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Sample records for mg-based amorphous ball-milled

  1. Crystallization of amorphous Fe90Zr10 under ball milling.

    PubMed

    Kwon, Young-Soon; Kim, Ji-Soon; Kim, Jin-Chun; Kwon, Yong-Jae; Povstugar, Ivan; Yelsukov, Eugene; Kim, Cheol-Eeh; Lee, Hyung-Soon

    2010-01-01

    The present study deals with structural transformations induced by high-energy ball-milling of an amorphous Fe90Zr10 alloy prepared by melt-spinning. The amorphous melt-spun ribbons were found to undergo crystallization into BCC alpha-Fe(Zr) nanocrystallites under high-energy ball milling. The decomposition degree of the amorphous phase increased with increasing milling time and intensity. Our results suggest that the observed crystallization is a deformation-induced process rather than a thermally induced one.

  2. Athermal character of the solid state amorphization of lactose induced by ball milling

    NASA Astrophysics Data System (ADS)

    Willart, J. F.; Caron, V.; Lefort, R.; Danède, F.; Prévost, D.; Descamps, M.

    2004-12-01

    In this paper, we report the possibility to reach pure glassy amorphous lactose by ball milling of crystalline α lactose under a dry nitrogen atmosphere. This route to the glassy state is found to be free of mutarotation towards the anomer β while this mutarotation is unavoidable using the usual thermal route, i.e. the quench of the liquid. This result definitely makes the 'local quench melting' hypothesis unsuitable to account for amorphization by ball milling.

  3. Microstructural characterization of amorphous and nanocrystalline boron nitride prepared by high-energy ball milling

    SciTech Connect

    Ghosh, J. Mazumdar, S.; Das, M.; Ghatak, S.; Basu, A.K.

    2008-04-01

    Microstructural parameters like crystallite size, lattice strain, stacking faults and dislocation density were evaluated from the X-ray diffraction data of boron nitride (BN) powder milled in a high-energy vibrational ball mill for different length of time (2-120 h), using different model based approaches like Scherrer analysis, integral breadth method, Williamson-Hall technique and modified Rietveld technique. From diffraction line-broadening analysis of the successive patterns of BN with varying milling time, it was observed that overall line broadening was an operative cause for crystallite size reduction at lower milling time ({approx}5 h), whereas lattice strains were the prominent cause of line broadening at higher milling times (>19 h). For intermediate milling time (7-19 h), both crystallite size and lattice strain influence the profile broadening although their relative contribution vary with milling time. Microstructural information showed that after long time milling (>19 h) BN becomes mixture of nanocrystalline and amorphous BN. The accumulations of defects cause this crystalline to amorphous transition. It has been found that twin fault ({beta}') and deformation fault ({alpha}) significantly contributed to BN powder as synthesized by a high-energy ball-milling technique. Present study consider only three ball-milled (0, 2 and 3 h) BN powder for faults calculation because fault effected reflections (1 0 1, 1 0 2, 1 0 3) disappear with milling time (>3 h). The morphology and particle size of the BN powders before and after ball milling were also observed in a field emission scanning electron microscope (FESEM)

  4. HRTEM and TEM studies of amorphous structures in ZrNiTiCu base alloys obtained by rapid solidification or ball milling.

    PubMed

    Dutkiewicz, J; Lityńska, L; Maziarz, W; Kocisko, R; Molnarová, M; Kovácová, A

    2009-01-01

    Amorphous structure of Ti(25)Zr(17)Ni(29)Cu(29) composition was studied. Alloys were prepared either by rapid solidification using melt spinning or by high-energy ball milling. The composition of multi-component eutectic in slowly cooled samples of ZrNiTiCu alloy was determined using EDS measurements in scanning microscope of slowly cooled cast samples. The alloys of eutectic composition were melt-spun or ball-milled. Transmission electron microscopy (TEM) studies of melt-spun ribbons from alloys near eutectic composition did not show presence of nanocrystals within the amorphous structure. TEM studies of ball-milled powders showed presence of nanocrystallites of size 2-5 nm. The electron diffraction pattern showed intense diffused ring due to the presence of the amorphous phase and a weak spot due to crystalline phases which were difficult to identify. The high temperature high-pressure compaction in vacuum of amorphous ball-milled powders resulted in a similar structure like in the powders showing nanocrystals embedded in the amorphous matrix. The crystallites were imaged using HREM. Interplanar distances were measured in pictures obtained by inverse fast Fourier transform (IFFT) of atomic planes to obtain better contrast. Analysis of the IFFT from high-resolution micrographs allowed to identify Cu(10)Zr(7) phase. Point analysis and elemental mapping performed using nondispersive X-ray energy spectroscopy showed uniform elements distribution indicating that chemical segregation to nanocrystals is within measurement error. PMID:18614372

  5. A comparison of the amorphization of zeolitic imidazolate frameworks (ZIFs) and aluminosilicate zeolites by ball-milling.

    PubMed

    Baxter, Emma F; Bennett, Thomas D; Cairns, Andrew B; Brownbill, Nick J; Goodwin, Andrew L; Keen, David A; Chater, Philip A; Blanc, Frédéric; Cheetham, Anthony K

    2016-03-14

    X-ray diffraction has been used to investigate the kinetics of amorphization through ball-milling at 20 Hz, for five zeolitic imidazolate frameworks (ZIFs) - ZIF-8, ZIF-4, ZIF-zni, BIF-1-Li and CdIF-1. We find that the rates of amorphization for the zinc-containing ZIFs increase with increasing solvent accessible volume (SAV) in the sequence ZIF-8 > ZIF-4 > ZIF-zni. The Li-B analogue of the dense ZIF-zni amorphizes more slowly than the corresponding zinc phase, with the behaviour showing a correlation with their relative bulk moduli and SAVs. The cadmium analogue of ZIF-8 (CdIF-1) amorphizes more rapidly than the zinc counterpart, which we ascribe primarily to its relatively weak M-N bonds as well as the higher SAV. The results for the ZIFs are compared to three classical zeolites - Na-X, Na-Y and ZSM-5 - with these taking up to four times longer to amorphize. The presence of adsorbed solvent in the pores is found to render both ZIF and zeolite frameworks more resistant to amorphization. X-ray total scattering measurements show that amorphous ZIF-zni is structurally indistinguishable from amorphous ZIF-4 with both structures retaining the same short-range order that is present in their crystalline precursors. By contrast, both X-ray total scattering measurements and (113)Cd NMR measurements point to changes in the local environment of amorphous CdIF-1 compared with its crystalline CdIF-1 precursor.

  6. A comparison of the amorphization of zeolitic imidazolate frameworks (ZIFs) and aluminosilicate zeolites by ball-milling.

    PubMed

    Baxter, Emma F; Bennett, Thomas D; Cairns, Andrew B; Brownbill, Nick J; Goodwin, Andrew L; Keen, David A; Chater, Philip A; Blanc, Frédéric; Cheetham, Anthony K

    2016-03-14

    X-ray diffraction has been used to investigate the kinetics of amorphization through ball-milling at 20 Hz, for five zeolitic imidazolate frameworks (ZIFs) - ZIF-8, ZIF-4, ZIF-zni, BIF-1-Li and CdIF-1. We find that the rates of amorphization for the zinc-containing ZIFs increase with increasing solvent accessible volume (SAV) in the sequence ZIF-8 > ZIF-4 > ZIF-zni. The Li-B analogue of the dense ZIF-zni amorphizes more slowly than the corresponding zinc phase, with the behaviour showing a correlation with their relative bulk moduli and SAVs. The cadmium analogue of ZIF-8 (CdIF-1) amorphizes more rapidly than the zinc counterpart, which we ascribe primarily to its relatively weak M-N bonds as well as the higher SAV. The results for the ZIFs are compared to three classical zeolites - Na-X, Na-Y and ZSM-5 - with these taking up to four times longer to amorphize. The presence of adsorbed solvent in the pores is found to render both ZIF and zeolite frameworks more resistant to amorphization. X-ray total scattering measurements show that amorphous ZIF-zni is structurally indistinguishable from amorphous ZIF-4 with both structures retaining the same short-range order that is present in their crystalline precursors. By contrast, both X-ray total scattering measurements and (113)Cd NMR measurements point to changes in the local environment of amorphous CdIF-1 compared with its crystalline CdIF-1 precursor. PMID:26575842

  7. High performance amorphous-Si@SiOx/C composite anode materials for Li-ion batteries derived from ball-milling and in situ carbonization

    NASA Astrophysics Data System (ADS)

    Wang, Dingsheng; Gao, Mingxia; Pan, Hongge; Wang, Junhua; Liu, Yongfeng

    2014-06-01

    Amorphous-Si@SiOx/C composites with amorphous Si particles as core and coated with a double layer of SiOx and carbon are prepared by ball-milling crystal micron-sized silicon powders and carbonization of the citric acid intruded in the ball-milled Si. Different ratios of Si to citric acid are used in order to optimize the electrochemical performance. It is found that SiOx exists naturally at the surfaces of raw Si particles and its content increases to ca. 24 wt.% after ball-milling. With an optimized Si to citric acid weight ratio of 1/2.5, corresponding to 8.4 wt.% C in the composite, a thin carbon layer is coated on the surfaces of a-Si@SiOx particles, moreover, floc-like carbon also forms and connects the carbon coated a-Si@SiOx particles. The composite provides a capacity of 1450 mA h g-1 after 100 cycles at a current density of 100 mA g1, and a capacity of 1230 mA h g-1 after 100 cycles at 500 mA g1 as anode material for lithium-ion batteries. Effects of ball-milling and the addition of citric acid on the microstructure and electrochemical properties of the composites are revealed and the mechanism of the improvement in electrochemical properties is discussed.

  8. Role of local heating in crystallization of amorphous alloys under ball milling: An experiment on Fe{sub 90}Zr{sub 10}

    SciTech Connect

    Kwon, Y. S.; Kim, J. S.; Povstugar, I. V.; Yelsukov, E. P.; Choi, P. P.

    2007-04-01

    Fe{sub 90}Zr{sub 10} was chosen as a model system to elucidate the roles of mechanical deformation and local heating in the phenomenon of ball-milling-induced crystallization of amorphous alloys. The structural evolution of melt-spun amorphous Fe{sub 90}Zr{sub 10} ribbons under different milling conditions and high-pressure torsion was investigated by means of x-ray diffraction, Moessbauer spectroscopy, and magnetic measurements. Despite a considerable difference in the local temperatures for high-energy and low-energy ball millings, cryomilling (under liquid nitrogen-cooling), and high-pressure torsion, amorphous Fe{sub 90}Zr{sub 10} crystallizes into a supersaturated {alpha}-Fe(Zr) solid solution in all cases. Local heating occurring under high- and low-energy millings only plays a minor role and leads to a slight shift of the crystallization products towards equilibrium state. Mechanical deformation was established as the primary cause of crystallization of the amorphous Fe-Zr alloy under ball milling.

  9. Polymorphic form of piroxicam influences the performance of amorphous material prepared by ball-milling.

    PubMed

    Naelapää, Kaisa; Boetker, Johan Peter; Veski, Peep; Rantanen, Jukka; Rades, Thomas; Kogermann, Karin

    2012-06-15

    The objective of this study was to investigate the influence of the starting solid state form of piroxicam (anhydrate form I: PRXAH I vs form II: PRXAH II) on the properties of the resulting amorphous material. The second objective was to obtain further insight into the impact of critical factors like thermal stress, dissolution medium and storage conditions on the thermal behavior, solid state transformations and physical stability of amorphous materials. For analysis differential scanning calorimetry (DSC), Raman spectroscopy and X-ray powder diffractometry (XRPD) were used. Pair-wise distribution function (PDF) analysis of the XRPD data was performed. PDF analysis indicated that the recrystallization behavior of amorphous samples was influenced by the amount of residual order in the samples. The recrystallization behavior of amorphous samples prepared from PRXAH I showed similarity to the starting material, whereas the recrystallization behavior of amorphous samples prepared from PRXAH II resembled to that of the PRX form III (PRXAH III). Multivariate data analysis (MVDA) helped to identify that the influence of storage time and temperature was more pronounced in the case of amorphous PRX prepared from PRXAH I. Furthermore, the wet slurry experiments with amorphous materials revealed the recrystallization of amorphous material as PRXMH in the biorelevant medium. PMID:22433471

  10. Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering.

    PubMed

    Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

    2015-09-15

    The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 °C, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase.

  11. Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering.

    PubMed

    Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

    2015-01-01

    The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 °C, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase. PMID:26369360

  12. Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering

    NASA Astrophysics Data System (ADS)

    Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

    2015-09-01

    The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 oC, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase.

  13. Magnetic properties of ball-milled SrFe12O19 particles consolidated by Spark-Plasma Sintering

    PubMed Central

    Stingaciu, Marian; Topole, Martin; McGuiness, Paul; Christensen, Mogens

    2015-01-01

    The room-temperature magnetic properties of ball-milled strontium hexaferrite particles consolidated by spark-plasma sintering are strongly influenced by the milling time. Scanning electron microscopy revealed the ball-milled SrFe12O19 particles to have sizes varying over several hundred nanometers. X-Ray powder-diffraction studies performed on the ball-milled particles before sintering clearly demonstrate the occurrence of a pronounced amorphization process. During sintering at 950 oC, re-crystallization takes place, even for short sintering times of only 2 minutes and transformation of the amorphous phase into a secondary phase is unavoidable. The concentration of this secondary phase increases with increasing ball-milling time. The remanence and maximum magnetization values at 1T are weakly influenced, while the coercivity drops dramatically from 2340 Oe to 1100 Oe for the consolidated sample containing the largest amount of secondary phase. PMID:26369360

  14. Ball milling synthesis of silica nanoparticle from rice husk ash for drug delivery application.

    PubMed

    Salavati-Niasari, Masoud; Javidi, Jaber; Dadkhah, Mahnaz

    2013-07-01

    Silica nanoparticles were synthesized from rice husk ash at room temperature by using high energy planetary ball mill. The milling time and mill rotational speed were varied in four levels. The morphology of the synthesized powders was investigated by the FE-SEM and TEM image as well as XRD patterns. The results have revealed that the nano-sized amorphous silica particles are formed after about 6 h ball milling and they are spherical in shape. The average particle size of the silica powders is found to be around 70 nm which decreases with increasing ball milling time or mill rotational speed. The as-synthesized silica nanoparticles were subsequently employed as drug carrier to investigate in vitro release behavior of Penicillin-G in simulated body fluid. UV-Vis spectroscopy was used to determine the amount of Penicillin-G released from the carrier. Penicillin-G release profile from silica nanoparticles exhibited a delayed release effect. PMID:22931308

  15. Formation of budesonide/α-lactose glass solutions by ball-milling

    NASA Astrophysics Data System (ADS)

    Dudognon, E.; Willart, J. F.; Caron, V.; Capet, F.; Larsson, T.; Descamps, M.

    2006-04-01

    The possibility to obtain amorphous budesonide stabilised by blending with an excipient characterised by a higher glass transition temperature, namely α-lactose, has been studied. We carried out the mixing of the two compounds at room temperature by ball-milling. The four obtained blends (containing, respectively, 10, 30, 50 and 70% w of budesonide) are X-ray amorphous and exhibit a single glass transition located between the ones of pure milled crystalline compounds. This revealed that the two amorphous phases are miscible whatever the composition and sufficiently mixed to relax as a whole. Ball-milling thus appears as a powerful tool to form amorphous molecular alloys with enhanced stability properties.

  16. Multifractal properties of ball milling dynamics

    SciTech Connect

    Budroni, M. A. Pilosu, V.; Rustici, M.; Delogu, F.

    2014-06-15

    This work focuses on the dynamics of a ball inside the reactor of a ball mill. We show that the distribution of collisions at the reactor walls exhibits multifractal properties in a wide region of the parameter space defining the geometrical characteristics of the reactor and the collision elasticity. This feature points to the presence of restricted self-organized zones of the reactor walls where the ball preferentially collides and the mechanical energy is mainly dissipated.

  17. DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, AND ORE BIN CHUTE, LOOKING EAST NORTHEAST. CRUSHED ORE FROM THE SECONDARY ORE BIN WAS INTRODUCED INTO THE FEED TROUGH VIA A CHUTE. AS THE BALL MILL TURNED, THE ROUND SCOOP ALSO TURNED IN THE TROUGH TO CHANNEL ORE INTO THE BALL MILL. SEE CA-292-14 FOR IDENTICAL B&W NEGATIVE. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

  18. DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    DETAIL VIEW OF BALL MILL FEED SYSTEM, MOUTH OF CLASSIFIER, AND ORE BIN CHUTE, LOOKING EAST NORTHEAST. CRUSHED ORE FROM THE SECONDARY ORE BIN WAS INTRODUCED INTO THE FEED TROUGH VIA A CHUTE. AS THE BALL MILL TURNED, THE ROUND SCOOP ALSO TURNED IN THE TROUGH TO CHANNEL ORE INTO THE BALL MILL. SEE CA-292-20 (CT) FOR IDENTICAL COLOR TRANSPARENCY. - Gold Hill Mill, Warm Spring Canyon Road, Death Valley Junction, Inyo County, CA

  19. Investigation of phase composition and nanoscale microstructure of high-energy ball-milled MgCu sample.

    PubMed

    Ma, Zongqing; Liu, Yongchang; Yu, Liming; Cai, Qi

    2012-07-13

    The ball milling technique has been successfully applied to the synthesis of various materials such as equilibrium intermetallic phases, amorphous compounds, nanocrystalline materials, or metastable crystalline phases. However, how the phase composition and nanoscale microstructure evolute during ball milling in various materials is still controversial due to the complex mechanism of ball milling, especially in the field of solid-state amorphization caused by ball milling. In the present work, the phase evolution during the high-energy ball milling process of the Mg and Cu (atomic ratio is 1:1) mixed powder was investigated. It was found that Mg firstly reacts with Cu, forming the Mg2Cu alloy in the primary stage of ball milling. As the milling time increases, the diffracted peaks of Mg2Cu and Cu gradually disappear, and only a broad halo peak can be observed in the X-ray diffraction pattern of the final 18-h milled sample. As for this halo peak, lots of previous studies suggested that it originated from the amorphous phase formed during the ball milling. Here, a different opinion that this halo peak results from the very small size of crystals is proposed: As the ball milling time increases, the sizes of Mg2Cu and Cu crystals become smaller and smaller, so the diffracted peaks of Mg2Cu and Cu become broader and broader and result in their overlap between 39° and 45°, at last forming the amorphous-like halo peak. In order to determine the origin of this halo peak, microstructure observation and annealing experiment on the milled sample were carried out. In the transmission electron microscopy dark-field image of the milled sample, lots of very small nanocrystals (below 20 nm) identified as Mg2Cu and Cu were found. Moreover, in the differential scanning calorimetry curve of the milled sample during the annealing process, no obvious exothermic peak corresponding to the crystallization of amorphous phase is observed. All the above results confirm that the broad

  20. Microstructure and martensitic transformation in Si-coated TiNi powders prepared by ball milling

    SciTech Connect

    Kim, Jae-hyun; Cho, Gyu-bong; Im, Yeon-min; Chun, Byong-sun; Kim, Yeon-wook; Nam, Tae-hyun

    2013-12-15

    Graphical abstract: - Highlights: • Amorphous Si-coated TiNi powders were prepared successfully by ball milling. • Ti{sub 4}Ni{sub 4}Si{sub 7} was formed at the interface between Si and TiNi after annealing. • Si-coated Ti–Ni powders displayed the R phase after annealing. - Abstract: Si was coated on the surface of Ti–49Ni (at%) alloy powders by ball milling in order to improve the electrochemical properties of the Si electrodes of secondary Li ion batteries and then the microstructure and martensitic transformation behavior were investigated by means of scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Ti–Ni powders coated with Si were fabricated successfully by ball milling. As-milled powders consisted of highly deformed Ti–Ni powders with the B2 phase and amorphous Si layers. The thickness of the Si layer coated on the surface of the Ti–Ni powders increased from 3–5 μm to 10–15 μm by extending the milling time from 3 h to 48 h. However, severe contamination from the grinding media, ZrO{sub 2} occurred when the ball milling time was as long as 48 h. By heating as-milled powders to various temperatures in the range of 673–873 K, the highly deformed Ti–Ni powders were recovered and Ti{sub 4}Ni{sub 4}Si{sub 7} was formed. Two-stage B2–R–B19′ transformation occurred when as-milled Si-coated Ti–49Ni alloy powders were heated to temperatures below 873 K, above this temperature one-stage B2–B19′ transformation occurred.

  1. DETAIL OF CYCLONE CLASSIFIER, WITH MARCY NO. 86 BALL MILL ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    DETAIL OF CYCLONE CLASSIFIER, WITH MARCY NO. 86 BALL MILL BELOW AND BEHIND IT. STRAIGHT HORIZONTAL PIPE IS SLIME FEED FROM ROD MILL. PIPE OUT TOP OF CYCLONE AND CURVING AT LOWER RIGHT CARRIED FINELY GROUND SLIME TO FLOTATION CONDITIONER TANK. PIPE NOT VISIBLE OUT BOTTOM OF CYCLONE CONVEYED COARSER SLIME TO BALL MILL. - Shenandoah-Dives Mill, 135 County Road 2, Silverton, San Juan County, CO

  2. Powder properties of hydrogenated ball-milled graphite

    SciTech Connect

    Zhang, Y.; Wedderburn, J.; Harris, R.; Book, D.

    2014-12-15

    Ball milling is an effective way of producing defective and nanostructured graphite. In this work, the hydrogen storage properties of graphite, ball-milled in a tungsten carbide milling pot under 3 bar hydrogen for various times (0–40 h), were investigated by TGA-Mass Spectrometry, XRD, SEM and laser diffraction particle size analysis. For the conditions used in this study, 10 h is the optimum milling time resulting in desorption of 5.5 wt% hydrogen upon heating under argon to 990 °C. After milling for 40 h, the graphite became significantly more disordered, and the amount of desorbed hydrogen decreased. After milling up to 10 h, the BET surface area increased while particle size decreased; however, there is no apparent correlation between these parameters, and the hydrogen storage properties of the hydrogenated ball-milled graphite.

  3. Preparation and Characterization of Nano structured Materials from Fly Ash: A Waste from Thermal Power Stations, by High Energy Ball Milling

    PubMed Central

    2007-01-01

    The Class F fly ash has been subjected to high energy ball milling and has been converted into nanostructured material. The nano structured fly ash has been characterized for its particle size by using particle size analyzer, specific surface area with the help of BET surface area apparatus, structure by X-ray diffraction studies and FTIR, SEM and TEM have been used to study particle aggregation and shape of the particles. On ball milling, the particle size got reduced from 60 μm to 148 nm by 405 times and the surface area increased from 0.249 m2/gm to 25.53 m2/gm i.e. by more than 100%. Measurement of surface free energy as well as work of adhesion found that it increased with increased duration of ball milling. The crystallite was reduced from 36.22 nm to 23.01 nm for quartz and from 33.72 nm to 16.38 nm for mullite during ball milling to 60 h. % crystallinity reduced from 35% to 16% during 60 h of ball milling because of destruction of quartz and hematite crystals and the nano structured fly ash is found to be more amorphous. Surface of the nano structured fly ash has become more active as is evident from the FTIR studies. Morphological studies revealed that the surface of the nano structured fly ash is more uneven and rough and shape is irregular, as compared to fresh fly ash which are mostly spherical in shape.

  4. 6. FF coal pulverizer (ball mill inside). GG building in ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    6. FF coal pulverizer (ball mill inside). GG building in background did preliminary crushing; pulverizer to left, coal conveyor and air cleaning towers to right; conveyor on left brought crushed coal to FF. Looking north/northeast - Rouge Steel Company, 3001 Miller Road, Dearborn, MI

  5. Phase evolution in carbide dispersion strengthened nanostructured copper composite by high energy ball milling

    NASA Astrophysics Data System (ADS)

    Hussain, Zuhailawati; Nur Hawadah, M. S.

    2012-09-01

    In this study, high-energy ball milling was applied to synthesis in situ nanostructured copper based composite reinforced with metal carbides. Cu, M (M=W or Ti) and graphite powder mixture were mechanically alloyed for various milling time in a planetary ball mill with composition of Cu-20vol%WC and Cu-20vol%TiC. Then the as-milled powder were compacted at 200 to 400 MPa and sintered in a vacuum furnace at 900°C. The results of X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy analysis showed that formation of tungsten carbides (W2C and WC phases) was observed after sintering of Cu-W-C mixture while TiC precipitated in as-milled powder of Cu-Ti-C composite after 5 h and become amorphous with longer milling. Mechanism of MA explained the cold welding and fracturing event during milling. Cu-W-C system shows fracturing event is more dominant at early stage of milling and W particle still existed after milling up to 60 h. While in Cu-Ti-C system, cold welding is more dominant and all Ti particles dissolved into Cu matrix.

  6. Ball-milled sulfur-doped graphene materials contain metallic impurities originating from ball-milling apparatus: their influence on the catalytic properties.

    PubMed

    Chua, Chun Kiang; Sofer, Zdeněk; Khezri, Bahareh; Webster, Richard D; Pumera, Martin

    2016-07-21

    Graphene materials have found applications in a wide range of devices over the past decade. In order to meet the demand for graphene materials, various synthesis methods are constantly being improved or invented. Ball-milling of graphite to obtain graphene materials is one of the many versatile methods to easily obtain bulk quantities. In this work, we show that the graphene materials produced by ball-milling are spontaneously contaminated with metallic impurities originating from the grinding bowls and balls. Ball-milled sulfur-doped graphene materials obtained from two types of ball-milling apparatus, specifically made up of stainless steel and zirconium dioxide, were investigated. Zirconium dioxide-based ball-milled sulfur-doped graphene materials contain a drastically lower amount of metallic impurities than stainless steel-based ball-milled sulfur-doped graphene materials. The presence of metallic impurities is demonstrated by their catalytic effects toward the electrochemical catalysis of hydrazine and cumene hydroperoxide. The general impression toward ball-milling of graphite as a versatile method for the bulk production of 'metal-free' graphene materials without the need for post-processing and the selection of ball-milling tools should be cautioned. These findings would have wide-reaching implications for graphene research. PMID:27314607

  7. Ball-milled sulfur-doped graphene materials contain metallic impurities originating from ball-milling apparatus: their influence on the catalytic properties.

    PubMed

    Chua, Chun Kiang; Sofer, Zdeněk; Khezri, Bahareh; Webster, Richard D; Pumera, Martin

    2016-07-21

    Graphene materials have found applications in a wide range of devices over the past decade. In order to meet the demand for graphene materials, various synthesis methods are constantly being improved or invented. Ball-milling of graphite to obtain graphene materials is one of the many versatile methods to easily obtain bulk quantities. In this work, we show that the graphene materials produced by ball-milling are spontaneously contaminated with metallic impurities originating from the grinding bowls and balls. Ball-milled sulfur-doped graphene materials obtained from two types of ball-milling apparatus, specifically made up of stainless steel and zirconium dioxide, were investigated. Zirconium dioxide-based ball-milled sulfur-doped graphene materials contain a drastically lower amount of metallic impurities than stainless steel-based ball-milled sulfur-doped graphene materials. The presence of metallic impurities is demonstrated by their catalytic effects toward the electrochemical catalysis of hydrazine and cumene hydroperoxide. The general impression toward ball-milling of graphite as a versatile method for the bulk production of 'metal-free' graphene materials without the need for post-processing and the selection of ball-milling tools should be cautioned. These findings would have wide-reaching implications for graphene research.

  8. Solvent-free mechanochemical glycosylation in ball mill.

    PubMed

    Tyagi, Mohit; Khurana, Darpan; Kartha, K P Ravindranathan

    2013-09-20

    Starting from acetobromosugars and an alcohol (alkyl/substituted alkyl/akenyl/alkynyl/glyceryl/cyclohexyl/steryl) various O-glycosides have been prepared mechanochemically under solvent-free conditions employing a planetary ball mill in the presence of metal carbonates (environmentally benign or otherwise) as promoters. The method was proven to be mild and efficient and applicable on preparative scale for the synthesis of various mono- and disaccharide glycosides. 4-Pentenyl glycoside so produced could, in four successive reactions in the same pot, be converted in high isolated yields into triazole-substituted pentyl glycoside that can find application in the area of medicinal chemistry.

  9. Preparation and solid-state characterization of ball milled saquinavir mesylate for solubility enhancement.

    PubMed

    Branham, Michael Lee; Moyo, Thomas; Govender, Thirumala

    2012-01-01

    Saquinavir is an anti-retroviral drug with very low oral bioavailability (e.g. 0.7-4.0%) due to its affinity toward efflux transporters (P-gp) and metabolic enzymes (CYP3A4). The aim of this study was to characterize the effects of high-energy ball milling on saquinavir solid-state characteristics and aqueous solubility for the design of effective buccal drug delivery systems. The solubility of saquinavir mesylate was evaluated in simulated saliva before and after milling for 1, 3, 15, 30, 50, and 60 h. To elucidate changes in crystallinity and long-range structure in the drug, analyses of the milled powders were performed using XRD, ATR-IR, DSC/TGA, BET surface area, EDX and SEM. In addition, the effects of milling time on saquinavir solubility were statistically correlated using repeated measures ANOVA. Results of this study indicate that the milling of saquinavir mesylate produces nanoporous particles with unique surface structures, thermal properties, and increased aqueous solubility. Optimal milling time occurred at 3h and corresponded to a 9-fold solubility enhancement in simulated saliva. Thermal analysis revealed only a slight decrease in melting point (T(m)) from 242 °C to 236 °C after 60 h milling. XRD diffractograms indicate a gradual crystalline-to-amorphous transition with some residual crystallinity remaining after 60 h milling time. Unstable polymorphic structures appeared between 15 and 30 h which were converted to more stable isomorphs at 60 h. Aggregate formation also seems to occur after 15 h but no metal contamination of the drug was observed during the milling process as determined by EDX analysis. In conclusion, high-energy ball milling may be a method of choice for improving the solubility of saquinavir and facilitating novel drug formulations design.

  10. Effects and mechanism of ball milling on torrefaction of pine sawdust.

    PubMed

    Gong, Chunxiao; Huang, Jing; Feng, Chen; Wang, Guanghui; Tabil, Lope; Wang, Decheng

    2016-08-01

    The effects and mechanism of ball milling on the torrefaction process were studied. Ball- and hammer-milled (screen size 1mm) pine sawdust samples were torrefied at three temperatures (230, 260, and 290°C) and two durations (30 and 60min) to investigate into their torrefaction behavior and physicochemical properties. The results showed that, under identical torrefaction conditions, torrefied ball-milled pine sawdust had a higher carbon content and fixed carbon, and lower hydrogen and oxygen contents than torrefied hammer-milled pine sawdust. Torrefied ball-milled pine sawdust produced lower mass and energy yields, but higher heating values than torrefied hammer-milled pine sawdust. Ball milling destroyed the crystalline structure of cellulose and thus reduced the thermal stability of hemicellulose, cellulose, and lignin, causing them to degrade at relatively lower temperatures. In conclusion, biomass pretreated with a combination of ball milling and torrefaction has the potential to produce an alternative fuel to coal. PMID:27136611

  11. Effects and mechanism of ball milling on torrefaction of pine sawdust.

    PubMed

    Gong, Chunxiao; Huang, Jing; Feng, Chen; Wang, Guanghui; Tabil, Lope; Wang, Decheng

    2016-08-01

    The effects and mechanism of ball milling on the torrefaction process were studied. Ball- and hammer-milled (screen size 1mm) pine sawdust samples were torrefied at three temperatures (230, 260, and 290°C) and two durations (30 and 60min) to investigate into their torrefaction behavior and physicochemical properties. The results showed that, under identical torrefaction conditions, torrefied ball-milled pine sawdust had a higher carbon content and fixed carbon, and lower hydrogen and oxygen contents than torrefied hammer-milled pine sawdust. Torrefied ball-milled pine sawdust produced lower mass and energy yields, but higher heating values than torrefied hammer-milled pine sawdust. Ball milling destroyed the crystalline structure of cellulose and thus reduced the thermal stability of hemicellulose, cellulose, and lignin, causing them to degrade at relatively lower temperatures. In conclusion, biomass pretreated with a combination of ball milling and torrefaction has the potential to produce an alternative fuel to coal.

  12. A comparison of cellulose nanocrystals and cellulose nanofibres extracted from bagasse using acid and ball milling methods

    NASA Astrophysics Data System (ADS)

    Rahimi Kord Sofla, M.; Brown, R. J.; Tsuzuki, T.; Rainey, T. J.

    2016-09-01

    This study compared the fundamental properties of cellulose nanocrystals (CNC) and cellulose nanofibrils (CNF) extracted from sugarcane bagasse. Conventional hydrolysis was used to extract CNC while ball milling was used to extract CNF. Images generated by scanning electron microscope and transmission electron microscope showed CNC was needle-like with relatively lower aspect ratio and CNF was rope-like in structure with higher aspect ratio. Fourier-transformed infrared spectra showed that the chemical composition of nanocellulose and extracted cellulose were identical and quite different from bagasse. Dynamic light scattering studies showed that CNC had uniform particle size distribution with a median size of 148 nm while CNF had a bimodal size distribution with median size 240 ± 12 nm and 10 μm. X-ray diffraction showed that the amorphous portion was removed during hydrolysis; this resulted in an increase in the crystalline portion of CNC compared to CNF. Thermal degradation of cellulose initiated at a much lower temperature, in the case of the nanocrystals while the CNF prepared by ball milling were not affected, indicating higher thermal stability.

  13. A new approach for remediation of As-contaminated soil: ball mill-based technique.

    PubMed

    Shin, Yeon-Jun; Park, Sang-Min; Yoo, Jong-Chan; Jeon, Chil-Sung; Lee, Seung-Woo; Baek, Kitae

    2016-02-01

    In this study, a physical ball mill process instead of chemical extraction using toxic chemical agents was applied to remove arsenic (As) from contaminated soil. A statistical analysis was carried out to establish the optimal conditions for ball mill processing. As a result of the statistical analysis, approximately 70% of As was removed from the soil at the following conditions: 5 min, 1.0 cm, 10 rpm, and 5% of operating time, media size, rotational velocity, and soil loading conditions, respectively. A significant amount of As remained in the grinded fine soil after ball mill processing while more than 90% of soil has the original properties to be reused or recycled. As a result, the ball mill process could remove the metals bound strongly to the surface of soil by the surface grinding, which could be applied as a pretreatment before application of chemical extraction to reduce the load. PMID:26667646

  14. Properties of high-energy ball-milled Fe-Se based superconductors.

    PubMed

    Ahn, Jung-Ho; Sangjun-Oh

    2012-02-01

    We have synthesized FeSe0.5Te0.5 superconductors by high-energy ball-milling and subsequent annealing. High-energy ball-milling of elemental powder mixtures resulted in the formation of metastable and/or nanocrystalline phases. Both XRD and DSC results show that the ball-milled powers were completely transformed to FeSe0.5Te0.5 with the grain size of a few nanometers during sintering at low temperatures. The resulting materials exhibited superconducting transition at 14 K. The enhancement of critical current density was observed for the high-energy ball-milled powder, compared with the un-milled powders.

  15. Dioxins reformation and destruction in secondary copper smelting fly ash under ball milling

    NASA Astrophysics Data System (ADS)

    Cagnetta, Giovanni; Hassan, Mohammed Mansour; Huang, Jun; Yu, Gang; Weber, Roland

    2016-03-01

    Secondary copper recovery is attracting increasing interest because of the growth of copper containing waste including e-waste. The pyrometallurgical treatment in smelters is widely utilized, but it is known to produce waste fluxes containing a number of toxic pollutants due to the large amount of copper involved, which catalyses the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans (“dioxins”). Dioxins are generated in secondary copper smelters on fly ash as their major source, resulting in highly contaminated residues. In order to assess the toxicity of this waste, an analysis of dioxin-like compounds was carried out. High levels were detected (79,090 ng TEQ kg‑1) in the ash, above the Basel Convention low POPs content (15,000 ng TEQ kg‑1) highlighting the hazardousness of this waste. Experimental tests of high energy ball milling with calcium oxide and silica were executed to assess its effectiveness to detoxify such fly ash. Mechanochemical treatment obtained 76% dioxins reduction in 4 h, but longer milling time induced a partial de novo formation of dioxins catalysed by copper. Nevertheless, after 12 h treatment the dioxin content was substantially decreased (85% reduction) and the copper, thanks to the phenomena of incorporation and amorphization that occur during milling, was almost inactivated.

  16. Effect of ball milling materials and methods on powder processing of Bi2223 superconductors

    NASA Astrophysics Data System (ADS)

    Yavuz, M.; Maeda, H.; Vance, L.; Liu, H. K.; Dou, S. X.

    1998-10-01

    Various milling systems consisting of agate and polypropylene grinding containers, agate and YSZ balls, and dry and wet milling were used in planetary ball-milling and YSZ balls and YSZ container were used in wet and dry attrition milling. The differently milled powders were then evaluated by measurements of particle size, surface area, porosity, size distribution and chemical analysis of the Si, Zr and C contents. The results show that dry milling is much more efficient for particle size reduction in planetary milling than wet milling, whereas wet milling and dry milling gave quite similar results in attrition milling. Meanwhile 0953-2048/11/10/056/img6 contamination was found in powder milled with an agate container with agate balls. Some C contamination from the polypropylene container was detected after milling, but negligible Zr from YSZ balls and C from the grinding carrier (hexane). It was found that after 1 h milling in the planetary mill fracture mechanisms transform from the elastic to the plastic region. Therefore, further milling is not very effective. It was also shown that the Bi2212 phase decomposes into several non-superconducting oxides such as 0953-2048/11/10/056/img7, CuO and a main amorphous phase after extensive dry milling.

  17. Dioxins reformation and destruction in secondary copper smelting fly ash under ball milling

    PubMed Central

    Cagnetta, Giovanni; Hassan, Mohammed Mansour; Huang, Jun; Yu, Gang; Weber, Roland

    2016-01-01

    Secondary copper recovery is attracting increasing interest because of the growth of copper containing waste including e-waste. The pyrometallurgical treatment in smelters is widely utilized, but it is known to produce waste fluxes containing a number of toxic pollutants due to the large amount of copper involved, which catalyses the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans (“dioxins”). Dioxins are generated in secondary copper smelters on fly ash as their major source, resulting in highly contaminated residues. In order to assess the toxicity of this waste, an analysis of dioxin-like compounds was carried out. High levels were detected (79,090 ng TEQ kg−1) in the ash, above the Basel Convention low POPs content (15,000 ng TEQ kg−1) highlighting the hazardousness of this waste. Experimental tests of high energy ball milling with calcium oxide and silica were executed to assess its effectiveness to detoxify such fly ash. Mechanochemical treatment obtained 76% dioxins reduction in 4 h, but longer milling time induced a partial de novo formation of dioxins catalysed by copper. Nevertheless, after 12 h treatment the dioxin content was substantially decreased (85% reduction) and the copper, thanks to the phenomena of incorporation and amorphization that occur during milling, was almost inactivated. PMID:26975802

  18. Dioxins reformation and destruction in secondary copper smelting fly ash under ball milling.

    PubMed

    Cagnetta, Giovanni; Hassan, Mohammed Mansour; Huang, Jun; Yu, Gang; Weber, Roland

    2016-03-15

    Secondary copper recovery is attracting increasing interest because of the growth of copper containing waste including e-waste. The pyrometallurgical treatment in smelters is widely utilized, but it is known to produce waste fluxes containing a number of toxic pollutants due to the large amount of copper involved, which catalyses the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans ("dioxins"). Dioxins are generated in secondary copper smelters on fly ash as their major source, resulting in highly contaminated residues. In order to assess the toxicity of this waste, an analysis of dioxin-like compounds was carried out. High levels were detected (79,090 ng TEQ kg(-1)) in the ash, above the Basel Convention low POPs content (15,000 ng TEQ kg(-1)) highlighting the hazardousness of this waste. Experimental tests of high energy ball milling with calcium oxide and silica were executed to assess its effectiveness to detoxify such fly ash. Mechanochemical treatment obtained 76% dioxins reduction in 4 h, but longer milling time induced a partial de novo formation of dioxins catalysed by copper. Nevertheless, after 12 h treatment the dioxin content was substantially decreased (85% reduction) and the copper, thanks to the phenomena of incorporation and amorphization that occur during milling, was almost inactivated.

  19. Dioxins reformation and destruction in secondary copper smelting fly ash under ball milling.

    PubMed

    Cagnetta, Giovanni; Hassan, Mohammed Mansour; Huang, Jun; Yu, Gang; Weber, Roland

    2016-01-01

    Secondary copper recovery is attracting increasing interest because of the growth of copper containing waste including e-waste. The pyrometallurgical treatment in smelters is widely utilized, but it is known to produce waste fluxes containing a number of toxic pollutants due to the large amount of copper involved, which catalyses the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans ("dioxins"). Dioxins are generated in secondary copper smelters on fly ash as their major source, resulting in highly contaminated residues. In order to assess the toxicity of this waste, an analysis of dioxin-like compounds was carried out. High levels were detected (79,090 ng TEQ kg(-1)) in the ash, above the Basel Convention low POPs content (15,000 ng TEQ kg(-1)) highlighting the hazardousness of this waste. Experimental tests of high energy ball milling with calcium oxide and silica were executed to assess its effectiveness to detoxify such fly ash. Mechanochemical treatment obtained 76% dioxins reduction in 4 h, but longer milling time induced a partial de novo formation of dioxins catalysed by copper. Nevertheless, after 12 h treatment the dioxin content was substantially decreased (85% reduction) and the copper, thanks to the phenomena of incorporation and amorphization that occur during milling, was almost inactivated. PMID:26975802

  20. Raman spectroscopy of ball-milled TiO 2

    NASA Astrophysics Data System (ADS)

    Gajović, A.; Stubičar, M.; Ivanda, M.; Furić, K.

    2001-05-01

    Raman spectroscopy was applied to study structural and dimensional changes during high-energy ball milling of TiO 2 anatase. Milling was performed for up to 10 h using two different sets of grinding tools (wolfram carbide (WC) and agate). The diminution of the TiO 2 particle to nanometric size was monitoring by low-frequency Raman spectroscopy. The nanometric sizes were confirmed by transmission electron microscopy (TEM). After short milling time by WC the bands of high-pressure TiO 2 II phase (α-PbO 2 structure) were detected in Raman spectrum. Prolonged milling time was needed for transformation to rutil. When milling was performed by agate, the time necessary for both phase transitions was longer, presumably because of lower ball-to-powder weight ratio. The low-frequency Raman band of the prolonged milled samples was broad, which suggests the wide dispersion in nano-particle dimensions. The position of the low-frequency band in longer-milled samples indicated dimensions smaller than 20 nm, since the diameter of the particle is inversely proportional to the low-frequency mode of the spherical particles. These results were in agreement with the TEM results.

  1. Crystal structure of ball-milled mixture of sodium chloride and magnesium chloride-ethanol adduct

    SciTech Connect

    Jiang Xue; Tian Xiuzhi; Fan Zhiqiang

    2008-02-05

    NaCl doped MgCl{sub 2}.nEtOH adducts were prepared by ball-milling MgCl{sub 2}.2.5EtOH with NaCl. Both the ball-milled MgCl{sub 2}.nEtOH/NaCl mixture and pure MgCl{sub 2}.2.5EtOH adducts were analyzed by X-ray diffraction (XRD), transmission electron microscope (TEM), thermogravimetry (TG) and differencial scanning calorimetry (DSC). A simple MgCl{sub 2}.nEtOH/NaCl mixture without ball-milling treatment was also studied for comparison. Two kinds of mixed crystals, Na{sub 2}MgCl{sub 4} and NaMgCl{sub 3}, were found to be formed in a ball-milled mixture that contained 16 mol.% NaCl. TG and DSC analysis of the samples also provided indirect evidences supporting the presence of the mixed crystals in the ball-milled mixture. Adding certain amounts of NaCl in MgCl{sub 2}.2.5EtOH adduct, either by co-milling or by simple mixing, greatly increased the thermal stability of the adduct, but thermal decomposition behaviour of the ball-milled mixture was still different from that of a simple mixture.

  2. Response to Thermal Exposure of Ball-Milled Aluminum-Borax Powder Blends

    NASA Astrophysics Data System (ADS)

    Birol, Yucel

    2013-04-01

    Aluminum-borax powder mixtures were ball milled and heated above 873 K (600 °C) to produce Al-B master alloys. Ball-milled powder blends reveal interpenetrating layers of deformed aluminum and borax grains that are increasingly refined with increasing milling time. Thermal exposure of the ball-milled powder blends facilitates a series of thermite reactions between these layers. Borax, dehydrated during heating, is reduced by Al, and B thus generated reacts with excess Al to produce AlB2 particles dispersed across the aluminum grains starting at 873 K (600 °C). AlB2 particles start to form along the interface of the aluminum and borax layers. Once nucleated, these particles grow readily to become hexagonal-shaped crystals that traverse the aluminum grains with increasing temperatures as evidenced by the increase in the size as well as in the number of the AlB2 particles. Ball milling for 1 hour suffices to achieve a thermite reaction between borax and aluminum. Ball milling further does not impact the response of the powder blend to thermal exposure. The nucleation-reaction sites are multiplied, however, with increasing milling time and thus insure a higher number of smaller AlB2 particles. The size of the AlB2 platelets may be adjusted with the ball milling time.

  3. Investigation of griseofulvin and hydroxypropylmethyl cellulose acetate succinate miscibility in ball milled solid dispersions.

    PubMed

    Al-Obaidi, Hisham; Lawrence, M Jayne; Al-Saden, Noor; Ke, Peng

    2013-02-25

    Solid dispersions of varying weight ratios compositions of the nonionic drug, griseofulvin and the hydrophilic, anionic polymer, hydroxylpropylmethyl cellulose acetate succinate, have been prepared by ball milling and the resulting samples characterized using a combination of Fourier transform infra-red spectroscopy, X-ray powder diffraction and differential scanning calorimetry. The results suggest that griseofulvin forms hydrogen bonds with the hydroxylpropylmethyl cellulose acetate succinate polymer when prepared in the form of a solid dispersion but not when prepared in a physical mixture of the same composition. As anticipated, the actual measured glass transition temperature of the solid dispersions displayed a linear relationship between that predicted using the Gordon-Taylor and Fox equations assuming ideal mixing, but interestingly only at griseofulvin contents less than 50 wt%. At griseofulvin concentrations greater than this, the measured glass transition temperature of the solid dispersions was almost constant. Furthermore, the crystalline content of the solid dispersions, as determined by differential scanning calorimetry and X-ray powder diffraction followed a similar trend in that the crystalline content significantly decreased at ratios less than 50 wt% of griseofulvin. When the physical mixtures of griseofulvin and the hydroxylpropylmethyl cellulose acetate succinate polymer were analyzed using the Flory-Huggins model, a negative free energy of mixing with an interaction parameter of -0.23 were obtained. Taken together these results suggest that anionic hydrophilic hydroxylpropylmethyl cellulose acetate succinate polymer is a good solvent for crystalline nonionic griseofulvin with the solubility of griseofulvin in the solid dispersion being was estimated to be within the range 40-50 wt%. Below this solubility limit, the amorphous drug exists as amorphous glassy solution while above these values the system is supersaturated and glassy suspension and

  4. Anisotropy induced large exchange bias behavior in ball milled Ni-Co-Mn-Sb alloys

    SciTech Connect

    Nayak, Ajaya K.; Sahoo, Roshnee; Suresh, K. G.; Nigam, A. K.; Chen, X.; Ramanujan, R. V.

    2011-06-06

    We report the effect of decrease in the grain size on the structural, magnetic and exchange bias (EB) behavior in ball milled Ni{sub 50-x}Co{sub x}Mn{sub 38}Sb{sub 12} (x=0 and 5) Heusler alloys. The existence of a wide range of grain sizes in the ball milled samples results in dramatic changes in the structural and magnetic properties. For x=0, a large EB field of 3.2 kOe is observed in the ball milled sample, compared to a value of 245 Oe of the bulk sample. This increase is attributed to the enhanced exchange coupling between the soft and hard magnetic particles.

  5. Structural and magnetic stability of high energy ball milled Co2MnSi

    NASA Astrophysics Data System (ADS)

    Vinesh, A.; Sudheesh, V. D.; Sebastian, Varkey; Lakshmi, N.; Venugopalan, K.

    2015-07-01

    Structural and magnetic properties of ball milled Co2MnSi have been studied and compared with that of ordered bulk sample. The milled sample (with average size determined using the Williamson-Hall method) shows that the chemical ordering for this sample is very stable and is little effected by high energy ball milling. However, the reduction in the saturation magnetic moment of the milled sample shows that there is spin disordering induced on ball milling - attributable to the formation of a magnetically dead layer at the surface of the nano-sized samples. The ordered sample (unmilled) has a saturation moment value of 4.4 μB per formula unit at room temperature and is in agreement with the prediction of Slater Pauling curve. On milling it reduces to ~3 μB per formula unit at room temperature with an accompanying increase in the coercivity, retentivity and squareness factor.

  6. Remediation of oil-contaminated sand by coal agglomeration using ball milling.

    PubMed

    Shin, Yu-Jen; Shen, Yun-Hwei

    2011-10-01

    The mechanical shear force provided by a less energy intensive device (usually operating at 20-200 rpm), a ball mill, was used toperform coal agglomeration and its effects on remediation of a model fuel oil-contaminated sand were evaluated. Important process parameters such as the amount of coal added, milling time, milling speed and the size of milling elements are discussed. The results suggested that highly hydrophobic oil-coal agglomerates, formed by adding suitable amounts of coal into the oil-contaminated sand, could be mechanically liberated from cleaned sand during ball milling and recovered as a surface coating on the steel balls. Over 90% removal of oil from oil-contaminated sand was achieved with 6 wt% of coal addition and an optimum ball milling time of 20 min and speed of 200 rpm. This novel process has considerable potential for cleaning oil-contaminated sands.

  7. Phase Transformation and Magnetic Property of Ni-Mn-Ga Powders Prepared by Dry Ball Milling

    NASA Astrophysics Data System (ADS)

    Tian, B.; Chen, F.; Tong, Y. X.; Li, L.; Zheng, Y. F.

    2012-12-01

    This study investigated the phase transformations and magnetic properties of Ni-Mn-Ga alloy powders prepared by dry ball milling in argon atmosphere. The Fe and Cr elements were found to be introduced in the alloy after ball milling, which should result from the severe collision and friction among the particles, balls, and vial. The x-ray diffraction result indicated that the Fe and Cr elements should have alloyed with the Ni-Mn-Ga matrix. The martensitic transformation temperature and Curie temperature of the 800 °C annealed powders decreased by ~33 °C and increased by ~28 °C, respectively, as compared to that of the bulk alloy. The comprehensive effect of the changing of valence electron concentration of the alloy due to the introduction of Fe and Cr and the grain refinement of the alloy caused by ball milling should be responsible for the reduction of martensitic transformation temperature. The saturation magnetization of the 800 °C annealed powders became larger (~5 emu/g) than that of the bulk alloy. The enhancement of magnetic properties, such as the increase of Curie temperature and enhancement of saturation magnetization of the annealed Ni-Mn-Ga powders, should be attributed to the increase of magnetic exchange caused by introduction of Fe in the alloy. The contaminations of Fe and Cr elements emerging from the dry ball milling process changed the phase transformation and magnetic properties of the Ni-Mn-Ga alloy. Therefore, the dry ball milling process is difficult to control the contamination from the milling medium and not suitable to prepare Ni-Mn-Ga powders. On the contrary, the wet ball milling method under liquid medium should be a better method to prevent the contamination and fabricate pure Ni-Mn-Ga ferromagnetic shape memory alloy powders.

  8. Nitrogen-doped graphene by ball-milling graphite with melamine for energy conversion and storage

    NASA Astrophysics Data System (ADS)

    Xue, Yuhua; Chen, Hao; Qu, Jia; Dai, Liming

    2015-12-01

    N-doped graphene was prepared by ball milling of graphite with melamine. It was found that ball-milling reduced the size of graphite particles from 30 to 1 μm and facilitated the exfoliation of the resultant small particles into few-layer N-doped graphene nanosheets under ultrasonication. The as-prepared N-doped graphene nanoplatelets (NGnPs) exhibited a nitrogen content as high as 11.4 at.%, making them attractive as efficient electrode materials in supercapacitors for energy storage and as highly-active metal-free catalysts for oxygen reduction in fuel cells for energy conversion.

  9. Factors influencing the ball milling of Si3N4 in water

    NASA Technical Reports Server (NTRS)

    Freedman, M. R.; Kiser, J. D.; Herbell, T. P.

    1985-01-01

    A statistical study of the ball milling of Si3N4 powder in Si3N4 hardware was undertaken to understand how the resulting increase in specific surface area is related to solids loading and mill speed. An attempt was made to optimize milling conditions. The degree of communication was more dependent upon solids loading than mill speed. A practical grinding limit between 0.5 and 0.75 microns was achieved in 144 hr independent of solids loading. Ball mill wear and media wear were independent of both solids loading and mill speed.

  10. Structural and microstructural changes in monoclinic ZrO{sub 2} during the ball-milling with stainless steel assembly

    SciTech Connect

    Stefanic, G. . E-mail: stefanic@irb.hr; Music, S.; Gajovic, A.

    2006-04-13

    High-energy ball-milling of monoclinic ZrO{sub 2} was performed in air using the planetary ball mill with a stainless steel milling assembly. Structural and microstructural changes during the ball-milling were monitored using X-ray powder diffraction, Raman spectroscopy, Moessbauer spectroscopy, field emission scanning electron microscopy and energy dispersive X-ray spectrometry. The results of line broadening analysis indicated a decrease in the crystallite size and an increase in the microstrains with the ball-milling time increased up to {approx}150 min. The results of quantitative phase analysis indicated the presence of a very small amount of tetragonal ZrO{sub 2} phase in this early stage of ball-milling. The onset of m-ZrO{sub 2} {sup {yields}} t-ZrO{sub 2} transition occurred between 10 and 15 h of ball-milling, which resulted in a complete transition after 20 h of ball-milling. Further ball-milling caused a decrease of the t-ZrO{sub 2} lattice parameters followed by a probable transition into c-ZrO{sub 2}. It was concluded that the stabilization of t- and c-ZrO{sub 2} polymorphs at RT can be attributed to the incorporation of aliovalent cations (Fe{sup 2+}, Fe{sup 3+} and Cr{sup 3+}) introduced into the sample due to the wear and oxidation of the milling media.

  11. Synthesis of Fe/SiO{sub 2} and iron oxides/SiO{sub 2} nanocomposites by long-term ball milling

    SciTech Connect

    Pozo López, G.; Condó, A.M.; Urreta, S.E.; Silvetti, S.P.

    2014-01-01

    Graphical abstract: - Highlights: • Iron–iron oxides/silica composites are synthesized by long term dry ball-milling. • Bcc iron and α-quartz powders are used as precursors. • Surface effects enhance coercivity in iron/silica nanocomposites. • In spite of their small size, about 10 nm, iron particles are ferromagnetic. • Ferro and superparamagnetic particles are found in maghemite/silica composites. - Abstract: Iron oxide/SiO{sub 2} nanocomposites are synthesized by dry ball-milling a mixture of bcc Fe and α-quartz powders for prolonged times. A sequence of nanocomposites is obtained, with small magnetic particles dispersed in a non magnetic, amorphous matrix. The powders are characterized by X-ray diffraction and transmission electron microscopy. The magnetic hysteresis properties are investigated in the range 50–300 K. After 120 h milling, deformed, non-spherical, α-Fe nanocrystallites of about 10 nm in size and very few small (<10 nm) maghemite particles are found. At room temperature, iron particles are ferromagnetic and a large effective magnetic anisotropy is estimated, which is mainly attributed to surface effects. Between 160 and 200 h milling, maghemite nanoparticles are observed while after 220 h grinding, hematite phase appears; after 340 h milling, the sample consists of ferromagnetic hematite particles with a broad size distribution (5–50 nm) embedded in an amorphous matrix.

  12. Synthesis of aluminum nitride powders from a plasma-assisted ball milled precursor through carbothermal reaction

    SciTech Connect

    Liu, Zhi-jie; Dai, Le-yang; Yang, De-zheng; Wang, Sen; Zhang, Bao-jian; Wang, Wen-chun; Cheng, Tie-han

    2015-01-15

    Highlights: • A novel and high efficiency synthesizing AlN powders method combining mechanical ball milling and DBDP has been developed. • The particle size, the crystallite size, the lattice distortion, the morphology of Al{sub 2}O{sub 3} powders, and the AlN conversion rate are investigated and compared under the ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP. • The ball milled Al{sub 2}O{sub 3} powders with DBDP have small spherical structure morphology with very fine particles size and high specific surface area, which result in a higher chemical efficiency and a higher AlN conversion rate at lower thermal temperature. - Abstract: In this paper, aluminum nitride (AlN) powers have been produced with a novel and high efficiency method by thermal annealing at 1100–1600 °C of alumina (Al{sub 2}O{sub 3}) powders which were previously ball milled for various time up to 40 h with and without the assistant of dielectric barrier discharge plasma (DBDP). The ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP and the corresponding synthesized AlN powers are characterized by X-ray diffraction, scanning electron microscope, and transmission electron microscopy. From the characteristics of the ball milled Al{sub 2}O{sub 3} powders with DBDP and without DBDP, it can be seen that the ball milled Al{sub 2}O{sub 3} powders with DBDP have small spherical structure morphology with very fine particles size and high specific surface area, which result in a higher chemical efficiency and a higher AlN conversion rate at lower thermal temperature. Meanwhile, the synthesized AlN powders can be known as hexagonal AlN with fine crystal morphology and irregular lump-like structure, and have uniform distribution with the average particle size of about between 500 nm and 1000 nm. This provides an important method for fabricating ultra fine powders and synthesizing nitrogen compounds.

  13. Magnetic property and microstructure of single crystalline Nd2Fe14B ultrafine particles ball milled from HDDR powders

    NASA Astrophysics Data System (ADS)

    Li, W. F.; Hu, X. C.; Cui, B. Z.; Yang, J. B.; Han, J. Z.; Hadjipanayis, G. C.

    2013-08-01

    In this work we report the microstructure and magnetic property of single crystalline Nd2Fe14B ultrafine particles ball milled from HDDR Nd-Fe-B alloys. The average size of the particles is 283 nm, and TEM observation reveals that these particles are single crystalline. The coercivity of these particles is 6.0 kOe, which is much higher than that of the particles ball milled from sintered and hot pressed Nd-Fe-B magnets. Micromagnetic analysis shows that the coercivity degradation is caused by surface damage during ball milling.

  14. Comparative Study by MS and XRD of Fe50Al50 Alloys Produced by Mechanical Alloying, Using Different Ball Mills

    NASA Astrophysics Data System (ADS)

    Rojas Martínez, Y.; Pérez Alcázar, G. A.; Bustos Rodríguez, H.; Oyola Lozano, D.

    2005-02-01

    In this work we report a comparative study of the magnetic and structural properties of Fe50Al50 alloys produced by mechanical alloying using two different planetary ball mills with the same ball mass to powder mass relation. The Fe50Al50 sample milled during 48 h using the Fritsch planetary ball mill pulverisette 5 and balls of 20 mm, presents only a bcc alloy phase with a majority of paramagnetic sites, whereas that sample milled during the same time using the Fritsch planetary ball mill pulverisette 7 with balls of 15 mm, presents a bcc alloy phase with paramagnetic site (doublet) and a majority of ferromagnetic sites which include pure Fe. However for 72 h of milling this sample presents a bcc paramagnetic phase, very similar to that prepared with the first system during 48 h. These results show that the conditions used in the first ball mill equipment make more efficient the milling process.

  15. Excess lithium storage in LiFePO4-Carbon interface by ball-milling

    NASA Astrophysics Data System (ADS)

    Guo, Hua; Song, Xiaohe; Zheng, Jiaxin; Pan, Feng

    2016-07-01

    As one of the most popular cathode materials for high power lithium ion batteries (LIBs) of the electrical-vehicle (EV), lithium iron phosphate (LiFePO4 (LFP)) is limited to its relatively lower theoretical specific capacity of 170mAh g‑1. To break the limits and further improve the capacity of LFP is promising but challenging. In this study, the ball-milling method is applied to the mixture of LFP and carbon, and the effective capacity larger than the theoretical one by 30mAh g‑1 is achieved. It is demonstrated that ball-milling leads to the LFP-Carbon interface to store the excess Li-ions.

  16. Electromagnetic properties of Co flaky particles prepared via ball-milling method

    NASA Astrophysics Data System (ADS)

    Liu, Chao; Jiang, Jian-Tang; Yuan, Yong; Gong, Yuan-Xun; Zhen, Liang

    2016-10-01

    Flaky cobalt particles with different aspect ratio were produced with ball-milling method. The phase structure and morphology of the particles were identified by XRD analysis and SEM observation. The static magnetic and electromagnetic properties of the particles were measured and effects of shape, microstructure and filling fraction were investigated. Phase transition from fcc lattice to hcp lattice occur due to the drive of ball-milling is responsible for the largely increased coercivity. Particles with high aspect ratio are found to possess high permittivity and permeability, compelling the frequency of absorption peak to shift to low frequency. Coatings using cobalt particles milled for 20 h as fillers present a RL peak of -33 dB at 8 GHz at the thickness of 2.5 mm together with a broad effective absorbing (RL below -10 dB) bandwidth covering 6-10 GHz.

  17. High energy ball milling study of Fe{sub 2}MnSn Heusler alloy

    SciTech Connect

    Jain, Vivek Kumar Lakshmi, N.; Jain, Vishal; Sijo, A. K.; Venugopalan, K.

    2015-06-24

    The structural and magnetic properties of as-melted and high energy ball milled alloy samples have been studied by X-ray diffraction, DC magnetization and electronic structure calculations by means of density functional theory. The observed properties are compared to that of the bulk sample. There is a very good enhancement of saturation magnetization and coercivity in the nano-sized samples as compared to bulk which is explained in terms of structural disordering and size effect.

  18. High energy ball milling study of Fe2MnSn Heusler alloy

    NASA Astrophysics Data System (ADS)

    Jain, Vivek Kumar; Lakshmi, N.; Jain, Vishal; Sijo A., K.; Venugopalan, K.

    2015-06-01

    The structural and magnetic properties of as-melted and high energy ball milled alloy samples have been studied by X-ray diffraction, DC magnetization and electronic structure calculations by means of density functional theory. The observed properties are compared to that of the bulk sample. There is a very good enhancement of saturation magnetization and coercivity in the nano-sized samples as compared to bulk which is explained in terms of structural disordering and size effect.

  19. Dielectric properties of vanadium doped barium titanate synthesized via high-energy ball milling

    NASA Astrophysics Data System (ADS)

    Dulian, Piotr; Bąk, Wojciech; Wieczorek-Ciurowa, Krystyna; Kajtoch, Czesław

    2014-06-01

    The study shows the advisability of using a mechanochemical synthesis method, based on a high-energy planetary ball milling, to a modification of barium titanate by a vanadium doping. This method improves useful properties of BaTi0:95V0:05O3 as a capacitor material. It has a high value of electric permittivity ɛ' in the wide range of temperature and low dielectric losses ɛ″ as well as a low electrical conductivity.

  20. The effect of oxygen on ball milling of a near-equiatomic FeV sigma phase

    SciTech Connect

    Costa, B. F. O.; Le Caeer, G.; Malaman, B.

    2008-10-15

    A coarse-grained near-equiatomic tetragonal sigma phase Fe{sub 48}V{sub 52} is milled in argon in a vibratory mill with a small steady air supply. The oxygen content increases regularly at a rate of about 0.25 at. %/h. Besides a classical short step, during which the sigma phase transforms into an alpha phase, two main steps occur. During the first step, from {approx}40 to {approx}140 h of milling, the bcc alpha phase is enriched in iron and heterogeneous because of a preferential oxidation of vanadium atoms. The bcc phase is partially amorphized as it is when milling in the absence of oxygen and nanocrystalline vanadium oxides do form. The second step is characterized by the coarsening of vanadium oxide particles and by the formation of ternary ferrous oxides. The results are discussed in the light of a vacancy mechanism proposed recently to account for the high stability of oxide nanoclusters in oxide dispersion strengthened Fe-based alloys processed by ball milling.

  1. Ball-milled solid dispersions of BCS Class IV drugs: Impact on the dissolution rate and intestinal permeability of acyclovir.

    PubMed

    Nart, Viviane; França, Maria Terezinha; Anzilaggo, Daiane; Riekes, Manoela Klüppel; Kratz, Jadel Müller; de Campos, Carlos Eduardo Maduro; Simões, Cláudia Maria Oliveira; Stulzer, Hellen Karine

    2015-08-01

    Acyclovir, an analog of 2'-deoxyguanosine, is one of the most important drugs in the current approved antiviral treatment. However, it's biopharmaceutical properties, contribute to acyclovir's poor oral bioavailability, which restricts the clinical use of the drug. In this view, the aim of this work was to improve the dissolution rate and intestinal permeability of acyclovir through the development of ball milling solid dispersions with the hydrophilic carriers Pluronic F68®, hydroxypropylmethyl cellulose K100M® and chitosan. Solid dispersions were obtained and completely characterized through different solid state techniques. The solid state data demonstrated a decrease in the crystallinity (amorphous phase and defects) and the presence of hydrogen bonds for SD HPMC and SD CTS. The enhancement of dissolution rates was observed for all SDs developed. In addition, no detrimental effects over the in vitro antiviral activity were detected. The solid dispersions with Pluronic F68® significantly improved the intestinal permeability of acyclovir across Caco-2 cells. In summary, the SDs developed in this study could be considered as potential systems for solid dosage forms containing acyclovir with superior biopharmaceutical properties.

  2. Magnetoresistivity and microstructure of YBa2Cu3Oy prepared using planetary ball milling

    NASA Astrophysics Data System (ADS)

    Hamrita, A.; Ben Azzouz, F.; Madani, A.; Ben Salem, M.

    2012-01-01

    We have studied the microstructure and the magnetoresistivity of polycrystalline YBa2Cu3Oy (YBCO or Y-123 for brevity) embedded with nanoparticles of Y-deficient YBCO, generated by the planetary ball milling technique. Bulk samples were synthesized from a precursor YBCO powder, which was prepared from commercial high purity Y2O3, Ba2CO3 and CuO via a one-step annealing process in air at 950 °C. After planetary ball milling of the precursor, the powder was uniaxially pressed and subsequently annealed at 950 °C in air. Phase analysis by X-ray diffraction (XRD), granular structure examination by scanning electron microscopy (SEM), microstructure investigation by transmission electron microscopy (TEM) coupled with energy dispersive X-ray spectroscopy (EDXS) were carried out. TEM analyses show that nanoparticles of Y-deficient YBCO, generated by ball milling, are embedded in the superconducting matrix. Electrical resistance as a function of temperature, ρ(T), revealed that the zero resistance temperature, Tco, is 84.5 and 90 K for the milled and unmilled samples respectively. The milled ceramics exhibit a large magnetoresistance in weak magnetic fields at liquid nitrogen temperature. This attractive effect is of high significance as it makes these materials promising candidates for practical application in magnetic field sensor devices.

  3. Microstructure and Physical Properties of Tb2TiO5 Neutron Absorber Synthesized by Ball Milling and Sintering

    NASA Astrophysics Data System (ADS)

    Huang, Jinghua; Ran, Guang; Liu, Tengjiao; Shen, Qiang; Li, Ning

    2016-10-01

    Tb2TiO5 neutron absorber was synthesized by ball milling and sintering. Microstructure character of ball-milled Tb4O7-17.605%TiO2 (mass fraction, %) powders and sintered bulks was analyzed using XRD, SEM and TEM. The microhardness, coefficient of thermal expansion and thermal conductivity of sintered bulks were measured. The experiment results showed that the nanocrystalline solid solution was obtained during ball milling. After 96 h of ball milling, TiO2 was completely solved in Tb4O7 and the crystal size of Tb4O7 was up to 37 nm. The bulk materials prepared by cold isostatic pressing were sintered at 1300 °C. Tb2TiO5 bulks with an orthorhombic structure were obtained. The microhardness of sintered bulks, as well as the thermal conductivity, increased firstly with increasing ball milling time and then decreased. The coefficient of thermal expansion decreased initially and then increased with increasing ball milling time. For the sintered bulk with powder milled for 48 h, the highest values of both microhardness and thermal conductivity were observed, whereas the lowest coefficient of thermal expansion was exhibited. In addition, with increasing testing temperature, the thermal conductivity of sintered bulks initially fell and then rebounded while an opposite trend was found in the coefficient of thermal expansion.

  4. Microstructure and Physical Properties of Tb2TiO5 Neutron Absorber Synthesized by Ball Milling and Sintering

    NASA Astrophysics Data System (ADS)

    Huang, Jinghua; Ran, Guang; Liu, Tengjiao; Shen, Qiang; Li, Ning

    2016-08-01

    Tb2TiO5 neutron absorber was synthesized by ball milling and sintering. Microstructure character of ball-milled Tb4O7-17.605%TiO2 (mass fraction, %) powders and sintered bulks was analyzed using XRD, SEM and TEM. The microhardness, coefficient of thermal expansion and thermal conductivity of sintered bulks were measured. The experiment results showed that the nanocrystalline solid solution was obtained during ball milling. After 96 h of ball milling, TiO2 was completely solved in Tb4O7 and the crystal size of Tb4O7 was up to 37 nm. The bulk materials prepared by cold isostatic pressing were sintered at 1300 °C. Tb2TiO5 bulks with an orthorhombic structure were obtained. The microhardness of sintered bulks, as well as the thermal conductivity, increased firstly with increasing ball milling time and then decreased. The coefficient of thermal expansion decreased initially and then increased with increasing ball milling time. For the sintered bulk with powder milled for 48 h, the highest values of both microhardness and thermal conductivity were observed, whereas the lowest coefficient of thermal expansion was exhibited. In addition, with increasing testing temperature, the thermal conductivity of sintered bulks initially fell and then rebounded while an opposite trend was found in the coefficient of thermal expansion.

  5. Ball milling: a green mechanochemical approach for synthesis of nitrogen doped carbon nanoparticles

    NASA Astrophysics Data System (ADS)

    Xing, Tan; Sunarso, Jaka; Yang, Wenrong; Yin, Yongbai; Glushenkov, Alexey M.; Li, Lu Hua; Howlett, Patrick C.; Chen, Ying

    2013-08-01

    Technological and scientific challenges coupled with environmental considerations have attracted a search for robust, green and energy-efficient synthesis and processing routes for advanced functional nanomaterials. In this article, we demonstrate a high-energy ball milling technique for large-scale synthesis of nitrogen doped carbon nanoparticles, which can be used as an electro-catalyst for oxygen reduction reactions after a structural refinement with controlled thermal annealing. The resulting carbon nanoparticles exhibited competitive catalytic activity (5.2 mA cm-2 kinetic-limiting current density compared with 7.6 mA cm-2 on Pt/C reference) and excellent methanol tolerance compared to a commercial Pt/C catalyst. The proposed synthesis route by ball milling and annealing is an effective process for carbon nanoparticle production and efficient nitrogen doping, providing a large-scale production method for the development of highly efficient and practical electrocatalysts.Technological and scientific challenges coupled with environmental considerations have attracted a search for robust, green and energy-efficient synthesis and processing routes for advanced functional nanomaterials. In this article, we demonstrate a high-energy ball milling technique for large-scale synthesis of nitrogen doped carbon nanoparticles, which can be used as an electro-catalyst for oxygen reduction reactions after a structural refinement with controlled thermal annealing. The resulting carbon nanoparticles exhibited competitive catalytic activity (5.2 mA cm-2 kinetic-limiting current density compared with 7.6 mA cm-2 on Pt/C reference) and excellent methanol tolerance compared to a commercial Pt/C catalyst. The proposed synthesis route by ball milling and annealing is an effective process for carbon nanoparticle production and efficient nitrogen doping, providing a large-scale production method for the development of highly efficient and practical electrocatalysts. Electronic

  6. Effect of adding ball-milled achenes to must on bioactive compounds and antioxidant activities in fruit wine.

    PubMed

    Lee, Pao-Ju; Chen, Shaun

    2016-03-01

    This study reports the utilization of ball-milled achenes in fermentation to increase the levels of ellagic acid and total phenol content, as well as to enhance the antioxidant capacity of strawberry wine. Achenes were micronized using ball-milling process, and then added to strawberry must prior to fermentation. The effects of the addition of ball-milled achenes on the ellagic acid and total phenol content in strawberry wine were determined, and the free radical scavenging and iron chelation activities were also analyzed. Quality attributes and acceptance were studied in comparison with a leading commercial strawberry wine for market application. The particle sizes of achenes were reduced from 1.1 mm to 400 nm after 30 min of ball-milling, and this led to an increase in the amount of extracted ellagic acid from 550.72 to 915.24 μg/g. The addition of ball-milled achenes to must led to a 19.72 % and 52.37 % increase in ellagic acid and total phenol content in strawberry wine, respectively. The increase in bioactive compounds resulted in increases of 54.09 %, 51.49 % and 56.97 % in ABTS and DPPH radical scavenging, and ferrous ion chelating activities, respectively. Although the commercial strawberry wine showed greater aroma intensity, no significant differences in overall quality and acceptance among the conventional process, added ball-milled achenes and the leading commercial strawberry wines were found. This study demonstrates that supplementation of ball-milled achenes in fermentation can be beneficial in increasing the levels of bioactive compounds and antioxidative capacity, indicating a good market potential. PMID:27570280

  7. Ball Mill Synthesis of Bulk Quaternary Cu2ZnSnSe4 and Thermoelectric Studies

    NASA Astrophysics Data System (ADS)

    Tiwari, Kunal J.; Prem Kumar, D. S.; Mallik, Ramesh Chandra; Malar, P.

    2016-08-01

    In this work, quaternary chalcogenide Cu2ZnSnSe4 (CZTSe) was synthesized using a mechanochemical ball milling process and its thermoelectric properties were studied by electrical resistivity, Seebeck coefficient, and thermal conductivity measurements. The synthesis process comprises three steps viz., wet ball milling of the elemental precursors, vacuum annealing, and densification by hot pressing. The purpose of this is to evaluate the feasibility of introducing wet milling in place of vacuum melting in solid state synthesis for the reaction of starting elements. We report the structural characterization and thermoelectric studies conducted on samples that were milled at 300 rpm and 500 rpm. X-ray diffraction (XRD) analysis showed the existence of multiple phases in the as-milled samples, indicating the requirement for heat treatment. Therefore, the ball milled powders were cold pressed and vacuum annealed to eliminate the secondary phases. Annealed samples were hot pressed and made into dense pellets for further investigations. In addition to XRD, energy dispersive spectroscopy (EDS) studies were performed on hot pressed samples to study the composition. XRD and EDS studies confirm CZTSe phase formation along with ZnSe secondary phase. Electrical resistivity and Seebeck coefficient measurements were done on the hot pressed samples in the temperature range 340-670 K to understand the thermoelectric behaviour. Thermal conductivity was calculated from the specific heat capacity and thermal diffusivity values. The thermoelectric figure of merit zT values for samples milled at 300 rpm and 500 rpm are ˜0.15 and ˜0.16, respectively, at 630 K, which is in good agreement with the values reported for solid state synthesized compounds.

  8. A study of the mechanism of microwave-assisted ball milling preparing ZnFe2O4

    NASA Astrophysics Data System (ADS)

    Zhang, Yingzhe; Wu, Yujiao; Qin, Qingdong; Wang, Fuchun; Chen, Ding

    2016-07-01

    In this paper, well dispersed ZnFe2O4 nano-particles with high magnetization saturation of 82.23 emu/g were first synthesized by microwave assisted ball milling and then the influences of pre-treatments and microwave powers to the progress were studied. It was found that under the both function of crack effect induced by ball milling and rotary motion induced by microwave the synthesized ferrtie nano-particles were well dispersed that is much different from the powders synthesized by normal high energy ball milling. The pre-treatment of ball milling can only enhance the reaction rate in the first several hours but the pre-irradiation of microwave can enhance the hole reaction rate. Further more, it was also been found that with increasing the microwave power, the more raw materials will converted into zinc ferrite in the first 5 h. 5 h latter the microwave power of 720 W is high enough for the coupling effect of microwave and ball milling with stirrer rotation speed of 256 rpm.

  9. Electrochemical properties of the TiO2(B) powders ball mill treated for lithium-ion battery application

    PubMed Central

    2013-01-01

    Background Belt or wire shaped TiO2(B) particles were synthesized for lithium ion battery application by a hydrothermal and heat treatment process. In order to facilitate TiO2(B)/C composites fabrication, the synthesized TiO2(B) particles were crushed into smaller sizes by ball milling. Results Ball mill treated TiO2(B) particles of less than 1.0 μm with a fraction of anatase phase, compared to as-synthesized TiO2(B) particles with about 24 μm in average particle size, showed a significant improvement in the electrochemical properties. They showed a much improved stability in the charge–discharge cycles and irreversibility. They maintained about 98% of the initial capacity during 50 cycles while as-synthesized sample before ball mill treatment showed a gradual decrease in the capacity with the cycles. The irreversibility of 12.4% of as-synthesized sample was also greatly improved to 7% after ball milling treatment. Conclusions Our results indicate ball mill treatment can be an economical way to improve electrochemical properties of TiO2(B) anode materials for lithium ion battery application. PMID:24196343

  10. Energy efficiency of cement finish grinding in a dry batch ball mill

    SciTech Connect

    Touil, D.; Belaadi, S.; Frances, C. . E-mail: Christine.Frances@ensiacet.fr

    2006-03-15

    Dry grinding experiments on cement clinker were carried out using a laboratory batch ball mill equipped with torque measurement. The specific energy was found to be dependent on operating parameters and clinker environment. Additional compounds such as gypsum and pozzolanic tuff improve energy efficiency. The optimal parameters allowing maximising the energy efficiency factor were determined. Energy efficiency factors were obtained both on the crude material (size minus 2.8 mm) and on a sieved fraction (1-0.71 mm). They demonstrate that a low initial rate of breakage implies higher energy efficiency. On the contrary, conditions ensuring an initial maximal rate of breakage lead to an increase of the energy consumption.

  11. Generation of drugs coated iron nanoparticles through high energy ball milling

    NASA Astrophysics Data System (ADS)

    Radhika Devi, A.; Chelvane, J. A.; Prabhakar, P. K.; Padma Priya, P. V.; Doble, Mukesh; Murty, B. S.

    2014-03-01

    The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.

  12. Parametric evaluation of ball milling of SiC in water

    NASA Technical Reports Server (NTRS)

    Kiser, J. D.; Herbell, T. P.; Freedman, M. R.

    1985-01-01

    A statistically designed experiment was conducted to determine optimum conditions for ball milling alpha-SiC in water. The influence of pH adjustment, volume percent solids loading, and mill rotational speed on grinding effectiveness was examined. An equation defining the effect of those milling variables on specific surface area was obtained. The volume percent solids loading of the slurry had the greatest influence on the grinding effectiveness in terms of increase in specific surface area. As grinding effectiveness improved, mill and media wear also increased. Contamination was minimized by use of sintered alpha-SiC milling hardware.

  13. Ball Milling Assisted Solvent and Catalyst Free Synthesis of Benzimidazoles and Their Derivatives.

    PubMed

    El-Sayed, Taghreed H; Aboelnaga, Asmaa; Hagar, Mohamed

    2016-01-01

    Benzoic acid and o-phenylenediamine efficiently reacted under the green solvent-free Ball Milling method. Several reaction parameters were investigated such as rotation frequency; milling balls weight and milling time. The optimum reaction condition was milling with 56.6 g weight of balls at 20 Hz frequency for one hour milling time. The study was extended for synthesis of a series of benzimidazol-2-one or benzimidazol-2-thione using different aldehydes; carboxylic acids; urea; thiourea or ammonium thiocyanate with o-phenylenediamine. Moreover; the alkylation of benzimidazolone or benzimidazolthione using ethyl chloroacetate was also studied. PMID:27563861

  14. Generation of drugs coated iron nanoparticles through high energy ball milling

    SciTech Connect

    Radhika Devi, A.; Murty, B. S.; Chelvane, J. A.; Prabhakar, P. K.; Padma Priya, P. V.; Doble, Mukesh

    2014-03-28

    The iron nanoparticles coated with oleic acid and drugs such as folic acid/Amoxicillin were synthesized by high energy ball milling and characterized by X-ray diffraction, Transmission electron microscope, zeta potential, dynamic light scattering, Fourier Transform Infra red (FT-IR) measurements, and thermo gravimetric analysis (TGA). FT-IR and TGA measurements show good adsorption of drugs on oleic acid coated nanoparticles. Magnetic measurements indicate that saturation magnetization is larger for amoxicillin coated particles compared to folic acid coated particles. The biocompatibility of the magnetic nanoparticles prepared was evaluated by in vitro cytotoxicity assay using L929 cells as model cells.

  15. Magnetic and Magnetocaloric Properties of High-Energy Ball-Milled Nanocrystalline CeMn2Ge2 Compound

    NASA Astrophysics Data System (ADS)

    Kaya, Melike; Dincer, Ilker; Akturk, Selcuk; Elerman, Yalcin

    2016-10-01

    CeMn2Ge2 nanopowders have been obtained by high-energy ball milling for 5 and 10 hours from bulk compound to investigate the effect of milling time on magnetic and magnetocaloric properties. CeMn2Ge2 nanopowders have been characterized by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy, transmission electron microscopy, and magnetization measurements. The average grain size of the nanoparticles from XRD measurements is about 12.2 and 8 nm for 5-hour and 10-hour ball-milled samples, respectively. The investigations reveal that magnetic entropy change (∆ S m) can be altered by changing the particle size of the compound. Maximum ∆ S m is -2.45 and -1.30 J kg-1 K-1 for the 5- and 10-hour ball-milled nanopowders, respectively.

  16. Magnetic and Magnetocaloric Properties of High-Energy Ball-Milled Nanocrystalline CeMn2Ge2 Compound

    NASA Astrophysics Data System (ADS)

    Kaya, Melike; Dincer, Ilker; Akturk, Selcuk; Elerman, Yalcin

    2016-07-01

    CeMn2Ge2 nanopowders have been obtained by high-energy ball milling for 5 and 10 hours from bulk compound to investigate the effect of milling time on magnetic and magnetocaloric properties. CeMn2Ge2 nanopowders have been characterized by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy, transmission electron microscopy, and magnetization measurements. The average grain size of the nanoparticles from XRD measurements is about 12.2 and 8 nm for 5-hour and 10-hour ball-milled samples, respectively. The investigations reveal that magnetic entropy change (∆S m) can be altered by changing the particle size of the compound. Maximum ∆S m is -2.45 and -1.30 J kg-1 K-1 for the 5- and 10-hour ball-milled nanopowders, respectively.

  17. Strong textured SmCo5 nanoflakes with ultrahigh coercivity prepared by multistep (three steps) surfactant-assisted ball milling

    NASA Astrophysics Data System (ADS)

    Zuo, Wen-Liang; Zhao, Xin; Xiong, Jie-Fu; Zhang, Ming; Zhao, Tong-Yun; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

    2015-08-01

    The high coercivity of 26.2 kOe for SmCo5 nanoflakes are obtained by multistep (three steps) surfactant-assisted ball milling. The magnetic properties, phase structure and morphology are studied by VSM, XRD and SEM, respectively. The results demonstrate that the three step ball-milling can keep more complete crystallinity (relatively less defects) during the process of milling compared with one step high energy ball-milling, which enhances the texture degree and coercivity. In addition, the mechanism of coercivity are also studied by the temperature dependence of demagnetization curves for aligned SmCo5 nanoflakes/resin composite, the result indicates that the magnetization reversal could be controlled by co-existed mechanisms of pinning and nucleation.

  18. Bioethanol production from ball milled bagasse using an on-site produced fungal enzyme cocktail and xylose-fermenting Pichia stipitis.

    PubMed

    Buaban, Benchaporn; Inoue, Hiroyuki; Yano, Shinichi; Tanapongpipat, Sutipa; Ruanglek, Vasimon; Champreda, Verawat; Pichyangkura, Rath; Rengpipat, Sirirat; Eurwilaichitr, Lily

    2010-07-01

    Sugarcane bagasse is one of the most promising agricultural by-products for conversion to biofuels. Here, ethanol fermentation from bagasse has been achieved using an integrated process combining mechanical pretreatment by ball milling, with enzymatic hydrolysis and fermentation. Ball milling for 2 h was sufficient for nearly complete cellulose structural transformation to an accessible amorphous form. The pretreated cellulosic residues were hydrolyzed by a crude enzyme preparation from Penicillium chrysogenum BCC4504 containing cellulase activity combined with Aspergillus flavus BCC7179 preparation containing complementary beta-glucosidase activity. Saccharification yields of 84.0% and 70.4% for glucose and xylose, respectively, were obtained after hydrolysis at 45 degrees C, pH 5 for 72 h, which were slightly higher than those obtained with a commercial enzyme mixture containing Acremonium cellulase and Optimash BG. A high conversion yield of undetoxified pretreated bagasse (5%, w/v) hydrolysate to ethanol was attained by separate hydrolysis and fermentation processes using Pichia stipitis BCC15191, at pH 5.5, 30 degrees C for 24 h resulting in an ethanol concentration of 8.4 g/l, corresponding to a conversion yield of 0.29 g ethanol/g available fermentable sugars. Comparable ethanol conversion efficiency was obtained by a simultaneous saccharification and fermentation process which led to production of 8.0 g/l ethanol after 72 h fermentation under the same conditions. This study thus demonstrated the potential use of a simple integrated process with minimal environmental impact with the use of promising alternative on-site enzymes and yeast for the production of ethanol from this potent lignocellulosic biomass.

  19. Influence of Iron Oxide Particles on the Strength of Ball-Milled Iron

    SciTech Connect

    Lesuer, D R; Syn, C K; Sherby, O D

    2005-12-07

    Detailed microstructural and mechanical property studies of ball-milled iron, in the powder and consolidated states, are reviewed and assessed. The analyses cover three and one-half orders of magnitude of grain size (from 6 nm to 20 mm) and focus on the influence of oxide particles on the strength. The study includes the early work of Koch and Yang, Kimura and Takaki and continues with the more recent work of Umemoto et al and Belyakov, Sakai et al. It is shown that the major contributors to strength are the nanooxide particles. These particles are created by adiabatic shear banding during ball-milling leading to a bimodal distribution of particles. The predicted strength from particles, {sigma}{sub p}, is given by {sigma}{sub p} = B {center_dot} (D*{sub S}){sup -1/2} where D*{sub S} is the surface-to-surface interparticle spacing, and B = 395 MPa {center_dot} {micro}m{sup -1/2}. A model is proposed that accounts for the influence of the bimodal particle size distribution on strength.

  20. Effect of ball milling energy on rheological and thermal properties of amaranth flour.

    PubMed

    Roa, Diego F; Baeza, Rosa I; Tolaba, Marcela P

    2015-12-01

    Pearled amaranth grains obtained by abrasive milling were processed by planetary ball milling to produce amaranth flours. The influence of milling energy on rheological and thermal behavior of amaranth flour dispersions and stability during 24 h storage at 4 °C were investigated based on a factorial design. The rheological behavior of flour dispersions (4 % and 8 % w/v) was determined using a rotational viscometer, while gelatinization degree was determined by differential scanning calorimetry as a measure of structural changes.The power law model was found to be suitable in expressing the relationship between shear stress and shear rate. Flour dispersions showed a pseudoplastic behavior. However this character decreased with the storage being dependent on flour concentration and milling energy. A decrease of the consistency index and an increase of the flow behavior index were observed as a result of the increasing milling energy. Gelatinization enthalpy decrease showed the loss of crystalline structure due to ball milling. Amaranth flour dispersions presented increasing stability during storage. It was observed, that the stability changed with the concentration of amaranth flours.Thus, more stable dispersions were obtained as the flour concentration increased. The highly milled sample was the most stable sample during the storage.

  1. Fast sample preparation for analysis of tablets and capsules: the ball-mill extraction method.

    PubMed

    Kok, S J; Debets, A J

    2001-11-01

    A new ball-mill extraction method for solid dosage forms was developed. It was used for tablets, and compared with a conventional (powdering and sonication) method applied in pharmaceutical analysis of solid dosage forms. The ball-mill sample preparation procedure is both quantitative and fast. No powdering, weighing and sonication steps are needed in the sample preparation. The complete procedure takes 2 min (milling and extraction) and 5 min (centrifugation), respectively, much less than the conventional method in which sample preparation takes approximately 45-90 min. The samples are centrifuged in the mill vial, which saves time and avoids evaporation of solvent. Stainless steel extraction vials with different diameters were fabricated to enable the use of various extraction volumes. The extraction recovery was tested using various types of tablets (small, large and extended release tablets) with active compounds at low and higher concentrations, recoveries were comparable with the conventional method. The relative small investment and simplicity of the method makes it excellently suited for use in various pharmaceutical (development and quality assurance) laboratories. PMID:11516911

  2. Ball mill assisted rapid mechanochemical extraction method for natural products from plants.

    PubMed

    Wang, Man; Bi, Wentao; Huang, Xiaohua; Chen, David Da Yong

    2016-06-01

    A ball mill assisted mechanochemical extraction method was developed to extract compounds of natural product (NP) from plant using ionic liquid (IL). A small volume ball mill, also known as PastPrep(®) Homogenizer, which is often used for high-speed lysis of biological samples and for other applications, was used to dramatically increase the speed, completeness and reproducibility of the extraction process at room temperature to preserve the chemical integrity of the extracted compounds. In this study, tanshinones were selected as target compounds to evaluate the performance of this extraction method. Factors affecting the extraction efficiency, such as the duration, IL concentration and solid/liquid ratio were systematically optimized using the response surface methodology. Under the optimized conditions, the described method was more efficient and much faster than the conventional extraction methods such as methanol based ultrasound assisted extraction (UAE) and heat reflux extraction (HRE) that consumes a lot more organic solvent. In addition, the natural products of interest were enriched by anion metathesis of ionic liquids, combining extraction and preconcentration in the same process. The extractant was analyzed by HPLC and LC-MS. The reproducibility (RSD, n=5), correlation coefficient (r(2)) of the calibration curve, and the limit of detection, were determined to be in the range of 4.7-5.2%, 0.9992-0.9995, and 20-51ng/mL, respectively. PMID:27157426

  3. Ball mill assisted rapid mechanochemical extraction method for natural products from plants.

    PubMed

    Wang, Man; Bi, Wentao; Huang, Xiaohua; Chen, David Da Yong

    2016-06-01

    A ball mill assisted mechanochemical extraction method was developed to extract compounds of natural product (NP) from plant using ionic liquid (IL). A small volume ball mill, also known as PastPrep(®) Homogenizer, which is often used for high-speed lysis of biological samples and for other applications, was used to dramatically increase the speed, completeness and reproducibility of the extraction process at room temperature to preserve the chemical integrity of the extracted compounds. In this study, tanshinones were selected as target compounds to evaluate the performance of this extraction method. Factors affecting the extraction efficiency, such as the duration, IL concentration and solid/liquid ratio were systematically optimized using the response surface methodology. Under the optimized conditions, the described method was more efficient and much faster than the conventional extraction methods such as methanol based ultrasound assisted extraction (UAE) and heat reflux extraction (HRE) that consumes a lot more organic solvent. In addition, the natural products of interest were enriched by anion metathesis of ionic liquids, combining extraction and preconcentration in the same process. The extractant was analyzed by HPLC and LC-MS. The reproducibility (RSD, n=5), correlation coefficient (r(2)) of the calibration curve, and the limit of detection, were determined to be in the range of 4.7-5.2%, 0.9992-0.9995, and 20-51ng/mL, respectively.

  4. Dissipation mechanisms in polycrystalline YBCO prepared by sintering of ball-milled precursor powder

    NASA Astrophysics Data System (ADS)

    Hannachi, E.; Ben Salem, M. K.; Slimani, Y.; Hamrita, A.; Zouaoui, M.; Ben Azzouz, F.; Ben Salem, M.

    2013-12-01

    Magnetoresistivity (ρ(T,H)) measurements of polycrystalline YBa2Cu3Oy (Y-123) and YBa2Cu3Oy embedded with nanoparticles of Y-deficient Y-123, generated by the planetary ball milling, have been compared and analyzed by the Ambegaokar and Halperin phase slip model (AH) and thermally activated flux creep (TAFC). Phase analysis by X-ray diffraction (XRD), granular structure examination by scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDXS), were carried out. SEM analyses show that nanoparticles of Y-deficient Y-123, generated by ball milling, are embedded in the superconducting matrix. The broadening of the resistive transition under magnetic field is found to possess two distinct regions, which suggests that dissipation phenomenon in milled and unmilled samples is caused by two mechanisms: the order parameter fluctuations and the vortex-dynamics separated by a crossover temperature T. The critical current Jc(0) at zero temperature in the grain boundaries decreases as a power law, H, which is an indication of the sensitivity of a single junction between the superconducting grains to the applied magnetic field. Jc(0) of the milled material is higher than the one of the unmilled and the activation energies of vortex flux motion U(H) behavior in the applied magnetic field is enhanced by the presence of the nanoparticles embedded in the matrix.

  5. Characterization of ball-milled carbon nanotube dispersed aluminum mixed powders

    NASA Astrophysics Data System (ADS)

    Maleque, M. A.; Abdullah, U.; Yaacob, I.; Ali, Y.

    2016-04-01

    Currently, carbon nanotube (CNT) is attracting much interest as fibrous materials for reinforcing aluminum matrix composites due to unique properties, such as high strength, elastic modulus, flexibility and high aspect ratios. However, the quality of the dispersion is the major concerning factor which determines the homogeneity of the enhanced mechanical and tribological properties of the composite. This work study and characterized carbon nanotube dispersion in ballmilled CNT-aluminum mixed powders with four different formulations such as 1, 1.5, 2 and 2.5 wt% CNT under high energy planetary ball milling operations. The ball milling was performed for two hours at constant milling speed of 250 rpm under controlled atmosphere. The characterization is performed using FESEM and EDX analyzer for mapping, elemental and line analysis. The experimental results showed homogeneous dispersion of CNTs in aluminum matrix. The composite mixture showed similar pattern from mapping, elemental and line analysis. Identification of only two peaks proved that controlled atmosphere during milling prevented the formation of inter metallic compounds such as aluminum carbide in the composite mixture. Therefore, this CNT-A1 composite powder mixture can be used for new nano-composite development without any agglomeration problem.

  6. Structure and hard magnetic properties of barium hexaferrite with and without La 2O 3 prepared by ball milling

    NASA Astrophysics Data System (ADS)

    Babu, V.; Padaikathan, P.

    2002-03-01

    The barium hexaferrites have been prepared by ball milling of a BaO 2 and Fe 2O 3 mixture followed by thermal heat treatments. The structure and magnetic properties were investigated using X-ray diffraction, scanning electron microscopy and vibrating sample magnetometer techniques. The effect of grain refiner was also studied and it was found that the hard magnetic properties were improved significantly. The sintered product of barium hexaferrite powders prepared from ball milling has higher coercive force than that of other barium hexaferrite made from oxide/carbonate.

  7. Preparation of chiral amino esters by asymmetric phase-transfer catalyzed alkylations of Schiff bases in a ball mill.

    PubMed

    Nun, Pierrick; Pérez, Violaine; Calmès, Monique; Martinez, Jean; Lamaty, Frédéric

    2012-03-19

    The asymmetric alkylation of Schiff bases under basic conditions in a ball mill was performed. The starting Schiff bases of glycine were prepared beforehand by milling protected glycine hydrochloride and benzophenone imine, in the absence of solvent. The Schiff base was then reacted with a halogenated derivative in a ball mill in the presence of KOH. By adding a chiral ammonium salt derived from cinchonidine, the reaction proceeded asymmetrically under phase-transfer catalysis conditions, giving excellent yields and enantiomeric excesses up to 75 %. Because an equimolar amount of starting material was used, purification was greatly simplified.

  8. Reaction between LiBH4 and MgH2 induced by high-energy ball milling

    NASA Astrophysics Data System (ADS)

    Ding, Zhao; Zhao, Xuzhe; Shaw, Leon L.

    2015-10-01

    Previous studies of ab initio density functional theory (DFT) calculations have predicted that reactions between LiBH4 and MgH2 can take place at temperature near 200 °C. However, such predictions have been shown to be inconsistent with many experiments. Herein, we have designed a novel process termed as ball milling with aerosol spraying (BMAS) to prove, for the first time, that the reaction between LiBH4 and MgH2 can indeed occur during ball milling at room temperature. Through this BMAS process we have demonstrated unambiguously the formation of MgB2 and LiH during ball milling of MgH2 while aerosol spraying of the LiBH4/THF solution. In this BMAS process, aerosol spraying of the LiBH4/THF solution leads to the formation of LiBH4 nanoparticles which decompose to form Li2B12H12. The Li2B12H12 formed then reacts with MgH2 in situ during ball milling to form MgB2 and LiH. The discovery made in this study has significant implications in making LiBH4 + MgH2 as a viable system for reversible hydrogen storage applications near ambient temperature in the future.

  9. Effect of ball-milling surfactants on the interface chemistry in hot-compacted SmCo5 magnets

    SciTech Connect

    Li, WF; Sepehri-Amin, H; Zheng, LY; Cui, BZ; Gabay, AM; Hono, K; Huang, WJ; Ni, C; Hadjipanayis, GC

    2012-11-01

    Anisotropic SmCo5 nanoflakes prepared by high-energy ball-milling with surfactants have great potential in applications for high-performance nanocomposite magnets. For such "nanocomposite" applications, the surface structure and chemistry of nanoflakes are crucial for achieving high coercivity. In this study, hot-pressed samples from anisotropic SmCo5 nanoflakes, ball-milled with different surfactants, oleic acid (OA) and oleylamine (OY), were investigated. Interface layers between the SmCo5 nanoflakes were found to consist of samarium oxides and a soft magnetic Co phase. These surface layers contribute to the degradation of hard magnetic performance, which is confirmed by scanning transmission electron microscopy-energy dispersive X-ray spectroscopy analysis of the cross-section of a single flake ball-milled with OA. Samples milled with OY show a much thinner interface layer in compacted samples, which means that the surface degradation during ball-milling with OY is much less than that with OA. The results show clearly that the choice of proper surfactant and the control of processing parameters are the key factors for improving the surface condition of the nanoflakes and the resulting hard magnetic properties. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  10. One step conversion of wheat straw to sugars by simultaneous ball milling, mild acid, and fungus Penicillium simplicissimum treatment.

    PubMed

    Yuan, Li; Chen, Zhenhua; Zhu, Yonghua; Liu, Xuanming; Liao, Hongdong; Chen, Ding

    2012-05-01

    Wheat straw is one of the major lignocellulosic plant residues in many countries including China. An attractive alternative is the utilization of wheat straw for bioethanol production. This article mainly studies a simple one-step wet milling with Penicillium simplicissimum and weak acid to hydrolysis of wheat straw. The optimal condition for hydrolysis was ball milling 48 h in citrate solvent (pH = 4) with P. simplicissimum H5 at the speed of 500 rpm and the yield of sugar increased with increased milling time. Corresponding structure transformations before and after milling analyzed by X-ray diffraction, transmission Fourier transform infrared spectroscopy, and environmental scanning electron microscopy clearly indicated that this combined treatment could be attributed to the crystalline and chemical structure changes of cellulose in wheat straw during ball milling. This combined treatment of ball milling, mild acid, and fungus hydrolysis enabled the conversion of the wheat straw. Compared with traditional method of ball milling, this work showed a more simple, novel, and environmentally friendly way in mechanochemical treatment of wheat straw.

  11. Hydrophobic cellulose films with excellent strength and toughness via ball milling activated acylation of microfibrillated cellulose.

    PubMed

    Deng, Sha; Huang, Rui; Zhou, Mi; Chen, Feng; Fu, Qiang

    2016-12-10

    Cellulose films with excellent mechanical strength are of interest to many researchers, but unfortunately they often lack the ductility and water resistance. This work demonstrates an efficient and easily industrialized method for hydrophobic cellulose films made of modified microfibrillated cellulose (MFC). Prior to film fabrication, the simultaneous exfoliation and acylation of MFC was achieved through the synergetic effect of mechanical and chemical actions generated from ball milling in the presence of hexanoyl chloride. Largely enhanced tensile strength and elongation at break have been achieved (4.98MPa, 4.37% for original MFC films, 140MPa, 21.3% for modified ones). Due to hydrophobicity and compact structure, modified films show excellent water resistance and decreased water vapor permeability. Moreover, optical performance of modified films is also improved compared with the original MFC films. Our work can largely expand the application of this biodegradable resource and ultimately reduce the need for petroleum-based plastics. PMID:27577904

  12. Dehydrogenation kinetics of as-received and ball-milled LiAlH4

    NASA Astrophysics Data System (ADS)

    Andreasen, A.; Vegge, T.; Pedersen, A. S.

    2005-12-01

    In this paper, we investigate the dehydrogenation kinetics of LiAlH4 into Li3AlH6 (reaction I) and further into LiH (reaction II). We find the apparent activation energies to be ∼ 80 and 100 kJ/mol for reactions I and II, respectively. Furthermore, we investigate the effect of ball milling on crystallite size and the dehydrogenation kinetics of both reactions I and II. We find a clear correlation between crystallite size and dehydrogenation kinetics of reaction I. On the other hand, we find the kinetics of reaction II to be independent of the crystallite size. This indicates that reaction I is limited by a mass transfer process, while reaction II is limited by the intrinsic kinetics.

  13. EXAFS study of metal-coated particles produced by ball milling

    SciTech Connect

    Heald, S.M.; Jayanetti, S.; Pandya, K.I.

    1992-01-01

    EXAFS measurements have been carried out on mixtures of Sa with Ge and Si, and Pt with SiO[sub 2] which have been ball milled for extended periods. In these systems the brittle component (Ge, Si, or SiO[sub 2]) is ground to nanocrystalline dimensions while the ductile metal is found to coat the outer surface the particles. Analysis shows that in the Sn-Ge and Sn-Si systems, mixing at the interface is found to form apparently cubic SnGe and SnSi alloys respectively. In the Pt-SiO[sub 2] system while no mixing is observed, the Pt is found to be highly dispersed on the surface of SiO[sub 2] particles.

  14. EXAFS study of metal-coated particles produced by ball milling

    SciTech Connect

    Heald, S.M.; Jayanetti, S.; Pandya, K.I.

    1992-11-01

    EXAFS measurements have been carried out on mixtures of Sa with Ge and Si, and Pt with SiO{sub 2} which have been ball milled for extended periods. In these systems the brittle component (Ge, Si, or SiO{sub 2}) is ground to nanocrystalline dimensions while the ductile metal is found to coat the outer surface the particles. Analysis shows that in the Sn-Ge and Sn-Si systems, mixing at the interface is found to form apparently cubic SnGe and SnSi alloys respectively. In the Pt-SiO{sub 2} system while no mixing is observed, the Pt is found to be highly dispersed on the surface of SiO{sub 2} particles.

  15. Hydrogen storage materials discovery via high throughput ball milling and gas sorption.

    PubMed

    Li, Bin; Kaye, Steven S; Riley, Conor; Greenberg, Doron; Galang, Daniel; Bailey, Mark S

    2012-06-11

    The lack of a high capacity hydrogen storage material is a major barrier to the implementation of the hydrogen economy. To accelerate discovery of such materials, we have developed a high-throughput workflow for screening of hydrogen storage materials in which candidate materials are synthesized and characterized via highly parallel ball mills and volumetric gas sorption instruments, respectively. The workflow was used to identify mixed imides with significantly enhanced absorption rates relative to Li2Mg(NH)2. The most promising material, 2LiNH2:MgH2 + 5 atom % LiBH4 + 0.5 atom % La, exhibits the best balance of absorption rate, capacity, and cycle-life, absorbing >4 wt % H2 in 1 h at 120 °C after 11 absorption-desorption cycles.

  16. Microwave Absorption Properties of Iron Nanoparticles Prepared by Ball-Milling

    NASA Astrophysics Data System (ADS)

    Chu, Xuan T. A.; Ta, Bach N.; Ngo, Le T. H.; Do, Manh H.; Nguyen, Phuc X.; Nam, Dao N. H.

    2016-05-01

    A nanopowder of iron was prepared using a high-energy ball milling method, which is capable of producing nanoparticles at a reasonably larger scale compared to conventional chemical methods. Analyses using x-ray diffraction and magnetic measurements indicate that the iron nanoparticles are a single phase of a body-centered cubic structure and have quite stable magnetic characteristics in the air. The iron nanoparticles were then mixed with paraffin and pressed into flat square plates for free-space microwave transmission and reflection measurements in the 4-8 GHz range. Without an Al backing plate, the Fe nanoparticles seem to only weakly absorb microwave radiation. The reflected signal S 11 drops to zero and a very large negative value of reflection loss ( RL) are observed for Al-backed samples, suggesting the existence of a phase matching resonance near frequency f ˜ 6 GHz.

  17. Solid acid-catalyzed depolymerization of barley straw driven by ball milling.

    PubMed

    Schneider, Laura; Haverinen, Jasmiina; Jaakkola, Mari; Lassi, Ulla

    2016-04-01

    This study describes a time and energy saving, solvent-free procedure for the conversion of lignocellulosic barley straw into reducing sugars by mechanocatalytical pretreatment. The catalytic conversion efficiency of several solid acids was tested which revealed oxalic acid dihydrate as a potential catalyst with high conversion rate. Samples were mechanically treated by ball milling and subsequently hydrolyzed at different temperatures. The parameters of the mechanical treatment were optimized in order to obtain sufficient amount of total reducing sugar (TRS) which was determined following the DNS assay. Additionally, capillary electrophoresis (CE) and Fourier transform infrared spectrometry (FT-IR) were carried out. Under optimal conditions TRS 42% was released using oxalic acid dihydrate as a catalyst. This study revealed that the acid strength plays an important role in the depolymerization of barley straw and in addition, showed, that the oxalic acid-catalyzed reaction generates low level of the degradation product 5-hydroxymethylfurfural (HMF). PMID:26859328

  18. Structural, microstructural and magnetocaloric investigations in high-energy ball milled NiMnGa powders

    NASA Astrophysics Data System (ADS)

    de Santanna, Y. V. B.; de Melo, M. A. C.; Santos, I. A.; Coelho, A. A.; Gama, S.; Cótica, L. F.

    2008-11-01

    In this paper, structural, microstrucutural and magnetocaloric properties of Ni 2.18Mn 0.82Ga alloys submitted to high-energy ball milling are reported. A 7-layered orthorhombic martensitic ( Pnnm) phase was detected in post-milling annealed samples, which reached a microstrucuture composed predominantly by nanograins. The magnetocaloric effect is strongly weakened in comparison with as-cast samples of similar composition. This effect can be attributed to the absence of the mesoscale twin-related martensitic variants in the nanostructurated powders. However, post-milled samples annealed at 1123 K for 4 h present relative cooling powers as high as those observed for manganites. Therefore, these materials can be considered as potential candidates for use as regenerators in prototypal magnetic refrigerators.

  19. Solvent-free ball-milling subcomponent synthesis of metallosupramolecular complexes.

    PubMed

    Giri, Chandan; Sahoo, Prasit Kumar; Puttreddy, Rakesh; Rissanen, Kari; Mal, Prasenjit

    2015-04-20

    Subcomponent self-assembly from components A, B, C, D, and Fe(2+) under solvent-free conditions by self-sorting leads to the construction of three structurally different metallosupramolecular iron(II) complexes. Under carefully selected ball-milling conditions, tetranuclear [Fe4 (AD2 )6 ](4-) 22-component cage 1, dinuclear [Fe2 (BD2 )3 ](2-) 11-component helicate 2, and 5-component mononuclear [Fe(CD3 )](2+) complex 3 were prepared simultaneously in a one-pot reaction from 38 components. Through subcomponent substitution reaction by adding subcomponent B, the [Fe4 (AD2 )6 ](4-) cage converts quantitatively to the [Fe2 (BD2 )3 ](2-) helicate, which, in turn, upon addition of subcomponent C, transforms to [Fe(CD3 )](2+) , following the hierarchical preference based on the thermodynamic stability of the complexes.

  20. Cross-Coupling Biarylation of Nitroaryl Chlorides Through High Speed Ball Milling

    PubMed Central

    Lam, Solita; Puplampu-Dove, Yvonne; Morris, Adrienne; Epps, Ayunna; Mandouma, Ghislain

    2016-01-01

    Solvent-free reaction using a high-speed ball milling technique has been applied to the classical Ullmann coupling reaction. Cross-coupling biarylation of several nitroaryl chlorides was achieved in good yields when performed in custom-made copper vials through continuous shaking without additional copper or solvent. Cross-coupling products were obtained almost pure and NMR-ready. These reactions were cleaner than solution phase coupling which require longer reaction time in high boiling solvents, and added catalysts as well as lengthy extraction and purification steps. Gram quantities of cross biaryl compounds have been synthesized with larger copper vials, a proof that this method can be used to reduce industrial waste and for sustainability. PMID:27294205

  1. Influence of milling time on fineness of Centella Asiatica particle size produced using planetary ball mill

    NASA Astrophysics Data System (ADS)

    Borhan, M. Z.; Ahmad, R.; Rusop, M.; Abdullah, S.

    2012-11-01

    Centella Asiatica (C. Asiatica)contains asiaticoside as bioactive constituent which can be potentially used in skin healing process. Unfortunately, the normal powders are difficult to be absorbed by the body effectively. In order to improve the value of use, nano C. Asiatica powder was prepared. The influence of milling time was carried out at 0.5, 2, 4, 6, 8 hours and 10 hours. The effect of ball milling at different times was characterized using particles size analysis and FTIR Spectroscopy. The fineness of ground product was evaluated by recording the z-Average (nm), undersize distribution and polydispersity index (PdI). The results show that the smallest size particles by mean is 233 nm while FTIR spectra shows that there is no changing in the major component in the C. Asiatica powders with milling time.

  2. Preparation, characterization and optoelectronic properties of nanodiamonds doped zinc oxide nanomaterials by a ball milling technique

    NASA Astrophysics Data System (ADS)

    Ullah, Hameed; Sohail, Muhammad; Malik, Uzma; Ali, Naveed; Bangash, Masroor Ahmad; Nawaz, Mohsan

    2016-07-01

    Zinc oxide (ZnO) is one of the very important metal oxides (MOs) for applications in optoelectronic devices which work in the blue and UV regions. However, to meet the challenges of obtaining ZnO nanomaterials suitable for practical applications, various modifications in physico-chemical properties are highly desirable. One of the ways adopted for altering the properties is to synthesize composite(s) of ZnO with various reinforcements. Here we report on the tuning of optoelectronic properties of ZnO upon doping by nanodiamonds (NDs) using the ball milling technique. A varying weight percent (wt.%) of NDs were ball milled for 2 h with ZnO nanoparticles prepared by a simple precipitation method. The effects of different parameters, the calcination temperature of ZnO, wt.% of NDs and mechanical milling upon the optoelectronic properties of the resulting ZnO-NDs nanocomposites have been investigated. The ZnO-NDs nanocomposites were characterized by IR spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDX). The UV-vis spectroscopy revealed the alteration in the bandgap energy (Eg ) of ZnO as a function of the calcination temperature of ZnO, changing the concentration of NDs, and mechanical milling of the resulting nanocomposites. The photoluminescence (PL) spectroscopy showed a decrease in the deep level emission (DLE) peaks and an increase in near-band-edge transition peaks as a result of the increasing concentration of NDs. The decrease in DLE and increase in band to band transition peaks were due to the strong interaction between the NDs and the Zn+; consequently, the Zn+ concentration decreased on the interstitial sites.

  3. Preparation, characterization and optoelectronic properties of nanodiamonds doped zinc oxide nanomaterials by a ball milling technique

    NASA Astrophysics Data System (ADS)

    Ullah, Hameed; Sohail, Muhammad; Malik, Uzma; Ali, Naveed; Bangash, Masroor Ahmad; Nawaz, Mohsan

    2016-07-01

    Zinc oxide (ZnO) is one of the very important metal oxides (MOs) for applications in optoelectronic devices which work in the blue and UV regions. However, to meet the challenges of obtaining ZnO nanomaterials suitable for practical applications, various modifications in physico-chemical properties are highly desirable. One of the ways adopted for altering the properties is to synthesize composite(s) of ZnO with various reinforcements. Here we report on the tuning of optoelectronic properties of ZnO upon doping by nanodiamonds (NDs) using the ball milling technique. A varying weight percent (wt.%) of NDs were ball milled for 2 h with ZnO nanoparticles prepared by a simple precipitation method. The effects of different parameters, the calcination temperature of ZnO, wt.% of NDs and mechanical milling upon the optoelectronic properties of the resulting ZnO–NDs nanocomposites have been investigated. The ZnO–NDs nanocomposites were characterized by IR spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDX). The UV-vis spectroscopy revealed the alteration in the bandgap energy (Eg ) of ZnO as a function of the calcination temperature of ZnO, changing the concentration of NDs, and mechanical milling of the resulting nanocomposites. The photoluminescence (PL) spectroscopy showed a decrease in the deep level emission (DLE) peaks and an increase in near-band-edge transition peaks as a result of the increasing concentration of NDs. The decrease in DLE and increase in band to band transition peaks were due to the strong interaction between the NDs and the Zn+; consequently, the Zn+ concentration decreased on the interstitial sites.

  4. Seebeck and thermal conductivity analysis in amorphous/crystalline {beta}-K{<_2}Bi{<_8}Se{<_13} nanocomposite materials.

    SciTech Connect

    Kyratsi, Th.; Hatzikraniotis, E.; Ioannou, M.; Chung, D. Y.; Tsiaoussis, I.

    2011-01-01

    In this work, ball milling is applied on {beta}-K{sub 2}Bi{sub 8}Se{sub 13} compounds in order to explore the potential of the process for the fabrication of nano-based material. Polycrystalline {beta}-K{sub 2}Bi{sub 8}Se{sub 13}, synthesized from melt, was ball milled under inert atmosphere. Powder x-ray diffraction showed a significantly increased disorder with ball milling time. TEM studies confirmed the presence of nanocrystalline material in an amorphous matrix, suggesting the development of crystalline/amorphous {beta}-K{sub 2}Bi{sub 8}Se{sub 13} nanocomposite material via ball milling process. Seebeck coefficient and thermal conductivity were analyzed based on the effective medium theory and show a significant contribution of a nanocrystalline phase.

  5. Enhanced Piezoelectric Properties and Tunability of Lead-Free Ceramics Prepared by High-Energy Ball Milling

    NASA Astrophysics Data System (ADS)

    Mahesh, M. L. V.; Bhanuprasad, V. V.; James, A. R.

    2013-12-01

    Zirconium-doped barium titanate Ba(Zr0.15Ti0.85)O3 lead-free ceramics (hereinafter referred to as BZT) were synthesized using the solid-state reaction method by adopting the high-energy ball milling technique. Nanosized BZT powders resulted from high-energy ball milling, which in turn enhanced the dielectric and piezoelectric properties of the ceramics. A single-phase perovskite structure free from secondary phase peaks was observed for sintered BZT samples, and a relative density of ˜94% of the theoretical density was achieved. The electric-field-induced polarization-current data indicate the ferroelectric nature of the samples. Unipolar strain as high as 0.12% was realized for the ceramics sintered at 1350°C, indicating their potential for use in actuator applications. Very high tunability of >70% for these ceramics is also reported.

  6. Acid-Assisted Ball Milling of Cellulose as an Efficient Pretreatment Process for the Production of Butyl Glycosides.

    PubMed

    Boissou, Florent; Sayoud, Nassim; De Oliveira Vigier, Karine; Barakat, Abdellatif; Marinkovic, Sinisa; Estrine, Boris; Jérôme, François

    2015-10-12

    Ball milling of cellulose in the presence of a catalytic amount of H2SO4 was found to be a promising pre-treatment process to produce butyl glycosides in high yields. Conversely to the case of water, n-butanol has only a slight effect on the recrystallization of ball-milled cellulose. As a result, thorough depolymerization of cellulose prior the glycosylation step is no longer required, which is a pivotal aspect with respect to energy consumption. This process was successfully transposed to wheat straw from which butyl glycosides and xylosides were produced in good yields. Butyl glycosides and xylosides are important chemicals as they can be used as hydrotropes but also as intermediates in the production of valuable amphiphilic alkyl glycosides.

  7. Acid-Assisted Ball Milling of Cellulose as an Efficient Pretreatment Process for the Production of Butyl Glycosides.

    PubMed

    Boissou, Florent; Sayoud, Nassim; De Oliveira Vigier, Karine; Barakat, Abdellatif; Marinkovic, Sinisa; Estrine, Boris; Jérôme, François

    2015-10-12

    Ball milling of cellulose in the presence of a catalytic amount of H2SO4 was found to be a promising pre-treatment process to produce butyl glycosides in high yields. Conversely to the case of water, n-butanol has only a slight effect on the recrystallization of ball-milled cellulose. As a result, thorough depolymerization of cellulose prior the glycosylation step is no longer required, which is a pivotal aspect with respect to energy consumption. This process was successfully transposed to wheat straw from which butyl glycosides and xylosides were produced in good yields. Butyl glycosides and xylosides are important chemicals as they can be used as hydrotropes but also as intermediates in the production of valuable amphiphilic alkyl glycosides. PMID:26346950

  8. Study on the influence of volume size of the milling jar in purifying Tronoh silica sand using ball milling process

    NASA Astrophysics Data System (ADS)

    Hashim, Nazratulhuda; Mamat, Othman

    2015-07-01

    Tronoh silica sand is the potential source for the SiO2. Purification is an important step in expanding the usage of the Tronoh silica sand. Since the residual impurities are the obstacle in achieving high purity silica, the low speed ball mill will be introduced as a main equipment in purifying Tronoh silica sand. The objective of this study is to understand the influence of volume size of the milling jar in purifying Tronoh silica sand by using ball milling process. The chemical composition of the samples were analyzed by using XRF and SEM. The results showed that the highest purity of the Tronoh silica sand can be achieved by using the 1.0 ℓ milling jar.

  9. ZnO nanoparticles obtained by ball milling technique: Structural, micro-structure, optical and photo-catalytic properties

    NASA Astrophysics Data System (ADS)

    Balamurugan, S.; Joy, Josny; Godwin, M. Anto; Selvamani, S.; Raja, T. S. Gokul

    2016-05-01

    The ZnO nanoparticles were obtained by ball milling of commercial grade ZnO powder at 250 rpm for 20 h and studied their structural, micro-structure, optical and photo-catalytic properties. Due to ball milling significant decrease in lattice parameters and average crystalline size is noticed for the as-milled ZnO nano powder. The HRSEM images of the as-milled powder consist of agglomerated fine spherical nanoparticles in the range of ~10-20 nm. The room temperature PL spectrum of as-milled ZnO nano powder excited under 320 nm reveals two emission bands at ~406 nm (violet emission) and ~639 nm (green emission). Interestingly about 98 % of photo degradation of methylene (MB) by the ZnO catalyst is achieved at 100 minutes of solar light irradiation.

  10. Self-sintering-assisted high intergranular connectivity in ball-milled ex situ MgB2 bulks

    NASA Astrophysics Data System (ADS)

    Mizutani, Shunsuke; Yamamoto, Akiyasu; Shimoyama, Jun-ichi; Ogino, Hiraku; Kishio, Kohji

    2014-11-01

    To understand the mechanisms leading to higher intergranular connectivity in polycrystalline ex situ MgB2 prepared using a pressure-less self-sintering technique, the influence of the initial particle size of the MgB2 powder was investigated. MgB2 bulks sintered at 900 °C for 24 h using ball-milled powders exhibited a network structure with both qualitatively and quantitatively improved intergranular couplings. The connectivity calculated using normal-state transport measurements reached a high value of ˜40%, which is comparable to that of MgB2 bulks fabricated via Mg diffusion or high-pressure-assisted processes. Moreover, the sintering time required to achieve a reasonably high connectivity of 25-30% was less than 1 h. Notably, microstructural analyses confirmed the formation of intergranular necks and grain boundaries during the early stage of sintering. These results suggested self-sintering of the ball-milled MgB2 bulks proceeded much more rapidly than those sintered using an MgB2 powder without ball-milling. Increased intergranular contact points and decreased gap length between grains in green compact are assumed to be the origins for the stimulated self-sintering and corresponding increase in the electrical connectivity.

  11. Crystallization and microstructure of 8YSZ nanopowders synthesized by ball-mill assisted constant pH route

    NASA Astrophysics Data System (ADS)

    Mohanty, Subrat K.; Nayak, Bibhuti B.

    2013-06-01

    8 mol% Y2O3 stabilized ZrO2 (8YSZ) nanopowders were prepared by two ways of precipitation technique namely conventional precipitation (i.e. stepwise increase of pH) and constant pH precipitation (i.e. precipitation at constant pH). The crystallization, microstructure and density of both the powders were studied with and without ball milling. The ball milled powders prepared in conventional method were found to be sintered upto 92% of the theoretical density, whereas the powders prepared in constant pH precipitation method after ball milling showed 97% of the theoretical density, at 1600°C. The presence of fine and uniformly distributed pores were observed, for the 8YSZ pellets synthesized via conventional precipitation method, whereas a relatively dense microstructure was observed for that synthesized via constant pH precipitation method, from the SEM micrographs. Constant pH route shows better results as compared to conventional route and seems to be effective way of synthesis to prepare 8YSZ for electrolyte in solid oxide fuel cell (SOFC) application.

  12. Characterization of cationic starch flocculants synthesized by dry process with ball milling activating method.

    PubMed

    Su, Yuting; Du, Hongying; Huo, Yinqiang; Xu, Yongliang; Wang, Jie; Wang, Liying; Zhao, Siming; Xiong, Shanbai

    2016-06-01

    The cationic starch flocculants were synthesized by the reaction of maize starch which was activated by a ball-milling treatment with 2,3-epoxypropyl trimethyl ammonium chlorides (ETMAC) using the dry method. The cationic starches were characterized by several approaches including scanning electron microscope (SEM), degree of substitution (DS), infrared spectrum (IR), X-ray diffraction (XRD), flocculating activity, electron spin resonance (ESR), and solid-state nuclear magnetic resonance (NMR). The effect of mechanical activation on starch etherifying modification was investigated. The mechanical activation cracked starch granules and destructed their crystal structures. This resulted in enhancements to the reaction activity and reaction efficiency, which was approved by ESR and solid state NMR. The starch flocculants, synthesized by the reaction of mechanically activated starches at 90°C for 2.5h with ETMAC at molar ratio of 0.40:1.00, showed good flocculation activity. The substitution degree (0.300) and reaction efficiency (75.06%) of starch flocculants synthesized with mechanically activated starches were significantly greater than those of starch flocculants with native starches (P<0.05).

  13. Experimental study of residence time distributions of ball-mill circuits grinding coal-water mixtures

    SciTech Connect

    Shoji, K.; Takahashi, Y.; Ohtake, A.; Austin, L.G.

    2008-08-15

    Residence time distributions (RTDs) were estimated by water tracing in a number of wet overflow ball mills (diameters 0.38 to 4.65 m) producing dense, coal-water slurries. In open-circuit mills of 0.38 m diameter and various length-diameter (LID) ratios, the mean residence times of solid were also determined from measured mill holdups. Holdup increased with increased mill feed rate, but the mean residence times of coal and water were still equal to each other. The experimental residence time distributions were fitted to the Mori-Jimbo-Yamazaki semi-infinite, axial mixing model, and the dimensionless mixing coefficient was determined for each of 25 tests in single- and two-compartment mills. This coefficient was found to be independent to the feed rate but linearly proportional to the D/L ratio. The mixing coefficient was smaller for two-compartment mills than for single-compartment mills, showing that there was reduced mixing introduced by the diaphragm separating the compartments. Equations are given to scale residence time distributions for changes in mill diameter and length.

  14. Insertion compounds and composites made by ball milling for advanced sodium-ion batteries.

    PubMed

    Zhang, Biao; Dugas, Romain; Rousse, Gwenaelle; Rozier, Patrick; Abakumov, Artem M; Tarascon, Jean-Marie

    2016-01-18

    Sodium-ion batteries have been considered as potential candidates for stationary energy storage because of the low cost and wide availability of Na sources. However, their future commercialization depends critically on control over the solid electrolyte interface formation, as well as the degree of sodiation at the positive electrode. Here we report an easily scalable ball milling approach, which relies on the use of metallic sodium, to prepare a variety of sodium-based alloys, insertion layered oxides and polyanionic compounds having sodium in excess such as the Na4V2(PO4)2F3 phase. The practical benefits of preparing sodium-enriched positive electrodes as reservoirs to compensate for sodium loss during solid electrolyte interphase formation are demonstrated by assembling full C/P'2-Na1[Fe0.5Mn0.5]O2 and C/'Na3+xV2(PO4)2F3' sodium-ion cells that show substantial increases (>10%) in energy storage density. Our findings may offer electrode design principles for accelerating the development of the sodium-ion technology.

  15. Insertion compounds and composites made by ball milling for advanced sodium-ion batteries

    PubMed Central

    Zhang, Biao; Dugas, Romain; Rousse, Gwenaelle; Rozier, Patrick; Abakumov, Artem M.; Tarascon, Jean-Marie

    2016-01-01

    Sodium-ion batteries have been considered as potential candidates for stationary energy storage because of the low cost and wide availability of Na sources. However, their future commercialization depends critically on control over the solid electrolyte interface formation, as well as the degree of sodiation at the positive electrode. Here we report an easily scalable ball milling approach, which relies on the use of metallic sodium, to prepare a variety of sodium-based alloys, insertion layered oxides and polyanionic compounds having sodium in excess such as the Na4V2(PO4)2F3 phase. The practical benefits of preparing sodium-enriched positive electrodes as reservoirs to compensate for sodium loss during solid electrolyte interphase formation are demonstrated by assembling full C/P′2-Na1[Fe0.5Mn0.5]O2 and C/‘Na3+xV2(PO4)2F3' sodium-ion cells that show substantial increases (>10%) in energy storage density. Our findings may offer electrode design principles for accelerating the development of the sodium-ion technology. PMID:26777573

  16. Iron Nanoparticles Fabricated by High-Energy Ball Milling for Magnetic Hyperthermia

    NASA Astrophysics Data System (ADS)

    Tung, D. K.; Manh, D. H.; Phong, L. T. H.; Nam, P. H.; Nam, D. N. H.; Anh, N. T. N.; Nong, H. T. T.; Phan, M. H.; Phuc, N. X.

    2016-05-01

    Iron nanoparticles (FeNPs) have been successfully prepared by high-energy ball milling in air for various milling times from 1 h to 32 h. Their structure, particle size, elemental composition, magnetic, and inductive heating properties were investigated by means of x-ray diffraction (XRD) analysis, field-emission scanning electron microscopy, energy-dispersive x-ray (EDX) spectroscopy, vibrating-sample magnetometry, and magnetic induction heating, respectively. XRD analysis showed that the average crystallite size decreased to 11 nm after 10 h of milling, then remained almost unchanged for longer milling times. Coexistence of iron (Fe) and iron oxide (FeO) phases was detected after 12 h of milling. EDX analysis also confirmed the occurrence of oxidation, which can be reconciled with the corresponding decrease and increase in saturation magnetization ( M s) with milling time when exposed to oxygen and when annealed under H2 ambient due to oxygen reduction. The time-dependent magnetic and inductive heating responses of the FeNPs were investigated for prospective application in magnetic hyperthermia. The effect of varying the alternating-current (AC) magnetic field strength on the saturation heating temperature and specific loss power of FeNP-containing ferrofluid with concentration of 4 mg/mL was also studied and is discussed.

  17. Analysis of the Magnetocaloric Effect in Powder Samples Obtained by Ball Milling

    NASA Astrophysics Data System (ADS)

    Blázquez, J. S.; Ipus, J. J.; Moreno-Ramírez, L. M.; Borrego, J. M.; Lozano-Pérez, S.; Franco, V.; Conde, C. F.; Conde, A.

    2015-06-01

    Since the discovery of the giant magnetocaloric effect (MCE) close to room temperature in FeRh and particularly in Gd5Si2Ge2 compounds, the study of this phenomenon has experienced an exponential growth. Among the different techniques used to produce magnetocaloric materials, ball milling has been shown as a very versatile one and presents several advantages over other preparation techniques ( e.g., easy scale-up to industrial production). Although a general decrease of the peak value of the magnetic entropy change is observed for milled samples, it can be compensated by the large broadening of the MCE peak, leading to an increase of the refrigeration capacity. In this short review, several aspects inherent to powder samples affecting MCE will be discussed, such as the relevant effect of the demagnetizing field, the possible multiphase character, and the presence of Curie temperature distributions. In mechanically alloyed samples, the two latter factors are typically affected by the degree of integration of the different starting constituents.

  18. Effective high-energy ball milling in air of Fe65Co35 alloys

    NASA Astrophysics Data System (ADS)

    Sirvent, P.; Berganza, E.; Aragón, A. M.; Bollero, A.; Moure, A.; García-Hernández, M.; Marín, P.; Fernández, J. F.; Quesada, A.

    2014-05-01

    Fe65Co35 alloys are technologically relevant, especially in magnetic storage and composite permanent magnets, due to the fact that they present higher saturation magnetization per volume than any other material. Out of the various approaches undertaken for its production, mechanical ball milling remains the most common and efficient method, especially considering the large industrial scale of the applications. With the development of cost-efficient processing in mind, the influence of performing the synthesis of the FeCo alloys in air instead of the standard argon atmosphere is studied. The structural and magnetic characterization, along with the study of the oxygen content of the samples, proves that synthesizing FeCo alloys in air produce materials with nearly identical magnetic performance as their argon-milled counterpart, with the oxidation extent of the materials consisting almost exclusively of the oxide passivating layer located at the surface. In addition, no aging effect was observed in the saturation magnetization up to 6 months. It is concluded that the use of argon atmospheres, desiccators and/or glove boxes may be entirely removed from the process without affecting the magnetic properties.

  19. Curie temperature and magnetic properties of aluminum doped barium ferrite particles prepared by ball mill method

    NASA Astrophysics Data System (ADS)

    Chen, Daming; Harward, Ian; Baptist, Joshua; Goldman, Sara; Celinski, Zbigniew

    2015-12-01

    Barium ferrite has attracted considerable interest in the fields of permanent magnets and perpendicular magnetic recording due to its strong uniaxial anisotropy and high Curie temperature (Tc). We prepared aluminum doped barium ferrite ceramics (BaAlxFe12-xO19, 0≤x≤6) by the ball mill method. The powder was milled for 96 h, and after forming pellets, annealed for 48 h in air at 1000 °C. The X-ray diffraction (XRD) data show that there are only single hexagonal phases in the samples without any impurity phase. The crystal lattice constants, a and c, were calculated by Cohen's method. Both a and c decrease with increasing x, ranging from 0.588 nm and 2.318 nm to 0.573 nm and 2.294 nm, respectively. A Vibrating Sample Magnetometer (VSM) and Superconducting Quantum Interference Device (SQUID) were used to investigate Tc and magnetic properties of BaFe12-xAlxO19. It is found that Tc decreases with increasing x, from 425 °C to 298 °C. It is also found that the saturated magnetization (4πMs) decreases with increasing x, while the coercivity (Hc) increases with the increase in x. The anisotropy field was also determined from the SQUID measurement.

  20. Fluid mechanics of slurry flow through the grinding media in ball mills

    SciTech Connect

    Songfack, P.K.; Rajamani, R.K.

    1995-12-31

    The slurry transport within the ball mill greatly influences the mill holdup, residence time, breakage rate, and hence the power draw and the particle size distribution of the mill product. However, residence-time distribution and holdup in industrial mills could not be predicted a priori. Indeed, it is impossible to determine the slurry loading in continuously operating mills by direct measurement, especially in industrial mills. In this paper, the slurry transport problem is solved using the principles of fluid mechanics. First, the motion of the ball charge and its expansion are predicted by a technique called discrete element method. Then the slurry flow through the porous ball charge is tackled with a fluid-flow technique called the marker and cell method. This may be the only numerical technique capable of tracking the slurry free surface as it fluctuates with the motion of the ball charge. The result is a prediction of the slurry profile in both the radial and axial directions. Hence, it leads to the detailed description of slurry mass and ball charge within the mill. The model predictions are verified with pilot-scale experimental work. This novel approach based on the physics of fluid flow is devoid of any empiricism. It is shown that the holdup of industrial mills at a given feed percent solids can be predicted successfully.

  1. Anisotropic SmCo{sub 5} nanoflakes by surfactant-assisted high energy ball milling

    SciTech Connect

    Cui, B. Z.; Gabay, A. M.; Li, W. F.; Hadjipanayis, G. C.; Marinescu, M.; Liu, J. F.

    2010-05-15

    Crystallographically anisotropic SmCo{sub 5} nanoflakes were fabricated directly by one-step surfactant-assisted high energy ball milling (HEBM) of Sm{sub 17}Co{sub 83} ingot powders for 5 h in heptane and oleic acid (OA) without preprocessing or further annealing. The SmCo{sub 5} nanoflakes have a strong [001] out-of-plane texture. The thickness of nanoflakes is in the range of 8-80 nm while their length is 0.5-8 {mu}m. The surfactant OA plays an important role in the formation of SmCo{sub 5} nanoflakes. HEBM of SmCo{sub 5} ingots in heptane without OA resulted in the formation of magnetically isotropic more or less equiaxed SmCo{sub 5} particles with a size of 2-30 {mu}m. Closely packed 'kebablike' SmCo{sub 5} nanoflakes were formed by HEBM in heptane with 15 wt % OA. HEBM in 150 wt % OA led to well-separated nanoflakes instead of the closely packed kebablike nanostructure. This resulted in the enhanced [001] out-of-plane texture. In-plane transmission electron microscope examination showed that the SmCo{sub 5} nanoflakes were composed of grains with sizes in the range of 4-8 nm. Coercivities of about 18.0 kOe were obtained for the anisotropic SmCo{sub 5} nanoflakes.

  2. Room temperature dual ferroic behaviour of ball mill synthesized NdFeO3 orthoferrite

    NASA Astrophysics Data System (ADS)

    Aparnadevi, N.; Saravana Kumar, K.; Manikandan, M.; Paul Joseph, D.; Venkateswaran, C.

    2016-07-01

    Phase pure NdFeO3 has been achieved using high energy ball milling of oxide precursors with subsequent sintering. It is established that structural arrangement of NdFeO3 regulates the multifunctional feature of the material. Rietveld refinement of the room temperature X-ray diffraction pattern shows that the Fe-O-Fe bond angle significantly favors the super exchange interaction, which is predominantly antiferromagnetic in nature. Magnetization measurement illustrates antiferromagnetic behaviour with a weak ferromagnetic component caused by the canted nature of the Fe3+ spins at room temperature. Absorption bands in the visible ambit, apparent from the UV-Vis diffuse reflectance studies, is found due to the crystal ligand field of octahedral oxygen environment of Fe3+ ions. The direct band gap is estimated to be 2.39 eV from the diffuse reflectance spectrum. The lossy natured ferroelectric loop having a maximum polarization of 0.23 μC/cm2 at room temperature is found to be driven by the non-collinear magnetic structure with reverse Dzyaloshinskii-Moriya effect. Magnetic field has influence on the dielectric constant as evident from the impedance spectroscopy, indicating the strong coupling between ferroelectric and the magnetic structure of NdFeO3.

  3. Synthesis of Highly Active Mg-BASED Hydrides Using Hydriding Combustion Synthesis and NbF5 Additives

    NASA Astrophysics Data System (ADS)

    Chourashiya, M. G.; Park, C. N.; Park, C. J.

    2012-09-01

    Superiority of the hydriding combustion (HC) technique over conventional metallurgical approach to the synthesis of cost-effective Mg based hydrides, which show promise as hydrogen storage materials, is well known. In the present research, we report further improvements in HC prepared Mg-based materials, achieved by optimizing the preparative parameters of HC and by catalytic addition. Mg90-Ni60-C40 composites prepared using optimized processing parameters were ball-milled with NbF5 (10 h) and characterized for their micro-structural and hydriding properties. The ball-milled/catalyzed powder showed decreased crystallinity with CNTs on its surfaces. Surface area of the ball-milled powder decreased to almost half of the as-HC powder, while TG analysis revealed a four-fold decrease in the desorption temperature of the milled powder compared to that of the as-HC prepared powder. Activated samples achieved the maximum absorption/desorption limits (5.3 wt.%) at as low as 100°C, underlining the possibility of the use of these materials in portable hydrogen storage devices.

  4. Ball-milled CuPc/TiO{sub 2} hybrid nanocomposite and its photocatalytic degradation of aqueous Rhodamine B

    SciTech Connect

    Mekprasart, W.; Vittayakorn, N.; Pecharapa, W.

    2012-11-15

    Graphical abstract: This work reports on the synthesis of hybrid composites of titanium dioxide and copper phthalocyanine via ball-milling assisted process in combination with mechanical mixing process. Their structural properties and photocatalytic degradation of aqueous RhB were investigated. The significant enhancement of the photocatalytic performance of the composite may be related to the charge recombination suppression guiding to the increase of free functional radicals participated in degradation process. Highlights: ► CuPc/TiO{sub 2} nanocomposite was synthesized by ball-milling assisted process and mechanical mixing method. ► Ball milling process can reduce CuPc size and assist the formation of well-dispersed composite. ► Loaded CuPc has inconsiderable influence on basic crystal structure of TiO{sub 2} matrix. ► The optical absorption properties of TiO{sub 2} in UV and visible light is improved with the existence of CuPc. ► CuPc/TiO{sub 2} nanocomposite can efficiently heighten the catalytic performance of TiO{sub 2} in the photodegradation of RhB. -- Abstract: Hybrid composites of titanium dioxide and copper phthalocyanine were synthesized by ball-milling assisted process in combination with mechanically stirring method. Structural properties of as-synthesized composites were characterized by X-ray diffraction (XRD), X-ray absorption fine structure (XANES) and scanning electron microscope (SEM). The optical absorbance of as-prepared composites and their photocatalytic activities were investigated by UV–vis spectroscopy. XRD and XANES results confirm that CuPc/TiO{sub 2} nanocomposite is still in the same structure of TiO{sub 2} and CuPc. SEM result reveals that the decreasing particle size of ball-milled CuPc has good dispersion on the surface of TiO{sub 2}. Absorptivity in UV region of the composites is heightened and shifted to visible light due to strong absorbance in blue-green spectrum of CuPc. The photocatalytic degradation of Rhodamine

  5. Amorphous metal-organic frameworks for drug delivery.

    PubMed

    Orellana-Tavra, Claudia; Baxter, Emma F; Tian, Tian; Bennett, Thomas D; Slater, Nigel K H; Cheetham, Anthony K; Fairen-Jimenez, David

    2015-09-21

    We report the encapsulation of the hydrophilic model molecule calcein in the Zr-based MOF UiO-66, followed by amorphization of the framework by ball-milling. We show controlled release of calcein over more than 30 days, compared with the 2 day release period from crystalline UiO-66.

  6. Ball milling effects for induced carriers and reduced grain size on thermoelectric properties in Bi1‑ x Sr x CuSeO (x = 0,0.1)

    NASA Astrophysics Data System (ADS)

    Mizuno, Shu; Ishizawa, Mamoru; Fujishiro, Hiroyuki; Naito, Tomoyuki; Katsui, Hirokazu; Goto, Takashi

    2016-11-01

    We have investigated the ball milling effects for thermoelectric Bi1‑ x Sr x CuSeO (x = 0,0.1) materials. The characteristic rotation speed R for the ball milling exists, at which the crystallite size of the starting powder suddenly decreased. The grain size in the bulks sintered using ball-milled powders also decreased and thermoelectric properties were enhanced mainly by the induced carriers, rather than by the reduction in thermal conductivity. The ball milling effects of carrier doping on thermoelectricity are discussed.

  7. Study of morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled compound

    SciTech Connect

    Bajorek, Anna; Skornia, Paweł; Prusik, Krystian; Wojtyniak, Marcin; Chełkowska, Grażyna

    2015-03-15

    The morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled intermetallic compounds are presented. The polycrystalline HoNi{sub 3} bulk compound crystallizes in the rhombohedral PuNi{sub 3} — type of crystal structure and indicates ferrimagnetic arrangement with the Curie temperature of T{sub C} = 57 ± 2 K, the helimagnetic temperature T{sub h} = 23 ± 2 K with the total saturation magnetic moment of 6.84 μ{sub B}/f.u. at 2 K. The use of the ball-milling method leads to the formation of HoNi{sub 3} nanoflakes with typical thickness of less than 100 nm prone to agglomeration upon milling. The increase of grinding duration leads to the reduction in crystallite size, which was confirmed by various complementary microscopical and diffraction studies. Moreover, the increase in milling duration results in the emergence of the relatively small coercivity (H{sub C}), remanence (M{sub r}) and a variation of the saturation magnetization (M{sub S}). - Graphical abstract: Display Omitted - Highlights: • The ball-milling method exhibits significant potential for producing RT{sub 3} nanopowders. • The AFM method was used for the first time in analysis of R–T nanoflakes morphology. • HoNi{sub 3} compound forms polycrystalline and textured nanoflakes evolving upon milling. • The decrease in crystallite size via grinding is confirmed by XRD, TEM and AFM. • The magnetic parameters were sensitive to the extension of pulverization b.

  8. Bismuth-ceramic nanocomposites through ball milling and liquid crystal synthetic methods

    NASA Astrophysics Data System (ADS)

    Dellinger, Timothy Michael

    Three methods were developed for the synthesis of bismuth-ceramic nanocomposites, which are of interest due to possible use as thermoelectric materials. In the first synthetic method, high energy ball milling of bismuth metal with either MgO or SiO2 was found to produce nanostructured bismuth dispersed on a ceramic material. The morphology of the resulting bismuth depended on its wetting behavior with respect to the ceramic: the metal wet the MgO, but did not wet on the SiO2. Differential Scanning Calorimetry measurements on these composites revealed unusual thermal stability, with nanostructure retained after multiple cycles of heating and cooling through the metal's melting point. The second synthesis methodology was based on the use of lyotropic liquid crystals. These mixtures of water and amphiphilic molecules self-assemble to form periodic structures with nanometer-scale hydrophilic and hydrophobic domains. A novel shear mixing methodology was developed for bringing together reactants which were added to the liquid crystals as dissolved salts. The liquid crystals served to mediate synthesis by acting as nanoreactors to confine chemical reactions within the nanoscale domains of the mesophase, and resulted in the production of nanoparticles. By synthesizing lead sulfide (PbS) and bismuth (Bi) particles as proof-of-concept, it was shown that nanoparticle size could be controlled by controlling the dimensionality of the nanoreactors through control of the liquid crystalline phase. Particle size was shown to decrease upon going from three-dimensionally percolating nanoreactors, to two dimensional sheet-like nanoreactors, to one dimensional rod-like nanoreactors. Additionally, particle size could be controlled by varying the precursor salt concentration. Since the nanoparticles did not agglomerate in the liquid crystal immediately after synthesis, bismuth-ceramic nanocomposites could be prepared by synthesizing Bi nanoparticles and mixing in SiO2 particles which

  9. Facile and Cost-Effective Synthesis and Deposition of a YBCO Superconductor on Copper Substrates by High-Energy Ball Milling

    NASA Astrophysics Data System (ADS)

    Alami, Abdul Hai; Assad, Mhd Adel; Aokal, Camilia

    2016-09-01

    The article investigates the synthesis and deposition of YBCO on a copper substrate for various functional purposes. The superconductor is first prepared by mechanically alloying elemental components (yttrium, barium, and copper) for 50 hours in a high-energy ball mill with subsequent protocol of heat treatment in an oxygen-rich atmosphere to arrive at stoichiometric ratios of YBa2Cu3O7. The material is then deposited on a thin copper substrate also by ball milling under various parameters of rotational speed and deposition time to select the best and most homogenous substrate coverage. Atomic force microscopy has confirmed the desired results, and other microstructural, thermal, and electrical techniques are used to characterize the obtained material. High-energy ball milling proved to be a versatile means to synthesize and deposit the material in a straightforward manner and controllable parameters for different deposit thicknesses and coverages.

  10. Preparation of Si nano-crystals with controlled oxidation state from SiO disproportionated by ZrO2 ball-milling

    NASA Astrophysics Data System (ADS)

    Okamoto, Yuji; Harada, Yoshitomo; Ohta, Narumi; Takada, Kazunori; Sumiya, Masatomo

    2016-09-01

    We demonstrate that a SiO disproportionation reaction can be achieved simply by high energy mechanochemical milling. The planetary ball-milling of ZrO2 for a few minutes generated Si nano-crystals. Milling conditions including rotation speed, ball number, milling time, and type of ball material were able to control the oxidation states of Si. The ball-milled SiO powder was tested as an anode of a lithium battery. ZrO2 contamination from the vial and balls was eliminated by dipping the ball-milled SiO powder in (NH4)HSO4 molten salt and heating for 5 min. The disproportionated SiO powder showed characteristics comparable to those of a powder prepared by a conventional heating process taking several hours.

  11. Selective ensemble modeling load parameters of ball mill based on multi-scale frequency spectral features and sphere criterion

    NASA Astrophysics Data System (ADS)

    Tang, Jian; Yu, Wen; Chai, Tianyou; Liu, Zhuo; Zhou, Xiaojie

    2016-01-01

    It is difficult to model multi-frequency signal, such as mechanical vibration and acoustic signals of wet ball mill in the mineral grinding process. In this paper, these signals are decomposed into multi-scale intrinsic mode functions (IMFs) by the empirical mode decomposition (EMD) technique. A new adaptive multi-scale spectral features selection approach based on sphere criterion (SC) is applied to these IMFs frequency spectra. The candidate sub-models are constructed by the partial least squares (PLS) with the selected features. Finally, the branch and bound based selective ensemble (BBSEN) algorithm is applied to select and combine these ensemble sub-models. This method can be easily extended to regression and classification problems with multi-time scale signal. We successfully apply this approach to a laboratory-scale ball mill. The shell vibration and acoustic signals are used to model mill load parameters. The experimental results demonstrate that this novel approach is more effective than the other modeling methods based on multi-scale frequency spectral features.

  12. Effect of high-energy ball milling time on structural and magnetic properties of nanocrystalline cobalt ferrite powders

    NASA Astrophysics Data System (ADS)

    Cedeño-Mattei, Yarilyn; Perales-Pérez, Oscar; Uwakweh, Oswald N. C.

    2013-09-01

    Cobalt ferrite nanocrystals synthesized by conventional and size-controlled coprecipitation methods were treated by high-energy ball milling, HEBM, in order to study the effect of crystal size reduction and/or strain on the resulting magnetic properties. Processed nanocrystals were characterized by X-ray diffraction, Brunauer, Emmett, and Teller surface area analysis, transmission electron microscopy (TEM), and vibrating sample magnetometry. The cobalt ferrite nanocrystals exhibited crystal size reduction from initial values (average crystallite sizes of 12±1 nm and 18±3 nm, respectively) down to 10 nm after HEBM for 10 h. The specific surface area was decreased by milling (from 96.5 to 59.4 m2/g; for the 12 nm cobalt ferrite nanocrystals), due to particles aggregation. TEM analyses corroborated the aggregation of the nanoparticles at such long milling times. The same cobalt ferrite nanocrystals exhibited a rise in coercivity from 394 to 560 Oe after 5 h ball milling which was attributed to the introduction of strain anisotropy, namely point defects, as suggested by the systematic shift of the diffraction peaks towards higher angles. In turn, the magnetic characterization of the starting 18 nm-nanocrystals reported a drop in coercivity from 4506 Oe to 491 Oe that was attributed predominantly to size reduction within the single domain region. A correlation between particle size, cationic distribution, and HEBM processing conditions became evident.

  13. Preparation of natural pyrite nanoparticles by high energy planetary ball milling as a nanocatalyst for heterogeneous Fenton process

    NASA Astrophysics Data System (ADS)

    Fathinia, Siavash; Fathinia, Mehrangiz; Rahmani, Ali Akbar; Khataee, Alireza

    2015-02-01

    In the present study pyrite nanoparticles were prepared by high energy mechanical ball milling utilizing a planetary ball mill. Various pyrite samples were produced by changing the milling time from 2 h to 6 h, in the constant milling speed of 320 rpm. X-ray diffraction (XRD), scanning electron microscopy (SEM) linked with energy dispersive X-ray (EDX), Fourier transform infrared spectroscopy (FT-IR) analysis and Brunauer-Emmett-Teller (BET) were performed to explain the characteristics of primary (unmilled) and milled pyrite samples. The average particle size distribution of the produced pyrite during 6 h milling was found to be between 20 nm and 100 nm. The catalytic performance of the different pyrite samples was examined in the heterogeneous Fenton process for degradation of C.I. Acid Orange 7 (AO7) solution. Results showed that the decolorization efficiency of AO7 in the presence of 6 h-milled pyrite sample was the highest. The impact of key parameters on the degradation efficiency of AO7 by pyrite nanoparticles catalyzed Fenton process was modeled using central composite design (CCD). Accordingly, the maximum removal efficiency of 96.30% was achieved at initial AO7 concentration of 16 mg/L, H2O2 concentration of 5 mmol/L, catalyst amount of 0.5 g/L and reaction time of 25 min.

  14. Highly Al-doped TiO{sub 2} nanoparticles produced by Ball Mill Method: structural and electronic characterization

    SciTech Connect

    Santos, Desireé M. de los Navas, Javier Sánchez-Coronilla, Antonio; Alcántara, Rodrigo; Fernández-Lorenzo, Concha; Martín-Calleja, Joaquín

    2015-10-15

    Highlights: • Highly Al-doped TiO{sub 2} nanoparticles were synthesized using a Ball Mill Method. • Al doping delayed anatase to rutile phase transformation. • Al doping allow controlling the structural and electronic properties of nanoparticles. - Abstract: This study presents an easy method for synthesizing highly doped TiO{sub 2} nanoparticles. The Ball Mill method was used to synthesize pure and Al-doped titanium dioxide, with an atomic percentage up to 15.7 at.% Al/(Al + Ti). The samples were annealed at 773 K, 973 K and 1173 K, and characterized using ICP-AES, XRD, Raman spectroscopy, FT-IR, TG, STEM, XPS, and UV–vis spectroscopy. The effect of doping and the calcination temperature on the structure and properties of the nanoparticles were studied. The results show high levels of internal doping due to the substitution of Ti{sup 4+} ions by Al{sup 3+} in the TiO{sub 2} lattice. Furthermore, anatase to rutile transformation occurs at higher temperatures when the percentage of doping increases. Therefore, Al doping allows us to control the structural and electronic properties of the nanoparticle synthesized. So, it is possible to obtain nanoparticles with anatase as predominant phase in a higher range of temperature.

  15. Effects of process control agent on the synthesis of AIN-carbon nanotube by ball-milling.

    PubMed

    Nam, Hye Rim; Kim, Young Jin; Ahn, Jung-Ho

    2013-09-01

    Aluminum and its alloy are of importance due to high specific strength. In particular, aluminum matrix composites have good corrosion resistance and mechanical property at high temperatures. However, enhanced mechanical strength and wear resistance via proper heat treatments are strongly required for many structural applications. For this purpose, we synthesized carbon nanotube (CNT)-reinforced aluminum matrix composites by employing a new method. We employed controlled ball-milling and sintering: the use of some specific process control agents (PCAs) for ball-milling and sintering in a specific atmosphere. The use of our PCAs was beneficial both for homogeneous mixing and for the formation of hard dispersoids. Hardened layers was formed at the surface of the present aluminum-CNT composites as a result of reaction of aluminum with PCAs and nitrogen in the processing atmosphere. The resulting materials after sintering showed interesting mechanical properties, combined with surface hardening. The hardening mainly stems from the formation of Al-N-O phase at the surface of specimens. PMID:24205586

  16. Impact of high energy ball milling on the nanostructure of magnetite–graphite and magnetite–graphite–molybdenum disulphide blends

    SciTech Connect

    Österle, W.; Orts-Gil, G.; Gross, T.; Deutsch, C.; Hinrichs, R.; Vasconcellos, M.A.Z.; Zoz, H.; Yigit, D.; Sun, X.

    2013-12-15

    Different, partly complementary and partly redundant characterization methods were applied to study the transition of magnetite, graphite and MoS{sub 2} powders to mechanically alloyed nanostructures. The applied methods were: Transmission electron microscopy (TEM), Mössbauer spectroscopy (MS), Raman spectroscopy (RS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The main objective was to prepare a model material providing the essential features of a typical tribofilm forming during automotive braking, and to assess the impact of different constituents on sliding behaviour and friction level. Irrespective of the initial grain size, the raw materials were transferred to a nanocrystalline structure and mixed on a nanoscopic scale during high energy ball milling. Whereas magnetite remained almost unchanged, graphite and molybdenum disulphide were transformed to a nanocrystalline and highly disordered structure. The observed increase of the coefficient of friction was attributed to a loss of lubricity of the latter ingredient due to this transformation and subsequent oxidation. - Highlights: • Characterization of microstructural changes induced by high energy ball milling • Assessment of the potential of different characterization methods • Impact of mechanical alloying on tribological performance revealed by tests • Preparation of an artificial third body resembling the one formed during braking.

  17. Synthesis of Nano-Size AlN Powders by Carbothermal Reduction from Plasma-Assisted Ball Milling Precursor

    NASA Astrophysics Data System (ADS)

    Liu, Zhijie; Wang, Wenchun; Yang, Dezheng; Wang, Sen; Dai, Leyang

    2016-07-01

    Nano-size aluminum nitride (AlN) powders have been successfully synthesized with a high efficiency method through annealing from milling assisted by discharge plasma (p-milling) alumina (Al2O3) precursors. The characterization of the p-milling Al2O3 powders and the synthesized AlN are investigated. Compared to conventional ball milling (c-milling), it can be found that the precursors by p-milling have a finer grain size with a higher specific surface area, which lead to a faster reaction efficiency and higher conversion to AlN at lower temperatures. The activation energy of p-milling Al2O3 is found to be 371.5 kJ/mol, a value that is much less than the reported value of the unmilled and the conventional milled Al2O3. Meanwhile, the synthesized AlN powders have unique features, such as an irregular lamp-like morphology with uniform particle distribution and fine average particle size. The results are attributed to the unique synergistic effect of p-milling, which is the effect of deformation, fracture, and cold welding of Al2O3 powders resulting from ball milling, that will be enhanced due to the introduction of discharge plasma. supported by National Natural Science Foundation of China (No. 51177008)

  18. Discrete element method based scale-up model for material synthesis using ball milling

    NASA Astrophysics Data System (ADS)

    Santhanam, Priya Radhi

    Mechanical milling is a widely used technique for powder processing in various areas. In this work, a scale-up model for describing this ball milling process is developed. The thesis is a combination of experimental and modeling efforts. Initially, Discrete Element Model (DEM) is used to describe energy transfer from milling tools to the milled powder for shaker, planetary, and attritor mills. The rolling and static friction coefficients are determined experimentally. Computations predict a quasisteady rate of energy dissipation, E d, for each experimental configuration. It is proposed that the milling dose defined as a product of Ed and milling time, t, divided by the mass of milled powder, mp characterizes the milling progress independently of the milling device or milling conditions used. Once the milling dose is determined for one experimental configuration, it can be used to predict the milling time required to prepare the same material in any milling configuration, for which Ed is calculated. The concept is validated experimentally for DEM describing planetary and shaker mills. For attritor, the predicted Ed includes substantial contribution from milling tool interaction events with abnormally high forces (>103 N). The energy in such events is likely dissipated to heat or plastically deform milling tools rather than refine material. Indeed, DEM predictions for the attritor correlate with experiments when such events are ignored in the analysis. With an objective of obtaining real-time indicators of milling progress, power, torque, and rotation speed of the impeller of an attritor mill are measured during preparation of metal matrix composite powders in the subsequent portion of this thesis. Two material systems are selected and comparisons made between in-situ parameters and experimental milling progress indicators. It is established that real-time measurements can certainly be used to describe milling progress. However, they need to be interpreted carefully

  19. GEL-STATE NMR OF BALL-MILLED WHOLE CELL WALLS IN DMSO-d6 USING 2D SOLUTION-STATE NMR SPECTROSCOPY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Plant cell walls were used for obtaining 2D solution-state NMR spectra without actual solubilization or structural modification. Ball-milled whole cell walls were swelled directly in the NMR tube with DMSO-d6 where they formed a gel. There are relatively few gel-state NMR studies. Most have involved...

  20. Manganese(III) Acetate-Promoted Cross-Coupling Reaction of Benzothiazole/Thiazole Derivatives with Organophosphorus Compounds under Ball-Milling Conditions.

    PubMed

    Li, Liang; Wang, Jun-Jie; Wang, Guan-Wu

    2016-07-01

    The first solvent-free manganese(III) acetate-promoted reaction of benzothiazole/thiazole derivatives with organophosphorus compounds including phosphine oxides, phosphinate ester, and phosphonate diester has been efficiently developed under ball-milling conditions, providing a highly efficient and green protocol to structurally diverse C2-phosphonylated benzothiazole/thiazole derivatives with remarkable functional group tolerance and excellent yields. PMID:27248000

  1. Stainless-Steel Ball-Milling Method for Hydro-/Deutero-genation using H2O/D2O as a Hydrogen/Deuterium Source.

    PubMed

    Sawama, Yoshinari; Kawajiri, Takahiro; Niikawa, Miki; Goto, Ryota; Yabe, Yuki; Takahashi, Tohru; Marumoto, Takahisa; Itoh, Miki; Kimura, Yuuichi; Monguchi, Yasunari; Kondo, Shin-ichi; Sajiki, Hironao

    2015-11-01

    A one-pot continuous-flow method for hydrogen (deuterium) generation and subsequent hydrogenation (deuterogenation) was developed using a stainless-steel (SUS304)-mediated ball-milling approach. SUS304, especially zero-valent Cr and Ni as constituents of the SUS304, and mechanochemical processing played crucial roles in the development of the reactions. PMID:26493945

  2. Properties of dispersion-strengthened chromium - 4-volume-percent-thoria alloys produced by ball milling in hydrogen iodide

    NASA Technical Reports Server (NTRS)

    Arias, A.

    1974-01-01

    The effects of processing variables on the tensile properties and ductile-to-brittle transition temperature (DBTT) of Cr + 4 vol. %ThO2 alloys and of pure Cr produced by ball milling in hydrogen iodide were investigated. Hot rolled Cr + ThO2 was stronger than either hot pressed Cr + ThO2 or pure Cr at temperatures up to 1537 C. Hot pressed Cr + ThO2 had a DBTT of 501 C as compared with minus 8 to 24 C for the hot rolled Cr + ThO2 and with 139 C for pure Cr. It is postulated that the dispersoid in the hot rolled alloys lowers the DBTT by inhibiting recovery and recrystallization of the strained structure.

  3. Two step meso-acidophilic bioleaching of chalcopyrite containing ball mill spillage and removal of the surface passivation layer.

    PubMed

    Panda, S; Parhi, P K; Nayak, B D; Pradhan, N; Mohapatra, U B; Sukla, L B

    2013-02-01

    Meso-acidophilic bacterial leaching of ball mill spillage (containing chalcopyrite >80%) was carried out in an innovative two-step bioleaching method. The major drawback of meso-acidophilic bioleaching limiting industrial application is the passivation phenomenon over the ore surfaces in iron-sulfur rich environments. In the present study, we present a novel wash solution that efficiently removed the passivation layer. FTIR characterization of the bioleached sample indicated that the residues could be further leached to recover extra copper after wash solution application. XRD study indicated accumulation of sulfates (SO(4)(-)) of Na, K, Fe and oxy hydroxides of iron [FeO(OH)] in the form of jarosite outlining the passivation layer. SEM, FESEM-EDS studies indicated severe corrosion effects of the wash solution on the passivation layer. Two step bioleaching of the ore sample yielded 32.6% copper in 68days in the first interlude and post wash solution application yielded 10.8% additional copper.

  4. The structure and magnetic properties of Sm-Fe-N powders prepared by ball milling at low temperature

    NASA Astrophysics Data System (ADS)

    Fang, Qiuli; An, Xiaoxin; Wang, Fang; Li, Ying; Du, Juan; Xia, Weixing; Yan, Aru; Liu, J. Ping; Zhang, Jian

    2016-07-01

    Sm-Fe-N powders have great potential to be used for preparing high-performance bonded permanent magnets because of their high anisotropy field and large saturation magnetization. In this work, we report the morphology, structure, oxygen content and magnetic properties of the Sm-Fe-N powders prepared by high energy ball milling at low temperature. Compared with the samples milled at room temperature, the Sm-Fe-N powders prepared at low temperature display more homogeneous morphology, less decomposition, lower oxygen content, and therefore enhanced magnetic performance. Our experimental results indicate that the low temperature milling will be a promising method for fabricating Sm-Fe-N bonded magnets with high-performance.

  5. Remarkable performance improvement of inexpensive ball-milled Si nanoparticles by carbon-coating for Li-ion batteries

    NASA Astrophysics Data System (ADS)

    Kasukabe, Takatoshi; Nishihara, Hirotomo; Iwamura, Shinichiroh; Kyotani, Takashi

    2016-07-01

    Si nanoparticles prepared by ball-milling (BM-Si) are expected as practical negative-electrode materials for lithium-ion batteries, but their performance is much lower than those of more expensive Si nanomaterials, such as chemical-vapor-deposition derived Si nanoparticles (CVD-Si) having a tight network structure. It is found that carbon-coating of aggregations of BM-Si forms a quasi-network structure, thereby making the performance comparable to that of CVD-Si under capacity restriction (to 1500 mAh g-1). In this case, the structural transition of BM-Si during charge/discharge cycling is characterized by the formation of a specific 'wrinkled structure', which is very similar to that formed in CVD-Si.

  6. Electric modulus formalism and electrical transport property of ball mill synthesized nanocrystalline Mn doped ZrO2 solid solution

    NASA Astrophysics Data System (ADS)

    Saha, S.; Nandy, A.; Meikap, A. K.; Pradhan, S. K.

    2015-12-01

    Here we report the formation of Mn doped nanocrystalline ZrO2 solid solution synthesized by high energy ball-milling method and the transport mechanism in the temperature range 298 K

  7. Superthermostability of nanoscale TIC-reinforced copper alloys manufactured by a two-step ball-milling process

    NASA Astrophysics Data System (ADS)

    Wang, Fenglin; Li, Yunping; Xu, Xiandong; Koizumi, Yuichiro; Yamanaka, Kenta; Bian, Huakang; Chiba, Akihiko

    2015-12-01

    A Cu-TiC alloy, with nanoscale TiC particles highly dispersed in the submicron-grained Cu matrix, was manufactured by a self-developed two-step ball-milling process on Cu, Ti and C powders. The thermostability of the composite was evaluated by high-temperature isothermal annealing treatments, with temperatures ranging from 727 to 1273 K. The semicoherent nanoscale TiC particles with Cu matrix, mainly located along the grain boundaries, were found to exhibit the promising trait of blocking grain boundary migrations, which leads to a super-stabilized microstructures up to approximately the melting point of copper (1223 K). Furthermore, the Cu-TiC alloys after annealing at 1323 K showed a slight decrease in Vickers hardness as well as the duplex microstructure due to selective grain growth, which were discussed in terms of hardness contributions from various mechanisms.

  8. Significantly improved dehydrogenation of ball-milled MgH2 doped with CoFe2O4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Shan, Jiawei; Li, Ping; Wan, Qi; Zhai, Fuqiang; Zhang, Jun; Li, Ziliang; Liu, Zhaojiang; Volinsky, Alex A.; Qu, Xuanhui

    2014-12-01

    CoFe2O4 nanoparticles are added to magnesium hydride (MgH2) by high-energy ball milling in order to improve its hydriding properties. The hydrogen storage properties and catalytic mechanism are investigated by pressure-composition-temperature (PCT), differential thermal analysis (DTA), X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The nonisothermal desorption results show that the onset desorption temperature of the MgH2 + 7 mol% CoFe2O4 is 160 °C, which is 200 °C lower than of the as-received MgH2. The dehydrogenation process of the MgH2 doped with the CoFe2O4 nanoparticles includes two steps. DTA curves and XRD patterns reveal that a chemical reaction happens between MgH2 and CoFe2O4, forming the final products of the ternary combination, corresponding to Co3Fe7, MgO and Co. The onset desorption temperature of the ball-milled MgH2 doped with Co3Fe7, MgO and Co is about 260 °C, approximately 100 °C lower than the un-doped MgH2, demonstrating that the ternary combination (Co3Fe7, MgO, and Co) also has a great catalytic effect on the MgH2 hydrogen storage properties. It is also confirmed that the various methods of adding the ternary combination have different effects on the MgH2 hydriding-dehydriding process.

  9. Sulfur-graphene nanostructured cathodes via ball-milling for high-performance lithium-sulfur batteries.

    PubMed

    Xu, Jiantie; Shui, Jianglan; Wang, Jianli; Wang, Min; Liu, Hua-Kun; Dou, Shi Xue; Jeon, In-Yup; Seo, Jeong-Min; Baek, Jong-Beom; Dai, Liming

    2014-10-28

    Although much progress has been made to develop high-performance lithium-sulfur batteries (LSBs), the reported physical or chemical routes to sulfur cathode materials are often multistep/complex and even involve environmentally hazardous reagents, and hence are infeasible for mass production. Here, we report a simple ball-milling technique to combine both the physical and chemical routes into a one-step process for low-cost, scalable, and eco-friendly production of graphene nanoplatelets (GnPs) edge-functionalized with sulfur (S-GnPs) as highly efficient LSB cathode materials of practical significance. LSBs based on the S-GnP cathode materials, produced by ball-milling 70 wt % sulfur and 30 wt % graphite, delivered a high initial reversible capacity of 1265.3 mAh g(-1) at 0.1 C in the voltage range of 1.5-3.0 V with an excellent rate capability, followed by a high reversible capacity of 966.1 mAh g(-1) at 2 C with a low capacity decay rate of 0.099% per cycle over 500 cycles, outperformed the current state-of-the-art cathode materials for LSBs. The observed excellent electrochemical performance can be attributed to a 3D "sandwich-like" structure of S-GnPs with an enhanced ionic conductivity and lithium insertion/extraction capacity during the discharge-charge process. Furthermore, a low-cost porous carbon paper pyrolyzed from common filter paper was inserted between the 0.7S-0.3GnP electrode and porous polypropylene film separator to reduce/eliminate the dissolution of physically adsorbed polysulfide into the electrolyte and subsequent cross-deposition on the anode, leading to further improved capacity and cycling stability.

  10. Scale-up of organic reactions in ball mills: process intensification with regard to energy efficiency and economy of scale.

    PubMed

    Stolle, Achim; Schmidt, Robert; Jacob, Katharina

    2014-01-01

    The scale-up of the Knoevenagel-condensation between vanillin and barbituric acid carried out in planetary ball mills is investigated from an engineering perspective. Generally, the reaction proceeded in the solid state without intermediate melting and afforded selectively only one product. The reaction has been used as a model to analyze the influence and relationship of different parameters related to operation in planetary ball mills. From the viewpoint of technological parameters the milling ball diameter, dMB, the filling degree with respect to the milling balls' packing, ΦMB,packing, and the filling degree of the substrates with respect to the void volume of the milling balls' packing, ΦGS, have been investigated at different reaction scales. It was found that milling balls with small dMB lead to higher yields within shorter reaction time, treaction, or lower rotation frequency, rpm. Thus, the lower limit is set considering the technology which is available for the separation of the milling balls from the product after the reaction. Regarding ΦMB,packing, results indicate that the optimal value is roughly 50% of the total milling beakers' volume, VB,total, independent of the reaction scale or reaction conditions. Thus, 30% of VB,total are taken by the milling balls. Increase of the initial batch sizes changes ΦGS significantly. However, within the investigated parameter range no negative influence on the yield was observed. Up to 50% of VB,total can be taken over by the substrates in addition to 30% for the total milling ball volume. Scale-up factors of 15 and 11 were realized considering the amount of substrates and the reactor volume, respectively. Beside technological parameters, variables which influence the process itself, treaction and rpm, were investigated also. Variation of those allowed to fine-tune the reaction conditions in order to maximize the yield and minimize the energy intensity.

  11. Dielectric and photocatalytic properties of sulfur doped TiO{sub 2} nanoparticles prepared by ball milling

    SciTech Connect

    Jalalah, Mohammed; Faisal, M.; Bouzid, Houcine; Ismail, Adel A.; Al-Sayari, Saleh A.

    2013-09-01

    Graphical abstract: - Highlights: • Designing of visible light responsive photocatalyst utilizing ball milling. • Sulphur used as dopant in commercial TiO{sub 2} P25 at different atomic percentage. • S doping resulted in an intense increase in absorption in the visible light region. • Newly design photocatalyst exhibited excellent photocatalytic performance. • 0.11 at.% S-doped TiO{sub 2} shows 3-times higher activity than that of TiO{sub 2} P25. - Abstract: Sulfur (S) doped commercial TiO{sub 2} P-25 has been achieved by changing the amount of thiourea using ball milling technique. The results of XRD clearly reveal biphasial anatase and rutile mixtures for all prepared samples and doping of S does not change the morphology of the TiO{sub 2}. The optical absorption edge of S-doped TiO{sub 2} was red shifted with indirect bandgap energy of 2.8 eV. The dielectric studies confirm that the dielectric constant of TiO{sub 2} increases after doping, however it becomes more conductive. Newly designed S-doped TiO{sub 2} photocatalysts exhibited excellent photocatalytic performance for the degradation of methylene blue (MB) under visible light. The overall photocatalytic activity of 0.11 at.% S-doped TiO{sub 2} was significantly 3-times higher than that of commercial TiO{sub 2} P-25 and complete degradation of MB has taken place after 90 min of irradiation under visible light while only 35% dye degraded when the reaction has been carried out in the presence of undoped TiO{sub 2}.

  12. Preparation of ultrafine magnetic biochar and activated carbon for pharmaceutical adsorption and subsequent degradation by ball milling.

    PubMed

    Shan, Danna; Deng, Shubo; Zhao, Tianning; Wang, Bin; Wang, Yujue; Huang, Jun; Yu, Gang; Winglee, Judy; Wiesner, Mark R

    2016-03-15

    Ball milling was used to prepare two ultrafine magnetic biochar/Fe3O4 and activated carbon (AC)/Fe3O4 hybrid materials targeted for use in pharmaceutical removal by adsorption and mechanochemical degradation of pharmaceutical compounds. Both hybrid adsorbents prepared after 2h milling exhibited high removal of carbamazepine (CBZ), and were easily separated magnetically. These adsorbents exhibited fast adsorption of CBZ and tetracycline (TC) in the initial 1h. The biochar/Fe3O4 had a maximum adsorption capacity of 62.7mg/g for CBZ and 94.2mg/g for TC, while values obtained for AC/Fe3O4 were 135.1mg/g for CBZ and 45.3mg/g for TC respectively when data were fitted using the Langmuir expression. Solution pH values slightly affected the sorption of TC on the adsorbents, while CBZ sorption was almost pH-independent. The spent adsorbents with adsorbed CBZ and TC were milled to degrade the adsorbed pollutants. The adsorbed TC itself was over 97% degraded after 3h of milling, while about half of adsorbed CBZ were remained. The addition of quartz sand was found to improve the mechanochemical degradation of CBZ on biochar/Fe3O4, and its degradation percent was up to 98.4% at the dose of 0.3g quarts sand/g adsorbent. This research provided an easy method to prepare ultrafine magnetic adsorbents for the effective removal of typical pharmaceuticals from water or wastewater and degrade them using ball milling.

  13. Sulfur-graphene nanostructured cathodes via ball-milling for high-performance lithium-sulfur batteries.

    PubMed

    Xu, Jiantie; Shui, Jianglan; Wang, Jianli; Wang, Min; Liu, Hua-Kun; Dou, Shi Xue; Jeon, In-Yup; Seo, Jeong-Min; Baek, Jong-Beom; Dai, Liming

    2014-10-28

    Although much progress has been made to develop high-performance lithium-sulfur batteries (LSBs), the reported physical or chemical routes to sulfur cathode materials are often multistep/complex and even involve environmentally hazardous reagents, and hence are infeasible for mass production. Here, we report a simple ball-milling technique to combine both the physical and chemical routes into a one-step process for low-cost, scalable, and eco-friendly production of graphene nanoplatelets (GnPs) edge-functionalized with sulfur (S-GnPs) as highly efficient LSB cathode materials of practical significance. LSBs based on the S-GnP cathode materials, produced by ball-milling 70 wt % sulfur and 30 wt % graphite, delivered a high initial reversible capacity of 1265.3 mAh g(-1) at 0.1 C in the voltage range of 1.5-3.0 V with an excellent rate capability, followed by a high reversible capacity of 966.1 mAh g(-1) at 2 C with a low capacity decay rate of 0.099% per cycle over 500 cycles, outperformed the current state-of-the-art cathode materials for LSBs. The observed excellent electrochemical performance can be attributed to a 3D "sandwich-like" structure of S-GnPs with an enhanced ionic conductivity and lithium insertion/extraction capacity during the discharge-charge process. Furthermore, a low-cost porous carbon paper pyrolyzed from common filter paper was inserted between the 0.7S-0.3GnP electrode and porous polypropylene film separator to reduce/eliminate the dissolution of physically adsorbed polysulfide into the electrolyte and subsequent cross-deposition on the anode, leading to further improved capacity and cycling stability. PMID:25290080

  14. HPMC as a potential enhancer of nimodipine biopharmaceutical properties via ball-milled solid dispersions.

    PubMed

    Riekes, Manoela Klüppel; Kuminek, Gislaine; Rauber, Gabriela Schneider; de Campos, Carlos Eduardo Maduro; Bortoluzzi, Adailton João; Stulzer, Hellen Karine

    2014-01-01

    The poor solubility of drugs remains one of the most challenging aspects of formulation development. Aiming at improving the biopharmaceutical limitations of the calcium channel blocker nimodipine, the development of solid dispersions is proposed herein. Three different proportions of nimodipine:HPMC were tested and all of them generated amorphous solid dispersions. Improvements of up 318% in the solubility and a 4-fold increase in the dissolution rate of nimodipine were achieved. Stability studies conducted over 90 days in a desiccator indicated that the initial characteristic of the formulations were maintained. However, at 40 °C/75% RH recrystallization was observed for solid dispersions with 70 and 80% of HPMC, whilst the formulation composed of 90% of the carrier remained amorphous. The increase in the stability observed when the HPMC concentration was increased from 70 to 90% in the solid dispersions was attributed to the dilution mechanism. PMID:24274533

  15. HPMC as a potential enhancer of nimodipine biopharmaceutical properties via ball-milled solid dispersions.

    PubMed

    Riekes, Manoela Klüppel; Kuminek, Gislaine; Rauber, Gabriela Schneider; de Campos, Carlos Eduardo Maduro; Bortoluzzi, Adailton João; Stulzer, Hellen Karine

    2014-01-01

    The poor solubility of drugs remains one of the most challenging aspects of formulation development. Aiming at improving the biopharmaceutical limitations of the calcium channel blocker nimodipine, the development of solid dispersions is proposed herein. Three different proportions of nimodipine:HPMC were tested and all of them generated amorphous solid dispersions. Improvements of up 318% in the solubility and a 4-fold increase in the dissolution rate of nimodipine were achieved. Stability studies conducted over 90 days in a desiccator indicated that the initial characteristic of the formulations were maintained. However, at 40 °C/75% RH recrystallization was observed for solid dispersions with 70 and 80% of HPMC, whilst the formulation composed of 90% of the carrier remained amorphous. The increase in the stability observed when the HPMC concentration was increased from 70 to 90% in the solid dispersions was attributed to the dilution mechanism.

  16. Phase development during high-energy ball-milling of zinc oxide and iron - the impact of grain size on the source and the degree of contamination.

    PubMed

    Štefanić, G; Krehula, S; Štefanić, I

    2015-11-21

    High-energy ball-milling of powder mixtures of zincite (ZnO) and iron (α-Fe) at different weight ratios was performed in air using a planetary ball mill with a stainless steel milling assembly. Structural and microstructural changes during the ball-milling (up to 30 h) were monitored using X-ray powder diffraction, field emission scanning electron microscopy (FE-SEM) and UV-Vis diffuse reflectance spectroscopy. The mechanism of iron oxidation was determined from the results of Mössbauer spectroscopy. It was found that an early phase of ball-milling caused the oxidation of iron from Fe(0) to Fe(2+) followed by the formation of a solid solution structurally similar to wüstite. The wüstite-type phase rapidly disappeared upon prolonged milling, which was accompanied by further oxidation of iron from Fe(2+) to Fe(3+) and the formation of spinel-type ferrite structurally similar to franklinite (ZnFe2O4) in the products with a high zinc content, or magnetite (Fe3O4) in the products with a high iron content. Further milling or annealing had a low impact on the franklinite-type phase, but caused the transition of the magnetite-type phase to the phase structurally similar to hematite (α-Fe2O3). The results of energy dispersive X-ray spectrometry (EDS) showed a dramatic increase in the degree of contamination with the increase in the proportion of the starting iron (∼9 times higher contamination during the milling of pure iron compared with pure zincite). It was shown that the source of contamination (balls or vial) strongly depends on the type of milled sample. Ball-milling of relatively big and heavy grains (starting iron) caused preferential contamination from the vial whereas ball-milling of smaller and lighter grains (products obtained after prolonged milling) caused preferential contamination from the balls. After prolonged milling the contamination due to wear of the balls was dominant in all the products. An explanation for the observed impact of grain size on

  17. Phase development during high-energy ball-milling of zinc oxide and iron - the impact of grain size on the source and the degree of contamination.

    PubMed

    Štefanić, G; Krehula, S; Štefanić, I

    2015-11-21

    High-energy ball-milling of powder mixtures of zincite (ZnO) and iron (α-Fe) at different weight ratios was performed in air using a planetary ball mill with a stainless steel milling assembly. Structural and microstructural changes during the ball-milling (up to 30 h) were monitored using X-ray powder diffraction, field emission scanning electron microscopy (FE-SEM) and UV-Vis diffuse reflectance spectroscopy. The mechanism of iron oxidation was determined from the results of Mössbauer spectroscopy. It was found that an early phase of ball-milling caused the oxidation of iron from Fe(0) to Fe(2+) followed by the formation of a solid solution structurally similar to wüstite. The wüstite-type phase rapidly disappeared upon prolonged milling, which was accompanied by further oxidation of iron from Fe(2+) to Fe(3+) and the formation of spinel-type ferrite structurally similar to franklinite (ZnFe2O4) in the products with a high zinc content, or magnetite (Fe3O4) in the products with a high iron content. Further milling or annealing had a low impact on the franklinite-type phase, but caused the transition of the magnetite-type phase to the phase structurally similar to hematite (α-Fe2O3). The results of energy dispersive X-ray spectrometry (EDS) showed a dramatic increase in the degree of contamination with the increase in the proportion of the starting iron (∼9 times higher contamination during the milling of pure iron compared with pure zincite). It was shown that the source of contamination (balls or vial) strongly depends on the type of milled sample. Ball-milling of relatively big and heavy grains (starting iron) caused preferential contamination from the vial whereas ball-milling of smaller and lighter grains (products obtained after prolonged milling) caused preferential contamination from the balls. After prolonged milling the contamination due to wear of the balls was dominant in all the products. An explanation for the observed impact of grain size on

  18. Solvent-free cross-dehydrogenative coupling reactions under high speed ball-milling conditions applied to the synthesis of functionalized tetrahydroisoquinolines.

    PubMed

    Su, Weike; Yu, Jingbo; Li, Zhenhua; Jiang, Zhijiang

    2011-11-01

    Solvent-free reaction using a high-speed ball milling technique has been first applied to cross-dehydrogenative coupling (CDC) reactions between tetrahydroisoquinolines and three types of pronucleophiles such as nitroalkanes, alkynes, and indoles. All coupling products were obtained in good yields at short reaction times (no more than 40 min). When alkynes and indoles were used as pronucleophile, the reactions can be catalyzed efficiently by recoverable copper balls without any additional metal catalyst. PMID:21961457

  19. Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching.

    PubMed

    Swain, Basudev; Mishra, Chinmayee; Kang, Leeseung; Park, Kyung-Soo; Lee, Chan Gi; Hong, Hyun Seon

    2015-04-01

    Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium, two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na2CO3, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na2CO3, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4M HCl, 100°C and pulp density of 20g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching.

  20. Preparation and characterization of nanocrystalline ZrO2-7%Y2O3 powders for thermal barrier coatings by high-energy ball milling

    NASA Astrophysics Data System (ADS)

    Bobzin, Kirsten; Zhao, Lidong; Schlaefer, Thomas; Warda, Thomas

    2011-06-01

    High-energy ball milling is an effective method to produce nanocrystalline oxides. In this study, a conventional ZrO2-7%Y2O3 spray powder was ball-milled to produce nanocrystalline powders with high levels of crystalline disorders for deposition of thermal barrier coatings. The powder was milled both with 100Cr6 steel balls and with ZrO2-3%Y2O3 ceramic balls as grinding media. The milling time was varied in order to investigate the effect of the milling time on the crystallite size. The powders were investigated in terms of their crystallite sizes and morphologies by X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results show that under given milling conditions the powder was already nanostructured after 40 min milling. The crystallite size decreased significantly with increasing milling time within first 120 min. After that, a further increase of milling time did not lead to a significant reduction of the crystallite size. Ball-milling led to lattice microstrains. Milling with the steel balls resulted in finer nano-sized crystal grains, but caused the contamination of the powder. The nano-sized crystal grains coarsened during the heat-treatment at 1250°C.

  1. Magnetically enhanced hard-soft SmCo5-FeNi composites obtained via high energy ball milling and heat treatment

    NASA Astrophysics Data System (ADS)

    Rai, B. K.; Mishra, S. R.

    2013-10-01

    The effect of high energy ball milling on the structure and magnetic properties of SmCo5-x%FeNi (x: 5,15), magnetically hard-soft phase composites, has been investigated as a function of composition ratio, ball milling time, and annealing temperature using x-ray diffraction and room temperature magnetometry. The milling resulted in decomposition of SmCo5 and FeNi phases. Heat treatment of ball-milled composites resulted in a secondary soft magnetic phase FeCo. High remanence and coercivity values are obtained at a low annealing temperature of ˜650 °C and short annealing time (20 min). Magnetic measurements of annealed composite sample, SmCo5-5%FeNi, show enhancement in magnetization (178%), remanence (127%), and coercivity (67%) as compared to that of pure SmCo5. The enhancement in coercivity and remanence is attributed to the effective exchange coupling between hard SmCo5 and soft FeCo/FeNi phases. Overall better magnetic properties were presented by composites with low FeNi content. The facile synthesis process represents a general process toward SmCo5 based exchange-spring nanocomposites for high performance bulk permanent magnet.

  2. Synthesis of Nd2Fe14C compound by high-energy ball-milling Nd-Fe alloy in heptane and annealing under vacuum

    NASA Astrophysics Data System (ADS)

    Geng, H. M.; Ji, Y.; Feng, X. Y.; Zhang, J. J.; Ran, Z.; Yan, Y.; Wang, W. Q.; Su, F.; Du, X. B.

    2016-06-01

    A simple synthesis route for the Nd2Fe14C compound with good permanent magnetic properties is presented. Being high-energy ball-milled in heptane (C7H16) for 8 h, the NdFe3.5 alloy consisting of Nd2Fe17 and Nd phases disproportionates into NdH2+δ and α-Fe. Subsequently, NdH2+δ decomposes when annealed from room temperature to 900 °C under vacuum, and H2 is released. Meanwhile Nd2Fe14C, NdC and little α-Fe phases are formed in the final product. H and C atoms come from the decomposition of heptane. Coercivity of 1.39 T and maximum magnetic energy product of 62.7 kJ m-3 have been achieved. Too short a ball-milling time results in the insufficient disproportionation of NdFe3.5 alloy and the residue of Nd2Fe17 phase in the final product. Too long a ball-milling time results in the appearance of NdC2 and more α-Fe phases besides Nd2Fe14C and NdC phases. Hexane (C6H14), octane (C8H18) and nonane (C9H20) have been proved to have a similar effect to heptane.

  3. Solid-state synthesis of Mg{sub 2}Si via short-duration ball-milling and low-temperature annealing

    SciTech Connect

    Ioannou, M.; Chrissafis, K.; Pavlidou, E.; Gascoin, F.; Kyratsi, Th.

    2013-01-15

    In this work, a short duration ball-milling of elemental Mg and Si followed by a thermal treatment is suggested in order to synthesize magnesium silicide via solid-state reaction. The formation of magnesium silicide was studied in terms of its structure and thermal characteristics by powder X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy and differential scanning calorimetry. Pure Mg{sub 2}Si was formed after short milling and heating at temperatures as low as 280 Degree-Sign C. Differential scanning calorimetry analysis was performed to study the kinetics of the reaction. The activation energy of the reaction was calculated using the Ozawa-Flynn-Wall and Friedman methods. The thermoelectric properties suggested semiconducting behavior whereas thermal conductivity values of highly dense hot-pressed pellets are consistent with the literature. - Graphical abstract: Thermographs of ball-milled Mg and Si powders (1 and 2) show exothermic areas suggesting Mg{sub 2}Si formation at low temperatures. Unmilled Mg and Si mixture (3) forms Mg{sub 2}Si at higher temperatures. Highlights: Black-Right-Pointing-Pointer Ball-milling process is crucial for the formation of pure Mg{sub 2}Si at low temperatures. Black-Right-Pointing-Pointer Synthesis profiles based on different temperature settings and duration are suggested. Black-Right-Pointing-Pointer Thermal analysis confirms the shift of the Mg{sub 2}Si formation at low temperatures.

  4. Quantification of residual crystallinity in ball milled commercially sourced lactose monohydrate by thermo-analytical techniques and terahertz spectroscopy.

    PubMed

    Smith, Geoff; Hussain, Amjad; Bukhari, Nadeem Irfan; Ermolina, Irina

    2015-05-01

    The quantification of crystallinity is necessary in order to be able to control the milling process. The use of thermal analysis for this assessment presents certain challenges, particularly in the case of crystal hydrates. In this study, the residual crystallinity on ball milling of lactose monohydrate (LMH), for periods up to 90min, was evaluated by thermo-analytical techniques (TGA, DSC) and terahertz spectroscopy (THz). In general, the results from one of the DSC analysis and the THz measurements agree showing a monotonous decrease in relative residual crystallinity with milling time (∼80% reduction after 60min milling) and a slight increase at the 90min time point. However, the estimates from TGA and two other methods of analyzing DSC curve do not agree with the former techniques and show variability with significantly higher estimates for crystallinity. It was concluded that, the thermal techniques require more complex treatment of the data in the evaluation of changes in crystallinity of a milled material (in particular to account for the de-vitrification and mutarotation of the material that inevitably occurs during the measurement cycle) while the analysis of THz data is more straightforward, with the measurement having no impact on the native state of the material. PMID:25784570

  5. Removal of fluoride from drinking water using modified ultrafine tea powder processed using a ball-mill

    NASA Astrophysics Data System (ADS)

    Cai, Huimei; Xu, Lingyun; Chen, Guijie; Peng, Chuanyi; Ke, Fei; Liu, Zhengquan; Li, Daxiang; Zhang, Zhengzhu; Wan, Xiaochun

    2016-07-01

    A low-cost and highly efficient biosorbent was prepared by loading zirconium(IV) onto ball-milled, ultrafine tea powder (UTP-Zr) for removal of fluoride from drinking water. To evaluate the fluoride adsorption capacity of UTP-Zr over a wide range of conditions, the biosorbent dosage, contact time, initial pH, initial fluoride concentration and presence of other ions were varied. UTP-Zr performed well over the considerably wide pH range of 3-10. The residual concentration of Zr in the treated water was below the limit of detection (0.01 mg/L). Fluoride adsorption by the UTP-Zr biosorbent followed the Langmuir model, with a maximum adsorption capacity of 12.43 mgF/g at room temperature. The fluoride adsorption kinetics fit the pseudo-second-order kinetic model. The synthesized biosorbent was characterized by BET, SEM, EDS, XRD and XPS to reveal how UTP-Zr interacts with fluoride. Results from this study demonstrated that UTP-based biosorbents will be useful and safe for the removal of fluoride from drinking water.

  6. A comparison between different X-ray diffraction line broadening analysis methods for nanocrystalline ball-milled FCC powders

    NASA Astrophysics Data System (ADS)

    Soleimanian, V.; Mojtahedi, M.

    2015-06-01

    The microstructural characteristics of aluminum, copper and nickel powders are investigated using different X-ray diffraction line broadening analysis approaches. Prior to analysis, the powders were ball-milled to produce a nanocrystalline structure with high density of probable types of lattice defects. A variety of methods, including Scherrer, Williamson-Smallman, Williamson-Hall, Warren-Averbach, modified Williamson-Hall, modified Warren-Averbach, Rietveld refinement and whole powder pattern modeling (WPPM) approaches are applied. In this way, microstructural characteristics such as crystallite size, microstrain, dislocation density, effective outer cut-off radius of dislocations and the probability of twining and stacking faults are calculated. On the other hand, the results of conventional and advanced line broadening analysis methods are compared. It is revealed that the density of linear and planar defects in the mechanically deformed aluminum powder is significantly smaller than that of copper and nickel, as well as the level of anisotropic strain broadening. Moreover, the WPPM procedure provided a better profile fitting with more accurate results.

  7. Synthesis, characterization and performance of high energy ball milled meso-scale zero valent iron in Fenton reaction.

    PubMed

    Ambika, Selvaraj; Devasena, M; Nambi, Indumathi Manivannan

    2016-10-01

    Understanding contaminant degradation by different sized zero valent iron (ZVI) particles is one important aspect in addressing the long-term stability of these particles in field studies. In this study, meso zero valent iron (mZVI) particles were synthesised in a milling time of 10 h using ball milling technique. The efficacy of mZVI particles for removal of phenol was quantitatively evaluated in comparison with coarse zero valent iron (cZVI) and nano zero valent iron (nZVI) particles. Phenol degradation experiments were carried out in sacrificial batch mode at room temperature independently with cZVI, nZVI and mZVI under varied pH conditions of 3, 4, 6, 7, 8 and 10. Batch experiments substantiating the reactivity of mZVI under unbuffered pH system were also carried out and compared with buffered and poorly buffered pH systems. mZVI particles showed consistent phenol degradation at circum-neutral pH with efficiency of 44%, 67%, and 89% in a span of 5, 10 and 20 min respectively. The dissolved iron species and residual iron formation were also measured as a function of pH. Unbuffered systems at circum-neutral pH produced less residual iron when compared to buffered and poorly buffered systems. At this pH, oxidation of Fe(2+) produced a different oxidant Ferryl ion, which was found to effectively participate in phenol degradation. PMID:27397842

  8. A novel combined pretreatment of ball milling and microwave irradiation for enhancing enzymatic hydrolysis of microcrystalline cellulose.

    PubMed

    Peng, Huadong; Li, Hongqiang; Luo, Hao; Xu, Jian

    2013-02-01

    Microcrystalline cellulose (MCC) was performed as a mode substrate to investigate its potential ability of bioconversion in a novel combined pretreatment of ball milling (BM) and/or microwave irradiation (MWI). The variation of structure characteristics of MCC before/after pretreatment were investigated, including crystallinity index (CrI), size of crystal (S(C)), specific surface area (SSA) and degree of polymerization (DP). Their correlation with the rate of enzymatic hydrolysis was differentiated by an optimized equation which indicated the rate of hydrolysis was much more sensitive to CrI than SSA and DP. To achieve the same or higher glucose yield of BM for 3h and 6h, BM for 1h with MWI for 20min could save 54.8% and 77.40% energy consumption, respectively. Moreover, chemicals were not required in this process. It is concluded that the combination of BM and short time MWI is an environment-friendly, economical and effective approach to treat biomass. PMID:23306114

  9. Textured PrCo{sub 5} nanoflakes with large coercivity prepared by low power surfactant-assisted ball milling

    SciTech Connect

    Zuo, Wen-Liang Liu, Rong-Ming; Zheng, Xin-Qi; Wu, Rong-Rong; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

    2014-05-07

    The effect of the milling time on the structure, morphology, coercivity, and remanence ratio of textured PrCo{sub 5} nanoflakes produced by low power surfactant-assisted ball milling (SABM) was investigated. The X-ray powder diffraction (XRD) patterns indicate that the SABM PrCo{sub 5} samples are all CaCu{sub 5}-type hexagonal structure. The average grain size is smaller than 10 nm when the SABM time is equal to or longer than 5.5 h. The thickness of nanoflakes is mainly in the range of 50−100 nm while the length is 0.5−5 μm when the SABM time reaches 8 h. For the field-aligned PrCo{sub 5} nanoflakes, the out-of-plane texture is indicated from the increasing (0 0 l) peaks in the XRD patterns, and the easy magnetization direction is perpendicular to the flake surface. The strong texture of PrCo{sub 5} nanoflakes leads to a large coercivity H{sub c} (7.8 kOe) and obvious anisotropic magnetic behaviors for the aligned samples.

  10. Effects of high-energy ball-milling on injectability and strength of β-tricalcium-phosphate cement.

    PubMed

    Bae, Jiyoung; Ida, Yumika; Sekine, Kazumitsu; Kawano, Fumiaki; Hamada, Kenichi

    2015-07-01

    Calcium phosphate cement (CPC) offers many advantages as a bone-substitution material. The objective of this study is to develop a new CPC that simultaneously exhibits fine injectability, a short setting time, and high strength. β-tricalcium phosphate (β-TCP, control) powder was ball-milled for 24h to produce a new cement powder. The modified β-TCP after 24h milling (mβ-TCP-24h) exhibited excellent injectability even 1h after mixing. The mechanical properties of the set cement (compact) were evaluated using compressive strength (CS) and diametral tensile strength (DTS) testing. The CS and DTS values of the mβ-TCP-24h compacts were 8.02MPa and 2.62MPa, respectively, at 5h after mixing, and were 49.6MPa and 7.9MPa, respectively, at 2 weeks after mixing. All the CS and DTS values of the mβ-TCP-24h compacts were significantly higher than those of the control for the same duration after mixing. These results suggest that the mechano-chemically modified β-TCP powder dissolves rapidly and accelerates hydroxyapatite precipitation, which successfully shortens the cement setting time and enhances the strength. This study supports that mβ-TCP-24h is a promising candidate for use in injectable CPCs with improved strength. PMID:25855467

  11. Preparation of CNT/AlSi10Mg composite powders by high-energy ball milling and their physical properties

    NASA Astrophysics Data System (ADS)

    Wang, Lin-zhi; Liu, Ying; Wei, Wen-hou; An, Xu-guang; Zhang, Tao; Pu, Ya-yun

    2016-03-01

    This study investigated the effects of carbon nanotube (CNT) concentration on the micro-morphologies and laser absorption properties of CNT/AlSi10Mg composite powders produced by high-energy ball milling. A scanning electron microscope, X-ray diffractometer, laser particle size analyzer, high-temperature synchronous thermal analyzer, and UV/VIS/NIR spectrophotometer were used for the analysis of micrographs, phases, granulometric parameters, thermal properties, and laser absorption properties of the composite powders, respectively. The results showed that the powders gradually changed from flake- to granule-like morphology and the average particle size sharply decreased with increases in milling rotational speed and milling time. Moreover, a uniform dispersion of CNTs in AlSi10Mg powders was achieved only for a CNT content of 1.5wt%. Laser absorption values of the composite powders were also observed to gradually increase with the increase of CNT concentration, and different spectra displayed characteristic absorption peaks at a wavelength of approximately 826 nm.

  12. DEM modeling of ball mills with experimental validation: influence of contact parameters on charge motion and power draw

    NASA Astrophysics Data System (ADS)

    Boemer, Dominik; Ponthot, Jean-Philippe

    2016-07-01

    Discrete element method simulations of a 1:5-scale laboratory ball mill are presented in this paper to study the influence of the contact parameters on the charge motion and the power draw. The position density limit is introduced as an efficient mathematical tool to describe and to compare the macroscopic charge motion in different scenarios, i.a. with different values of the contact parameters. While the charge motion and the power draw are relatively insensitive to the stiffness and the damping coefficient of the linear spring-slider-damper contact law, the coefficient of friction has a strong influence since it controls the sliding propensity of the charge. Based on the experimental calibration and validation by charge motion photographs and power draw measurements, the descriptive and predictive capabilities of the position density limit and the discrete element method are demonstrated, i.e. the real position of the charge is precisely delimited by the respective position density limit and the power draw can be predicted with an accuracy of about 5 %.

  13. Quenching ilmenite with a high-temperature and high-pressure phase using super-high-energy ball milling.

    PubMed

    Hashishin, Takeshi; Tan, Zhenquan; Yamamoto, Kazuhiro; Qiu, Nan; Kim, Jungeum; Numako, Chiya; Naka, Takashi; Valmalette, Jean Christophe; Ohara, Satoshi

    2014-04-25

    The mass production of highly dense oxides with high-temperature and high-pressure phases allows us to discover functional properties that have never been developed. To date, the quenching of highly dense materials at the gramme-level at ambient atmosphere has never been achieved. Here, we provide evidence of the formation of orthorhombic Fe2TiO4 from trigonal FeTiO3 as a result of the high-temperature (>1250 K) and high-pressure (>23 GPa) condition induced by the high collision energy of 150 gravity generated between steel balls. Ilmenite was steeply quenched by the surrounding atmosphere, when iron-rich ilmenite (Fe2TiO4) with a high-temperature and high-pressure phase was formed by planetary collisions and was released from the collision points between the balls. Our finding allows us to infer that such intense planetary collisions induced by high-energy ball milling contribute to the mass production of a high-temperature and high-pressure phase.

  14. Quenching ilmenite with a high-temperature and high-pressure phase using super-high-energy ball milling

    NASA Astrophysics Data System (ADS)

    Hashishin, Takeshi; Tan, Zhenquan; Yamamoto, Kazuhiro; Qiu, Nan; Kim, Jungeum; Numako, Chiya; Naka, Takashi; Valmalette, Jean Christophe; Ohara, Satoshi

    2014-04-01

    The mass production of highly dense oxides with high-temperature and high-pressure phases allows us to discover functional properties that have never been developed. To date, the quenching of highly dense materials at the gramme-level at ambient atmosphere has never been achieved. Here, we provide evidence of the formation of orthorhombic Fe2TiO4 from trigonal FeTiO3 as a result of the high-temperature (>1250 K) and high-pressure (>23 GPa) condition induced by the high collision energy of 150 gravity generated between steel balls. Ilmenite was steeply quenched by the surrounding atmosphere, when iron-rich ilmenite (Fe2TiO4) with a high-temperature and high-pressure phase was formed by planetary collisions and was released from the collision points between the balls. Our finding allows us to infer that such intense planetary collisions induced by high-energy ball milling contribute to the mass production of a high-temperature and high-pressure phase.

  15. Grinding Wear Behaviour of Stepped Austempered Ductile Iron as Media Material During Comminution of Iron Ore in Ball Mills

    NASA Astrophysics Data System (ADS)

    Raghavendra, H.; Bhat, K. L.; Udupa, K. Rajendra; Hegde, M. M. Rajath

    2011-01-01

    An attempt has been made to evaluate the suitability of austempered ductile iron (ADI) as media material for grinding iron ore in a ball mill. Spheroidal graphite (S.G) iron balls are austenitised at 900° C for 60 minutes and given stepped austempering treatment at 280° C for 30 minutes and 60 minutes followed by 380° C for 60 minutes in each case. These materials are characterised by measuring hardness, analysing X-ray diffraction (X-RD), studying microstructure using optical and scanning electron microscope (SEM). Grinding wear behaviour of these materials was assessed for wear loss in wet condition at different pH value of the mineral slurry and found that the wear rate of grinding media material decreases with increase in pH of the slurry. The wear resistance of ADI balls were compared with forged En31 steel balls and found that the stepped austempered ductile iron is superior to forged En31 steel balls.

  16. Grinding Wear Behaviour of Stepped Austempered Ductile Iron as Media Material During Comminution of Iron Ore in Ball Mills

    SciTech Connect

    Raghavendra, H.; Bhat, K. L.; Udupa, K. Rajendra; Hegde, M. M. Rajath

    2011-01-17

    An attempt has been made to evaluate the suitability of austempered ductile iron (ADI) as media material for grinding iron ore in a ball mill. Spheroidal graphite (S.G) iron balls are austenitised at 900 deg. C for 60 minutes and given stepped austempering treatment at 280 deg. C for 30 minutes and 60 minutes followed by 380 deg. C for 60 minutes in each case. These materials are characterised by measuring hardness, analysing X-ray diffraction (X-RD), studying microstructure using optical and scanning electron microscope (SEM). Grinding wear behaviour of these materials was assessed for wear loss in wet condition at different pH value of the mineral slurry and found that the wear rate of grinding media material decreases with increase in pH of the slurry. The wear resistance of ADI balls were compared with forged En31 steel balls and found that the stepped austempered ductile iron is superior to forged En31 steel balls.

  17. The phase analysis of spark plasma sintered MgB2 after ball milling.

    PubMed

    Kang, Deuk-Kyun; Kim, Dong-Woong; Kim, Cheol-Jin; Ahn, In-Shup

    2010-01-01

    Mg and amorphous B powders below 10 and 3 micro meter were used as raw materials, and mixed by planetary-mill for 9 hours at argon atmosphere. MgB2 bulk was fabricated at the various temperatures by Spark Plasma Sintering. In the sintering process, mixed powders were sintered in graphite mold, at the pressure of 55 Mpa. The fabricated MgB2 samples were evaluated with XRD, EDS, FE-SEM, PPMS. MgB2, MgO and Fe phases were observed from XRD result. In the results, MgO and Fe were impurity which may affect superconducting properties of MgB2 samples, and it's distribution could be confirmed from EDS mapping result. In order to confirm the formation of MgB2 phase, DTA was used as heating rate of 10 degrees C/min at Ar atmosphere from room temperature to 1200 degrees C. In the PPMS result, the Tc (critical temperature) was about 21 K, and the density of spark plasma sintered samples increased to 1.87 g/cm3 by increasing sintering temperature.

  18. Mechanical ball-milling preparation of fullerene/cobalt core/shell nanocomposites with high electrochemical hydrogen storage ability.

    PubMed

    Bao, Di; Gao, Peng; Shen, Xiande; Chang, Cheng; Wang, Longqiang; Wang, Ying; Chen, Yujin; Zhou, Xiaoming; Sun, Shuchao; Li, Guobao; Yang, Piaoping

    2014-02-26

    The design and synthesis of new hydrogen storage nanomaterials with high capacity at low cost is extremely desirable but remains challenging for today's development of hydrogen economy. Because of the special honeycomb structures and excellent physical and chemical characters, fullerenes have been extensively considered as ideal materials for hydrogen storage materials. To take the most advantage of its distinctive symmetrical carbon cage structure, we have uniformly coated C60's surface with metal cobalt in nanoscale to form a core/shell structure through a simple ball-milling process in this work. The X-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectra, high-solution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectrometry (EDX) elemental mappings, and X-ray photoelectron spectroscopy (XPS) measurements have been conducted to evaluate the size and the composition of the composites. In addition, the blue shift of C60 pentagonal pinch mode demonstrates the formation of Co-C chemical bond, and which enhances the stability of the as-obtained nanocomposites. And their electrochemical experimental results demonstrate that the as-obtained C60/Co composites have excellent electrochemical hydrogen storage cycle reversibility and considerably high hydrogen storage capacities of 907 mAh/g (3.32 wt % hydrogen) under room temperature and ambient pressure, which is very close to the theoretical hydrogen storage capacities of individual metal Co (3.33 wt % hydrogen). Furthermore, their hydrogen storage processes and the mechanism have also been investigated, in which the quasi-reversible C60/Co↔C60/Co-Hx reaction is the dominant cycle process.

  19. Physical and electrochemical properties of LiFePO 4 nanoparticles synthesized by a combination of spray pyrolysis with wet ball-milling

    NASA Astrophysics Data System (ADS)

    Konarova, Muxina; Taniguchi, Izumi

    A novel preparation technique was developed to synthesize LiFePO 4 nanoparticles through a combination of spray pyrolysis (SP) with wet ball-milling (WBM). Using this technique, the preparation of LiFePO 4 nanoparticles was investigated for a wide range of process parameters such as ball-milling time and sintering temperature. The effect of process parameters on the physical and electrochemical properties of LiFePO 4 was then discussed through analysis using by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), the Brunauer-Emmet-Teller (BET) method, Raman spectroscopy and using an electrochemical cell of Li|1 M LiClO 4 in EC:DEC = 1:1|LiFePO 4. LiFePO 4 nanoparticles with a geometric mean diameter of 58 nm were prepared at a rotating speed of 800 rpm and a ball-milling time of 12 h in an Ar atmosphere followed by heat treatment at 500 °C for 4 h in a N 2 + 3% H 2 atmosphere. The sample delivered first discharge capacities of 164 and 100 mAh g -1 at charge-discharge rates of 0.1 and 10 C in the test cells, respectively. The electrochemical properties of LiFePO 4 nanoparticles were strongly affected by the formation of Fe 2P, Fe 3P and α-Fe 2O 3 at higher charge-discharge rates.

  20. Facile synthesis and regeneration of Mg(BH4)2 by high energy reactive ball milling of MgB2.

    PubMed

    Gupta, Shalabh; Hlova, Ihor Z; Kobayashi, Takeshi; Denys, Roman V; Chen, Fu; Zavaliy, Ihor Y; Pruski, Marek; Pecharsky, Vitalij K

    2013-01-28

    We report direct hydrogenation of MgB(2) in a planetary ball mill. Magnesium borohydride, Mg(BH(4))(2), and various polyhedral borane anion salts have been synthesized at pressures between 50 and 350 bar H(2) without the need for subsequent isothermal hydrogenation at elevated temperature and pressure. The obtained products release ∼4 wt% H(2) below 390 °C, and a major portion of Mg(BH(4))(2) transforms back to MgB(2) at around 300 °C, demonstrating the possibility of reversible hydrogen storage in an Mg(BH(4))(2)-MgB(2) system.

  1. Mechanical and Microstructure Study of Nickel-Based ODS Alloys Processed by Mechano-Chemical Bonding and Ball Milling

    NASA Astrophysics Data System (ADS)

    Amare, Belachew N.

    Due to the need to increase the efficiency of modern power plants, land-based gas turbines are designed to operate at high temperature creating harsh environments for structural materials. The elevated turbine inlet temperature directly affects the materials at the hottest sections, which includes combustion chamber, blades, and vanes. Therefore, the hottest sections should satisfy a number of material requirements such as high creep strength, ductility at low temperature, high temperature oxidation and corrosion resistance. Such requirements are nowadays satisfied by implementing superalloys coated by high temperature thermal barrier coating (TBC) systems to protect from high operating temperature required to obtain an increased efficiency. Oxide dispersive strengthened (ODS) alloys are being considered due to their high temperature creep strength, good oxidation and corrosion resistance for high temperature applications in advanced power plants. These alloys operating at high temperature are subjected to different loading systems such as thermal, mechanical, and thermo-mechanical combined loads at operation. Thus, it is critical to study the high temperature mechanical and microstructure properties of such alloys for their structural integrity. The primary objective of this research work is to investigate the mechanical and microstructure properties of nickel-based ODS alloys produced by combined mechano-chemical bonding (MCB) and ball milling subjected to high temperature oxidation, which are expected to be applied for high temperature turbine coating with micro-channel cooling system. Stiffness response and microstructure evaluation of such alloy systems was studied along with their oxidation mechanism and structural integrity through thermal cyclic exposure. Another objective is to analyze the heat transfer of ODS alloy coatings with micro-channel cooling system using finite element analysis (FEA) to determine their feasibility as a stand-alone structural

  2. Size effect on the melting temperature depression of Al12Mg17 complex metallic alloy nanoparticles prepared by planetary ball milling

    NASA Astrophysics Data System (ADS)

    Zolriasatein, Ashkan; Shokuhfar, Ali

    2015-11-01

    This research investigates the synthesis and size-dependent melting point depression of complex metallic alloy (CMA) nanoparticles. Al12Mg17 which belongs to this new category of intermetallic materials was initially produced as pre-alloyed ingot, then homogenized to achieve single phase compound and crushed into small size powder and finally, mechanically milled in a planetary ball mill to synthesize nanoparticles. Phase and microstructural characterizations of the as-crushed and milled powders were performed using X-ray diffractometry (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). Effects of the mechanical milling on thermal behavior of the Al12Mg17 nanoparticles in comparison with as-cast Al12Mg17 ingot has been investigated by differential scanning calorimetry (DSC) measurement. It was found that an average particle size of 24 nm with crystallite size of 16 nm was achieved after 20 h of ball milling process. The size- dependent melting point depression of the Al12Mg17 nanoparticles has been experimentally observed and also comparison of the obtained results with theoretical models was carried out.

  3. Structural; magnetic and catalytic properties of nanocrystalline Cu0.5Zn0.5Fe2O4 synthesized by microwave combustion and ball milling methods

    NASA Astrophysics Data System (ADS)

    Mahmoud, M. H.; Hassan, Azza M.; Said, Abd El-Aziz A.; Hamdeh, H. H.

    2016-06-01

    Effects of high energy ball-milling on nanosized Cu0.5Zn0.5Fe2O4 powders were studied at 30 and 330 min of milling. The powders were initially synthesized from its stoichiometric metal nitrates and urea mixtures, using a microwave assisted combustion method. Ball-milling induced electromechanical reaction was examined by XRD, TEM, Mössbauer spectroscopy, magnetization, and catalytic performance by exploring potential changes in size, phases and chemical structure. Before Milling, the as-prepared powders were comprised of small grains of poor spinel crystallinity and very small crystallite size, and a minor α-Fe2O3 phase. Progressive milling significantly reduced the grain size, increased chemical disorder, and reduced the hematite phase. These changes are also manifested in the magnetization measurements. The Catalytic activity performance was carried out using dehydrogenation of isopropyl alcohol. The observed activity was correlated to the presence of Cu2+ and Fe3+ catalysts at octahedral sites before and after milling.

  4. Detailed Investigation of Ion Exchange in Ball Milled LiH+MgB2 System using Ultra-High Field NMR Spectroscopy

    SciTech Connect

    Hu, Jian Z.; Kwak, Ja Hun; Yang, Zhenguo; Wan, Xiufeng; Shaw, Leonard D.

    2010-06-01

    The present study with the detailed 1H-6Li cross polarization NMR analysis confirms the formation of a ternary compound, (Mg1-xLi2x)B2, during ball milling of LiH + ½ MgB2 at room temperature. The 6Li sites in (Mg1-xLi2x)B2 exhibit spinning sidebands (SSBs), whereas the 6Li sites in LiH do not. The SSBs and the very short spin-lattice relaxation time manifested by the 6Li sites in (Mg1-xLi2x)B2 indicate that the Li ions in (Mg1-xLi2x)B2 are located between the layered boron structures and close to Mg ions. The formation of (Mg1-xLi2x)B2 explains the previous observation that the LiH + ½ MgB2 mixture ball milled effectively has a greatly enhanced hydriding kinetics at temperatures below the melting point of LiBH4.

  5. Synthesis of boron suboxide (B{sub 6}O) with ball milled boron oxide (B{sub 2}O{sub 3}) under lower pressure and temperature

    SciTech Connect

    Jiao Xiaopeng; Jin Hua; Liu Fuyang; Ding Zhanhui; Yang Bin; Lu Fengguo; Zhao Xudong; Liu Xiaoyang

    2010-07-15

    Boron reacted with ball milled boron oxide under pressures between 1 and 5 GPa and at temperatures between 1300 and 1700 {sup o}C to afford boron suboxide (B{sub 6}O). Icosahedral B{sub 6}O grains with diameters ranging from 100 nm to 1.3 {mu}m were prepared. The factors that affect the synthesis of B{sub 6}O are investigated. The best sample with crystal size up to 1.3 {mu}m is obtained at 2 GPa and 1400 {sup o}C for 6 h. The indentation experiment gave an average Vickers hardness of 32.3 GPa for bulk B{sub 6}O sample, which is consistent with previous reports. Bulk B{sub 6}O sample exhibits oxidation resistance in air up to 1000 {sup o}C and mild oxidation in the temperatures of 1000-1200 {sup o}C, which is more oxidation resistant than diamond. It is possible that B{sub 6}O could be used as a substitute for diamond in industry because of its relatively mild synthesis conditions, high thermal stability and high hardness. - Graphical abstract: Icosahedral B{sub 6}O grains were prepared for mixtures of boron and ball milled boron oxide at 2 GPa and 1400 {sup o}C, a milder synthesis condition in comparison with previous works.

  6. Neutron diffraction study of the interaction of iron with amorphous fullerite

    NASA Astrophysics Data System (ADS)

    Borisova, P. A.; Agafonov, S. S.; Blanter, M. S.; Somenkov, V. A.

    2014-01-01

    The amorphous fullerite C60 has been prepared by mechanical activation (grinding in a ball mill), and its interaction with iron during sintering of powders with 0-95 at % Fe has been studied. After sintering in the range 800-1200°C under a pressure of 70 MPa, the samples have nonequilibrium structures different from the structures of both annealed and quenched steels. In this case, the carbon phase, i.e., amorphous fullerite, undergoes a polyamorphous transition to amorphous graphite. It has also been shown that the interaction of amorphous fullerite with iron is weaker compared to crystalline fullerite or crystalline graphite.

  7. Calorimetry study of the synthesis of amorphous Ni-Ti alloys by mechanical alloying. [Ni33 Ti67

    SciTech Connect

    Schwarz, R.B.; Petrich, R.R.

    1988-01-01

    We synthesized amorphous Ni/sub 33/Ti/sub 67/ alloy powder by ball milling (a) a mixture of elemental nickel and titanium powders and (b) powders of the crystalline intermetallic NiTi/sub 2/. We characterized the reaction products as a function of ball-milling time by differential scanning calorimetry and x-ray diffraction. The measurements suggest that in process (a) the amorphous alloy forms by a solid-state interdiffusion reaction at the clean Ni/Ti interfaces generated by the mechanical attrition. In process (b), the crystalline alloy powder stores energy in the form of chemical disorder and lattice and point defects. The crystal-to-amorphous transformation occurs when the stored energy reaches a critical value. The achievement of the critical stored energy competes with the dynamic recovery of the lattice. 23 refs., 7 figs.

  8. Iron-based amorphous alloys and methods of synthesizing iron-based amorphous alloys

    DOEpatents

    Saw, Cheng Kiong; Bauer, William A.; Choi, Jor-Shan; Day, Dan; Farmer, Joseph C.

    2016-05-03

    A method according to one embodiment includes combining an amorphous iron-based alloy and at least one metal selected from a group consisting of molybdenum, chromium, tungsten, boron, gadolinium, nickel phosphorous, yttrium, and alloys thereof to form a mixture, wherein the at least one metal is present in the mixture from about 5 atomic percent (at %) to about 55 at %; and ball milling the mixture at least until an amorphous alloy of the iron-based alloy and the at least one metal is formed. Several amorphous iron-based metal alloys are also presented, including corrosion-resistant amorphous iron-based metal alloys and radiation-shielding amorphous iron-based metal alloys.

  9. Recycling process for recovery of gallium from GaN an e-waste of LED industry through ball milling, annealing and leaching

    SciTech Connect

    Swain, Basudev Mishra, Chinmayee; Kang, Leeseung; Park, Kyung-Soo Lee, Chan Gi; Hong, Hyun Seon

    2015-04-15

    Waste dust generated during manufacturing of LED contains significant amounts of gallium and indium, needs suitable treatment and can be an important resource for recovery. The LED industry waste dust contains primarily gallium as GaN. Leaching followed by purification technology is the green and clean technology. To develop treatment and recycling technology of these GaN bearing e-waste, leaching is the primary stage. In our current investigation possible process for treatment and quantitative leaching of gallium and indium from the GaN bearing e-waste or waste of LED industry dust has been developed. To recycle the waste and quantitative leaching of gallium, two different process flow sheets have been proposed. In one, process first the GaN of the waste the LED industry dust was leached at the optimum condition. Subsequently, the leach residue was mixed with Na{sub 2}CO{sub 3}, ball milled followed by annealing, again leached to recover gallium. In the second process, the waste LED industry dust was mixed with Na{sub 2}CO{sub 3}, after ball milling and annealing, followed acidic leaching. Without pretreatment, the gallium leaching was only 4.91 w/w % using 4 M HCl, 100 °C and pulp density of 20 g/L. After mechano-chemical processing, both these processes achieved 73.68 w/w % of gallium leaching at their optimum condition. The developed process can treat and recycle any e-waste containing GaN through ball milling, annealing and leaching. - Highlights: • Simplest process for treatment of GaN an LED industry waste developed. • The process developed recovers gallium from waste LED waste dust. • Thermal analysis and phase properties of GaN to Ga{sub 2}O{sub 3} and GaN to NaGaO{sub 2} revealed. • Solid-state chemistry involved in this process reported. • Quantitative leaching of the GaN was achieved.

  10. Structure-Property Correlation in Fe-Al2O3 In Situ Nanocomposite Synthesized by High-Energy Ball Milling and Spark Plasma Sintering

    NASA Astrophysics Data System (ADS)

    Udhayabanu, V.; Ravi, K. R.; Murty, B. S.

    2016-07-01

    In the present study, Fe-10 vol pct Al2O3 in situ nanocomposite has been derived by high-energy ball milling of Fe2O3-Fe-Al powder mixture followed by the consolidation using spark plasma sintering (SPS). The consolidated nanocomposite has bimodal-grained structure consisting of nanometer- and submicron-sized Fe grains along with nanometer-sized Al2O3, and Fe3O4 particles. The mechanical property analysis reveals that compressive yield strength of Fe-10 vol pct Al2O3 nanocomposite is 2100 MPa which is nearly two times higher than that of monolithic Fe processed by Mechanical Milling and SPS. The strengthening contributions obtained from matrix, grain size, and particles in the synthesized nanocomposite have been calculated theoretically, and are found to be matching well with the experimental strength levels.

  11. Multiphase transformation and hybrid nanostructure under non-equilibrium and equilibrium condition during high-energy ball milling of BaTiO3 powders

    NASA Astrophysics Data System (ADS)

    Ghosh, Jiten; Bysakh, Sandip; Mazumder, Sujata

    2014-04-01

    BaTiO3 is a well-known technologically important electroceramic material. In the present study high-energy ball-milling processing for producing distortion in the parent thermodynamically stable tetragonal BaTiO3 has been followed. This has produced nano-sized particles as well as a reactive surface. The intention of the present work is to study (i) structural changes on mechanical activation of perovskite BaTiO3 phase and (ii) possible formation of lattice defect as a result of lattice strain generated during milling that can serve peculiar channels of enhanced diffusion of gas molecules at ambient condition. Catalytic activity of nano-sized BaTiO3 has been explained on a result of high structural distortion brought into solid by milling.

  12. Effect of ball milling and thermal treatment on exchange bias and magnetocaloric properties of Ni48Mn39.5Sn10.5Al2 ribbons

    NASA Astrophysics Data System (ADS)

    Czaja, P.; Przewoźnik, J.; Fitta, M.; Bałanda, M.; Chrobak, A.; Kania, B.; Zackiewicz, P.; Wójcik, A.; Szlezynger, M.; Maziarz, W.

    2016-03-01

    The combined effect of ball milling and subsequent heat treatment on microstructure, magnetic, magnetocaloric and exchange bias properties of Ni48Mn39.5Sn10.5Al2 ribbons is reported. The annealing treatment results in the increase of the critical martensitic transformation temperature. The magnetic entropy change ΔSM of the order of 7.9 and -2.3 J kg K-1 for the annealed 50-32 μm powder fraction is determined. This is less than in the as melt spun ribbon but appears at a considerably higher temperature. At the same time EB is decreased due to annealing treatment. This decrease is attributed to the strengthened ferromagnetic exchange coupling due heat induced stress and structural relaxation.

  13. Structure-Property Correlation in Fe-Al2O3 In Situ Nanocomposite Synthesized by High-Energy Ball Milling and Spark Plasma Sintering

    NASA Astrophysics Data System (ADS)

    Udhayabanu, V.; Ravi, K. R.; Murty, B. S.

    2016-10-01

    In the present study, Fe-10 vol pct Al2O3 in situ nanocomposite has been derived by high-energy ball milling of Fe2O3-Fe-Al powder mixture followed by the consolidation using spark plasma sintering (SPS). The consolidated nanocomposite has bimodal-grained structure consisting of nanometer- and submicron-sized Fe grains along with nanometer-sized Al2O3, and Fe3O4 particles. The mechanical property analysis reveals that compressive yield strength of Fe-10 vol pct Al2O3 nanocomposite is 2100 MPa which is nearly two times higher than that of monolithic Fe processed by Mechanical Milling and SPS. The strengthening contributions obtained from matrix, grain size, and particles in the synthesized nanocomposite have been calculated theoretically, and are found to be matching well with the experimental strength levels.

  14. Ultrathin SmCo5 nanoflakes with high-coercivity prepared by solid particle (NaCl) and surfactant co-assisted ball milling.

    PubMed

    Zuo, Wen-Liang; Zhao, Xin; Zhao, Tong-Yun; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

    2016-01-01

    The ultrathin SmCo5 nanoflakes with average thickness smaller than 50 nm are prepared by a novel method of solid particle (NaCl) and surfactant co-assisted ball milling. The as-prepared nanoflakes exhibit a narrower thickness distribution of 10-50 nm and high coercivity of 23 kOe. The possible formation mechanism of nanoflakes are proposed. Temperature dependence of demagnetization curves indicate that the magnetization reversal may be controlled by both nucleation and pinning. The results of X-ray powder diffraction and magnetic measurement for aligned SmCo5 nanoflakes resin composite indicate that the nanoflakes have a high texture degree. The ultrathin thickness and high coercivity are beneficial for preparing the high performance soft/hard coupling magnets and nanocomposite magnets. PMID:27174410

  15. Ultrathin SmCo5 nanoflakes with high-coercivity prepared by solid particle (NaCl) and surfactant co-assisted ball milling

    PubMed Central

    Zuo, Wen-Liang; Zhao, Xin; Zhao, Tong-Yun; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

    2016-01-01

    The ultrathin SmCo5 nanoflakes with average thickness smaller than 50 nm are prepared by a novel method of solid particle (NaCl) and surfactant co-assisted ball milling. The as-prepared nanoflakes exhibit a narrower thickness distribution of 10–50 nm and high coercivity of 23 kOe. The possible formation mechanism of nanoflakes are proposed. Temperature dependence of demagnetization curves indicate that the magnetization reversal may be controlled by both nucleation and pinning. The results of X-ray powder diffraction and magnetic measurement for aligned SmCo5 nanoflakes resin composite indicate that the nanoflakes have a high texture degree. The ultrathin thickness and high coercivity are beneficial for preparing the high performance soft/hard coupling magnets and nanocomposite magnets. PMID:27174410

  16. Ultrathin SmCo5 nanoflakes with high-coercivity prepared by solid particle (NaCl) and surfactant co-assisted ball milling

    NASA Astrophysics Data System (ADS)

    Zuo, Wen-Liang; Zhao, Xin; Zhao, Tong-Yun; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

    2016-05-01

    The ultrathin SmCo5 nanoflakes with average thickness smaller than 50 nm are prepared by a novel method of solid particle (NaCl) and surfactant co-assisted ball milling. The as-prepared nanoflakes exhibit a narrower thickness distribution of 10–50 nm and high coercivity of 23 kOe. The possible formation mechanism of nanoflakes are proposed. Temperature dependence of demagnetization curves indicate that the magnetization reversal may be controlled by both nucleation and pinning. The results of X-ray powder diffraction and magnetic measurement for aligned SmCo5 nanoflakes resin composite indicate that the nanoflakes have a high texture degree. The ultrathin thickness and high coercivity are beneficial for preparing the high performance soft/hard coupling magnets and nanocomposite magnets.

  17. Use of cellobiohydrolase-free cellulase blends for the hydrolysis of microcrystalline cellulose and sugarcane bagasse pretreated by either ball milling or ionic liquid [Emim][Ac].

    PubMed

    Teixeira, Ricardo Sposina Sobral; da Silva, Ayla Sant'Ana; Kim, Han-Woo; Ishikawa, Kazuhiko; Endo, Takashi; Lee, Seung-Hwan; Bon, Elba P S

    2013-12-01

    This study investigated the requirement of cellobiohydrolases (CBH) for saccharification of microcrystalline cellulose and sugarcane bagasse pretreated either by ball milling (BM) or by ionic liquid (IL) [Emim][Ac]. Hydrolysis was done using CBH-free blends of Pyrococcus horikoshii endoglucanase (EG) plus Pyrococcus furiosus β-glucosidase (EGPh/BGPf) or Optimash™ BG while Acremonium Cellulase was used as control. IL-pretreated substrates were hydrolyzed more effectively by CBH-free enzymes than were the BM-pretreated substrates. IL-treatment decreased the crystallinity and increased the specific surface area (SSA), whereas BM-treatment decreased the crystallinity without increasing the SSA. The hydrolysis of IL-treated cellulose by EGPh/BGPf showed a saccharification rate of 3.92 g/Lh and a glucose yield of 81% within 9h. These results indicate the efficiency of CBH-free enzymes for the hydrolysis of IL-treated substrates.

  18. X-ray absorption, neutron diffraction, and M{umlt o}ssbauer effect studies of MnZn{endash}ferrite processed through high-energy ball milling

    SciTech Connect

    Fatemi, D.J.; Harris, V.G.; Chen, M.X.; Malik, S.K.; Yelon, W.B.; Long, G.J.; Mohan, A.

    1999-04-01

    MnZn{endash}ferrite has been prepared via high-energy ball milling of elemental oxides MnO, ZnO, and {alpha}-Fe{sub 2}O{sub 3}. Neutron diffraction measurements suggest a high density of vacancies in a spinel structure. The spinel phase appears to comprise 99.8 wt;{percent} of the material in the sample milled for 40 h, with the remainder attributable to unreacted {alpha}-Fe{sub 2}O{sub 3}. The x-ray absorption near-edge structure was analyzed to provide an understanding of the charge state of the constituent Fe ions. This analysis reveals about 2/3 of Fe cations to be trivalent, increasing to about 3/4 after a 5 h anneal at 450;{degree}C. The heat treatment is also observed to induce a cation redistribution in the ball-milled ferrite toward that of a standard processed via ceramics methods. Results from M{umlt o}ssbauer spectroscopy determine the average hyperfine fields in the sample milled 40 h to be 289 and 487 kOe at 295 and 78 K, respectively. The average isomer shift is 0.32 mm/s at 295 K and 0.46 mm/s at 78 K, values which are typical of iron (III) in a spinel oxide lattice. As expected for a cubic-like environment, the quadrupole shifts are very small, ranging from 0.07 mm/s at 295 K to 0.00 mm/s at 78 K. {copyright} {ital 1999 American Institute of Physics.}

  19. Layered-Layered-Spinel Cathode Materials Prepared by a High-Energy Ball-Milling Process for Lithium-ion Batteries.

    PubMed

    Kim, Soo; Noh, Jae-Kyo; Aykol, Muratahan; Lu, Zhi; Kim, Haesik; Choi, Wonchang; Kim, Chunjoong; Chung, Kyung Yoon; Wolverton, Chris; Cho, Byung-Won

    2016-01-13

    In this work, we report the electrochemical properties of 0.5Li2MnO3·0.25LiNi0.5Co0.2Mn0.3O2·0.25LiNi0.5Mn1.5O4 and 0.333Li2MnO3·0.333LiNi0.5Co0.2Mn0.3O2·0.333LiNi0.5Mn1.5O4 layered-layered-spinel (L*LS) cathode materials prepared by a high-energy ball-milling process. Our L*LS cathode materials can deliver a large and stable capacity of ∼200 mAh g(-1) at high voltages up to 4.9 V, and do not show the anomalous capacity increase upon cycling observed in previously reported three-component cathode materials synthesized with different routes. Furthermore, we have performed synchrotron-based in situ X-ray diffraction measurements and found that there are no significant structural distortions during charge/discharge runs. Lastly, we carry out (opt-type) van der Waals-corrected density functional theory (DFT) calculations to explain the enhanced cycle characteristics and reduced phase transformations in our ball-milled L*LS cathode materials. Our simple synthesis method brings a new perspective on the use of the high-power L*LS cathodes in practical devices.

  20. Study of magnetic behavior in ball-milled nanocrystalline Fe-50 at.%Al alloy as a function of milling time

    NASA Astrophysics Data System (ADS)

    Rajan, S.; Shukla, R.; Kumar, A.; Vyas, A.; Brajpuriya, R.

    2015-04-01

    Ball milling technique has been extensively used to prepare different metastable states with nanocrystalline microstructures from intermetallic compounds. The present study was made on the identification of the changes in magnetic and electronic properties as a result of high-energy ball milling of Fe-50 at.%Al alloy samples. The phase formation and physical properties of the alloys were determined as a function of milling time by means of Mössbauer and X-ray photoelectron spectroscopy (XPS). The Mössbauer results show the formation of nanostructured body-centered cubic (BCC) FeAl alloy only after 5 h of mechanical milling and the same is also confirmed by Scanning electron microscope (SEM) and Transmission electron microscopy (TEM) studies. Mössbauer studies further confirm that there is magnetic behavior retention in the FeAl alloy samples even after 5 h of milling but magnetization decreases as the milling time increases. The reason for the same is due to the shocks and fracturing of the Al atoms embedded in the sites of Fe and as a result of which Fe-Fe nearest neighbors decreases. Secondly, with the increase in milling time, the particle size and the number density of equiatomic BCC Fe50Al50 grains decrease while the volume of grain boundary containing a solid solution of BCC FeAl and concentration of Al in a solid solution of BCC FeAl at the grain boundary increases as a result of which magnetization decreases. The shift in the binding energy of Fe2p and Al2p core level towards higher binding energy also supports the alloy formation after milling.

  1. Solid state amorphization in the Al-Fe binary system during high energy milling

    SciTech Connect

    Urban, P. Montes, J. M.; Cintas, J.

    2013-12-16

    In the present study, mechanical alloying (MA) of Al75Fe25 elemental powders mixture was carried out in argon atmosphere, using a high energy attritor ball mill. The microstructure of the milled products at different stages of milling was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The results showed that the amorphous phase content increased by increasing the milling time, and after 50 hours the amorphization process became complete. Heating the samples resulted in the crystallization of the synthesized amorphous alloys and the appearance of the equilibrium intermetallic compounds Al{sub 5}Fe{sub 2}.

  2. The studies of high-frequency magnetic properties and absorption characteristics for amorphous-filler composites

    NASA Astrophysics Data System (ADS)

    Li, Z. W.; Yang, Z. H.

    2015-10-01

    Pure amorphous flake fillers and amorphous flakes coated by ferrite nanoparticles with core-shell-like structure were fabricated using mechanical ball-milling. The later with core-shell-like structure can greatly decrease permittivity and improve the absorption properties, as compared to the former. The absorption of all amorphous-filler composites has its origin in a quarter-wavelength resonator. Based on the resonator model, absorption frequency fA and the corresponding return loss RL are calculated, which are well consistent with observed values. It is also found that the resonance frequency is proportional to effective resistivity, based on William-Shockley-Kittel's eddy model.

  3. Phase transformations in amorphous fullerite C60 under high pressure and high temperature

    NASA Astrophysics Data System (ADS)

    Borisova, P. A.; Blanter, M. S.; Brazhkin, V. V.; Somenkov, V. A.; Filonenko, V. P.

    2015-08-01

    First phase transformations of amorphous fullerite C60 at high temperatures (up to 1800 K) and high pressures (up to 8 GPa) have been investigated and compared with the previous studies on the crystalline fullerite. The study was conducted using neutron diffraction and Raman spectroscopy. The amorphous fullerite was obtained by ball-milling. We have shown that under thermobaric treatment no crystallization of amorphous fullerite into С60 molecular modification is observed, and it transforms into amorphous-like or crystalline graphite. A kinetic diagram of phase transformation of amorphous fullerite in temperature-pressure coordinates was constructed for the first time. Unlike in crystalline fullerite, no crystalline polymerized phases were formed under thermobaric treatment on amorphous fullerite. We found that amorphous fullerite turned out to be less resistant to thermobaric treatment, and amorphous-like or crystalline graphite were formed at lower temperatures than in crystalline fullerite.

  4. 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. PMID:21983262

  5. Magnetic properties of Co1-xZnxFe2O4 spinel ferrite nanoparticles synthesized by starch-assisted sol-gel autocombustion method and its ball milling

    NASA Astrophysics Data System (ADS)

    Yadav, Raghvendra Singh; Havlica, Jaromir; Hnatko, Miroslav; Šajgalík, Pavol; Alexander, Cigáň; Palou, Martin; Bartoníčková, Eva; Boháč, Martin; Frajkorová, Františka; Masilko, Jiri; Zmrzlý, Martin; Kalina, Lukas; Hajdúchová, Miroslava; Enev, Vojtěch

    2015-03-01

    In this article, Co1-xZnxFe2O4 (x=0.0 and 0.5) spinel ferrite nanoparticles were achieved at 800 °C by starch-assisted sol-gel autocombustion method. To further reduce the particle size, these synthesized ferrite nanoparticles were ball-milled for 2 h. X-ray diffraction patterns demonstrated single phase formation of Co1-xZnxFe2O4 (x=0.0 and 0.5) spinel ferrite nanoparticles. FE-SEM analysis indicated the nanosized spherical particles formation with spherical morphology. The change in Raman modes and relative intensity were observed due to ball milling and consequently decrease of particle size and cationic redistribution. An X-ray Photoelectron Spectroscopy (XPS) result indicated that Co2+, Zn2+ and Fe3+ exist in octahedral and tetrahedral sites. The cationic redistribution of Zn2+ and consequently Fe3+ occurred between octahedral and tetrahedral sites after ball-milling. The change in saturation magnetization (Ms) and coercivity (Hc) with decrease of nanocrystalline size and distribution of cations in spinel ferrite were observed.

  6. Effect of ball-milling and Fe-/Al-doping on the structural aspect and visible light photocatalytic activity of TiO2 towards Escherichia coli bacteria abatement.

    PubMed

    Schlur, Laurent; Begin-Colin, Sylvie; Gilliot, Pierre; Gallart, Mathieu; Carré, Gaëlle; Zafeiratos, Spiros; Keller, Nicolas; Keller, Valérie; André, Philippe; Greneche, Jean-Marc; Hezard, Bernard; Desmonts, Marie-Hélène; Pourroy, Geneviève

    2014-05-01

    Escherichia coli abatement was studied in liquid phase under visible light in the presence of two commercial titania photocatalysts, and of Fe- and Al-doped titania samples prepared by high energy ball-milling. The two commercial titania photocatalysts, Aeroxide P25 (Evonik industries) exhibiting both rutile and anatase structures and MPT625 (Ishihara Sangyo Kaisha), a Fe-, Al-, P- and S-doped titania exhibiting only the rutile phase, are active suggesting that neither the structure nor the doping is the driving parameter. Although the MPT625 UV-visible spectrum is shifted towards the visible domain with respect to the P25 one, the effect on bacteria is not increased. On the other hand, the ball milled iron-doped P25 samples exhibit low activities in bacteria abatement under visible light due to charge recombinations unfavorable to catalysis as shown by photoluminescence measurements. While doping elements are in interstitial positions within the rutile structure in MPT625 sample, they are located at the surface in ball milled samples and in isolated octahedral units according to (57)Fe Mössbauer spectrometry. The location of doping elements at the surface is suggested to be responsible for the sample cytotoxicity observed in the dark.

  7. Effects of zero-valent metals together with quartz sand on the mechanochemical destruction of dechlorane plus coground in a planetary ball mill.

    PubMed

    Wang, Haizhu; Huang, Jun; Zhang, Kunlun; Yu, Yunfei; Liu, Kai; Yu, Gang; Deng, Shubo; Wang, Bin

    2014-01-15

    Mechanochemical destruction by grinding with additives in high energy ball milling has been identified as a good alternative to traditional incineration for the disposal of wastes containing halogenated organic pollutants. Despite CaO normally used as an additive, recently Fe+SiO2 has been used to replace CaO for a faster destruction. In the present study, zero-valent metals (Al, Zn, besides Fe) together with SiO2 were investigated for their efficiencies of prompting the destruction of dechlorane plus (DP). Aluminum was found of be the best with a destruction percentage of nearly 99% for either syn- or anti-DP after 2.5h milling. In comparison, only 88/85% and 37/32% of syn-/anti-DP were destroyed when using zinc and iron after the same time, respectively. The detected water soluble chloride was lower than the stoichiometric amount containing in the original DP samples, due to the Si-Cl bond formed during the process. The potential fate of C and Cl present in DP is in the form of inorganic carbon, inorganic Cl and formation of Si-Cl bonds, respectively. The results suggested that Al+SiO2 is promising in the mechanochemical destruction of chlorinated organic pollutants like DP. PMID:24295775

  8. The grinding behavior of ground copper powder for Cu/CNT nanocomposite fabrication by using the dry grinding process with a high-speed planetary ball mill

    NASA Astrophysics Data System (ADS)

    Choi, Heekyu; Bor, Amgalan; Sakuragi, Shiori; Lee, Jehyun; Lim, Hyung-Tae

    2016-01-01

    The behavior of ground copper powder for copper-carbon nanotube (copper-CNT) nanocomposite fabrication during high-speed planetary ball milling was investigated because the study of the behavior characteristics of copper powder has recently gained scientific interest. Also, studies of Cu/CNT composites have widely been done due to their useful applications to enhanced, advanced nano materials and components, which would significantly improve the properties of new mechatronics-integrated materials and components. This study varied experimental conditions such as the rotation speed and the grinding time with and without CNTs, and the particle size distribution, median diameter, crystal structure and size, and particle morphology were monitored for a given grinding time. We observed that pure copper powders agglomerated and that the morphology changed with changing rotation speed. The particle agglomerations were observed with maximum experiment conditions (700 rpm, 60 min) in this study of the grinding process for mechanical alloys in the case of pure copper powders because the grinding behavior of Cu/CNT agglomerations was affected by the addition of CNTs. Indeed, the powder morphology and the crystal size of the composite powder could be changed by increasing the grinding time and the rotation speed.

  9. Effect of ball milling and dynamic compaction on magnetic properties of Al{sub 2}O{sub 3}/Co(P) composite particles

    SciTech Connect

    Denisova, E. A.; Kuzovnikova, L. A.; Iskhakov, R. S. Eremin, E. V.; Bukaemskiy, A. A.; Nemtsev, I. V.

    2014-05-07

    The evolution of the magnetic properties of composite Al{sub 2}O{sub 3}/Co(P) particles during ball milling and dynamic compaction is investigated. To prepare starting composite particles, the Al{sub 2}O{sub 3} granules were coated with a Co{sub 95}P{sub 5} shell by electroless plating. The magnetic and structural properties of the composite particles are characterized by scanning electron microscopy, X-ray diffraction, and the use of the Physical Property Measurement System. The use of composite core-shell particles as starting powder for mechanoactivation allows to decrease treatment duration to 1 h and to produce a more homogeneous bulk sample than in the case of the mixture of Co and Al{sub 2}O{sub 3} powders. The magnetic properties of the milled composite particles are correlated with changes in the microstructure. Reduction in grain size of Co during milling leads to an increase of the volume fraction of superparamagnetic particles and to a decrease of the saturation magnetization. The local magnetic anisotropy field depends on the amount of hcp-Co phase in sample. The anisotropy field value decreases from 8.4 kOe to 3.8 kOe with an increase in milling duration up to 75 min. The regimes of dynamic compaction were selected so that the magnetic characteristics—saturation magnetization and coercive field—remained unchanged.

  10. Covalent modification of glassy carbon spheres through ball milling under solvent free conditions: A novel electrochemical interface for mercury(II) quantification.

    PubMed

    Kempegowda, Raghu G; Malingappa, Pandurangappa

    2014-08-01

    A simple and green chemistry protocol has been proposed based on the covalent anchoring of benzamide molecule on glassy carbon spheres through ball milling under solvent free condition. The modification proceeds through the formation of an amide bond between carboxylic group of glassy carbon spheres and the amino group of modifier molecule. The formation of covalent bond was ascertained using X-ray photoelectron spectroscopy. Scanning electron microscopy was used to study the surface morphology of milled glassy carbon spheres. The aqueous colloidal solution of modified glassy carbon spheres was used in the preparation of thin film electrodes and subsequently used as a novel electrochemical interface in the quantification of mercury at trace level using a differential pulse anodic stripping voltammetric technique. The modified electrode showed good sensitivity and selectivity towards mercury with a detection limit of 1nM with least interference from most of the ions. The analytical utility of the proposed electrode has been validated by determining the mercury levels in number of sample matrices. PMID:24881534

  11. Binding of carbon coated nano-silicon in graphene sheets by wet ball-milling and pyrolysis as high performance anodes for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Sun, Wei; Hu, Renzong; Zhang, Miao; Liu, Jiangwen; Zhu, Min

    2016-06-01

    A novel approach has been developed to prepare silicon@carbon/graphene sheets (Si@C/G) composite with a unique structure, in which carbon coated Si nanoparticles are uniformly dispersed in a matrix of graphene sheets, to enhance the cycleability and electronic conductivity of Si-based anodes for Li-ion batteries. In this study, Si nanoparticles and expanded graphite (EG) are treated by combining high-energy wet ball-milling in sucrose solution with subsequent pyrolysis treatment to produce this Si@C/G composite. To achieve better overall electrochemical performance, the carbon content of the composites is also studied systematically. The as-designed Si30@C40/G30 (Si:C:G = 30:40:30, by weight) composite exhibits a high Li-storage capacity of 1259 mAh g-1 at a current density of 0.2 A g-1 in the first cycle. Further, a stable cycleability with 99.1/88.2% capacity retention from initial reversible charge capacity can be achieved over 100/300 cycles, showing great promise for batteries applications. This good electrochemical performance can be attributed to the uniform coating and binding effect of pyrolytic carbon as well as the network of graphene sheets, which increase the electronic conductivity and Li+ diffusion in the composite, and effectively accommodated the volume change of Si nanoparticles during the Li+ alloying and dealloying processes.

  12. Effects of zero-valent metals together with quartz sand on the mechanochemical destruction of dechlorane plus coground in a planetary ball mill.

    PubMed

    Wang, Haizhu; Huang, Jun; Zhang, Kunlun; Yu, Yunfei; Liu, Kai; Yu, Gang; Deng, Shubo; Wang, Bin

    2014-01-15

    Mechanochemical destruction by grinding with additives in high energy ball milling has been identified as a good alternative to traditional incineration for the disposal of wastes containing halogenated organic pollutants. Despite CaO normally used as an additive, recently Fe+SiO2 has been used to replace CaO for a faster destruction. In the present study, zero-valent metals (Al, Zn, besides Fe) together with SiO2 were investigated for their efficiencies of prompting the destruction of dechlorane plus (DP). Aluminum was found of be the best with a destruction percentage of nearly 99% for either syn- or anti-DP after 2.5h milling. In comparison, only 88/85% and 37/32% of syn-/anti-DP were destroyed when using zinc and iron after the same time, respectively. The detected water soluble chloride was lower than the stoichiometric amount containing in the original DP samples, due to the Si-Cl bond formed during the process. The potential fate of C and Cl present in DP is in the form of inorganic carbon, inorganic Cl and formation of Si-Cl bonds, respectively. The results suggested that Al+SiO2 is promising in the mechanochemical destruction of chlorinated organic pollutants like DP.

  13. Facile solid state ball milling as a green strategy to prepare 2-(2,4-dichlorophenoxy)-N‧-(2-hydroxybenzylidene)acetohydrazide complexes

    NASA Astrophysics Data System (ADS)

    Fekri, Ahmed; Zaky, Rania

    2014-11-01

    2-(2,4-Dichlorophenoxy)-N‧-(2-hydroxybenzylidene)acetohydrazide (H2L) complexes were prepared by ball milling involving the reaction of ligand with Ni(II), Co(II), Cu(II) and VO(II) salts (mechanochemical syntheses). The compounds were elucidated by elemental analysis, spectroscopy (1H NMR, IR, UV-visible, MS spectra), and physical measurements (magnetic susceptibility and molar conductance). IR spectra suggested that the H2L behaved as a monodentate and/or bidentate ligand coordinating via azomethine nitrogen and/or deprotonated enolized carbonyl oxygen. The electronic spectra of the complexes and their magnetic moments provided information about geometries. The antimicrobial activities of the ligand and its complexes were studied against gram positive bacteria; Staphylococcus aureus, gram-negative bacteria; Escherichia coli and pathogenic fungi; Candida albicans by using minimum inhibition concentrations method (MIC). Also, the antioxidant (ABTS-derived free radical method) and cytotoxic (in vitro Ehrlich Ascites) activities of the isolated compounds were evaluated.

  14. Exfoliation of graphite with triazine derivatives under ball-milling conditions: preparation of few-layer graphene via selective noncovalent interactions.

    PubMed

    León, Verónica; Rodriguez, Antonio M; Prieto, Pilar; Prato, Maurizio; Vázquez, Ester

    2014-01-28

    A ball-milling treatment can be employed to exfoliate graphite through interactions with commercially available melamine under solid conditions. This procedure allows the fast production of relatively large quantities of material with a low presence of defects. The milling treatment can be modulated in order to achieve graphene flakes with different sizes. Once prepared, the graphene samples can be redispersed in organic solvents, water, or culture media, forming stable dispersions that can be used for multiple purposes. In the present work, we have screened electron-rich benzene derivatives along with triazine derivatives in their respective ability to exfoliate graphite. The results suggest that the formation of a hydrogen-bonding network is important for the formation of multipoint interactions with the surfaces of graphene, which can be used for the exfoliation of graphite and the stabilization of graphene in different solvents. Aminotriazine systems were found to be the best partners in the preparation and stabilization of graphene layers in different solvents, while the equivalent benzene derivatives did not show comparable exfoliation ability. Computational studies have also been performed to rationalize the experimental results. The results provide also the basis for further work in the preparation of noncovalently modified graphene, where derivatives of aminotriazines can be designed to form extensive hydrogen-bond 2D networks on the graphene surface with the aim of manipulating their electronic and chemical properties.

  15. Textured Pr{sub 2}Fe{sub 14}B flakes with submicron or nanosize thickness prepared by surfactant-assisted ball milling

    SciTech Connect

    Zuo, Wen-Liang E-mail: shenbg@aphy.iphy.ac.cn; Liu, Rong-Ming; Zheng, Xin-Qi; Wu, Rong-Rong; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen E-mail: shenbg@aphy.iphy.ac.cn

    2014-05-07

    The textured Pr{sub 2}Fe{sub 14}B nanoflakes were produced by surfactant-assisted ball milling (SABM). Single phase tetragonal structure was characterized for the samples before and after SABM by X-ray diffraction (XRD). The thickness and length of the as-milled flakes are mainly in the range of 50–150 nm and 0.5–2 μm, respectively. For the field-aligned Pr{sub 2}Fe{sub 14}B nanoflakes, the out-of-plane texture (the easy magnetization direction (EMD) along the c-axis) is indicated from the increasing (00l) peaks in the XRD patterns. SEM image demonstrates that the EMD is parallel to flaky surface, which is different from the RCo{sub 5} (R = rare earth) system with EMD perpendicular to the surface. We propose a hypothesis that the easy glide planes are related with the area of crystal planes. In addition, a large coercivity H{sub c} = 3.9 kOe is observed in the Pr{sub 2}Fe{sub 14}B flakes with strong texture.

  16. Formation of NiAl Intermetallic Compound by Cold Spraying of Ball-Milled Ni/Al Alloy Powder Through Postannealing Treatment

    NASA Astrophysics Data System (ADS)

    Zhang, Qiang; Li, Chang-Jiu; Wang, Xiu-Ru; Ren, Zhi-Liang; Li, Cheng-Xin; Yang, Guan-Jun

    2008-12-01

    Ni/Al alloy powders were synthesized by ball milling of nickel-aluminum powder mixture with a Ni/Al atomic ratio of 1:1. Ni/Al alloy coating was deposited by cold spraying using N2 as accelerating gas. NiAl intermetallic compound was evolved in situ through postspray annealing treatment of cold-sprayed Ni/Al alloy coating. The effect of annealing temperature on the phase transformation behavior from Ni/Al mechanical alloy to intermetallics was investigated. The microstructure of the mechanically alloying Ni/Al powder and NiAl coatings was characterized by scanning electron microscopy and x-ray diffraction analysis. The results show that a dense Ni/Al alloy coating can be successfully deposited by cold spraying using the mechanically alloyed powder as feedstocks. The as-sprayed alloy coating exhibited a laminated microstructure retained from the mechanically alloying powder. The annealing of the subsequent Ni/Al alloy coating at a temperature higher than 850 °C leads to complete transformation from Ni/Al alloy to NiAl intermetallic compound.

  17. Magnetic properties and coercivity mechanism of Sm1-xPrxCo5 (x=0-0.6) nanoflakes prepared by surfactant-assisted ball milling

    NASA Astrophysics Data System (ADS)

    Xu, M. L.; Yue, M.; Wu, Q.; Li, Y. Q.; Lu, Q. M.

    2016-05-01

    Sm1-xPrxCo5 (x=0-0.6) nanoflakes with CaCu5 structure were successfully prepared by surfactant-assisted high-energy ball milling (SAHEBM). The crystal structure and magnetic properties of Sm1-xPrxCo5 (x=0-0.6) nanoflakes were studied by X-ray diffraction and vibrating sample magnetometer. Effects of Pr addition on the structure, magnetic properties and coercivity mechanism of Sm1-xPrxCo5 nanoflakes were systematically investigated. XRD results show that all the nanoflakes have a hexagonal CaCu5-type (Sm, Pr)1Co5 main phase and the (Sm, Pr)2Co7 impurity phase, and all of the samples exhibit a strong (00l) texture after magnetic alignment. As the Pr content increases, remanence firstly increases, then slightly reduced, while anisotropy field (HA) and Hci of decrease monotonically. Maximum energy product [(BH)max] of the flakes increases first, peaks at 24.4 MGOe with Pr content of x = 0.4, then drops again. Magnetization behavior analysis indicate that the coercivity mechanism is mainly controlled by inhomogeneous domain wall pinning, and the pinning strength weakens with the increased Pr content, suggesting the great influence of HA on the coercivity of flakes.

  18. Influence of ball milling and annealing conditions on the properties of L10 FePt nanoparticles fabricated by a new green chemical synthesis method

    NASA Astrophysics Data System (ADS)

    Hu, X. C.; Capobianchi, A.; Gallagher, R.; Hadjipanayis, G. C.

    2014-05-01

    In this work, a new green chemical strategy for the synthesis of L10 FePt alloy nanoparticles is reported. The precursor is a polycrystalline molecular complex (Fe(H2O)6PtCl6), in which Fe and Pt atoms are arranged on alternating planes and milled with NaCl to form nanocrystals. Then the mixture was annealed under reducing atmosphere (5% H2 and 95% Ar) at temperatures varying from 350 °C to 500 °C for 2 h with a heating rate of 5 °C/min. After the reduction, the mixture was washed with water to remove the NaCl and L10 FePt nanoparticles were obtained. The X-Ray Diffraction pattern showed the presence of the characteristic peaks of the fct phase of FePt nanoparticles. Influence of precursor/NaCl ratio and ball milling time on particle size was investigated. Transmission electron microscopy images revealed that smaller precursor/NaCl ratio (10 mg/20 g) and longer milling time (15 h) lead to smaller particle size and narrower size distribution. Milling time does not influence the coercivity much but the decrease of the amount of precursor leads to a decrease of coercivity from 10.8 kOe to 4.8 kOe.

  19. Facile solid state ball milling as a green strategy to prepare 2-(2,4-dichlorophenoxy)-N'-(2-hydroxybenzylidene)acetohydrazide complexes.

    PubMed

    Fekri, Ahmed; Zaky, Rania

    2014-11-11

    2-(2,4-Dichlorophenoxy)-N'-(2-hydroxybenzylidene)acetohydrazide (H2L) complexes were prepared by ball milling involving the reaction of ligand with Ni(II), Co(II), Cu(II) and VO(II) salts (mechanochemical syntheses). The compounds were elucidated by elemental analysis, spectroscopy (1H NMR, IR, UV-visible, MS spectra), and physical measurements (magnetic susceptibility and molar conductance). IR spectra suggested that the H2L behaved as a monodentate and/or bidentate ligand coordinating via azomethine nitrogen and/or deprotonated enolized carbonyl oxygen. The electronic spectra of the complexes and their magnetic moments provided information about geometries. The antimicrobial activities of the ligand and its complexes were studied against gram positive bacteria; Staphylococcus aureus, gram-negative bacteria; Escherichia coli and pathogenic fungi; Candida albicans by using minimum inhibition concentrations method (MIC). Also, the antioxidant (ABTS-derived free radical method) and cytotoxic (in vitro Ehrlich Ascites) activities of the isolated compounds were evaluated.

  20. Influence of ball milling and annealing conditions on the properties of L1{sub 0} FePt nanoparticles fabricated by a new green chemical synthesis method

    SciTech Connect

    Hu, X. C.; Capobianchi, A.; Gallagher, R.; Hadjipanayis, G. C.

    2014-05-07

    In this work, a new green chemical strategy for the synthesis of L1{sub 0} FePt alloy nanoparticles is reported. The precursor is a polycrystalline molecular complex (Fe(H{sub 2}O){sub 6}PtCl{sub 6}), in which Fe and Pt atoms are arranged on alternating planes and milled with NaCl to form nanocrystals. Then the mixture was annealed under reducing atmosphere (5% H{sub 2} and 95% Ar) at temperatures varying from 350 °C to 500 °C for 2 h with a heating rate of 5 °C/min. After the reduction, the mixture was washed with water to remove the NaCl and L1{sub 0} FePt nanoparticles were obtained. The X-Ray Diffraction pattern showed the presence of the characteristic peaks of the fct phase of FePt nanoparticles. Influence of precursor/NaCl ratio and ball milling time on particle size was investigated. Transmission electron microscopy images revealed that smaller precursor/NaCl ratio (10 mg/20 g) and longer milling time (15 h) lead to smaller particle size and narrower size distribution. Milling time does not influence the coercivity much but the decrease of the amount of precursor leads to a decrease of coercivity from 10.8 kOe to 4.8 kOe.

  1. Size dependence of the magnetic and hyperfine properties of nanostructured hematite ( α-Fe 2 O 3 ) powders prepared by the ball milling technique

    NASA Astrophysics Data System (ADS)

    André-Filho, J.; León-Félix, L.; Coaquira, J. A. H.; Garg, V. K.; Oliveira, A. C.

    2014-01-01

    In this work we present the study of hematite ( α-Fe2O3) nanostructures synthesized by the ball milling technique. The structural characterization and the crystallite size estimation have been carried out using the X-ray diffraction (XRD) technique. Data analyses indicate that the hematite phase (space group, R-3C) is preserved after the milling process. As the milling time is increased, a second phase ( α-Fe) appears. The mean crystallite size shows a decreasing tendency as the milling time is increased. High-resolution transmission electron microscopy (HRTEM) images show the formation of grains composed of crystallites with irregular shapes. Mössbauer spectra of milled powders carried out at 297 and 77 K are well modeled with a histogram distribution of hyperfine fields. The presence of one additional sextet which corresponds to the ∝-Fe phase is also determined in agreement with XRD data analysis. Magnetic measurements suggest the suppression of the Morin transition in the milled samples and the absence of thermal relaxation effects in agreement with the Mössbauer spectroscopy results.

  2. Effect of the method of introduction of Y2O3 into NiAl-based powder alloys on their structure: I. Agitation in a ball mill

    NASA Astrophysics Data System (ADS)

    Povarova, K. B.; Vershinina, T. N.; Skachkov, O. A.; Drozdov, A. A.; Morozov, A. E.; Pozharov, S. V.

    2012-09-01

    The effect of the sintering temperature (1100-1400°C) of NiAl alloy samples with oxide Y2O3 produced by hydrostatic pressing on their structure and phase composition and the distribution of oxide particles in a NiAl-based intermetallic matrix alloyed with ˜0.5 at % Fe is considered. It is found that dispersed oxide particles in the compact material prepared from a mixture of oxide Y2O3 powder and a NiAl alloy (produced by calcium hydride reduction of a mixture of nickel and aluminum oxides) powder in a standard ball mill are nonuniformly distributed in the volume. The morphology of oxides changes during sintering: sintered samples contain rounded particles, which differ strongly from the clearly faceted angular particles of oxide Y2O3 added to a mixture (they represent conglomerates of single crystals). In the sintered samples, large aggregates of oxides are revealed along grain boundaries. Mass transfer is possible at the NiAl/Y2O3 interface in the system: it leads to partial substitution of aluminum and/or iron atoms for yttrium atoms in the Y2O3 lattice and to the formation of submicroscopic particles of (Fe,Al)5Y3O12-type oxides.

  3. Enhanced coercivity and remanence of PrCo5 nanoflakes prepared by surfactant-assisted ball milling with heat-treated starting powder

    NASA Astrophysics Data System (ADS)

    Zuo, Wen-Liang; Zhao, Xin; Xiong, Jie-Fu; Shang, Rong-Xiang; Zhang, Ming; Hu, Feng-Xia; Sun, Ji-Rong; Shen, Bao-Gen

    2015-07-01

    PrCo5 nanoflakes with strong texture and high coercivity of 8.15 kOe were prepared by surfactant-assisted ball milling with heat-treated starting powder. The thickness and length of the as-milled nanoflakes are mainly in the ranges of 50-100 nm and 0.5-3 μm, respectively. The x-ray diffraction patterns demonstrate that the heat treatment can increase the single phase and crystallinity of the PrCo5 compound, and combined with the demagnetization curves, indicate that the single phase and crystallinity are important for preparing high-coercivity and strong-textured rare earth permanent magnetic nanoflakes. In addition, the coercivity mechanism of the as-milled PrCo5 nanoflakes is studied by the angle dependence of coercivity for an aligned sample and the field dependence of coercivity, isothermal (IRM) and dc demagnetizing (DCD) remanence curves for an unaligned sample. The results indicate that the coercivity is dominated by co-existing mechanisms of pinning and nucleation. Furthermore, exchange coupling and dipolar coupling also co-exist in the sample. Project supported by the National Basic Research Program of China (Grant No. 2014CB643702), the National Natural Science Foundation of China (Grant No. 51401235), and Beijing Natural Science Foundation, China (Grant No. 2152034).

  4. Synthesis of boron suboxide (B 6O) with ball milled boron oxide (B 2O 3) under lower pressure and temperature

    NASA Astrophysics Data System (ADS)

    Jiao, Xiaopeng; Jin, Hua; Liu, Fuyang; Ding, Zhanhui; Yang, Bin; Lu, Fengguo; Zhao, Xudong; Liu, Xiaoyang

    2010-07-01

    Boron reacted with ball milled boron oxide under pressures between 1 and 5 GPa and at temperatures between 1300 and 1700 °C to afford boron suboxide (B 6O). Icosahedral B 6O grains with diameters ranging from 100 nm to 1.3 μm were prepared. The factors that affect the synthesis of B 6O are investigated. The best sample with crystal size up to 1.3 μm is obtained at 2 GPa and 1400 °C for 6 h. The indentation experiment gave an average Vickers hardness of 32.3 GPa for bulk B 6O sample, which is consistent with previous reports. Bulk B 6O sample exhibits oxidation resistance in air up to 1000 °C and mild oxidation in the temperatures of 1000-1200 °C, which is more oxidation resistant than diamond. It is possible that B 6O could be used as a substitute for diamond in industry because of its relatively mild synthesis conditions, high thermal stability and high hardness.

  5. Morphological, Thermal, and Magnetic Analysis of Ball-Milled γ-Fe2O3 and Fe3O4 Nanoparticles for Biomedical Application

    NASA Astrophysics Data System (ADS)

    Burnham, Philip; Papaefthymiou, Georgia C.; Viescas, Arthur; Li, Calvin; Dollahon, Norman

    2013-03-01

    Superparamagnetic iron oxide nanoparticles are promising agents for hyperthermia cancer treatment, because, when exposed to an alternating magnetic field, they impart heat to surrounding tissue. A comparison of γ-Fe2O3 and Fe3O4 nanoparticles for such application is presented. The particles were obtained via surfactant-assisted high energy ball-milling in a hexane/oleic acid carrier-fluid environment. Particles with diameters of 5 to 16 nm were prepared with mass ratios (oleic acid):(γ-Fe2O3) of 0:1, 1:5, 1:10 and 1:20, with milling times of 3, 6, 9, and 12 hours. TEM micrographs revealed spherical morphology and the effect of oleic acid shells. Optimal size distributions were obtained for high oleic acid contents. At room temperature, a reduced internal magnetic field ~480 kOe) was recorded via Mössbauer spectroscopy compared to bulk γ-Fe2O3 ~500 kOe), due to magnetic relaxation; Fe3O4 particles produced similar results. For the γ-Fe2O3 and Fe3O4 nanoparticles with 20% oleic acid by mass, comparative ZFC/FC magnetization (Happ = 200 Oe in temperature range from 2 to 400 K) and hysteresis loops (T = 2 K and 300 K up to Happ = 6 kOe) were obtained. Thermal transport characteristics were verified by Specific Absorption Rate (SAR) measurements using an AC magnetic field (f = 282 kHz). Differences and similarities in behavior will be discussed.

  6. Enhanced magnetic properties of NiO powders by the mechanical activation of aluminothermic reduction of NiO prepared by a ball milling process

    NASA Astrophysics Data System (ADS)

    Padhan, Aneeta Manjari; Ravikumar, P.; Saravanan, P.; Alagarsamy, Perumal

    2016-11-01

    We report the effect of mechanical activation on NiO-Al (x wt%) reduction reaction and resulting structural and magnetic properties by carrying out high-energy planetary ball milling. The pure NiO (un-milled) and milled NiO-Al (x≤2.5) powders exhibit face centered cubic structure, but the antiferromagnetic nature of pure NiO powder shows significant room temperature ferromagnetism with moderate moment and coercivity after milling due to non-stoichiometry in NiO caused by the defects, size reduction and oxidation of Ni. On the other hand, the addition of Al between 2.5 and 10% in NiO forms solid solution of NiO-Al with considerable reduction in the moment due to the atomic disorder. With increasing Al above 10%, NiO reduction reaction progresses gradually and as a result, the average magnetization increases from 0.57 to 4.3 emu/g with increasing Al up to 25%. A maximum of 91% reduction was observed for NiO-Al (40%) powders in 30 h of milling with a large increase in magnetization (~24 emu/g) along with the development of α-Al2O3. Thermomagnetization data reveal the presence of mixed magnetic phases in milled NiO powders and the component of induced ferromagnetic phase fades out with increasing Al due to the formation of Ni from the NiO-Al reduction reaction. The changes in the structural and magnetic properties are discussed on the basis of mechanical activation on the reduction of NiO by Al. The controlled reduction reaction with different Al content in NiO-Al is encouraging for the applications in catalysis and process of ore reduction.

  7. Effect of Gd-substitution on the ferroelectric and magnetic properties of BiFeO3 processed by high-energy ball milling

    NASA Astrophysics Data System (ADS)

    Sharma, Shiwani; Mishra, Alok; Saravanan, P.; Pandey, O. P.; Sharma, Puneet

    2016-11-01

    Multiferroic BiFeO3 was synthesized by means of high-energy ball milling (HEBM) followed by thermal annealing at various temperatures and the effect of Gd3+ substitution (x=0.0-0.20) at Bi3+ site was investigated in this study. It is found that the Gd-substitution tends to decrease the impurity phases and the crystallization of single phase BiFeO3 is observed at x=0.1. Scanning electron micrograph of Bi1-xGdxFeO3 sintered sample indicated a decrease in particle size and change in shape with increasing x. For all the studied samples, the measured dielectric constant values tend to increase from 110 (x=0.0) to 250 (x=0.10). The dielectric loss is found to be more for the pure BiFeO3 as compared to the Bi1-xGdxFeO3. Ferroelectric loops show a maximum polarization of 1.63 μC/cm2 for the Bi0.9Gd0.1FeO3. Magnetization (M) versus magnetic field (H) hysteresis loops at 300 K BiFeO3 and Bi0.9Gd0.1FeO3 demonstrated non-saturated loops, suggesting the antiferromagnetic nature of the samples. The M-H behavior of the Bi1-xGdxFeO3 at 300 K shows the antiferromagnetic nature of the samples. The estimated magnetization value at 10 kOe for the Bi0.9Gd0.1FeO3 sample (0.23 emu/g) is found to be higher than that of the pure BiFeO3 (0.037 emu/g).

  8. Cathode performance of LiMnPO 4/C nanocomposites prepared by a combination of spray pyrolysis and wet ball-milling followed by heat treatment

    NASA Astrophysics Data System (ADS)

    Doan, The Nam Long; Taniguchi, Izumi

    LiMnPO 4/C nanocomposites could be prepared by a combination of spray pyrolysis and wet ball-milling followed by heat treatment in the range of spray pyrolysis temperature from 200 to 500 °C. The ordered LiMnPO 4 olivine structure without any impurity phase could be identified by X-ray diffraction analysis for all samples. It could be also confirmed from scanning electron microscopy and transmission electron microscopy observations that the final samples were the LiMnPO 4/C nanocomposites with approximately 100 nm in primary particles size. The LiMnPO 4/C nanocomposite samples were used as cathode active materials for lithium batteries, and the electrochemical tests were carried out for the cell Li|1 M LiPF 6 in EC:DMC = 1:1|LiMnPO 4/C at various charge/discharge rates in three charge modes. As a result, the final sample which was synthesized at 300 °C by spray pyrolysis showed the best electrochemical performance due to the largest specific surface area, the smallest primary particle size and a well distribution of carbon. At galvanostatic charge/discharge rates of 0.05 C, the cell delivered first discharge capacities of 123 and 165 mAh g -1 in correspondence to charge cutoff voltages of 4.4 and 5.0 V, respectively. Furthermore, in a constant current-constant voltage charge mode at 4.4 V, the cells also exhibited initial discharge capacities of 147 mAh g -1 at 0.05 C, 145 mAh g -1 at 0.1 C, 123 mAh g -1 at 1 C and 65 mAh g -1 at 10 C. Moreover, the cells showed fair good cycleability over 100 cycles.

  9. Studies of superspin glass state and AC-losses in La0.7Sr0.3MnO3 nanoparticles obtained by high-energy ball-milling

    NASA Astrophysics Data System (ADS)

    Phong, P. T.; Manh, D. H.; Nguyen, L. H.; Tung, D. K.; Phuc, N. X.; Lee, I.-J.

    2014-11-01

    Single-phase perovskite compound La0.7Sr0.3MnO3 was synthesized by a high-energy ball milling method. Nanoparticle nature of this manganite with the average particle diameter of 11 nm was revealed from structure and morphology characterizations. The results of ac magnetic susceptibility measurements show that the system can be described as an ensemble of interacting magnetic nanoparticles, which indicates that the dipole-dipole interactions are strong enough to create superspin glass state in the sample. Furthermore, the specific loss power which is exhausted on the irradiation of an ensemble of particles with a magnetic field has been calculated and measured experimentally.

  10. Solution-state 2D NMR of ball-milled plant cell wall gels in DMSO-d6/pyridine-d5†

    PubMed Central

    Ralph, John

    2014-01-01

    NMR fingerprinting of the components of finely divided plant cell walls swelled in DMSO has been recently described. Cell wall gels, produced directly in the NMR tube with perdeutero-dimethylsulfoxide, allowed the acquisition of well resolved/dispersed 2D 13C–1H correlated solution-state NMR spectra of the entire array of wall polymers, without the need for component fractionation. That is, without actual solubilization, and without apparent structural modification beyond that inflicted by the ball milling and ultrasonication steps, satisfactorily interpretable spectra can be acquired that reveal compositional and structural details regarding the polysaccharide and lignin components in the wall. Here, the profiling method has been improved by using a mixture of perdeuterated DMSO and pyridine (4:1, v/v). Adding pyridine provided not only easier sample handling because of the better mobility compared to the DMSO-d6-only system but also considerably elevated intensities and improved resolution of the NMR spectra due to the enhanced swelling of the cell walls. This modification therefore provides a more rapid method for comparative structural evaluation of plant cell walls than is currently available. We examined loblolly pine (Pinus taeda, a gymnosperm), aspen (Populus tremuloides, an angiosperm), kenaf (Hibiscus cannabinus, an herbaceous plant), and corn (Zea mays L., a grass, i.e., from the Poaceae family). In principle, lignin composition (notably, the syringyl : guaiacyl : p-hydroxyphenyl ratio) can be quantified without the need for lignin isolation. Correlations for p-coumarate units in the corn sample are readily seen, and a variety of the ferulate correlations are also well resolved; ferulates are important components responsible for cell wall cross-linking in grasses. Polysaccharide anomeric correlations were tentatively assigned for each plant sample based on standard samples and various literature data. With the new potential for chemometric analysis

  11. Effects of processing parameters on the synthesis of (K0.5Na0.5)NbO3 nanopowders by reactive high-energy ball milling method.

    PubMed

    Nguyen, Duc Van

    2014-01-01

    The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C.

  12. Synthesis of SnFe2O4 Nanomaterials Via High Energy Ball Milling of SnO (Stannous) and α-Fe2O3 (Hematite) Solid Precursors

    NASA Astrophysics Data System (ADS)

    Uwakweh, Oswald N. C.; Más, Rita; Morales, Carolyn; Vargas, Pedro; Silva, Josue; Rosa, Angel; Lopez, Neshma; Moyet, Richard Perez; Cardona, Yenny

    2011-10-01

    The synthesis of single phase tin-ferrite, SnFe2O4, from tin (II) oxide or stannous oxide (SnO), and hematite (α-Fe2O3) solid precursors was carried out via high energy ball milling (HEBM) under wet condition involving the addition of controlled amounts of acetone. The stoichiometric amounts of the precursor materials were ball milled continuously for up to 22 h in a Spex-8000D mill using a ball-to-powder ratio of 40:1, with hardened stainless steel balls in WC-lined jars. The time-dependent formation of the SnFe2O4 based on combined X-ray diffraction and room temperature Mössbauer spectroscopy (MS) measurements revealed reaction enhancements associated with particles size reduction. The 22 h milled material indicated that synthesized SnFe2O4 had a particle size of 10.91 nm, coercivity of 4.44 mT, magnetic saturation/remanent ratio ( M r/ M s) of 0.085, while its superparamagnetic behavior was confirmed based on the combined MS and vibrating sample magnetometer measurements.

  13. Effects of Processing Parameters on the Synthesis of (K0.5Na0.5)NbO3 Nanopowders by Reactive High-Energy Ball Milling Method

    PubMed Central

    Duc Van, Nguyen

    2014-01-01

    The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C. PMID:24592146

  14. Characterization of Amorphous and Co-Amorphous Simvastatin Formulations Prepared by Spray Drying.

    PubMed

    Craye, Goedele; Löbmann, Korbinian; Grohganz, Holger; Rades, Thomas; Laitinen, Riikka

    2015-01-01

    In this study, spray drying from aqueous solutions, using the surface-active agent sodium lauryl sulfate (SLS) as a solubilizer, was explored as a production method for co-amorphous simvastatin-lysine (SVS-LYS) at 1:1 molar mixtures, which previously have been observed to form a co-amorphous mixture upon ball milling. In addition, a spray-dried formulation of SVS without LYS was prepared. Energy-dispersive X-ray spectroscopy (EDS) revealed that SLS coated the SVS and SVS-LYS particles upon spray drying. X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC) showed that in the spray-dried formulations the remaining crystallinity originated from SLS only. The best dissolution properties and a "spring and parachute" effect were found for SVS spray-dried from a 5% SLS solution without LYS. Despite the presence of at least partially crystalline SLS in the mixtures, all the studied formulations were able to significantly extend the stability of amorphous SVS compared to previous co-amorphous formulations of SVS. The best stability (at least 12 months in dry conditions) was observed when SLS was spray-dried with SVS (and LYS). In conclusion, spray drying of SVS and LYS from aqueous surfactant solutions was able to produce formulations with improved physical stability for amorphous SVS. PMID:26633346

  15. Amorphous red phosphorous embedded in carbon nanotubes scaffold as promising anode materials for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Yuan, Demao; Cheng, Jianli; Qu, Guoxing; Li, Xiaodong; Ni, Wei; Wang, Bin; Liu, Heng

    2016-01-01

    Amorphous red phosphorus/carbon nanotubes (ARPC) composites are prepared by planetary ball-milling technique with the pre-milling red phosphorus processes, consisting of uniformly distributing amorphous red phosphorus embedding in a three-dimensional conductive scaffold of interconnected carbon nanotubes (CNTs). Combining the three-dimensional conductive network with the amorphous red phosphorus can not only alleviate the volumetric change in the charging/discharging processes, but also provide conductive network for electron transport and dramatically improve the specific capacity, cycling stability and rate capability of the composite electrode. The ARPC composites deliver a high initial charge capacity of 2133.4 mAh g-1 at a current density of 0.05 C and maintain a reversible capacity of 998.5 mAh g-1 with a high Coulombic efficiency of approximately 99% after 50 cycles. Meanwhile, the composite can maintain high specific capacities of 1993.8 mAh g-1, 1896.9 mAh g-1, 1546.8 mAh g-1 and 816.6 mAh g-1 at 0.01 C, 0.05 C, 0.1 C and 0.5 C, respectively. Compared with that of the ball-milled amorphous red phosphorus with or without CNTs, the pre-milled ARPC composites show much better electrochemical performances.

  16. Inkjet-printed flexible organic thin-film thermoelectric devices based on p- and n-type poly(metal 1,1,2,2-ethenetetrathiolate)s/polymer composites through ball-milling

    PubMed Central

    Jiao, Fei; Di, Chong-an; Sun, Yimeng; Sheng, Peng; Xu, Wei; Zhu, Daoben

    2014-01-01

    In this article, we put forward a simple method for the synthesis of thermoelectric (TE) composite materials. Both n- and p-type composites were obtained by ball-milling the insoluble and infusible metal coordination polymers with other polymer solutions. The particle size, film morphology and composition were characterized by dynamic light scattering, scanning electron microscopy, transmission electron microscopy and energy-dispersive X-ray spectroscopy. The TE properties of the drop-cast composite film were measured at different temperatures. An inkjet-printed flexible device was fabricated and the output voltage and short-circuit current at various hot-side temperatures (Thot) and temperature gradients (ΔT) were tested. The composite material not only highly maintained the TE properties of the pristine material but also greatly improved its processability. This method can be extended to other insoluble and infusible TE materials for solution-processed flexible TE devices. PMID:24615147

  17. Effect of sintering in ball-milled K{sub 2}Bi{sub 8}Se{sub 13} thermoelectric nano-composites

    SciTech Connect

    Hatzikraniotis, E.; Ioannou, M.; Chrissafis, K.; Chung, D.Y.; Paraskevopoulos, K.M.; Kyratsi, Th.

    2012-09-15

    K{sub 2}Bi{sub 8}Se{sub 13} has many attractive features for thermoelectric applications. Recently, K{sub 2}Bi{sub 8}Se{sub 13}-based nanocomposite materials, consisting of nano-crystalline, micro-crystalline and amorphous phases, have been fabricated based on powder technology techniques. The Seebeck coefficient has been enhanced while the thermal conductivity has been decreased presenting, thus, interesting behavior. The behavior of the materials under heat treatment conditions is now of interest, as the application of sintering process is necessary for the development of thermoelectric modules. In this work, the crystallization of the K{sub 2}Bi{sub 8}Se{sub 13}-based nano-composites is studied using Differential Scanning Calorimetry. The results show that crystallization follows a multiple-step process with different activation energies. The thermoelectric properties are also discussed in the range that crystallization occurs. - Graphical Abstract: {beta}-K{sub 2}Bi{sub 8}Se{sub 13}-based nanocomposites follow a multiple-step crystallization process. Highlights: Black-Right-Pointing-Pointer K{sub 2}Bi{sub 8}Se{sub 13}-based composites consisting of nanocrystalline and amorphous phases. Black-Right-Pointing-Pointer Sintering results multiple-step crystallization with variable activation energies. Black-Right-Pointing-Pointer Thermoelectric properties follow a step-like behavior during sintering. Black-Right-Pointing-Pointer Properties are attributed to the strain relaxation, nucleation and grain growth.

  18. An x-ray photoemission electron microscopy study of the formation of Ti-Al phases in 4 mol% TiCl3 catalyzed NaAlH4 during high energy ball milling.

    PubMed

    Dobbins, Tabbetha; Abrecht, Mike; Uprety, Youaraj; Moore, Kristan

    2009-05-20

    This study reports reaction pathways to form TiAlx metallic complexes during the high energy ball milling of 4 mol% TiCl3 with NaAlH4 powders determined using local structure analysis of Tix+ and Alx+ species. Using x-ray photoemission electron microscopy (XPEEM) and x-ray diffraction (XRD), the oxidation state of Alx+ and Tix+ and the crystalline compounds existing in equilibrium with NaAlH4 were tracked for samples milled for times of 0 (i.e. mixing), 5, and 25 min. XPEEM analysis of the Al K edge after 5 min of milling reveals that Al remains in the 3+ oxidation state (i.e. in NaAlH4) around Ti0-rich regions of the sample. After 25 min of high energy milling, Ti0 has reacted with Al3+ (in nearby NaAlH4) to form TiAlx complexes. This study reports the pathway for TiAlx complex formation during milling of 4 mol% TiCl3catalyzed NaAlH4 to be as follows: (1) Ti3+ reduces to Ti0 (with Al3+ near Ti0 regions) and (2) Ti0 reacts with Al3+ in NaAlH4 to form TiAlx complexes.

  19. An x-ray photoemission electron microscopy study of the formation of Ti-Al phases in 4 mol% TiCl3 catalyzed NaAlH4 during high energy ball milling

    NASA Astrophysics Data System (ADS)

    Dobbins, Tabbetha; Abrecht, Mike; Uprety, Youaraj; Moore, Kristan

    2009-05-01

    This study reports reaction pathways to form TiAlx metallic complexes during the high energy ball milling of 4 mol% TiCl3 with NaAlH4 powders determined using local structure analysis of Tix+ and Alx+ species. Using x-ray photoemission electron microscopy (XPEEM) and x-ray diffraction (XRD), the oxidation state of Alx+ and Tix+ and the crystalline compounds existing in equilibrium with NaAlH4 were tracked for samples milled for times of 0 (i.e. mixing), 5, and 25 min. XPEEM analysis of the Al K edge after 5 min of milling reveals that Al remains in the 3+ oxidation state (i.e. in NaAlH4) around Ti0-rich regions of the sample. After 25 min of high energy milling, Ti0 has reacted with Al3+ (in nearby NaAlH4) to form TiAlx complexes. This study reports the pathway for TiAlx complex formation during milling of 4 mol% TiCl3 catalyzed NaAlH4 to be as follows: (1) Ti3+ reduces to Ti0 (with Al3+ near Ti0 regions) and (2) Ti0 reacts with Al3+ in NaAlH4 to form TiAlx complexes.

  20. Coexistence of short- and long-range ferromagnetic order in nanocrystalline Fe2Mn1-xCuxAl (x=0.0, 0.1 and 0.3) synthesized by high-energy ball milling

    NASA Astrophysics Data System (ADS)

    Thanh, Tran Dang; Nanto, Dwi; Tuyen, Ngo Thi Uyen; Nan, Wen-Zhe; Yu, YiKyung; Tartakovsky, Daniel M.; Yu, S. C.

    2015-11-01

    In this work, we prepared nanocrystalline Fe2Mn1-xCuxAl (x=0.0, 0.1 and 0.3) powders by the high energy ball milling technique, and then studied their critical properties. Our analysis reveals that the increase of Cu-doping concentration (up to x=0.3) in these powders leads to a gradual increase of the ferromagnetic-paramagnetic transition temperature from 406 to 452 K. The Banerjee criterion suggests that all the samples considered undergo a second-order phase transition. A modified Arrott plot and scaling analysis indicate that the critical exponents (β=0.419 and 0.442, γ=1.082 and 1.116 for x=0.0 and 0.1, respectively) are located in between those expected for the 3D-Heisenberg and the mean-field models; the values of β=0.495 and γ=1.046 for x=0.3 sample are very close to those of the mean-field model. These features reveal the coexistence of the short- and long-range ferromagnetic order in the nanocrystalline Fe2Mn1-xCuxAl powders. Particularly, as the concentration of Cu increases, values of the critical exponent shift towards those of the mean-field model. Such results prove the Cu doping favors establishing a long-range ferromagnetic order.

  1. The influence of amorphization methods on the apparent solubility and dissolution rate of tadalafil.

    PubMed

    Wlodarski, K; Sawicki, W; Paluch, K J; Tajber, L; Grembecka, M; Hawelek, L; Wojnarowska, Z; Grzybowska, K; Talik, E; Paluch, M

    2014-10-01

    This study for the first time investigates the solubility and dissolution rate of amorphous tadalafil (Td)--a poorly water soluble chemical compound which is commonly used for treating the erectile dysfunction. To convert the crystalline form of Td drug to its amorphous counterpart we have employed most of the commercially available amorphization techniques i.e. vitrification, cryogenic grinding, ball milling, spray drying, freeze drying and antisolvent precipitation. Among the mentioned methods only quenched cooling of the molten sample was found to be an inappropriate method of Td amorphization. This is due to the thermal decomposition of Td above 200°C, as proved by the thermogravimetric analysis (TGA). Disordered character of all examined samples was confirmed using differential scanning calorimetry (DSC) and X-ray powder diffraction (PXRD). In the case of most amorphous powders, the largest 3-fold increase of apparent solubility was observed after 5 min, indicating their fast recrystallization in water. On the other hand, the partially amorphous precipitate of Td and hypromellose enhanced the solubility of Td approximately 14 times, as compared with a crystalline substance, which remained constant for half an hour. Finally, disk intrinsic dissolution rate (DIDR) of amorphous forms of Td was also examined. PMID:24907679

  2. Connecting defects and amorphization in UiO-66 and MIL-140 metal–organic frameworks: a combined experimental and computational study.

    PubMed

    Bennett, Thomas D; Todorova, Tanya K; Baxter, Emma F; Reid, David G; Gervais, Christel; Bueken, Bart; Van de Voorde, B; De Vos, Dirk; Keen, David A; Mellot-Draznieks, Caroline

    2016-01-21

    The mechanism and products of the structural collapse of the metal–organic frameworks (MOFs) UiO-66, MIL-140B and MIL-140C upon ball-milling are investigated through solid state 13C NMR and pair distribution function (PDF) studies, finding amorphization to proceed by the breaking of a fraction of metal–ligand bonding in each case. The amorphous products contain inorganic–organic bonding motifs reminiscent of the crystalline phases. Whilst the inorganic Zr6O4(OH)4 clusters of UiO-66 remain intact upon structural collapse, the ZrO backbone of the MIL-140 frameworks undergoes substantial distortion. Density functional theory calculations have been performed to investigate defective models of MIL-140B and show, through comparison of calculated and experimental 13C NMR spectra, that amorphization and defects in the materials are linked. PMID:27144237

  3. Zn(1-x)Cu(x)O (0.02 ≤ x ≤ 0.1) Nanomaterials Prepared by Ball Milling, Citrate Sol Gel, and Molten Salt Flux Methods.

    PubMed

    Balamurugan, S; Melba, K

    2015-06-01

    The Cu doped ZnO, (Zn(1-x)Cu(x))O (x = 0.02, 0.04, 0.06, 0.08, and 0.1) nanomaterials were prepared by ball milling technique (BMT), citrate sol gel (CSG), and molten salt flux (MSF) methods. The various as-prepared (Zn(1-x)Cu(x))O materials were analyzed by powder X-ray diffraction (pXRD), FT-IR, and SEM-EDX measurements in order to check the phase formation, purity, surface morphology and elements present in the annealed materials. Due to the preparation methods as well as doping of 'x' slight variations in cell parameters are seen. The average crystalline size of CSG method shows smaller size (25-35 nm) than BMT and MSF approaches. The materials obtained by MSF technique reveal the average crystalline size in the range of 32-72 nm whereas the BMT materials exhibit 36-50 nm for the composition, 0.02 ≤ x ≤ 0.1. The presence of functional groups and the chemical bonding in (Zn(1-x)Cu(x))O system is confirmed through FT-IR measurements. It is evident from the FT-IR data that bands seen at 400-500 cm(-1) are characteristics of M-O (M = metal ion) bonding in the studied materials. The micro images observed by SEM exhibiting polycrystalline character as compared with the crystallite size obtained from XRD. Among the three approaches employed in the present investigations, in terms of average particle size the CSG method may be concluded as an efficient method for the preparation of Zn(1-x)Cu(x)O nanomaterials.

  4. Impact Ignition and Combustion Behavior of Amorphous Metal-Based Reactive Composites

    NASA Astrophysics Data System (ADS)

    Mason, Benjamin; Groven, Lori; Son, Steven

    2013-06-01

    Recently published molecular dynamic simulations have shown that metal-based reactive powder composites consisting of at least one amorphous component could lead to improved reaction performance due to amorphous materials having a zero heat of fusion, in addition to having high energy densities and potential uses such as structural energetic materials and enhanced blast materials. In order to investigate the feasibility of these systems, thermochemical equilibrium calculations were performed on various amorphous metal/metalloid based reactive systems with an emphasis on commercially available or easily manufactured amorphous metals, such as Zr and Ti based amorphous alloys in combination with carbon, boron, and aluminum. Based on the calculations and material availability material combinations were chosen. Initial materials were either mixed via a Resodyn mixer or mechanically activated using high energy ball milling where the microstructure of the milled material was characterized using x-ray diffraction, optical microscopy and scanning electron microscopy. The mechanical impact response and combustion behavior of select reactive systems was characterized using the Asay shear impact experiment where impact ignition thresholds, ignition delays, combustion velocities, and temperatures were quantified, and reported. Funding from the Defense Threat Reduction Agency (DTRA), Grant Number HDTRA1-10-1-0119. Counter-WMD basic research program, Dr. Suhithi M. Peiris, program director is gratefully acknowledged.

  5. Enhanced Physical Stability of Amorphous Drug Formulations via Dry Polymer Coating.

    PubMed

    Capece, Maxx; Davé, Rajesh

    2015-06-01

    Although amorphous solid drug formulations may be advantageous for enhancing the bioavailability of poorly soluble active pharmaceutical ingredients, they exhibit poor physical stability and undergo recrystallization. To address this limitation, this study investigates stability issues associated with amorphous solids through analysis of the crystallization behavior for acetaminophen (APAP), known as a fast crystallizer, using a modified form of the Avrami equation that kinetically models both surface and bulk crystallization. It is found that surface-enhanced crystallization, occurring faster at the free surface than in the bulk, is the major impediment to the stability of amorphous APAP. It is hypothesized that a novel use of a dry-polymer-coating process referred to as mechanical-dry-polymer-coating may be used to inhibit surface crystallization and enhance stability. The proposed process, which is examined, simultaneously mills and coats amorphous solids with polymer, while avoiding solvents or solutions, which may otherwise cause stability or crystallization issues during coating. It is shown that solid dispersions of APAP (64% loading) with a small particle size (28 μm) could be prepared and coated with the polymer, carnauba wax, in a vibratory ball mill. The resulting amorphous solid was found to have excellent stability as a result of inhibition of surface crystallization. PMID:25902736

  6. Enhanced Physical Stability of Amorphous Drug Formulations via Dry Polymer Coating.

    PubMed

    Capece, Maxx; Davé, Rajesh

    2015-06-01

    Although amorphous solid drug formulations may be advantageous for enhancing the bioavailability of poorly soluble active pharmaceutical ingredients, they exhibit poor physical stability and undergo recrystallization. To address this limitation, this study investigates stability issues associated with amorphous solids through analysis of the crystallization behavior for acetaminophen (APAP), known as a fast crystallizer, using a modified form of the Avrami equation that kinetically models both surface and bulk crystallization. It is found that surface-enhanced crystallization, occurring faster at the free surface than in the bulk, is the major impediment to the stability of amorphous APAP. It is hypothesized that a novel use of a dry-polymer-coating process referred to as mechanical-dry-polymer-coating may be used to inhibit surface crystallization and enhance stability. The proposed process, which is examined, simultaneously mills and coats amorphous solids with polymer, while avoiding solvents or solutions, which may otherwise cause stability or crystallization issues during coating. It is shown that solid dispersions of APAP (64% loading) with a small particle size (28 μm) could be prepared and coated with the polymer, carnauba wax, in a vibratory ball mill. The resulting amorphous solid was found to have excellent stability as a result of inhibition of surface crystallization.

  7. Aluminum Matrix Composites Strengthened with CuZrAgAl Amorphous Atomized Powder Particles

    NASA Astrophysics Data System (ADS)

    Dutkiewicz, Jan; Rogal, Łukasz; Wajda, Wojciech; Kukuła-Kurzyniec, Agata; Coddet, Christian; Dembinski, Lucas

    2015-06-01

    The Al-matrix composites were prepared by hot pressing in vacuum of an aluminum powder with 20 and 40 wt.% addition of the amorphous Cu43Zr43Ag7Al7 alloy (numbers indicate at.%) obtained using gas atomization method. The amorphous structure of the powder was confirmed using x-ray diffraction, DSC, and TEM. The average size of mostly spherical particles was 100 μm, so the powder was sieved to obtain maximum size of 60 μm. The composites were prepared using uniaxial cold pressing in vacuum and at a temperature of 400 °C. The composites of hardness from 43 to 53 HV were obtained for both additions of the amorphous phase. They reached compression strength of 150 MPa for 20% of amorphous phase and 250 MPa for the higher content. The modest hardening effect was caused by crack initiation at Al/amorphous interfaces. The amorphous phase was only partially crystallized in the hot-pressed composites, what did not cause hardness decrease. The application of nanocrystalline aluminum powders obtained by high-energy ball milling for the matrix of composites allowed obtaining nanocrystalline aluminum matrix composites of size near 150 nm, strengthened with the amorphous powders, whose compression strength was near 550 MPa for the composite containing 40% of the amorphous phase and slightly lower for the composite containing 20% of the phase. They showed much higher ductility of 23% in comparison with 7% for the composite containing 40% amorphous phase. The distribution of the strengthening phase in the nanocrystalline matrix was not homogeneous; the amorphous particles formed bands, where majority of cracks nucleated during compression test.

  8. M{umlt o}ssbauer investigation of intermixing during ball milling of Fe{sub 0.3}Cr{sub 0.7} and Fe{sub 0.5}W{sub 0.5} powder mixtures

    SciTech Connect

    Le Caeer, G.; Delcroix, P.; Shen, T.D.; Malaman, B.

    1996-11-01

    Intermixing of Fe and T (T=Cr,W) during ball milling of elemental powder mixtures Fe{sub 1{minus}x}T{sub x}, with x=0.70 for T=Cr and x=0.50 for T=W, has been followed by {sup 57}Fe M{umlt o}ssbauer spectroscopy at room temperature (RT) and by magnetization measurements for T=W. The chemical compositions have been chosen to yield final alloys or compounds which are nonmagnetic at RT to better follow the evolution of magnetic phases with milling times. For a long period of milling time t{sub m} before reaching the final stationary state, the hyperfine magnetic field distributions remain stationary in shape for both T=Cr and T=W. Only the relative weight of the magnetic contribution decreases with t{sub m}. For T=W, the average moment of magnetic Fe atoms is further shown to remain constant with t{sub m}. Stationary hyperfine field distribution shapes are found to be similar not only for {ital T}=Cr and W but also for T=Si (x=0.50) while published spectra suggest to add T=Al, Ti, V, Ta, Re to the latter nonexhaustive list. The stationary shape is characterized by a narrow peak located at a field close to the field of alpha iron at RT (330 kG) and by a broad, almost featureless, band from 50-100 kG to 300-320 kG. The broad band represents about 2/3 of the normalized field distribution. We deduce that the interpretation which consists in attributing the x-ray diffraction peaks of Fe-based bcc solid solutions to a single Fe-rich homogeneous solid solution must be done with care for intermediate milling times. We cannot infer from such hyperfine measurements a detailed description of the regions of the powders which are responsible for such magnetic features. We argue however that irregular interfaces between nanometer-sized Fe-rich zones and {ital T}-rich zones may play a role to explain the observed shape of the hyperfine field distributions.

  9. CONDENSED MATTER: STRUCTURE, MECHANICAL AND THERMAL PROPERTIES: Molecular Dynamics Study of Stability of Solid Solutions and Amorphous Phase in the Cu-Al System

    NASA Astrophysics Data System (ADS)

    Yang, Bin; Lai, Wen-Sheng

    2009-06-01

    The relative stability of fcc and bcc solid solutions and amorphous phase with different compositions in the Cu-Al system is studied by molecular dynamics simulations with n-body potentials. For Cu1-xAlx alloys, the calculations show that the fcc solid solution has the lowest energies in the composition region with x < 0.32 or x > 0.72, while the bee solid solution has the lowest energies in the central composition range, in agreement with the ball-milling experiments that a single bcc solid solution with 0.30 < x < 0.70 is obtained. The evolution of structures in solid solutions and amorphous phase is studied by the coordination number (CN) and bond-length analysis so as to unveil the underlying physics. It is found that the energy sequence among three phases is determined by the competition in energy change originating from the bond length and CNs (or the number of bonds).

  10. Microstructural characterization of Mg-based bulk metallic glass and nanocomposite

    SciTech Connect

    Babilas, Rafał; Nowosielski, Ryszard; Pawlyta, Mirosława; Fitch, Andy; Burian, Andrzej

    2015-04-15

    New magnesium-based bulk metallic glasses Mg{sub 60}Cu{sub 30}Y{sub 10} have been prepared by pressure casting. Glassy alloys were successfully annealed to become nanocomposite containing 200 nm crystallites in an amorphous matrix. The microstructure of bulk glassy alloy and nanocomposite obtained during heat treatment was examined by X-ray diffraction and scanning and high-resolution electron microscopy. Metallic glass has been also studied to explain the structural characteristics by the reverse Monte Carlo (RMC) modeling based on the diffraction data. The HRTEM images allow to indicate some medium-range order (MRO) regions about 2–3 nm in size and formation of local atomic clusters. The RMC modeling results confirmed some kinds of short range order (SRO) structures. It was found that the structure of bulk metallic glass formed by the pressure casting is homogeneous. The composite material contained very small particles in the amorphous matrix. Homogeneous glassy alloy had better corrosion resistance than a composite containing nanocrystalline particles in a glassy matrix. - Highlights: • RMC modeling demonstrates some kinds of SRO structures in Mg-based BMGs. • HRTEM indicated MRO regions about 2–3 nm and SRO regions about 0.5 nm in size. • Mg-based glassy alloys were successfully annealed to become nanocomposite material. • Crystalline particles have spherical morphology with an average diameter of 200 nm. • Glassy alloy had higher corrosion resistance than a nanocomposite sample.

  11. Influence of excipients in comilling on mitigating milling-induced amorphization or structural disorder of crystalline pharmaceutical actives.

    PubMed

    Balani, Prashant N; Ng, Wai Kiong; Tan, Reginald B H; Chan, Sui Yung

    2010-05-01

    The feasibility of using excipients to suppress the amorphization or structural disorder of crystalline salbutamol sulphate (SS) during milling was investigated. SS was subjected to ball-milling in the presence of alpha-lactose monohydrate (LAC), adipic acid (AA), magnesium stearate (MgSt), or polyvinyl pyrrolidone (PVP). X-ray powder diffraction, dynamic vapor sorption (DVS), high sensitivity differential scanning calorimetry (HSDSC) were used to analyze the crystallinity of the milled mixtures. Comilling with crystalline excipients, LAC, AA, and MgSt proved effective in reducing the amorphization of SS. LAC, AA, or MgSt acting as seed crystals to induce recrystallization of amorphous SS formed by milling. During comilling, both SS and LAC turned predominantly amorphous after 45 min but transformed back to a highly crystalline state after 60 min. Amorphous content was below the detection limits of DVS (0.5%) and HSDSC (5%). Comilled and physical mixtures of SS and ALM were stored under normal and elevated humidity conditions. This was found to prevent subsequent changes in crystallinity and morphology of comilled SS:LAC as compared to significant changes in milled SS and physical mixture. These results demonstrate a promising application of comilling with crystalline excipients in mitigating milling induced amorphization of pharmaceutical actives. PMID:19902526

  12. Impact of water on molecular dynamics of amorphous α-, β-, and γ-cyclodextrins studied by dielectric spectroscopy

    NASA Astrophysics Data System (ADS)

    Kaminski, K.; Adrjanowicz, K.; Kaminska, E.; Grzybowska, K.; Hawelek, L.; Paluch, M.; Tarnacka, M.; Gruszka, I.; Kasprzycka, A.

    2012-09-01

    Dielectric, calorimetric, and x-ray diffraction measurements were carried out on α-, β-, and γ-cyclodextrins, which are cyclic saccharides built by, respectively, six, seven, and eight glucose units connected via glycosidic linkage. Differential scanning calorimetry measurements indicated that each carbohydrate has a melting temperature located much above the temperature at which thermal decomposition begins. Moreover, calorimetric data revealed that it is possible to completely dehydrate each cyclodextrin by annealing them above 413 K. Unfortunately, it is impossible to obtain amorphous forms of cyclodextrin by simple cooling of the melt. Thus, a solid state amorphization method has been applied. X-ray diffraction studies demonstrated that by ball milling at room temperature we are able to obtain completely amorphous cyclodextrins. Finally, dielectric measurements were carried out to probe molecular dynamics in the amorphous state of cyclodextrins. It was found that there is only one relaxation process in amorphous hydrated cyclodextrins, while in dried samples two secondary relaxations are present. Moreover, we have shown that water has an enormous effect on the dynamics of both relaxation modes, i.e., with increasing content of water, the activation energy of the slow mode decreases, while that evaluated for the fast mode increases. We were not able to follow the dynamics of the structural relaxation process, because glass transition temperatures of amorphous cyclodextrins were found to lie above thermal degradation points.

  13. Formation of physically stable amorphous phase of ibuprofen by solid state milling with kaolin.

    PubMed

    Mallick, Subrata; Pattnaik, Satyanarayan; Swain, Kalpana; De, Pintu K; Saha, Arindam; Ghoshal, Gaurisankar; Mondal, Arijit

    2008-02-01

    Ibuprofen was milled in the solid state with kaolin (hydrated aluminium silicate) in different ratio to examine the extent of transformation from crystalline to amorphous state. The physical stability of the resultant drug was also investigated. X-ray powder diffractometry (XRD) and birefringence by Scanning Electron Microscopy (SEM) studies indicated almost complete amorphization of the drug on ball milling with kaolin at 1:2 ratio. Fourier transform infrared spectroscopy (FTIR) data showed a reduction in the absorbance of the free and the hydrogen-bonded acid carbonyl peak of carboxylic acid group accompanied by a corresponding increase in the absorbance of the carboxylate peak, indicating an acid-base reaction between the carboxylic acid containing ibuprofen and kaolin on milling. The extent of amorphization and reduction in the carbonyl peak and increase in carboxylate peak was a function of kaolin concentration in the milled powder. On storage of milled powder (at 40 degrees C and 75% RH for 10 weeks), XRD and birefringence of SEM study showed the absence of reversion to the crystalline state and FTIR data revealed continued reduction of carbonyl peak, whereas, ibuprofen converted from its crystalline acid form to amorphous salt form on milling with kaolin. Kaolin-bound state of ibuprofen was physically stable during storage. In-vitro dissolution studies revealed that percent release of ibuprofen from the kaolin co-milled powder is in the order: 1:2>1:1>1:0.5>1:0.1>milled alone ibuprofen>crystalline ibuprofen.

  14. Applicability of the one-step DVS method for the determination of amorphous amounts for further different hydrophilic and hydrophobic drugs.

    PubMed

    Müller, Thorsten; Scherließ, Regina; Schiewe, Jörg; Smal, Rüdiger; Weiler, Claudius; Steckel, Hartwig

    2015-08-01

    In a former publication the authors showed that low amounts of amorphous content (LOQ of 0.5%) in a hydrophobic model API (Ciclesonide) can be measured with an individually adjusted one-step dynamic organic vapor sorption (DVS). In this investigation the applicability is tested on various APIs which differ in lipophilicity (poor water solubility) and hygroscopicity (absorption of water). The vapor sorption method proved to be applicable in almost all cases. Moisture sorption isotherms were determined for all five investigated crystalline and amorphous APIs. However, it was necessary to select the parameters individually for each API. The used solvents (water, methanol, isopropanol and methylene chloride) and the humidity-levels (0.05 p/p0 until 0.5 p/p0) were chosen carefully because otherwise the amorphous amounts switch to their crystalline counterparts and are not detectable. The production of fully amorphous samples (absence of crystalline material measured by DSC, mDSC and XRPD) was optimized over several trials. As successfully methods proved ball-milling, freeze-drying, spray-drying and/or quench cooling. In the next step these fully amorphous amounts were blended with crystalline starting material to calibration curves (Turbula blender, influence of electrostatic charge to homogeneity) for the calculation of amorphous content. In summary, the following presented methods were used to determine and quantify low amorphous amounts (between 1.5% and 17.0%) in jet-milled powders (grinding pressure of 8bar, 1-3 grinding cycles), respectively.

  15. Improving Co-Amorphous Drug Formulations by the Addition of the Highly Water Soluble Amino Acid, Proline

    PubMed Central

    Jensen, Katrine Tarp; Löbmann, Korbinian; Rades, Thomas; Grohganz, Holger

    2014-01-01

    Co-amorphous drug amino acid mixtures were previously shown to be a promising approach to create physically stable amorphous systems with the improved dissolution properties of poorly water-soluble drugs. The aim of this work was to expand the co-amorphous drug amino acid mixture approach by combining the model drug, naproxen (NAP), with an amino acid to physically stabilize the co-amorphous system (tryptophan, TRP, or arginine, ARG) and a second highly soluble amino acid (proline, PRO) for an additional improvement of the dissolution rate. Co-amorphous drug-amino acid blends were prepared by ball milling and investigated for solid state characteristics, stability and the dissolution rate enhancement of NAP. All co-amorphous mixtures were stable at room temperature and 40 °C for a minimum of 84 days. PRO acted as a stabilizer for the co-amorphous system, including NAP–TRP, through enhancing the molecular interactions in the form of hydrogen bonds between all three components in the mixture. A salt formation between the acidic drug, NAP, and the basic amino acid, ARG, was found in co-amorphous NAP–ARG. In comparison to crystalline NAP, binary NAP–TRP and NAP–ARG, it could be shown that the highly soluble amino acid, PRO, improved the dissolution rate of NAP from the ternary co-amorphous systems in combination with either TRP or ARG. In conclusion, both the solubility of the amino acid and potential interactions between the molecules are critical parameters to consider in the development of co-amorphous formulations. PMID:25025400

  16. The Influence of Pressure on the Intrinsic Dissolution Rate of Amorphous Indomethacin

    PubMed Central

    Löbmann, Korbinian; Flouda, Konstantina; Qiu, Danwen; Tsolakou, Theodosia; Wang, Wenbo; Rades, Thomas

    2014-01-01

    New drug candidates increasingly tend to be poorly water soluble. One approach to increase their solubility is to convert the crystalline form of a drug into the amorphous form. Intrinsic dissolution testing is an efficient standard method to determine the intrinsic dissolution rate (IDR) of a drug and to test the potential dissolution advantage of the amorphous form. However, neither the United States Pharmacopeia (USP) nor the European Pharmacopeia (Ph.Eur) state specific limitations for the compression pressure in order to obtain compacts for the IDR determination. In this study, the influence of different compression pressures on the IDR was determined from powder compacts of amorphous (ball-milling) indomethacin (IND), a glass solution of IND and poly(vinylpyrrolidone) (PVP) and crystalline IND. Solid state properties were analyzed with X-ray powder diffraction (XRPD) and the final compacts were visually observed to study the effects of compaction pressure on their surface properties. It was found that there is no significant correlation between IDR and compression pressure for crystalline IND and IND–PVP. This was in line with the observation of similar surface properties of the compacts. However, compression pressure had an impact on the IDR of pure amorphous IND compacts. Above a critical compression pressure, amorphous particles sintered to form a single compact with dissolution properties similar to quench-cooled disc and crystalline IND compacts. In such a case, the apparent dissolution advantage of the amorphous form might be underestimated. It is thus suggested that for a reasonable interpretation of the IDR, surface properties of the different analyzed samples should be investigated and for amorphous samples the IDR should be measured also as a function of the compression pressure used to prepare the solid sample for IDR testing. PMID:25140536

  17. Phase transformation during mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si alloys

    SciTech Connect

    Amini, Rasool; Shamsipoor, Ali; Ghaffari, Mohammad; Alizadeh, Morteza; Okyay, Ali Kemal

    2013-10-15

    Mechano-synthesis of Fe–32Mn–6Si alloy by mechanical alloying of the elemental powder mixtures was evaluated by running the ball milling process under an inert argon gas atmosphere. In order to characterize the as-milled powders, powder sampling was performed at predetermined intervals from 0.5 to 192 h. X-ray florescence analyzer, X-ray diffraction, scanning electron microscope, and high resolution transmission electron microscope were utilized to investigate the chemical composition, structural evolution, morphological changes, and microstructure of the as-milled powders, respectively. According to the results, the nanocrystalline Fe–Mn–Si alloys were completely synthesized after 48 h of milling. Moreover, the formation of a considerable amount of amorphous phase during the milling process was indicated by quantitative X-ray diffraction analysis as well as high resolution transmission electron microscopy image and its selected area diffraction pattern. It was found that the α-to-γ and subsequently the amorphous-to-crystalline (especially martensite) phase transformation occurred by milling development. - Graphical abstract: Mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si shape memory alloys in the powder form: amorphous phase formation, α-to-γ phase transformation, mechano-crystallization of the amorphous, and martensite phase formation during the process. Highlights: • During MA, the α-to-γ phase transformation and amorphization occurred. • Mechano-crystallization of the amorphous phase occurred at sufficient milling time. • The formation of high amount of ε-martensite was evidenced at high milling times. • The platelet, spherical, and then irregular particle shapes was extended by MA. • By MA, the particles size was increased, then reduced, and afterward re-increased.

  18. Characterization and pharmacokinetic analysis of crystalline versus amorphous rapamycin dry powder via pulmonary administration in rats.

    PubMed

    Carvalho, Simone R; Watts, Alan B; Peters, Jay I; Liu, Sha; Hengsawas, Soraya; Escotet-Espinoza, Manuel S; Williams, Robert O

    2014-09-01

    The pharmacokinetics of inhaled rapamycin (RAPA) is compared for amorphous versus crystalline dry powder formulations. The amorphous formulation of RAPA and lactose (RapaLac) was prepared by thin film freezing (TFF) using lactose as the stabilizing agent in the weight ratio 1:1. The crystalline formulation was prepared by wet ball milling RAPA and lactose and posteriorly blending the mixture with coarse lactose (micronized RAPA/micronized lactose/coarse lactose=0.5:0.5:19). While both powders presented good aerosolization performance for lung delivery, TFF formulation exhibited better in vitro aerodynamic properties than the crystalline physical mixture. Single-dose 24h pharmacokinetic studies were conducted in Sprague-Dawley rats following inhalation of the aerosol mist in a nose-only inhalation exposure system. Lung deposition was higher for the crystalline group than for the TFF group. Despite higher pulmonary levels of drug that were found for the crystalline group, the systemic circulation (AUC₀₋₂₄) was higher for the amorphous group (8.6 ngh/mL) than for crystalline group (2.4 ngh/mL) based on a five-compartmental analysis. Lung level profiles suggest that TTF powder stays in the lung for the same period of time as the crystalline powder but it presented higher in vivo systemic bioavailability due to its enhanced solubility, faster dissolution rate and increased FPF at a more distal part of the lungs. PMID:24859653

  19. Magnetic Properties of Amorphous Fe-Si-B Powder Cores Mixed with Pure Iron Powder

    NASA Astrophysics Data System (ADS)

    Kim, Hyeon-Jun; Nam, Seul Ki; Kim, Kyu-Sung; Yoon, Sung Chun; Sohn, Keun-Yong; Kim, Mi-Rae; Sul Song, Yong; Park, Won-Wook

    2012-10-01

    Amorphous Fe-Si-B alloy was prepared by melt-spinning, and then the ribbons were pulverized and ball-milled to make the amorphous powder of ˜25 µm in size. Subsequently those were mixed with pure iron powders with an average particle size of 3 µm, and 1.5 wt % water glass diluted by distilled water at the ratio of 1:2. The powder mixtures were cold compacted at 650 MPa in toroid die, and heat treated at 430-440 °C under a nitrogen atmosphere for 1 h and 30 min, respectively. The soft magnetic properties of powder core were investigated using a B-H analyzer and a flux meter at the frequency range of ˜100 kHz. The microstructure was observed using scanning electron microscope (SEM), and the density of the core was measured using the principle of Archimedes. Based on the experimental results, the amorphous powder mixed with pure iron powder showed the improved powder compactability, which resulted in the increased permeability and the reduced core loss.

  20. 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.

  1. HRTEM studies of NiNbZr + Ag amorphous-nanocrystalline composites.

    PubMed

    Dutkiewicz, J; Lityńska-Dobrzyńska, L; Kovacova, A; Rogal, L; Maziarz, W

    2009-11-01

    Amorphous powder of composition corresponding to Ni60Ti20Zr20 (in at%) was obtained by ball milling in a high-energy mills starting from pure elements. Formation of the amorphous structure was observed already after 20 h of milling, although complete amorphization occurred after 40 h. The microhardness of powders increased from about 30 HV for pure elements to above 400 HV (1290 MPa) after 40 h of milling. Transmission electron microscopy (TEM) allowed to identify nanocrystalline inclusions of intermetallic phases of size 2-10 nm. Uniaxial hot pressing was performed in vacuum at temperature below the crystallization T(x) it is 510 degrees C and pressure of 600 MPa, Mixed amorphous powders and nanocrystalline silver powders were used to form a composite, in which microhardness was near 970 MPa HV and 400 HV for the amorphous phase and nanocrystalline silver, respectively. The compression strength of the composite containing 20 wt% of nanocrystalline Ag powder was equal to 600 MPa and plastic strain was 2%. Microstructure studies showed low porosity of composites of less than 1%, uniform distribution of the silver phase and a transition zone between both components, about 150 nm thick, where diffusion of nickel, niobium and zirconium into silver was observed. High-resolution TEM allowed identifying the structure of nanocrystalline inclusions in the amorphous matrix after hot pressing as either Ni(3)Zr or Ni(17)Nb(3). The identification was performed basing on measurements of angles and interatomic distances using inverse Fourier transformed images with enhanced contrast using Digital Micrograph computer program. PMID:19903239

  2. Micro-scale prediction method for API-solubility in polymeric matrices and process model for forming amorphous solid dispersion by hot-melt extrusion.

    PubMed

    Bochmann, Esther S; Neumann, Dirk; Gryczke, Andreas; Wagner, Karl G

    2016-10-01

    A new predictive micro-scale solubility and process model for amorphous solid dispersions (ASDs) by hot-melt extrusion (HME) is presented. It is based on DSC measurements consisting of an annealing step and a subsequent analysis of the glass transition temperature (Tg). The application of a complex mathematical model (BCKV-equation) to describe the dependency of Tg on the active pharmaceutical ingredient (API)/polymer ratio, enables the prediction of API solubility at ambient conditions (25°C). Furthermore, estimation of the minimal processing temperature for forming ASDs during HME trials could be defined and was additionally confirmed by X-ray powder diffraction data. The suitability of the DSC method was confirmed with melt rheological trials (small amplitude oscillatory system). As an example, ball milled physical mixtures of dipyridamole, indomethacin, itraconazole and nifedipine in poly(vinylpyrrolidone-co-vinylacetate) (copovidone) and polyvinyl caprolactam-polyvinyl acetate-polyethylene glycol graft copolymer (Soluplus®) were used.

  3. Amino acids as co-amorphous stabilizers for poorly water-soluble drugs--Part 2: molecular interactions.

    PubMed

    Löbmann, Korbinian; Laitinen, Riikka; Strachan, Clare; Rades, Thomas; Grohganz, Holger

    2013-11-01

    The formation of co-amorphous drug-drug mixtures has proved to be a powerful approach to stabilize the amorphous form and at the same time increase the dissolution of poorly water-soluble drugs. Molecular interactions in these co-amorphous formulations can play a crucial role in stabilization and dissolution enhancement. In this regard, Fourier-transform infrared spectroscopy (FTIR) is a valuable tool to analyze the molecular near range order of the compounds in the co-amorphous mixtures. In this study, several co-amorphous drugs--low molecular weight excipient blends--have been analyzed with FTIR spectroscopy. Molecular interactions of the drugs carbamazepine and indomethacin with the amino acids arginine, phenylalanine, and tryptophan were investigated. The amino acids were chosen from the biological target site of both drugs and prepared as co-amorphous formulations together with the drugs by vibrational ball milling. A detailed analysis of the FTIR spectra of these formulations revealed specific peak shifts in the vibrational modes of functional groups of drug and amino acid, as long as one amino acid from the biological target site was present in the blends. These peak shifts indicate that the drugs formed specific molecular interactions (hydrogen bonding and π-π interactions) with the amino acids. In the drug-amino acid mixtures that contained amino acids which were not present at the biological target site, no such interactions were identified. This study shows the potential of amino acids as small molecular weight excipients in co-amorphous formulations to stabilize the amorphous form of a poorly water-soluble drug through strong and specific molecular interactions with the drug.

  4. Surface functionalized amorphous nanosilica and microsilica with nanopores as promising tools in biomedicine

    NASA Astrophysics Data System (ADS)

    Rahman, Ayesha; Seth, Dipankar; Mukhopadhyaya, Sunit K.; Brahmachary, Ratan L.; Ulrichs, Christian; Goswami, Arunava

    2009-01-01

    Cellular interactions with engineered nanoparticles (NPs) are dependent on many properties, inherent to the nanoparticle (viz. size, shape, surface characteristics, degradation, agglomeration/dispersal, and charge, etc.). Modification of the surface reactivity via surface functionalization of the nanoparticles to be targeted seems to be important. Utilization of different surface functionalization methods of nanoparticles is an emerging field of basic and applied nanotechnology. It is well known that many disease-causing organisms induce host lipids and if deprived, their growth is inhibited in vivo. Amorphous nanosilica (ANS) and amorphous microsilica with nanopores (AMS) were prepared by a combination of wet chemistry and high-energy ball milling. Lipophilic moieties were attached to both ANS and AMS via chemical surface functionalization method. Lipophilic ANS and AMS were found to inhibit the growth of Bombyx mori nuclear polyhedrosis virus (BmNPV) and chicken malarial parasites via absorption of silkworm hemolymph and chicken serum lipids/lipoproteins, respectively, in vivo. Therefore, intelligent surface functionalization of NP is an important concept, and its application in curing chicken malaria and BmNPV is presented here. Surface functionalization method reported in this paper might serve as a valuable technology for treating many diseases where pathogens induce host lipid.

  5. Mg-based compounds for hydrogen and energy storage

    NASA Astrophysics Data System (ADS)

    Crivello, J.-C.; Denys, R. V.; Dornheim, M.; Felderhoff, M.; Grant, D. M.; Huot, J.; Jensen, T. R.; de Jongh, P.; Latroche, M.; Walker, G. S.; Webb, C. J.; Yartys, V. A.

    2016-02-01

    Magnesium-based alloys attract significant interest as cost-efficient hydrogen storage materials allowing the combination of high gravimetric storage capacity of hydrogen with fast rates of hydrogen uptake and release and pronounced destabilization of the metal-hydrogen bonding in comparison with binary Mg-H systems. In this review, various groups of magnesium compounds are considered, including (1) RE-Mg-Ni hydrides (RE = La, Pr, Nd); (2) Mg alloys with p-elements (X = Si, Ge, Sn, and Al); and (3) magnesium alloys with d-elements (Ti, Fe, Co, Ni, Cu, Zn, Pd). The hydrogenation-disproportionation-desorption-recombination process in the Mg-based alloys (LaMg12, LaMg11Ni) and unusually high-pressure hydrides synthesized at pressures exceeding 100 MPa (MgNi2H3) and stabilized by Ni-H bonding are also discussed. The paper reviews interrelations between the properties of the Mg-based hydrides and p- T conditions of the metal-hydrogen interactions, chemical composition of the initial alloys, their crystal structures, and microstructural state.

  6. Amorphization of ZrO2 + CeO2 Powders Through Mechanical Milling for the Use of Kinetic Spray

    NASA Astrophysics Data System (ADS)

    Li, Songlin; Wang, Lei; Xiong, Yuming; Bae, Gyuyeol; Lee, Changhee

    2013-12-01

    The coating formation in a kinetic spray process mainly depends on the impact of inflight particles at a high velocity. The plastic deformation at the impact interface would disrupt the native oxide scale on the particle and the substrate to generate the intimate contact of the atomic structures. Accordingly, it poses a challenge in producing ceramic coating during kinetic spray because of the lack of plasticity of ceramic powders at room temperature. In this study, we proposed to prepare ZrO2 ceramic coatings using partially amorphized powder with nanometer size in the kinetic spray process. To prepare the powder for the use of the kinetic spray, the amorphization and grain refinement of ZrO2 powder in mechanical ball milling were studied. The results showed that the amorphization and grain refinement were improved because of the formation of solid solution when the CeO2 agent was added. Subsequently, a nearly spherical powder was achieved via spray drying using the milled powders. The plasticity of the milled powders was tested in the kinetic spray process using Nitrogen as process gas. A dense ZrO2-CeO2 coating with a thickness of 50 μm was formed, whereas spraying milled ZrO2 powder can only lead to an inhomogeneous dispersion of the destructible particles on the surface of the substrate.

  7. Exploring several different routes to produce Mg- based nanomaterials for Hydrogen storage

    NASA Astrophysics Data System (ADS)

    Leiva, D. R.; Chanchetti, L. F.; Floriano, R.; Ishikawa, T. T.; Botta, W. J.

    2014-08-01

    Severe mechanical processing routes based on high-energy ball milling (HEBM) or severe plastic deformation (SPD) can be used to produce Mg nanomaterials for hydrogen storage applications. In the last few years, we have been exploring in our research group different SPD processing routes in Mg systems to achieve good activation (first hydrogenation) and fast H-absorption/desorption kinetics, combined with enhanced air resistance. In this paper, we compare SPD techniques applied to Mg with HEBM applied to MgH2. Both advanced - melt spinning (MS), high-pressure torsion (HPT) - and more conventional - cold rolling (CR), cold forging (CF)- techniques are evaluated as means of production of bulk samples with very refined microstructures and controlled textures. In the best SPD processing conditions, attractive H-absorption/desorption kinetic properties are obtained, which are comparable to the ones of MgH2 milled powders, even if the needed temperatures are higher - 350°C compared to 300°C.CR and CF stand out as the processes with higher potential for industrial application, considering the level of the attained hydrogen storage properties, its simplicity and low cost.

  8. Amorphic complexity

    NASA Astrophysics Data System (ADS)

    Fuhrmann, G.; Gröger, M.; Jäger, T.

    2016-02-01

    We introduce amorphic complexity as a new topological invariant that measures the complexity of dynamical systems in the regime of zero entropy. Its main purpose is to detect the very onset of disorder in the asymptotic behaviour. For instance, it gives positive value to Denjoy examples on the circle and Sturmian subshifts, while being zero for all isometries and Morse-Smale systems. After discussing basic properties and examples, we show that amorphic complexity and the underlying asymptotic separation numbers can be used to distinguish almost automorphic minimal systems from equicontinuous ones. For symbolic systems, amorphic complexity equals the box dimension of the associated Besicovitch space. In this context, we concentrate on regular Toeplitz flows and give a detailed description of the relation to the scaling behaviour of the densities of the p-skeletons. Finally, we take a look at strange non-chaotic attractors appearing in so-called pinched skew product systems. Continuous-time systems, more general group actions and the application to cut and project quasicrystals will be treated in subsequent work.

  9. Influence of small amorphous amounts in hydrophilic and hydrophobic APIs on storage stability of dry powder inhalation products.

    PubMed

    Müller, Thorsten; Krehl, Regina; Schiewe, Jörg; Weiler, Claudius; Steckel, Hartwig

    2015-05-01

    The effects of different manufacturing methods to induce formation of amorphous content, changes of physico-chemical characteristics of powder blends and changes of aerodynamic properties over storage time (6months) analyzed with the Next Generation Impactor (NGI) are investigated. Earlier studies have shown that standard pharmaceutical operations lead to structural disorders which may influence drug delivery and product stability. In this investigation, fully amorphous drug samples produced by spray-drying (SD) and ball-milling (BM) as well as semi-crystalline samples (produced by blending and micronization) are studied and compared to fully crystalline starting material. The amorphous content of these hydrophilic and hydrophobic active pharmaceutical ingredients (APIs) was determined using a validated one-step DVS-method. For the conducted blending and micronization tests, amorphous amounts up to a maximum of 5.1% for salbutamol sulfate (SBS) and 17.0% for ciclesonide (CS) were measured. In order to investigate the impact of small amorphous amounts, inhalable homogenous powder mixtures with very high and low amorphous content and a defined particle size were prepared with a Turbula blender for each API. These blends were stored (6months, 45% RH, room temperature) to evaluate the influence of amorphous amounts on storage stability. The fine particle fraction (FPF: % of emitted dose<5μm) was determined with the NGI at defined time points. The amorphous amounts showed a major effect on dispersion behavior, the mixtures of the two APIs showed differences at the beginning of the study and significant differences in storage stability. The FPF values for SBS decreased during storage (FPF: from 35% to <27%) for the blend with high amorphous amounts, in contrast the initially re-crystallized sample achieved a comparable constant level of about 25%. For the hydrophobic CS a constantly increasing FPF (from 6% to >15%) over storage time for both types of blends was

  10. Amino acids as co-amorphous stabilizers for poorly water soluble drugs--Part 1: preparation, stability and dissolution enhancement.

    PubMed

    Löbmann, Korbinian; Grohganz, Holger; Laitinen, Riikka; Strachan, Clare; Rades, Thomas

    2013-11-01

    Poor aqueous solubility of an active pharmaceutical ingredient (API) is one of the most pressing problems in pharmaceutical research and development because up to 90% of new API candidates under development are poorly water soluble. These drugs usually have a low and variable oral bioavailability, and therefore an unsatisfactory therapeutic effect. One of the most promising approaches to increase dissolution rate and solubility of these drugs is the conversion of a crystalline form of the drug into its respective amorphous form, usually by incorporation into hydrophilic polymers, forming glass solutions. However, this strategy only led to a small number of marketed products usually because of inadequate physical stability of the drug (crystallization). In this study, we investigated a fundamentally different approach to stabilize the amorphous form of drugs, namely the use of amino acids as small molecular weight excipients that form specific molecular interactions with the drug resulting in co-amorphous forms. The two poorly water soluble drugs carbamazepine and indomethacin were combined with amino acids from the binding sites of the biological receptors of these drugs. Mixtures of drug and the amino acids arginine, phenylalanine, tryptophan and tyrosine were prepared by vibrational ball milling. Solid-state characterization with X-ray powder diffraction (XRPD) and differential scanning calorimetry (DSC) revealed that the various blends could be prepared as homogeneous, single phase co-amorphous formulations indicated by the appearance of an amorphous halo in the XRPD diffractograms and a single glass transition temperature (Tg) in the DSC measurements. In addition, the Tgs of the co-amorphous mixtures were significantly increased over those of the individual drugs. The drugs remained chemically stable during the milling process and the co-amorphous formulations were generally physically stable over at least 6 months at 40 °C under dry conditions. The

  11. Synthesis of bulk nanostructured aluminum containing in situ crystallized amorphous particles

    NASA Astrophysics Data System (ADS)

    Zhang, Zhihui

    5083 Al containing in situ crystallized Al85Ni10La 5 amorphous particles (10% and 20% in volume fraction) was synthesized through a powder metallurgy route consisting of cold isostatic pressing, degassing and hot extrusion. The nanostructured 5083 Al powders (grain size ˜28 nm) were produced through mechanical milling in liquid nitrogen. The Al 85Ni10La5 powders were produced via gas atomization using helium gas and the fraction in the size range of <500 mesh (<25 mum), which appeared to be fully amorphous on the basis of X-ray diffraction studies, was isolated for further investigation. The amorphous Al85Ni10La5 alloy exhibited a glass transition at ˜259°C (at a heating rate of 40°C/min) and nanoscale crystallites (< 100 nm) with an equiaxed morphology formed during the subsequent crystallization reactions. At temperatures higher than 283°C, only the equilibrium phases Al, Al3Ni and Al11La 3 were formed. An unusually high nucleation density (1021-22 /m3) was recorded in the crystallization process. The copious nucleation sites were rationalized from the presence of quenched-in Al nuclei, which were evidenced by isothermal calorimetric tracing (235°C) and a direct HRTEM observation of the amorphous Al85Ni10La 5 powders. The feasibility of preparation of nanocrystalline/amorphous particles via melt spinning followed by ball milling was also studied. In the as-extruded composites, the amorphous Al85Ni10 La5 particles underwent complete crystallization resulting in a grain size of 100 ˜ 200 nm; the 5083 Al matrix had a grain size around 200 nm in the fine-grained region interspersed by coarse-grained region with a grain size of 600 ˜ 1500 nm. A metallurgical bond formed between the 5083 Al matrix and Al85Ni10La5 particles showing a grain-boundary-like interface. The compressive fracture strength of the as-extruded 10% and 20% Al85Ni10La5 composites were determined to be 1025 MPa and 837 MPa, respectively. The influence of secondary processing, i.e., swaging

  12. Amorphous metal composites

    DOEpatents

    Byrne, Martin A.; Lupinski, John H.

    1984-01-01

    An improved amorphous metal composite and process of making the composite. The amorphous metal composite comprises amorphous metal (e.g. iron) and a low molecular weight thermosetting polymer binder. The process comprises placing an amorphous metal in particulate form and a thermosetting polymer binder powder into a container, mixing these materials, and applying heat and pressure to convert the mixture into an amorphous metal composite.

  13. Chemical pretreatment of coal in a stirred ball mill

    SciTech Connect

    Birlingmair, D.; Chmielewski, T.; Pollard, J.

    1989-10-01

    Present studies on the electrochemical aspects of pyrite flotation in the presence of reducing agents were conducted to explain the effects observed during flotation of the separated organic and mineral-rich fractions of coal independently when sodium dithionite was used as an additive during and after grinding. In addition, the electrochemical phenomena occurring on the surface of pyrites of different origin was studied to aid in explaining the differences observed in the flotation of various coal-derived pyrite samples. Potentiometric and voltametric measurements have been conducted on electrodes prepared from natural pyrite samples of mineral and coal origin. Voltametric curves recorded on FeS{sub 2} electrodes indicate the presence of elemental sulfur, iron-oxy, and iron-hydroxy compounds, even on the freshly prepared surfaces. Comparison of voltametric curves with results of potentiometric measurements show that in the presence of dithionite several electrochemical processes are expected to take place on the pyrite surface. Voltametric curves recorded in solutions of different pH with and without sodium dithionite demonstrate that pyrite is a very good electrocatalyst in the anodic oxidation of dithionite. 13 refs., 12 figs.

  14. Amorphous Computing

    NASA Astrophysics Data System (ADS)

    Sussman, Gerald

    2002-03-01

    agents constructed by engineered cells, but we have few ideas for programming them effectively: How can one engineer prespecified, coherent behavior from the cooperation of immense numbers of unreliable parts that are interconnected in unknown, irregular, and time-varying ways? This is the challenge of Amorphous Computing.

  15. Nanocrystal dispersed amorphous alloys

    NASA Technical Reports Server (NTRS)

    Perepezko, John H. (Inventor); Allen, Donald R. (Inventor); Foley, James C. (Inventor)

    2001-01-01

    Compositions and methods for obtaining nanocrystal dispersed amorphous alloys are described. A composition includes an amorphous matrix forming element (e.g., Al or Fe); at least one transition metal element; and at least one crystallizing agent that is insoluble in the resulting amorphous matrix. During devitrification, the crystallizing agent causes the formation of a high density nanocrystal dispersion. The compositions and methods provide advantages in that materials with superior properties are provided.

  16. Hydrogen in amorphous silicon

    SciTech Connect

    Peercy, P. S.

    1980-01-01

    The structural aspects of amorphous silicon and the role of hydrogen in this structure are reviewed with emphasis on ion implantation studies. In amorphous silicon produced by Si ion implantation of crystalline silicon, the material reconstructs into a metastable amorphous structure which has optical and electrical properties qualitatively similar to the corresponding properties in high-purity evaporated amorphous silicon. Hydrogen studies further indicate that these structures will accomodate less than or equal to 5 at.% hydrogen and this hydrogen is bonded predominantly in a monohydride (SiH/sub 1/) site. Larger hydrogen concentrations than this can be achieved under certain conditions, but the excess hydrogen may be attributed to defects and voids in the material. Similarly, glow discharge or sputter deposited amorphous silicon has more desirable electrical and optical properties when the material is prepared with low hydrogen concentration and monohydride bonding. Results of structural studies and hydrogen incorporation in amorphous silicon were discussed relative to the different models proposed for amorphous silicon.

  17. Trehalose amorphization and recrystallization.

    PubMed

    Sussich, Fabiana; Cesàro, Attilio

    2008-10-13

    The stability of the amorphous trehalose prepared by using several procedures is presented and discussed. Amorphization is shown to occur by melting (T(m)=215 degrees C) or milling (room temperature) the crystalline anhydrous form TRE-beta. Fast dehydration of the di-hydrate crystalline polymorph, TRE-h, also produces an amorphous phase. Other dehydration procedures of TRE-h, such as microwave treatment, supercritical extraction or gentle heating at low scan rates, give variable fractions of the polymorph TRE-alpha, that undergo amorphization upon melting (at lower temperature, T(m)=130 degrees C). Additional procedures for amorphization, such as freeze-drying, spray-drying or evaporation of trehalose solutions, are discussed. All these procedures are classified depending on the capability of the undercooled liquid phase to undergo cold crystallization upon heating the glassy state at temperatures above the glass transition temperature (T(g)=120 degrees C). The recrystallizable amorphous phase is invariably obtained by the melt of the polymorph TRE-alpha, while other procedures always give an amorphous phase that is unable to crystallize above T(g). The existence of two different categories is analyzed in terms of the transformation paths and the hypothesis that the systems may exhibit different molecular mobilities.

  18. Amorphous diamond films

    DOEpatents

    Falabella, S.

    1998-06-09

    Amorphous diamond films having a significant reduction in intrinsic stress are prepared by biasing a substrate to be coated and depositing carbon ions thereon under controlled temperature conditions. 1 fig.

  19. Amorphous metal alloy

    DOEpatents

    Wang, R.; Merz, M.D.

    1980-04-09

    Amorphous metal alloys of the iron-chromium and nickel-chromium type have excellent corrosion resistance and high temperature stability and are suitable for use as a protective coating on less corrosion resistant substrates. The alloys are stabilized in the amorphous state by one or more elements of titanium, zirconium, hafnium, niobium, tantalum, molybdenum, and tungsten. The alloy is preferably prepared by sputter deposition.

  20. 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.

  1. Structural Amorphous Steels

    NASA Astrophysics Data System (ADS)

    Lu, Z. P.; Liu, C. T.; Thompson, J. R.; Porter, W. D.

    2004-06-01

    Recent advancement in bulk metallic glasses, whose properties are usually superior to their crystalline counterparts, has stimulated great interest in fabricating bulk amorphous steels. While a great deal of effort has been devoted to this field, the fabrication of structural amorphous steels with large cross sections has remained an alchemist’s dream because of the limited glass-forming ability (GFA) of these materials. Here we report the discovery of structural amorphous steels that can be cast into glasses with large cross-section sizes using conventional drop-casting methods. These new steels showed interesting physical, magnetic, and mechanical properties, along with high thermal stability. The underlying mechanisms for the superior GFA of these materials are discussed.

  2. Amorphous semiconductor solar cell

    DOEpatents

    Dalal, Vikram L.

    1981-01-01

    A solar cell comprising a back electrical contact, amorphous silicon semiconductor base and junction layers and a top electrical contact includes in its manufacture the step of heat treating the physical junction between the base layer and junction layer to diffuse the dopant species at the physical junction into the base layer.

  3. Amorphous silicon photovoltaic devices

    DOEpatents

    Carlson, David E.; Lin, Guang H.; Ganguly, Gautam

    2004-08-31

    This invention is a photovoltaic device comprising an intrinsic or i-layer of amorphous silicon and where the photovoltaic device is more efficient at converting light energy to electric energy at high operating temperatures than at low operating temperatures. The photovoltaic devices of this invention are suitable for use in high temperature operating environments.

  4. Mg-based multilayers and their thermal stabilities for EUV range

    NASA Astrophysics Data System (ADS)

    Zhu, Jingtao; Zhou, Sika; Li, Haochuan; Huang, Qiushi; Jiang, Li; Wang, Fengli; Zhang, Zhong; Wang, Zhanshan; Zhou, Hongjun; Huo, Tonglin

    2011-09-01

    We have investigated the optical properties and thermal stabilities of a serial of Mg-based multilayers including Mg/SiC, Mg/Co and Mg/Zr in extreme ultraviolet (EUV) range. Mg/X multilayer mirrors were deposited by magnetron sputtering technique onto polished silicon wafers. In order to study their stabilities under heat resistance, annealing experiments were carried out in vacuum environment keeping 1hour at different temperatures from 200°C to 550°C. Their EUV reflectivities were measured by using synchrotron radiation. Grazing incident X-ray and EUV reflection measurements were used to estimate the thermal stability of these multilayer systems. Mg/SiC and Mg/Co are stable up to 200°C and the reflectivity decreases drastically with the increase of temperature, while the reflectivity of Mg/Zr keeps constant during annealing at 300°C and falls slowly as the temperature increases. Up to 550°C, Bragg peaks of Mg/Zr multilayer are still sharp in X-ray reflectivity curve, and EUV reflectivity is 25% at 26.2nm at 30 degree incidence. These measurement results indicate that Mg/Co and Mg/SiC should be used in application requiring no heating above 200°C, while the new material combination Mg/Zr is a promising multilayer for practical application requiring stronger heat resistance in EUV range.

  5. Strengthening of Mg based alloy through grain refinement for orthopaedic application.

    PubMed

    Nayak, Soumyaranjan; Bhushan, Bharat; Jayaganthan, R; Gopinath, P; Agarwal, R D; Lahiri, Debrupa

    2016-06-01

    Magnesium is presently attracting a lot of interest as a replacement to clinically used orthopaedic implant materials, due to its ability to solve the stress shielding problems, biodegradability and osteocompatibility. However, the strength of Mg is still lower than the requirement and it becomes worse after it starts degrading fast, while being exposed in living body environment. This research explores the effectiveness of 'grain refinement through deformation', as a tool to modify the strength (while keeping elastic modulus unaffected) of Mg based alloys in orthopaedic application. Hot rolled Mg-3wt% Zn alloy (MZ3) has been investigated for its potential in orthopaedic implant. Microstructure, mechanical properties, bio-corrosion properties and biocompatibility of the rolled samples are probed into. Grain size gets refined significantly with increasing amount of deformation. The alloy experiences a marked improvement in hardness, yield strength, ultimate tensile strength, strain and toughness with finer grain size. An increment in accelerated corrosion rate is noted with decreasing grain size, which is correlated to the increased grain boundary area and mechano-chemical dissolution. However, immersion test in simulated body fluid (SBF) reveals reduction in corrosion rate after third day of immersion. This was possible owing to precipitation of protective hydroxyapatite (HA) layer, formed out of the interaction of SBF and the alloy. More nucleation sites at the grain boundary for fine grained samples help in forming more HA and thus reduce the corrosion rate. Human osteosarcoma cells show less viability and adhesion on grain refined alloy. PMID:26745721

  6. Amorphous silicon radiation detectors

    DOEpatents

    Street, R.A.; Perez-Mendez, V.; Kaplan, S.N.

    1992-11-17

    Hydrogenated amorphous silicon radiation detector devices having enhanced signal are disclosed. Specifically provided are transversely oriented electrode layers and layered detector configurations of amorphous silicon, the structure of which allow high electric fields upon application of a bias thereby beneficially resulting in a reduction in noise from contact injection and an increase in signal including avalanche multiplication and gain of the signal produced by incoming high energy radiation. These enhanced radiation sensitive devices can be used as measuring and detection means for visible light, low energy photons and high energy ionizing particles such as electrons, x-rays, alpha particles, beta particles and gamma radiation. Particular utility of the device is disclosed for precision powder crystallography and biological identification. 13 figs.

  7. Amorphous silicon radiation detectors

    DOEpatents

    Street, Robert A.; Perez-Mendez, Victor; Kaplan, Selig N.

    1992-01-01

    Hydrogenated amorphous silicon radiation detector devices having enhanced signal are disclosed. Specifically provided are transversely oriented electrode layers and layered detector configurations of amorphous silicon, the structure of which allow high electric fields upon application of a bias thereby beneficially resulting in a reduction in noise from contact injection and an increase in signal including avalanche multiplication and gain of the signal produced by incoming high energy radiation. These enhanced radiation sensitive devices can be used as measuring and detection means for visible light, low energy photons and high energy ionizing particles such as electrons, x-rays, alpha particles, beta particles and gamma radiation. Particular utility of the device is disclosed for precision powder crystallography and biological identification.

  8. Amorphous to amorphous transition in particle rafts

    NASA Astrophysics Data System (ADS)

    Varshney, Atul; Sane, A.; Ghosh, Shankar; Bhattacharya, S.

    2012-09-01

    Space-filling assemblies of athermal hydrophobic particles floating at an air-water interface, called particle rafts, are shown to undergo an unusual phase transition between two amorphous states, i.e., a low density “less-rigid” state and a high density “more-rigid” state, as a function of particulate number density (Φ). The former is shown to be a capillary bridged solid and the latter is shown to be a frictionally coupled one. Simultaneous studies involving direct imaging as well as measuring its mechanical response to longitudinal and shear stresses show that the transition is marked by a subtle structural anomaly and a weakening of the shear response. The structural anomaly is identified from the variation of the mean coordination number, mean area of the Voronoi cells, and spatial profile of the displacement field with Φ. The weakened shear response is related to local plastic instabilities caused by the depinning of the contact line of the underlying fluid on the rough surfaces of the particles.

  9. Amorphous to amorphous transition in particle rafts.

    PubMed

    Varshney, Atul; Sane, A; Ghosh, Shankar; Bhattacharya, S

    2012-09-01

    Space-filling assemblies of athermal hydrophobic particles floating at an air-water interface, called particle rafts, are shown to undergo an unusual phase transition between two amorphous states, i.e., a low density "less-rigid" state and a high density "more-rigid" state, as a function of particulate number density (Φ). The former is shown to be a capillary bridged solid and the latter is shown to be a frictionally coupled one. Simultaneous studies involving direct imaging as well as measuring its mechanical response to longitudinal and shear stresses show that the transition is marked by a subtle structural anomaly and a weakening of the shear response. The structural anomaly is identified from the variation of the mean coordination number, mean area of the Voronoi cells, and spatial profile of the displacement field with Φ. The weakened shear response is related to local plastic instabilities caused by the depinning of the contact line of the underlying fluid on the rough surfaces of the particles.

  10. Lightweight Mg-based composites with thermodynamically stable interfaces by in-situ combustion synthesis

    NASA Astrophysics Data System (ADS)

    Jo, Ilguk

    Lightweight Mg-based composites have been produced by in-situ combustion synthesis of the Al-Ti-C reaction system. The characteristics of the in-situ composites were investigated in terms of phase evolution and interfacial stability using various analysis techniques. The structural analysis results showed that full conversion of the Al-Ti-C reactants into spherical TiC reinforcements with sizes around 1mum was achieved by the combustion reaction. In-situ formed TiC had less oxygen and higher Al contents at the interface than ex-situ formed TiC; these clean interfaces with an Al layer on the reinforcements were shown to yield interfacial stability. For these reasons, the in-situ composites exhibited higher theoretical densities and also good mechanical properties compared with ex-situ produced composites. The interfacial characteristics of molten Mg with the Al-Ti-C reactants and the commercial TiC+Al substrates were evaluated using an infiltration technique under an argon atmosphere. Infiltration length increased with time at temperature, yielding activation energies (Ea) for each system. The value of Ea for the Al-Ti-C system (307.31kJ/mol) is lower than that for the other system (350.84kJ/mol); the high Ea value indicates that the infiltration is not a simple viscosity-controlled phenomenon but involves a chemical reaction. Formation of the Al3Ti phase was observed from the crystal structural analysis of the infiltrated area; thus, existence of reaction promoting the wetting of Mg. The phase evolution, reaction mechanism and kinetics of the Al-Ti-C reaction were studied using DSC and HT-XRD. It was confirmed that, along with the melting of Al, there was formation of Al3Ti by reaction between Al and Ti. A detailed structural analysis indicates that, the reaction mechanism involves melting of Al followed by formation and growth of Al 3Ti, which then contacts the graphite powder and initiates the combustion reaction. The effect of important process parameters, such

  11. 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.

  12. 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.

  13. 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.

  14. Bulk amorphous materials

    SciTech Connect

    Schwarz, R.B.; Archuleta, J.I.; Sickafus, K.E.

    1998-12-01

    This is the final report for a three-year, Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). The objective of this work was to develop the competency for the synthesis of novel bulk amorphous alloys. The authors researched their synthesis methods and alloy properties, including thermal stability, mechanical, and transport properties. The project also addressed the development of vanadium-spinel alloys for structural applications in hostile environments, the measurement of elastic constants and thermal expansion in single-crystal TiAl from 300 to 750 K, the measurement of elastic constants in gallium nitride, and a study of the shock-induced martensitic transformations in NiTi alloys.

  15. The effect of selected alloying element additions on properties of Mg-based alloy as bioimplants: A literature review

    NASA Astrophysics Data System (ADS)

    Zhang, Li-Nan; Hou, Zeng-Tao; Ye, Xin; Xu, Zhao-Bin; Bai, Xue-Ling; Shang, Peng

    2013-09-01

    This review investigates the current application limitations of Mg and Mg alloys. The key issues hindering the application of biodegradable Mg alloys as implants are their fast degradation rate and biological consideration. We have discussed the effect of some selected alloying element additions on the properties of the Mg-based alloy, especially the nutrient elements in human (Zn, Mn, Ca, Sr). Different grain sizes, phase constituents and distributions consequently influence the mechanical properties of the Mg alloys. Solution strengthening and precipitation strengthening are enhanced by the addition of alloying elements, generally improving the mechanical properties. Besides, the hot working process can also improve the mechanical properties. Combination of different processing steps is suggested to be adopted in the fabrication of Mg-based alloys. Corrosion properties of these Mg-based alloys have been measured in vitro and in vivo. The degradation mechanism is also discussed in terms of corrosion types, rates, byproducts and response of the surrounding tissues. Moreover, the clinical response and requirements of degradable implants are presented, especially for the nutrient elements (Ca, Mn, Zn, Sr). This review provides information related to different Mg alloying elements and presents the promising candidates for an ideal implant.

  16. Processing of amorphous PEEK and amorphous PEEK based composites

    SciTech Connect

    Kenny, J.; D'amore, A.; Nicolais, L.; Iannone, M.; Scatteia, B.; Aeritalia, S.p.A., Naples )

    1989-08-01

    An analysis of the crystallization behavior of amorphous PEEK, its carbon fiber composite, and its relationships with dynamic-mechanical properties of the system measured during and after processing is presented. The effect of the processing conditions, time and temperature, on the quality and on the amount of the crystallinity developed during cold crystallization has been investigated in order to evaluate the processability window of amorphous PEEK and amorphous PEEK based composite above the glass transition temperature and below the melting point. Also, the anomalous behavior of the amorphous matrix, crystallized at low temperatures, has been studied. Multiple melting peaks and changes of the glass transition during crystallization are explained in terms of crystalline morphology and molecular mobility. 20 refs.

  17. Apatite Formation from Amorphous Calcium Phosphate and Mixed Amorphous Calcium Phosphate/Amorphous Calcium Carbonate.

    PubMed

    Ibsen, Casper J S; Chernyshov, Dmitry; Birkedal, Henrik

    2016-08-22

    Crystallization from amorphous phases is an emerging pathway for making advanced materials. Biology has made use of amorphous precursor phases for eons and used them to produce structures with remarkable properties. Herein, we show how the design of the amorphous phase greatly influences the nanocrystals formed therefrom. We investigate the transformation of mixed amorphous calcium phosphate/amorphous calcium carbonate phases into bone-like nanocrystalline apatite using in situ synchrotron X-ray diffraction and IR spectroscopy. The speciation of phosphate was controlled by pH to favor HPO4 (2-) . In a carbonate free system, the reaction produces anisotropic apatite crystallites with large aspect ratios. The first formed crystallites are highly calcium deficient and hydrogen phosphate rich, consistent with thin octacalcium phosphate (OCP)-like needles. During growth, the crystallites become increasingly stoichiometric, which indicates that the crystallites grow through addition of near-stoichiometric apatite to the OCP-like initial crystals through a process that involves either crystallite fusion/aggregation or Ostwald ripening. The mixed amorphous phases were found to be more stable against phase transformations, hence, the crystallization was inhibited. The resulting crystallites were smaller and less anisotropic. This is rationalized by the idea that a local phosphate-depletion zone formed around the growing crystal until it was surrounded by amorphous calcium carbonate, which stopped the crystallization. PMID:27460160

  18. Fabrication of amorphous diamond films

    DOEpatents

    Falabella, S.

    1995-12-12

    Amorphous diamond films having a significant reduction in intrinsic stress are prepared by biasing a substrate to be coated and depositing carbon ions thereon under controlled temperature conditions. 1 fig.

  19. Amorphous metal alloy and composite

    DOEpatents

    Wang, Rong; Merz, Martin D.

    1985-01-01

    Amorphous metal alloys of the iron-chromium and nickel-chromium type have excellent corrosion resistance and high temperature stability and are suitable for use as a protective coating on less corrosion resistant substrates. The alloys are stabilized in the amorphous state by one or more elements of titanium, zirconium, hafnium, niobium, tantalum, molybdenum, and tungsten. The alloy is preferably prepared by sputter deposition.

  20. Bulk superhard B-C-N nanocomposite compact and method for preparing thereof

    DOEpatents

    Zhao, Yusheng; He, Duanwei

    2004-07-06

    Bulk, superhard, B-C-N nanocomposite compact and method for preparing thereof. The bulk, superhard, nanocomposite compact is a well-sintered compact and includes nanocrystalline grains of at least one high-pressure phase of B-C-N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compact has a Vicker's hardness of about 41-68 GPa. It is prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture, and sintering the encapsulated ball-milled mixture at a pressure of about 5-25 GPa and at a temperature of about 1000-2500 K.

  1. New horizon for high performance Mg-based biomaterial with uniform degradation behavior: Formation of stacking faults.

    PubMed

    Zhang, Jinghuai; Xu, Chi; Jing, Yongbin; Lv, Shuhui; Liu, Shujuan; Fang, Daqing; Zhuang, Jinpeng; Zhang, Milin; Wu, Ruizhi

    2015-01-01

    Designing the new microstructure is an effective way to accelerate the biomedical application of magnesium (Mg) alloys. In this study, a novel Mg-8Er-1Zn alloy with profuse nano-spaced basal plane stacking faults (SFs) was prepared by combined processes of direct-chill semi-continuous casting, heat-treatment and hot-extrusion. The formation of SFs made the alloy possess outstanding comprehensive performance as the biodegradable implant material. The ultimate tensile strength (UTS: 318 MPa), tensile yield strength (TYS: 207 MPa) and elongation (21%) of the alloy with SFs were superior to those of most reported degradable Mg-based alloys. This new alloy showed acceptable biotoxicity and degradation rate (0.34 mm/year), and the latter could be further slowed down through optimizing the microstructure. Most amazing of all, the uniquely uniform in vitro/vivo corrosion behavior was obtained due to the formation of SFs. Accordingly we proposed an original corrosion mechanism for the novel Mg alloy with SFs. The present study opens a new horizon for developing new Mg-based biomaterials with highly desirable performances. PMID:26349676

  2. New horizon for high performance Mg-based biomaterial with uniform degradation behavior: Formation of stacking faults

    PubMed Central

    Zhang, Jinghuai; Xu, Chi; Jing, Yongbin; Lv, Shuhui; Liu, Shujuan; Fang, Daqing; Zhuang, Jinpeng; Zhang, Milin; Wu, Ruizhi

    2015-01-01

    Designing the new microstructure is an effective way to accelerate the biomedical application of magnesium (Mg) alloys. In this study, a novel Mg–8Er–1Zn alloy with profuse nano-spaced basal plane stacking faults (SFs) was prepared by combined processes of direct-chill semi-continuous casting, heat-treatment and hot-extrusion. The formation of SFs made the alloy possess outstanding comprehensive performance as the biodegradable implant material. The ultimate tensile strength (UTS: 318 MPa), tensile yield strength (TYS: 207 MPa) and elongation (21%) of the alloy with SFs were superior to those of most reported degradable Mg-based alloys. This new alloy showed acceptable biotoxicity and degradation rate (0.34 mm/year), and the latter could be further slowed down through optimizing the microstructure. Most amazing of all, the uniquely uniform in vitro/vivo corrosion behavior was obtained due to the formation of SFs. Accordingly we proposed an original corrosion mechanism for the novel Mg alloy with SFs. The present study opens a new horizon for developing new Mg-based biomaterials with highly desirable performances. PMID:26349676

  3. New horizon for high performance Mg-based biomaterial with uniform degradation behavior: Formation of stacking faults.

    PubMed

    Zhang, Jinghuai; Xu, Chi; Jing, Yongbin; Lv, Shuhui; Liu, Shujuan; Fang, Daqing; Zhuang, Jinpeng; Zhang, Milin; Wu, Ruizhi

    2015-09-09

    Designing the new microstructure is an effective way to accelerate the biomedical application of magnesium (Mg) alloys. In this study, a novel Mg-8Er-1Zn alloy with profuse nano-spaced basal plane stacking faults (SFs) was prepared by combined processes of direct-chill semi-continuous casting, heat-treatment and hot-extrusion. The formation of SFs made the alloy possess outstanding comprehensive performance as the biodegradable implant material. The ultimate tensile strength (UTS: 318 MPa), tensile yield strength (TYS: 207 MPa) and elongation (21%) of the alloy with SFs were superior to those of most reported degradable Mg-based alloys. This new alloy showed acceptable biotoxicity and degradation rate (0.34 mm/year), and the latter could be further slowed down through optimizing the microstructure. Most amazing of all, the uniquely uniform in vitro/vivo corrosion behavior was obtained due to the formation of SFs. Accordingly we proposed an original corrosion mechanism for the novel Mg alloy with SFs. The present study opens a new horizon for developing new Mg-based biomaterials with highly desirable performances.

  4. Nanostructures having crystalline and amorphous phases

    DOEpatents

    Mao, Samuel S; Chen, Xiaobo

    2015-04-28

    The present invention includes a nanostructure, a method of making thereof, and a method of photocatalysis. In one embodiment, the nanostructure includes a crystalline phase and an amorphous phase in contact with the crystalline phase. Each of the crystalline and amorphous phases has at least one dimension on a nanometer scale. In another embodiment, the nanostructure includes a nanoparticle comprising a crystalline phase and an amorphous phase. The amorphous phase is in a selected amount. In another embodiment, the nanostructure includes crystalline titanium dioxide and amorphous titanium dioxide in contact with the crystalline titanium dioxide. Each of the crystalline and amorphous titanium dioxide has at least one dimension on a nanometer scale.

  5. Ball-milling modification of single-walled carbon nanotubes: purification, cutting, and functionalization.

    PubMed

    Rubio, Noelia; Fabbro, Chiara; Herrero, M Antonia; de la Hoz, Antonio; Meneghetti, Moreno; Fierro, Jose L G; Prato, Maurizio; Vázquez, Ester

    2011-03-01

    Single-walled carbon nanotubes (SWNTs) can be successfully cut with relatively homogeneous sizes using a planetary mill. The optimized conditions produce highly dispersible SWNTs that can be efficiently functionalized in a variety of synthetic ways. As clearly shown by Raman spectroscopy, the milling/cutting procedure compares very favorably with the most common way of purifying SWNTs, namely, treatment with strong oxidizing acids. Moreover a similar milling process can be used to functionalize and cut pristine SWNTs by one-step nitrene chemistry. PMID:21290599

  6. Optimizing particle size reduction of biochar using a planetary ball mill

    Technology Transfer Automated Retrieval System (TEKTRAN)

    With world demand for fossil fuels consistently growing, reducing our dependence on petroleum products is a necessary strategy. Our research group is currently studying the feasibility of biochar as rubber composite filler. If biochar can be used as a partial or complete substitute for carbon black ...

  7. Mechanochemical Strecker Reaction: Access to α-Aminonitriles and Tetrahydroisoquinolines under Ball-Milling Conditions.

    PubMed

    Hernández, José G; Turberg, Mathias; Schiffers, Ingo; Bolm, Carsten

    2016-10-01

    A mechanochemical version of the Strecker reaction for the synthesis of α-aminonitriles was developed. The milling of aldehydes, amines, and potassium cyanide in the presence of SiO2 gave the corresponding α-aminonitriles in good to high yields. The high efficiency of the mechanochemical Strecker-type multicomponent reaction allowed the one-pot synthesis of tetrahydroisoquinolines after a subsequent internal N-alkylation reaction.

  8. Degradation of trichloroethene with a noval ball milled Fe-C nanocomposite

    SciTech Connect

    Gao, Jie; Wang, Wei; Rondinone, Adam Justin; He, Feng; Liang, Liyuan

    2015-07-18

    Nanoscale zero-valent iron (NZVI) is effective in reductively degrading dense non-aqueous phase liquids (DNAPLs), such as trichloroethene (TCE), in groundwater (i.e., dechlorination) although the NZVI technology itself still suffers from high material costs and inability to target hydrophobic contaminants in source zones. To address these problems, we developed a novel, inexpensive iron-carbon (Fe-C) nanocomposite material by simultaneously milling micron-size iron and activated carbon powder. Microscopic and X-ray diffraction (XRD) characterization of the composite material revealed that nanoparticles of Fe were dispersed in activated carbon and a new iron carbide phase was formed. Bench-scale studies showed that this material instantaneously sorbed >90% of TCE from aqueous solutions and subsequently decomposed TCE into non-chlorinated products. Compared to milled Fe, Fe-C nanocomposite dechlorinated TCE at a slightly slower rate and favored the production of ethene over other TCE degradation products such as C3-C6 compounds. When placed in hexane-water mixture, the Fe-C nanocomposite materials are preferentially partitioned into the organic phase, indicating the ability of the composite materials to target DNAPL during remediation.

  9. Degradation of trichloroethene with a noval ball milled Fe-C nanocomposite

    DOE PAGES

    Gao, Jie; Wang, Wei; Rondinone, Adam Justin; He, Feng; Liang, Liyuan

    2015-07-18

    Nanoscale zero-valent iron (NZVI) is effective in reductively degrading dense non-aqueous phase liquids (DNAPLs), such as trichloroethene (TCE), in groundwater (i.e., dechlorination) although the NZVI technology itself still suffers from high material costs and inability to target hydrophobic contaminants in source zones. To address these problems, we developed a novel, inexpensive iron-carbon (Fe-C) nanocomposite material by simultaneously milling micron-size iron and activated carbon powder. Microscopic and X-ray diffraction (XRD) characterization of the composite material revealed that nanoparticles of Fe were dispersed in activated carbon and a new iron carbide phase was formed. Bench-scale studies showed that this material instantaneously sorbedmore » >90% of TCE from aqueous solutions and subsequently decomposed TCE into non-chlorinated products. Compared to milled Fe, Fe-C nanocomposite dechlorinated TCE at a slightly slower rate and favored the production of ethene over other TCE degradation products such as C3-C6 compounds. When placed in hexane-water mixture, the Fe-C nanocomposite materials are preferentially partitioned into the organic phase, indicating the ability of the composite materials to target DNAPL during remediation.« less

  10. Chemical reactions of metal powders with organic and inorganic liquids during ball milling

    NASA Technical Reports Server (NTRS)

    Arias, A.

    1975-01-01

    Chromium and/or nickel powders were milled in metal chlorides and in organic liquids representative of various functional groups. The powders always reacted with the liquid and became contaminated with elements from them. The milled powders had specific surface areas ranging from 0.14 to 37 sq m/g, and the total contamination with elements from the milling liquid ranged from 0.01 to 56 weight percent. Compounds resulting from substitution, addition, or elimination reactions formed in or from the milling liquid.

  11. Nanocomposite formation in haematite-Mg, Ti system induced by high-energy ball milling.

    PubMed

    Lee, Chung-Hyo

    2013-06-01

    Reactant materials of haematite and Mg, Ti powders have been milled, where pure metals are used as reducing agent. It is found that nanocomposite powders in which MgO and TiO2 are dispersed in alpha-Fe matrix with nano-sized grains are obtained by MA of Fe2O3 with Mg and Ti for 30 min and 5 hours, respectively. It is suggested that the shorter MA time for the nanocomposite formation in Fe2O3-Mg is due to a larger negative heat associated with the chemical reduction of reactant materials. X-ray diffraction results show that the average grain size of alpha-Fe in alpha-Fe/TiO2 nanocomposite powders is in the range of 40 nm. From magnetic measurement, we can also obtain indirect information about the details of the solid-state reduction process during MA.

  12. Degradation of Trichloroethene with a Novel Ball Milled Fe-C Nanocomposite.

    PubMed

    Gao, Jie; Wang, Wei; Rondinone, Adam J; He, Feng; Liang, Liyuan

    2015-12-30

    Nanoscale zero-valent iron (NZVI) is effective in reductively degrading dense non-aqueous phase liquids (DNAPLs), such as trichloroethene (TCE), in groundwater (i.e., dechlorination) although the NZVI technology itself still suffers from high material costs and inability to target hydrophobic contaminants in source zones. To address these problems, we developed a novel, inexpensive iron-carbon (Fe-C) nanocomposite material by simultaneously milling micron-size iron and activated carbon powder. Microscopic and X-ray diffraction (XRD) characterization of the composite material revealed that nanoparticles of Fe were dispersed in activated carbon and a new iron carbide phase was formed. Bench-scale studies showed that this material instantaneously sorbed >90% of TCE from aqueous solutions and subsequently decomposed TCE into non-chlorinated products. Compared to milled Fe, Fe-C nanocomposite dechlorinated TCE at a slightly slower rate and favored the production of ethene over other TCE degradation products such as C3--C6 compounds. When placed in hexane-water mixture, the Fe-C nanocomposite materials are preferentially partitioned into the organic phase, indicating the ability of the composite materials to target DNAPL during remediation.

  13. Amorphous-diamond electron emitter

    DOEpatents

    Falabella, Steven

    2001-01-01

    An electron emitter comprising a textured silicon wafer overcoated with a thin (200 .ANG.) layer of nitrogen-doped, amorphous-diamond (a:D-N), which lowers the field below 20 volts/micrometer have been demonstrated using this emitter compared to uncoated or diamond coated emitters wherein the emission is at fields of nearly 60 volts/micrometer. The silicon/nitrogen-doped, amorphous-diamond (Si/a:D-N) emitter may be produced by overcoating a textured silicon wafer with amorphous-diamond (a:D) in a nitrogen atmosphere using a filtered cathodic-arc system. The enhanced performance of the Si/a:D-N emitter lowers the voltages required to the point where field-emission displays are practical. Thus, this emitter can be used, for example, in flat-panel emission displays (FEDs), and cold-cathode vacuum electronics.

  14. Annealing studies of amorphous alloys

    SciTech Connect

    Wiley, J.D.; Perepezko, J.H.; Nordman, J.E.

    1983-04-01

    Amorphous films of the alloys Ni-Nb, Ni-Mo, Mo-Si, and W-Si were sputter deposited on single-crystal semiconductor substrates. One-hour crystallization temperatures of the films were determined to within +-25/sup 0/C by annealing and x-ray diffraction measurements. Interdiffusion between Au or Cu overlayers and the amorphous films were studied by annealing combined with Auger Electron Spectroscopy (AES) profiling, and by Rutherford Backscatter (RBS) analysis. Supplementary measurements used to study structural relaxation and crystallization included resistivity as a function of temperature; DTA and DSC; and electron microscopy.

  15. Comparison of Mg-based multilayers for solar He II radiation at 30.4 nm wavelength

    SciTech Connect

    Zhu Jingtao; Zhou Sika; Li Haochuan; Huang Qiushi; Wang Zhanshan; Le Guen, Karine; Hu, Min-Hui; Andre, Jean-Michel; Jonnard, Philippe

    2010-07-10

    Mg-based multilayers, including SiC/Mg, Co/Mg, B4C/Mg, and Si/Mg, are investigated for solar imaging and a He II calibration lamp at a 30.4 nm wavelength. These multilayers were fabricated by a magnetron sputtering method and characterized by x-ray reflection. The reflectivities of these multilayers were measured by synchrotron radiation. Near-normal-incidence reflectivities of Co/Mg and SiC/Mg multilayer mirrors are as high as 40.3% and 44.6%, respectively, while those of B4C/Mg and Si/Mg mirrors are too low for application. The measured results suggest that SiC/Mg, Co/Mg multilayers are promising for a 30.4 nm wavelength.

  16. Imprinting bulk amorphous alloy at room temperature

    PubMed Central

    Kim, Song-Yi; Park, Eun-Soo; Ott, Ryan T.; Lograsso, Thomas A.; Huh, Moo-Young; Kim, Do-Hyang; Eckert, Jürgen; Lee, Min-Ha

    2015-01-01

    We present investigations on the plastic deformation behavior of a brittle bulk amorphous alloy by simple uniaxial compressive loading at room temperature. A patterning is possible by cold-plastic forming of the typically brittle Hf-based bulk amorphous alloy through controlling homogenous flow without the need for thermal energy or shaping at elevated temperatures. The experimental evidence suggests that there is an inconsistency between macroscopic plasticity and deformability of an amorphous alloy. Moreover, imprinting of specific geometrical features on Cu foil and Zr-based metallic glass is represented by using the patterned bulk amorphous alloy as a die. These results demonstrate the ability of amorphous alloys or metallic glasses to precisely replicate patterning features onto both conventional metals and the other amorphous alloys. Our work presents an avenue for avoiding the embrittlement of amorphous alloys associated with thermoplastic forming and yields new insight the forming application of bulk amorphous alloys at room temperature without using heat treatment. PMID:26563908

  17. Imprinting bulk amorphous alloy at room temperature.

    PubMed

    Kim, Song-Yi; Park, Eun-Soo; Ott, Ryan T; Lograsso, Thomas A; Huh, Moo-Young; Kim, Do-Hyang; Eckert, Jürgen; Lee, Min-Ha

    2015-01-01

    We present investigations on the plastic deformation behavior of a brittle bulk amorphous alloy by simple uniaxial compressive loading at room temperature. A patterning is possible by cold-plastic forming of the typically brittle Hf-based bulk amorphous alloy through controlling homogenous flow without the need for thermal energy or shaping at elevated temperatures. The experimental evidence suggests that there is an inconsistency between macroscopic plasticity and deformability of an amorphous alloy. Moreover, imprinting of specific geometrical features on Cu foil and Zr-based metallic glass is represented by using the patterned bulk amorphous alloy as a die. These results demonstrate the ability of amorphous alloys or metallic glasses to precisely replicate patterning features onto both conventional metals and the other amorphous alloys. Our work presents an avenue for avoiding the embrittlement of amorphous alloys associated with thermoplastic forming and yields new insight the forming application of bulk amorphous alloys at room temperature without using heat treatment. PMID:26563908

  18. Imprinting bulk amorphous alloy at room temperature

    NASA Astrophysics Data System (ADS)

    Kim, Song-Yi; Park, Eun-Soo; Ott, Ryan T.; Lograsso, Thomas A.; Huh, Moo-Young; Kim, Do-Hyang; Eckert, Jürgen; Lee, Min-Ha

    2015-11-01

    We present investigations on the plastic deformation behavior of a brittle bulk amorphous alloy by simple uniaxial compressive loading at room temperature. A patterning is possible by cold-plastic forming of the typically brittle Hf-based bulk amorphous alloy through controlling homogenous flow without the need for thermal energy or shaping at elevated temperatures. The experimental evidence suggests that there is an inconsistency between macroscopic plasticity and deformability of an amorphous alloy. Moreover, imprinting of specific geometrical features on Cu foil and Zr-based metallic glass is represented by using the patterned bulk amorphous alloy as a die. These results demonstrate the ability of amorphous alloys or metallic glasses to precisely replicate patterning features onto both conventional metals and the other amorphous alloys. Our work presents an avenue for avoiding the embrittlement of amorphous alloys associated with thermoplastic forming and yields new insight the forming application of bulk amorphous alloys at room temperature without using heat treatment.

  19. Imprinting bulk amorphous alloy at room temperature

    SciTech Connect

    Kim, Song-Yi; Park, Eun-Soo; Ott, Ryan T.; Lograsso, Thomas A.; Huh, Moo-Young; Kim, Do-Hyang; Eckert, Jürgen; Lee, Min-Ha

    2015-11-13

    We present investigations on the plastic deformation behavior of a brittle bulk amorphous alloy by simple uniaxial compressive loading at room temperature. A patterning is possible by cold-plastic forming of the typically brittle Hf-based bulk amorphous alloy through controlling homogenous flow without the need for thermal energy or shaping at elevated temperatures. The experimental evidence suggests that there is an inconsistency between macroscopic plasticity and deformability of an amorphous alloy. Moreover, imprinting of specific geometrical features on Cu foil and Zr-based metallic glass is represented by using the patterned bulk amorphous alloy as a die. These results demonstrate the ability of amorphous alloys or metallic glasses to precisely replicate patterning features onto both conventional metals and the other amorphous alloys. In conclusion, our work presents an avenue for avoiding the embrittlement of amorphous alloys associated with thermoplastic forming and yields new insight the forming application of bulk amorphous alloys at room temperature without using heat treatment.

  20. Amorphous rare earth magnet powders

    SciTech Connect

    Sellers, C.H.; Branagan, D.J.; Hyde, T.A.; Lewis, L.H.; Panchanathan, V.

    1996-08-01

    Gas atomization (GA) processing does not generally have a high enough cooling rate to produce the initial amorphous microstructure needed to obtain optimal magnetic properties in RE{sub 2}Fe{sub 14}B alloys. Phase separation and an underquenched microstructure result from detrimental {alpha}-Fe precipitation, and the resulting magnetic domain structure is very coarse. Additionally, there is a dramatic dependence of the magnetic properties on the cooling rate (and therefore the particle size) and the powders can be sensitive to environmental degradation. Alloy compositions designed just for GA (as opposed to melt spinning) are necessary to produce an amorphous structure that can be crystallized to result in a fine structure with magnetic properties which are independent of particle size. The addition of titanium and carbon to the melt has been found to change the solidification process sufficiently to result in an ``overquenched`` state in which most of the powder size fractions have an amorphous component. Crystallization with a brief heat treatment produces a structure which has improved magnetic properties, in part due to the ability to use compositions with higher Fe contents without {alpha}-Fe precipitation. Results from magnetometry, magnetic force microscopy, and x-ray analyses will be used to contrast the microstructure, domain structure, and magnetic properties of this new generation of amorphous powders with their multiphase predecessors.

  1. Amorphous titanium-oxide supercapacitors

    PubMed Central

    Fukuhara, Mikio; Kuroda, Tomoyuki; Hasegawa, Fumihiko

    2016-01-01

    The electric capacitance of an amorphous TiO2-x surface increases proportionally to the negative sixth power of the convex diameter d. This occurs because of the van der Waals attraction on the amorphous surface of up to 7 mF/cm2, accompanied by extreme enhanced electron trapping resulting from both the quantum-size effect and an offset effect from positive charges at oxygen-vacancy sites. Here we show that a supercapacitor, constructed with a distributed constant-equipment circuit of large resistance and small capacitance on the amorphous TiO2-x surface, illuminated a red LED for 37 ms after it was charged with 1 mA at 10 V. The fabricated device showed no dielectric breakdown up to 1,100 V. Based on this approach, further advances in the development of amorphous titanium-dioxide supercapacitors might be attained by integrating oxide ribbons with a micro-electro mechanical system. PMID:27767103

  2. Tandem junction amorphous silicon solar cells

    DOEpatents

    Hanak, Joseph J.

    1981-01-01

    An amorphous silicon solar cell has an active body with two or a series of layers of hydrogenated amorphous silicon arranged in a tandem stacked configuration with one optical path and electrically interconnected by a tunnel junction. The layers of hydrogenated amorphous silicon arranged in tandem configuration can have the same bandgap or differing bandgaps.

  3. Density Functional Theory Study of Hydrogen Adsorption in a Ti-Decorated Mg-Based Metal-Organic Framework-74.

    PubMed

    Suksaengrat, Pitphichaya; Amornkitbamrung, Vittaya; Srepusharawoot, Pornjuk; Ahuja, Rajeev

    2016-03-16

    The Ti-binding energy and hydrogen adsorption energy of a Ti-decorated Mg-based metal-organic framework-74 (Mg-MOF-74) were evaluated by using first-principles calculations. Our results revealed that only three Ti adsorption sites were found to be stable. The adsorption site near the metal oxide unit is the most stable. To investigate the hydrogen-adsorption properties of Ti-functionalized Mg-MOF-74, the hydrogen-binding energy was determined. For the most stable Ti adsorption site, we found that the hydrogen adsorption energy ranged from 0.26 to 0.48 eV H2 (-1) . This is within the desirable range for practical hydrogen-storage applications. Moreover, the hydrogen capacity was determined by using ab initio molecular dynamics simulations. Our results revealed that the hydrogen uptake by Ti-decorated Mg-MOF-74 at temperatures of 77, 150, and 298 K and ambient pressure were 1.81, 1.74, and 1.29 H2  wt %, respectively. PMID:26717417

  4. Laser cladding of a Mg based Mg-Gd-Y-Zr alloy with Al-Si powders

    NASA Astrophysics Data System (ADS)

    Chen, Erlei; Zhang, Kemin; Zou, Jianxin

    2016-03-01

    In the present work, a Mg based Mg-Gd-Y-Zr alloy was subjected to laser cladding with Al-Si powders at different laser scanning speeds in order to improve its surface properties. It is observed that the laser clad layer mainly contains Mg2Si, Mg17Al12 and Al2(Gd,Y) phases distributed in the Mg matrix. The depth of the laser clad layer increases with decreasing the scanning speed. The clad layer has graded microstructures and compositions. Both the volume fraction and size of Mg2Si, Mg17Al12 and Al2(Gd,Y) phases decreases with the increasing depth. Due to the formation of these hardening phases, the hardness of clad layer reached a maximum value of HV440 when the laser scanning speed is 2 mm/s, more than 5 times of the substrate (HV75). Besides, the corrosion properties of the untreated and laser treated samples were all measured in a NaCl (3.5 wt.%) aqueous solution. The corrosion potential was increased from -1.77 V for the untreated alloy to -1.13 V for the laser clad alloy with scanning rate of 2 mm/s, while the corrosion current density was reduced from 2.10 × 10-5 A cm-2 to 1.64 × 10-6 A cm-2. The results show that laser cladding is an efficient method to improve surface properties of Mg-Rare earth alloys.

  5. Uranium incorporation into amorphous silica.

    PubMed

    Massey, Michael S; Lezama-Pacheco, Juan S; Nelson, Joey M; Fendorf, Scott; Maher, Kate

    2014-01-01

    High concentrations of uranium are commonly observed in naturally occurring amorphous silica (including opal) deposits, suggesting that incorporation of U into amorphous silica may represent a natural attenuation mechanism and promising strategy for U remediation. However, the stability of uranium in opaline silicates, determined in part by the binding mechanism for U, is an important factor in its long-term fate. U may bind directly to the opaline silicate matrix, or to materials such as iron (hydr)oxides that are subsequently occluded within the opal. Here, we examine the coordination environment of U within opaline silica to elucidate incorporation mechanisms. Precipitates (with and without ferrihydrite inclusions) were synthesized from U-bearing sodium metasilicate solutions, buffered at pH ∼ 5.6. Natural and synthetic solids were analyzed with X-ray absorption spectroscopy and a suite of other techniques. In synthetic amorphous silica, U was coordinated by silicate in a double corner-sharing coordination geometry (Si at ∼ 3.8-3.9 Å) and a small amount of uranyl and silicate in a bidentate, mononuclear (edge-sharing) coordination (Si at ∼ 3.1-3.2 Å, U at ∼ 3.8-3.9 Å). In iron-bearing synthetic solids, U was adsorbed to iron (hydr)oxide, but the coordination environment also contained silicate in both edge-sharing and corner-sharing coordination. Uranium local coordination in synthetic solids is similar to that of natural U-bearing opals that retain U for millions of years. The stability and extent of U incorporation into opaline and amorphous silica represents a long-term repository for U that may provide an alternative strategy for remediation of U contamination. PMID:24984107

  6. Stability study of amorphous valdecoxib.

    PubMed

    Ambike, Anshuman A; Mahadik, K R; Paradkar, Anant

    2004-09-10

    Formulation of poorly water-soluble drugs in the most stable dosage form for oral delivery perhaps presents the greatest challenge to pharmaceutical industry. Physical transformation of drug substance into its more soluble but metastable amorphous form is one of the approaches for improving dissolution rate of such drugs. The present study utilizes technique of spray drying for preparation of solid dispersions (SDs) and includes stability study of the same. Valdecoxib (VLD), a prototype of poorly water-soluble drugs, has been the drug of choice. The hydrophilic carriers selected were polyvinylpyrrolidone K30 (PVP) and hydroxypropylcellulose (HPC). SDs and pure VLD in the form of spray dried powder (SDVLD) in comparison with pure drug and corresponding physical mixtures (PMs) were initially characterized and then subjected to stability testing at ambient temperature and relative humidity up to 3 months. During initial characterization, increase in saturation solubility and dissolution rate was observed in all samples. DSC and XRPD studies of SDVLD and SDs suggested generation of amorphous form of drug. IR spectroscopy revealed presence of hydrogen bonding in SDs. During stability testing, there was gradual decrease in saturation solubility and dissolution rate of SDs, over the period of 3 months. While, saturation solubility of SDVLD dropped drastically within 15 days and was almost comparable with pure VLD. SD PVP retained the amorphous form of drug throughout stability period, whereas SD HPC and SDVLD presented incidence of crystallinity after 1 month and 15 days, respectively. This was justified by enthalpy relaxation studies in which, amorphous VLD showed considerable relaxation of enthalpy at Tg, while it was totally suppressed in SD PVP and partly in SD HPC. The study thus definitely reveals tremendous potential of solid dispersions of valdecoxib with PVP, from stability point of view.

  7. Visual Observations of the Amorphous-Amorphous Transition in H2O Under Pressure.

    PubMed

    Mishima, O; Takemura, K; Aoki, K

    1991-10-18

    The vapor-deposited low-density amorphous phase of H(2)O was directly compressed at 77 kelvin with a diamond-anvil cell, and the boundary between the low-density amorphous phase and the high-density amorphous phase was observed while the sample was warmed under compression. The transition from the low-density amorphous phase to the high-density amorphous phase was distinct and reversible in an apparently narrow pressure range at approximately 130 to approximately 150 kelvin, which provided experimental evidence for polymorphism in amorphous H(2)O. PMID:17742228

  8. The effect of treatment temperature on corrosion resistance and hydrophilicity of an ionic liquid coating for Mg-based stents.

    PubMed

    Zhang, Yafei; Forsyth, Maria; Hinton, Bruce R W

    2014-01-01

    Mg alloys are attractive candidate materials for biodegradable stents. However, there are few commercially available Mg-based stents in clinical use because Mg alloys generally undergo rapid localized corrosion in the body. In this study, we report a new surface coating for Mg alloy AZ31 based on a low-toxicity ionic liquid (IL), tributyl(methyl)phosphonium diphenyl phosphate (P1,4,4,4 dpp), to control its corrosion rate. Emphasis is placed on the effect of treatment temperature. We showed that enhancing the treatment temperature provided remarkable improvements in the performances of both corrosion resistance and biocompatibility. Increasing treatment temperature resulted in a thicker (although still nanometer scale) and more homogeneous IL film on the surface. Scanning electron microscopy and optical profilometry observations showed that there were many large, deep pits formed on the surface of bare AZ31 after 2 h of immersion in simulated body fluid (SBF). The IL coating (particularly when formed at 100 °C for 1 h) significantly suppressed the formation of these pits on the surface, making corrosion occur more uniformly. The P1,4,4,4 dpp IL film formed at 100 °C was more hydrophilic than the bare AZ31 surface, which was believed to be beneficial for avoiding the deposition of the proteins and cells on the surface and therefore improving the biocompatibility of AZ31 in blood. The interaction mechanism between this IL and AZ31 was also investigated using ATR-FTIR, which showed that both anion and cation of this IL were present in the film, and there was a chemical interaction between dpp(-) anion and the surface of AZ31 during the film formation.

  9. The effect of treatment temperature on corrosion resistance and hydrophilicity of an ionic liquid coating for Mg-based stents.

    PubMed

    Zhang, Yafei; Forsyth, Maria; Hinton, Bruce R W

    2014-01-01

    Mg alloys are attractive candidate materials for biodegradable stents. However, there are few commercially available Mg-based stents in clinical use because Mg alloys generally undergo rapid localized corrosion in the body. In this study, we report a new surface coating for Mg alloy AZ31 based on a low-toxicity ionic liquid (IL), tributyl(methyl)phosphonium diphenyl phosphate (P1,4,4,4 dpp), to control its corrosion rate. Emphasis is placed on the effect of treatment temperature. We showed that enhancing the treatment temperature provided remarkable improvements in the performances of both corrosion resistance and biocompatibility. Increasing treatment temperature resulted in a thicker (although still nanometer scale) and more homogeneous IL film on the surface. Scanning electron microscopy and optical profilometry observations showed that there were many large, deep pits formed on the surface of bare AZ31 after 2 h of immersion in simulated body fluid (SBF). The IL coating (particularly when formed at 100 °C for 1 h) significantly suppressed the formation of these pits on the surface, making corrosion occur more uniformly. The P1,4,4,4 dpp IL film formed at 100 °C was more hydrophilic than the bare AZ31 surface, which was believed to be beneficial for avoiding the deposition of the proteins and cells on the surface and therefore improving the biocompatibility of AZ31 in blood. The interaction mechanism between this IL and AZ31 was also investigated using ATR-FTIR, which showed that both anion and cation of this IL were present in the film, and there was a chemical interaction between dpp(-) anion and the surface of AZ31 during the film formation. PMID:25317893

  10. Narrow band gap amorphous silicon semiconductors

    DOEpatents

    Madan, A.; Mahan, A.H.

    1985-01-10

    Disclosed is a narrow band gap amorphous silicon semiconductor comprising an alloy of amorphous silicon and a band gap narrowing element selected from the group consisting of Sn, Ge, and Pb, with an electron donor dopant selected from the group consisting of P, As, Sb, Bi and N. The process for producing the narrow band gap amorphous silicon semiconductor comprises the steps of forming an alloy comprising amorphous silicon and at least one of the aforesaid band gap narrowing elements in amount sufficient to narrow the band gap of the silicon semiconductor alloy below that of amorphous silicon, and also utilizing sufficient amounts of the aforesaid electron donor dopant to maintain the amorphous silicon alloy as an n-type semiconductor.

  11. Amorphous silicon solar cell allowing infrared transmission

    DOEpatents

    Carlson, David E.

    1979-01-01

    An amorphous silicon solar cell with a layer of high index of refraction material or a series of layers having high and low indices of refraction material deposited upon a transparent substrate to reflect light of energies greater than the bandgap energy of the amorphous silicon back into the solar cell and transmit solar radiation having an energy less than the bandgap energy of the amorphous silicon.

  12. Preparation of amorphous sulfide sieves

    DOEpatents

    Siadati, Mohammad H.; Alonso, Gabriel; Chianelli, Russell R.

    2006-11-07

    The present invention involves methods and compositions for synthesizing catalysts/porous materials. In some embodiments, the resulting materials are amorphous sulfide sieves that can be mass-produced for a variety of uses. In some embodiments, methods of the invention concern any suitable precursor (such as thiomolybdate salt) that is exposed to a high pressure pre-compaction, if need be. For instance, in some cases the final bulk shape (but highly porous) may be same as the original bulk shape. The compacted/uncompacted precursor is then subjected to an open-flow hot isostatic pressing, which causes the precursor to decompose and convert to a highly porous material/catalyst.

  13. Is Mg-stabilized amorphous calcium carbonate a homogeneous mixture of amorphous magnesium carbonate and amorphous calcium carbonate?

    PubMed

    Yang, Sheng-Yu; Chang, Hsun-Hui; Lin, Cang-Jie; Huang, Shing-Jong; Chan, Jerry C C

    2016-10-01

    We find two types of carbonate ions in Mg stabilized amorphous calcium carbonate (Mg-ACC), whose short-range orders are identical to those of ACC and amorphous magnesium carbonate (AMC). Mg-ACC comprises a homogeneous mixture of the nano-clusters of ACC and AMC. Their relative amount varies systematically at different pH. PMID:27524162

  14. New bulk amorphous magnetic materials

    NASA Astrophysics Data System (ADS)

    Chiriac, H.; Lupu, N.

    2001-06-01

    The relationship between structure and magnetic properties of the melt-spun ribbons with thicknesses up to 200 μm and rods having up to 3 mm diameter prepared by mould casting and suction casting techniques, of nominal compositions Fe 56Co 7Ni 7Zr 6M 1.5Nb 2.5B 20 (M=Zr, Ti, Ta or Mo) and Nd 50Fe 40Si 10- xAl x was investigated. Saturation magnetisations up to 1.1 T, coercive fields of about 5 A/m, magnetic permeabilities of 25 000-30 000 in the as-cast state were measured for the Fe-based amorphous alloys. The large values over 200 kA/m of the intrinsic coercive field at room temperature and over 600 kA/m at 200 K measured in low magnetic fields for the Nd-Fe-based “X-ray amorphous” alloys, and its dependence on temperature and cooling rate are ascribed to the existence of very small ferromagnetic clusters embedded in an Nd-rich matrix. The thermal treatments applied to the amorphous samples below the crystallisation temperature cause an improvement in the magnetic properties as a consequence of structural relaxation.

  15. Laser surface treatment of amorphous metals

    NASA Astrophysics Data System (ADS)

    Katakam, Shravana K.

    Amorphous materials are used as soft magnetic materials and also as surface coatings to improve the surface properties. Furthermore, the nanocrystalline materials derived from their amorphous precursors show superior soft magnetic properties than amorphous counter parts for transformer core applications. In the present work, laser based processing of amorphous materials will be presented. Conventionally, the nanocrystalline materials are synthesized by furnace heat treatment of amorphous precursors. Fe-based amorphous/nanocrystalline materials due to their low cost and superior magnetic properties are the most widely used soft magnetic materials. However, achieving nanocrystalline microstructure in Fe-Si-B ternary system becomes very difficult owing its rapid growth rate at higher temperatures and sluggish diffusion at low temperature annealing. Hence, nanocrystallization in this system is achieved by using alloying additions (Cu and Nb) in the ternary Fe-Si-B system. Thus, increasing the cost and also resulting in reduction of saturation magnetization. laser processing technique is used to achieve extremely fine nanocrystalline microstructure in Fe-Si-B amorphous precursor. Microstructure-magnetic Property-laser processing co-relationship has been established for Fe-Si-B ternary system using analytical techniques. Laser processing improved the magnetic properties with significant increase in saturation magnetization and near zero coercivity values. Amorphous materials exhibit excellent corrosion resistance by virtue of their atomic structure. Fe-based amorphous materials are economical and due to their ease of processing are of potential interest to synthesize as coatings materials for wear and corrosion resistance applications. Fe-Cr-Mo-Y-C-B amorphous system was used to develop thick coatings on 4130 Steel substrate and the corrosion resistance of the amorphous coatings was improved. It is also shown that the mode of corrosion depends on the laser processing

  16. Efficient catalysis by MgCl2 in hydrogen generation via hydrolysis of Mg-based hydride prepared by hydriding combustion synthesis.

    PubMed

    Zhao, Zelun; Zhu, Yunfeng; Li, Liquan

    2012-06-01

    Magnesium chloride efficiently catalyzed the hydrolysis of Mg-based hydride prepared by hydriding combustion synthesis. Hydrogen yield of 1635 mL g(-1) was obtained (MgH(2)), i.e. with 96% conversion in 30 min at 303 K.

  17. Fluorination of amorphous thin-film materials with xenon fluoride

    DOEpatents

    Weil, Raoul B.

    1988-01-01

    A method is disclosed for producing fluorine-containing amorphous semiconductor material, preferably comprising amorphous silicon. The method includes depositing amorphous thin-film material onto a substrate while introducing xenon fluoride during the film deposition process.

  18. Fluorination of amorphous thin-film materials with xenon fluoride

    DOEpatents

    Weil, R.B.

    1987-05-01

    A method is disclosed for producing fluorine-containing amorphous semiconductor material, preferably comprising amorphous silicon. The method includes depositing amorphous thin-film material onto a substrate while introducing xenon fluoride during the film deposition process.

  19. Method of making amorphous metal composites

    DOEpatents

    Byrne, Martin A.; Lupinski, John H.

    1982-01-01

    The process comprises placing an amorphous metal in particulate form and a low molecular weight (e.g., 1000-5000) thermosetting polymer binder powder into a container, mixing these materials, and applying heat and pressure to convert the mixture into an amorphous metal composite.

  20. Electron tunnelling into amorphous germanium and silicon.

    NASA Technical Reports Server (NTRS)

    Smith, C. W.; Clark, A. H.

    1972-01-01

    Measurements of tunnel conductance versus bias, capacitance versus bias, and internal photoemission were made in the systems aluminum-oxide-amorphous germanium and aluminium-oxide-amorphous silicon. A function was extracted which expresses the deviation of these systems from the aluminium-oxide-aluminium system.

  1. Electron beam recrystallization of amorphous semiconductor materials

    NASA Technical Reports Server (NTRS)

    Evans, J. C., Jr.

    1968-01-01

    Nucleation and growth of crystalline films of silicon, germanium, and cadmium sulfide on substrates of plastic and glass were investigated. Amorphous films of germanium, silicon, and cadmium sulfide on amorphous substrates of glass and plastic were converted to the crystalline condition by electron bombardment.

  2. Imprinting bulk amorphous alloy at room temperature

    DOE PAGES

    Kim, Song-Yi; Park, Eun-Soo; Ott, Ryan T.; Lograsso, Thomas A.; Huh, Moo-Young; Kim, Do-Hyang; Eckert, Jürgen; Lee, Min-Ha

    2015-11-13

    We present investigations on the plastic deformation behavior of a brittle bulk amorphous alloy by simple uniaxial compressive loading at room temperature. A patterning is possible by cold-plastic forming of the typically brittle Hf-based bulk amorphous alloy through controlling homogenous flow without the need for thermal energy or shaping at elevated temperatures. The experimental evidence suggests that there is an inconsistency between macroscopic plasticity and deformability of an amorphous alloy. Moreover, imprinting of specific geometrical features on Cu foil and Zr-based metallic glass is represented by using the patterned bulk amorphous alloy as a die. These results demonstrate the abilitymore » of amorphous alloys or metallic glasses to precisely replicate patterning features onto both conventional metals and the other amorphous alloys. In conclusion, our work presents an avenue for avoiding the embrittlement of amorphous alloys associated with thermoplastic forming and yields new insight the forming application of bulk amorphous alloys at room temperature without using heat treatment.« less

  3. Compensated amorphous-silicon solar cell

    DOEpatents

    Devaud, G.

    1982-06-21

    An amorphous silicon solar cell including an electrically conductive substrate, a layer of glow discharge deposited hydrogenated amorphous silicon 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 elecrically 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.

  4. Structure, thermodynamics, and crystallization of amorphous hafnia

    SciTech Connect

    Luo, Xuhui; Demkov, Alexander A.

    2015-09-28

    We investigate theoretically amorphous hafnia using the first principles melt and quench method. We identify two types of amorphous structures of hafnia. Type I and type II are related to tetragonal and monoclinic hafnia, respectively. We find type II structure to show stronger disorder than type I. Using the phonon density of states, we calculate the specific heat capacity for type II amorphous hafnia. Using the nudged elastic band method, we show that the averaged transition barrier between the type II amorphous hafnia and monoclinic phase is approximately 0.09 eV/HfO{sub 2}. The crystallization temperature is estimated to be 421 K. The calculations suggest an explanation for the low thermal stability of amorphous hafnia.

  5. Solid-state diffusion in amorphous zirconolite

    SciTech Connect

    Yang, C.; Dove, M. T.; Trachenko, K.; Zarkadoula, E.; Todorov, I. T.; Geisler, T.; Brazhkin, V. V.

    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 find 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.

  6. Solid-state diffusion in amorphous zirconolite

    NASA Astrophysics Data System (ADS)

    Yang, C.; Zarkadoula, E.; Dove, M. T.; Todorov, I. T.; Geisler, T.; Brazhkin, V. V.; Trachenko, K.

    2014-11-01

    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 find 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.

  7. Neutron irradiation induced amorphization of silicon carbide

    SciTech Connect

    Snead, L.L.; Hay, J.C.

    1998-09-01

    This paper provides the first known observation of silicon carbide fully amorphized under neutron irradiation. Both high purity single crystal hcp and high purity, highly faulted (cubic) chemically vapor deposited (CVD) SiC were irradiated at approximately 60 C to a total fast neutron fluence of 2.6 {times} 10{sup 25} n/m{sup 2}. Amorphization was seen in both materials, as evidenced by TEM, electron diffraction, and x-ray diffraction techniques. Physical properties for the amorphized single crystal material are reported including large changes in density ({minus}10.8%), elastic modulus as measured using a nanoindentation technique ({minus}45%), hardness as measured by nanoindentation ({minus}45%), and standard Vickers hardness ({minus}24%). Similar property changes are observed for the critical temperature for amorphization at this neutron dose and flux, above which amorphization is not possible, is estimated to be greater than 130 C.

  8. Locomotion of Amorphous Surface Robots

    NASA Technical Reports Server (NTRS)

    Bradley, Arthur T. (Inventor)

    2016-01-01

    An amorphous robot includes a compartmented bladder containing fluid, a valve assembly, and an outer layer encapsulating the bladder and valve assembly. The valve assembly draws fluid from a compartment(s) and discharges the drawn fluid into a designated compartment to displace the designated compartment with respect to the surface. Another embodiment includes elements each having a variable property, an outer layer that encapsulates the elements, and a control unit. The control unit energizes a designated element to change its variable property, thereby moving the designated element. The elements may be electromagnetic spheres with a variable polarity or shape memory polymers with changing shape and/or size. Yet another embodiment includes an elongated flexible tube filled with ferrofluid, a moveable electromagnet, an actuator, and a control unit. The control unit energizes the electromagnet and moves the electromagnet via the actuator to magnetize the ferrofluid and lengthen the flexible tube.

  9. Biologically formed amorphous calcium carbonate.

    PubMed

    Weiner, Steve; Levi-Kalisman, Yael; Raz, Sefi; Addadi, Lia

    2003-01-01

    Many organisms from a wide variety of taxa produce amorphous calcium carbonate (ACC), despite the fact that it is inherently unstable and relatively soluble in its pure state. These properties also make it difficult to detect and characterize ACC. Raman spectroscopy is a particularly useful method for investigating ACC because the sample can be examined wet, and extended X-ray absorption fine structure (EXAFS) analysis can provide detailed information on the short-range order. Other methods for characterizing ACC include infrared spectroscopy, thermogravimetric analysis and differential thermal analysis (TGA and DTA), transmission electron microscopy (TEM), and electron and X-ray diffraction. Because of the difficulties involved, we suspect that ACC is far more widely distributed than is presently known, and a comparison of EXAFS spectra shows that different biogenic ACC phases have different short-range order structures. We also suspect that ACC fulfils many different functions, including as a transient precursor phase during the formation of crystalline calcium carbonate.

  10. Locomotion of Amorphous Surface Robots

    NASA Technical Reports Server (NTRS)

    Bradley, Arthur T. (Inventor)

    2014-01-01

    An amorphous robot includes a compartmented bladder containing fluid, a valve assembly, and an outer layer encapsulating the bladder and valve assembly. The valve assembly draws fluid from a compartment(s) and discharges the drawn fluid into a designated compartment to displace the designated compartment with respect to the surface. Another embodiment includes elements each having a variable property, an outer layer that encapsulates the elements, and a control unit. The control unit energizes a designated element to change its variable property, thereby moving the designated element. The elements may be electromagnetic spheres with a variable polarity or shape memory polymers with changing shape and/or size. Yet another embodiment includes an elongated flexible tube filled with ferrofluid, a moveable electromagnet, an actuator, and a control unit. The control unit energizes the electromagnet and moves the electromagnet via the actuator to magnetize the ferrofluid and lengthen the flexible tube.

  11. Quantification of surface amorphous content using dispersive surface energy: the concept of effective amorphous surface area.

    PubMed

    Brum, Jeffrey; Burnett, Daniel

    2011-09-01

    We investigate the use of dispersive surface energy in quantifying surface amorphous content, and the concept of effective amorphous surface area is introduced. An equation is introduced employing the linear combination of surface area normalized square root dispersive surface energy terms. This equation is effective in generating calibration curves when crystalline and amorphous references are used. Inverse gas chromatography is used to generate dispersive surface energy values. Two systems are investigated, and in both cases surface energy data collected for physical mixture samples comprised of amorphous and crystalline references fits the predicted response with good accuracy. Surface amorphous content of processed lactose samples is quantified using the calibration curve, and interpreted within the context of effective amorphous surface area. Data for bulk amorphous content is also utilized to generate a thorough picture of how disorder is distributed throughout the particle. An approach to quantifying surface amorphous content using dispersive surface energy is presented. Quantification is achieved by equating results to an effective amorphous surface area based on reference crystalline, and amorphous materials. PMID:21725707

  12. Observation of a rapid amorphization reaction

    SciTech Connect

    Hufnagel, T.C. ); Brennan, S. ); Payne, A.P.; Clemens, B.M. )

    1992-08-01

    We have observed a rapid amorphization reaction at ambient temperature in the Gd/Co system by employing grazing incidence x-ray scattering. We find that a 135 A crystalline Gd film is amporhized in less than 30 min by deposition of Co. We postulate that the rapidity of the reaction is due to surface diffusion of Co atoms after deposition to fast diffusion sites such as grain boundaries in the Gd film. Once the interfacial region has been amorphized these fast diffusion paths are sealed off from the surface, rapid diffusion of Co into the Gd crystalline layer is prevented, and the amorphization reaction stops.

  13. Pressure induced crystallization in amorphous silicon

    NASA Astrophysics Data System (ADS)

    Pandey, K. K.; Garg, Nandini; Shanavas, K. V.; Sharma, Surinder M.; Sikka, S. K.

    2011-06-01

    We have investigated the high pressure behavior of amorphous silicon (a-Si) using x-ray diffraction and Raman scattering techniques. Our experiments show that a-Si undergoes a polyamorphous transition from the low density amorphous to the high density amorphous phase, followed by pressure induced crystallization to the primitive hexagonal (ph) phase. On the release path, the sequence of observed phase transitions depends on whether the pressure is reduced slowly or rapidly. Using the results of our first principles calculations, pressure induced preferential crystallization to the ph phase is explained in terms of a thermodynamic model based on phenomenological random nucleation and the growth process.

  14. Selective laser sintering of amorphous metal powder

    NASA Astrophysics Data System (ADS)

    Fischer, P.; Blatter, A.; Romano, V.; Weber, H. P.

    2005-02-01

    For the first time, selective sintering of amorphous PtCuNiP powder with a pulsed Nd:YAG laser has been studied. Upon pulsed interaction, the grains melt only superficially to build necks between the grains. Depending on the laser parameters, the sintered material can be crystallized or retained amorphous. By contrast with crystalline powder, laser sintering of amorphous powder is achieved at substantially lower pulse energies due to its low melting point. The obtained results are compared with previous results from selective laser sintering of titanium powder.

  15. Method of producing hydrogenated amorphous silicon film

    DOEpatents

    Wiesmann, Harold J.

    1980-01-01

    This invention relates to hydrogenated amorphous silicon produced by thermally decomposing silane (SiH.sub.4) or other gases comprising H and Si, from a tungsten or carbon foil heated to a temperature of about 1400.degree.-1600.degree. C., in a vacuum of about 10.sup.-6 to 19.sup.-4 torr, to form a gaseous mixture of atomic hydrogen and atomic silicon, and depositing said gaseos mixture onto a substrate independent of and outside said source of thermal decomposition, to form hydrogenated amorphous silicon. The presence of an ammonia atmosphere in the vacuum chamber enhances the photoconductivity of the hydrogenated amorphous silicon film.

  16. MxMn8O16 (M = Ag or K) as promising cathode materials for secondary Mg based batteries: The role of the cation M

    DOE PAGES

    Huang, Jianping; Takeuchi, Esther S.; Altug S. Poyraz; Takeuchi, Kenneth J.; Marschilok, Amy C.

    2016-02-15

    Here, AgxMn8O16 (Ag-OMS-2) and KxMn8O16 (K-OMS-2) were investigated as high voltage cathode materials for Mg based batteries. Both MxMn8O16 materials delivered high initial capacities (>180 mA h g–1), and KxMn8O16 showed high cycle stability with a reversible capacity of >170 mA h g–1 after 20 cycles.

  17. Crystallization of amorphous solid films

    NASA Astrophysics Data System (ADS)

    Safarik, Douglas Joseph

    2003-06-01

    Below ˜130 K, H2O can exist for prolonged periods in a thermodynamically unstable, non-crystalline solid form known as amorphous solid water (ASW). When warmed to above 135 K, ASW crystallizes to the thermodynamically favored state, cubic ice I, on a laboratory time scale. Despite the relevance of ASW crystallization to a variety of scientific problems ranging from astrophysical phenomena to cryopreservation, the kinetics of this transformation are largely uncharacterized, and its mechanism is not fully understood. In the present work, the crystallization kinetics of vapor-deposited, nonporous ASW films less than one micron thick are investigated experimentally near 140 K. The amorphous to crystalline transition is characterized using a probe molecule, chlorodifluoromethane (CHF2Cl), whose adsorbed states and hence desorption kinetics are sensitive to the crystallinity of solid water surfaces. The transformation kinetics of very thick ASW films are found to be both independent of specimen size and consistent with simultaneous homogeneous nucleation and isotropic growth of crystalline ice grains. As the ASW film thickness is reduced from 385 nm to 55 nm, however, the rate of surface crystallization decelerates, in apparent conflict with a homogeneous nucleation and growth mechanism. In an attempt to explain this behavior, a geometrical model of phase transition kinetics at the surface of solids, with special consideration of finite specimen size in one dimension, is constructed. For materials in which nucleation occurs spatially randomly, phase change is predicted to decelerate when film thickness is reduced below the mean crystal grain size. This phenomenon originates from a reduction in the number of crystallites available to transform the surface as the sample becomes thinner. Good quantitative agreement between this simple model and the experimental data is attained using a minimum of kinetic parameters, suggesting it captures the essential physics of ASW

  18. Corrosion resistant amorphous metals and methods of forming corrosion resistant amorphous metals

    DOEpatents

    Farmer, Joseph C.; Wong, Frank M. G.; Haslam, Jeffery J.; Yang, Nancy; Lavernia, Enrique J.; Blue, Craig A.; Graeve, Olivia A.; Bayles, Robert; Perepezko, John H.; Kaufman, Larry; Schoenung, Julie; Ajdelsztajn, Leo

    2009-11-17

    A system for coating a surface comprises providing a source of amorphous metal, providing ceramic particles, and applying the amorphous metal and the ceramic particles to the surface by a spray. The coating comprises a composite material made of amorphous metal that contains one or more of the following elements in the specified range of composition: yttrium (.gtoreq.1 atomic %), chromium (14 to 18 atomic %), molybdenum (.gtoreq.7 atomic %), tungsten (.gtoreq.1 atomic %), boron (.ltoreq.5 atomic %), or carbon (.gtoreq.4 atomic %).

  19. Corrosion resistant amorphous metals and methods of forming corrosion resistant amorphous metals

    DOEpatents

    Farmer, Joseph C.; Wong, Frank M.G.; Haslam, Jeffery J.; Yang, Nancy; Lavernia, Enrique J.; Blue, Craig A.; Graeve, Olivia A.; Bayles, Robert; Perepezko, John H.; Kaufman, Larry; Schoenung, Julie; Ajdelsztajn, Leo

    2014-07-15

    A system for coating a surface comprises providing a source of amorphous metal, providing ceramic particles, and applying the amorphous metal and the ceramic particles to the surface by a spray. The coating comprises a composite material made of amorphous metal that contains one or more of the following elements in the specified range of composition: yttrium (.gtoreq.1 atomic %), chromium (14 to 18 atomic %), molybdenum (.gtoreq.7 atomic %), tungsten (.gtoreq.1 atomic %), boron (.ltoreq.5 atomic %), or carbon (.gtoreq.4 atomic %).

  20. Amorphization of silicon carbide by carbon displacement

    NASA Astrophysics Data System (ADS)

    Devanathan, R.; Gao, F.; Weber, W. J.

    2004-05-01

    We have used molecular dynamics simulations to examine the possibility of amorphizing silicon carbide (SiC) by exclusively displacing C atoms. At a defect generation corresponding to 0.2 displacements per atom, the enthalpy surpasses the level of melt-quenched SiC, the density decreases by about 15%, and the radial distribution function shows a lack of long-range order. Prior to amorphization, the surviving defects are mainly C Frenkel pairs (67%), but Si Frenkel pairs (18%) and antisite defects (15%) are also present. The results indicate that SiC can be amorphized by C sublattice displacements. Chemical short-range disorder, arising mainly from Frenkel pair production, plays a significant role in the amorphization.

  1. Amorphous Semiconductor Thin Films, an Introduction

    SciTech Connect

    Martin, Peter M.

    2003-12-01

    The field of amorphous semiconductors is so large that I cannot do it justice, but I hope this short column gives you some insight into the properties and materials available, and the issues involved.

  2. Fracture in Bulk Amorphous Alloys

    SciTech Connect

    Horton, J.A.; Wright, J.L.

    1998-11-30

    The fracture behavior of a Zr-based bulk amorphous alloy, Zr-10 AI-5 Ti-17.9 Cu-14.6 Ni, was examined by transmission electron microscopy (TEM) and x-ray diffraction for any evidence of crystallization preceding crack propagation. No evidence for crystallization was found in shear bands in compression specimens or at the fracture surface in tensile specimens. In- situ TEM deformation experiments were performed to more closely examine actual crack tip regions. During the in-situ deformation experiment controlled crack growth occurred to the point where the specimen was approximately 20 {micro}m thick at which point uncontrolled crack growth occurred. No evidence of any crystallization was found at the crack tips or the crack flanks. Subsequent scanning microscope examination showed that the uncontrolled crack growth region exhibited ridges and veins that appeared to have resulted from melting. Performing the deformations, both bulk and in-situ TEM, at liquid nitrogen temperatures (LN{sub 2}) resulted in an increase in the amount of controlled crack growth. The surface roughness of the bulk regions fractured at LN{sub 2} temperatures corresponded with the roughness of the crack propagation observed during the in-situ TEM experiment, suggesting that the smooth-appearing room temperature fracture sur-faces may also be a result of localized melting.

  3. Ductile crystalline–amorphous nanolaminates

    PubMed Central

    Wang, Yinmin; Li, Ju; Hamza, Alex V.; Barbee, Troy W.

    2007-01-01

    It is known that the room-temperature plastic deformation of bulk metallic glasses is compromised by strain softening and shear localization, resulting in near-zero tensile ductility. The incorporation of metallic glasses into engineering materials, therefore, is often accompanied by complete brittleness or an apparent loss of useful tensile ductility. Here we report the observation of an exceptional tensile ductility in crystalline copper/copper–zirconium glass nanolaminates. These nanocrystalline–amorphous nanolaminates exhibit a high flow stress of 1.09 ± 0.02 GPa, a nearly elastic-perfectly plastic behavior without necking, and a tensile elongation to failure of 13.8 ± 1.7%, which is six to eight times higher than that typically observed in conventional crystalline–crystalline nanolaminates (<2%) and most other nanocrystalline materials. Transmission electron microscopy and atomistic simulations demonstrate that shear banding instability no longer afflicts the 5- to 10-nm-thick nanolaminate glassy layers during tensile deformation, which also act as high-capacity sinks for dislocations, enabling absorption of free volume and free energy transported by the dislocations; the amorphous–crystal interfaces exhibit unique inelastic shear (slip) transfer characteristics, fundamentally different from those of grain boundaries. Nanoscale metallic glass layers therefore may offer great benefits in engineering the plasticity of crystalline materials and opening new avenues for improving their strength and ductility. PMID:17592136

  4. Ion-beam amorphization of semiconductors: A physical model based on the amorphous pocket population

    SciTech Connect

    Mok, K.R.C.; Jaraiz, M.; Martin-Bragado, I.; Rubio, J.E.; Castrillo, P.; Pinacho, R.; Barbolla, J.; Srinivasan, M.P.

    2005-08-15

    We introduce a model for damage accumulation up to amorphization, based on the ion-implant damage structures commonly known as amorphous pockets. The model is able to reproduce the silicon amorphous-crystalline transition temperature for C, Si, and Ge ion implants. Its use as an analysis tool reveals an unexpected bimodal distribution of the defect population around a characteristic size, which is larger for heavier ions. The defect population is split in both size and composition, with small, pure interstitial and vacancy clusters below the characteristic size, and amorphous pockets with a balanced mixture of interstitials and vacancies beyond that size.

  5. Amorphous Phases on the Surface of Mars

    NASA Technical Reports Server (NTRS)

    Rampe, E. B.; Morris, R. V.; Ruff, S. W.; Horgan, B.; Dehouck, E.; Achilles, C. N.; Ming, D. W.; Bish, D. L.; Chipera, S. J.

    2014-01-01

    Both primary (volcanic/impact glasses) and secondary (opal/silica, allophane, hisingerite, npOx, S-bearing) amorphous phases appear to be major components of martian surface materials based on orbital and in-situ measurements. A key observation is that whereas regional/global scale amorphous components include altered glass and npOx, local scale amorphous phases include hydrated silica/opal. This suggests widespread alteration at low water-to-rock ratios, perhaps due to snow/ice melt with variable pH, and localized alteration at high water-to-rock ratios. Orbital and in-situ measurements of the regional/global amorphous component on Mars suggests that it is made up of at least three phases: npOx, amorphous silicate (likely altered glass), and an amorphous S-bearing phase. Fundamental questions regarding the composition and the formation of the regional/global amorphous component(s) still remain: Do the phases form locally or have they been homogenized through aeolian activity and derived from the global dust? Is the parent glass volcanic, impact, or both? Are the phases separate or intimately mixed (e.g., as in palagonite)? When did the amorphous phases form? To address the question of source (local and/or global), we need to look for variations in the different phases within the amorphous component through continued modeling of the chemical composition of the amorphous phases in samples from Gale using CheMin and APXS data. If we find variations (e.g., a lack of or enrichment in amorphous silicate in some samples), this may imply a local source for some phases. Furthermore, the chemical composition of the weathering products may give insight into the formation mechanisms of the parent glass (e.g., impact glasses contain higher Al and lower Si [30], so we might expect allophane as a weathering product of impact glass). To address the question of whether these phases are separate or intimately mixed, we need to do laboratory studies of naturally altered samples made

  6. A Magnetic Sensor with Amorphous Wire

    PubMed Central

    He, Dongfeng; Shiwa, Mitsuharu

    2014-01-01

    Using a FeCoSiB amorphous wire and a coil wrapped around it, we have developed a sensitive magnetic sensor. When a 5 mm long amorphous wire with the diameter of 0.1 mm was used, the magnetic field noise spectrum of the sensor was about 30 pT/√Hz above 30 Hz. To show the sensitivity and the spatial resolution, the magnetic field of a thousand Japanese yen was scanned with the magnetic sensor. PMID:24940865

  7. Amorphous Carbon-Boron Nitride Nanotube Hybrids

    NASA Technical Reports Server (NTRS)

    Kim, Jae Woo (Inventor); Siochi, Emilie J. (Inventor); Wise, Kristopher E. (Inventor); Lin, Yi (Inventor); Connell, John (Inventor)

    2016-01-01

    A method for joining or repairing boron nitride nanotubes (BNNTs). In joining BNNTs, the nanotube structure is modified with amorphous carbon deposited by controlled electron beam irradiation to form well bonded hybrid a-C/BNNT structures. In repairing BNNTs, the damaged site of the nanotube structure is modified with amorphous carbon deposited by controlled electron beam irradiation to form well bonded hybrid a-C/BNNT structures at the damage site.

  8. Thermal transport in amorphous materials: a review

    NASA Astrophysics Data System (ADS)

    Wingert, Matthew C.; Zheng, Jianlin; Kwon, Soonshin; Chen, Renkun

    2016-11-01

    Thermal transport plays a crucial role in performance and reliability of semiconductor electronic devices, where heat is mainly carried by phonons. Phonon transport in crystalline semiconductor materials, such as Si, Ge, GaAs, GaN, etc, has been extensively studied over the past two decades. In fact, study of phonon physics in crystalline semiconductor materials in both bulk and nanostructure forms has been the cornerstone of the emerging field of ‘nanoscale heat transfer’. On the contrary, thermal properties of amorphous materials have been relatively less explored. Recently, however, a growing number of studies have re-examined the thermal properties of amorphous semiconductors, such as amorphous Si. These studies, which included both computational and experimental work, have revealed that phonon transport in amorphous materials is perhaps more complicated than previously thought. For instance, depending on the type of amorphous materials, thermal transport occurs via three types of vibrations: propagons, diffusons, and locons, corresponding to the propagating, diffusion, and localized modes, respectively. The relative contribution of each of these modes dictates the thermal conductivity of the material, including its magnitude and its dependence on sample size and temperature. In this article, we will review the fundamental principles and recent development regarding thermal transport in amorphous semiconductors.

  9. Amorphous boron nitride at high pressure

    NASA Astrophysics Data System (ADS)

    Durandurdu, Murat

    2016-06-01

    The pressure-induced phase transformation in hexagonal boron nitrite and amorphous boron nitrite is studied using ab initio molecular dynamics simulations. The hexagonal-to-wurtzite phase transformation is successfully reproduced in the simulation with a transformation mechanism similar to one suggested in experiment. Amorphous boron nitrite, on the other hand, gradually transforms to a high-density amorphous phase with the application of pressure. This phase transformation is irreversible because a densified amorphous state having both sp3 and sp2 bonds is recovered upon pressure release. The high-density amorphous state mainly consists of sp3 bonds and its local structure is quite similar to recently proposed intermediate boron nitrite phases, in particular tetragonal structure (P42/mnm), rather than the known the wurtzite or cubic boron nitrite due to the existence of four membered rings and edge sharing connectivity. On the basis of this finding we propose that amorphous boron nitrite might be best candidate as a starting structure to synthesize the intermediate phase(s) at high pressure and temperature (probably below 800 °C) conditions.

  10. Wear Resistant Amorphous and Nanocomposite Steel Coatings

    SciTech Connect

    Branagan, Daniel James; Swank, William David; Haggard, Delon C; Fincke, James Russell; Sordelet, D.

    2001-10-01

    In this article, amorphous and nanocomposite thermally deposited steel coatings have been formed by using both plasma and high-velocity oxy-fuel (HVOF) spraying techniques. This was accomplished by developing a specialized iron-based composition with a low critical cooling rate (?104 K/s) for metallic glass formation, processing the alloy by inert gas atomization to form micron-sized amorphous spherical powders, and then spraying the classified powder to form coatings. A primarily amorphous structure was formed in the as-sprayed coatings, independent of coating thickness. After a heat treatment above the crystallization temperature (568°C), the structure of the coatings self-assembled (i.e., devitrified) into a multiphase nanocomposite microstructure with 75 to 125 nm grains containing a distribution of 20 nm second-phase grain-boundary precipitates. Vickers microhardness testing revealed that the amorphous coatings were very hard (10.2 to 10.7 GPa), with further increases in hardness after devitrification (11.4 to 12.8 GPa). The wear characteristics of the amorphous and nanocomposite coatings were determined using both two-body pin-on-disk and three-body rubber wheel wet-slurry sand tests. The results indicate that the amorphous and nanocomposite steel coatings are candidates for a wide variety of wear-resistant applications.

  11. Electrons and phonons in amorphous semiconductors

    NASA Astrophysics Data System (ADS)

    Prasai, Kiran; Biswas, Parthapratim; Drabold, D. A.

    2016-07-01

    The coupling between lattice vibrations and electrons is one of the central concepts of condensed matter physics. The subject has been deeply studied for crystalline materials, but far less so for amorphous and glassy materials, which are among the most important for applications. In this paper, we explore the electron-lattice coupling using current tools of a first-principles computer simulation. We choose three materials to illustrate the phenomena: amorphous silicon (a-Si), amorphous selenium (a-Se) and amorphous gallium nitride (a-GaN). In each case, we show that there is a strong correlation between the localization of electron states and the magnitude of thermally induced fluctuations in energy eigenvalues obtained from the density-functional theory (i.e. Kohn–Sham eigenvalues). We provide a heuristic theory to explain these observations. The case of a-GaN, a topologically disordered partly ionic insulator, is distinctive compared to the covalent amorphous examples. Next, we explore the consequences of changing the charge state of a system as a proxy for tracking photo-induced structural changes in the materials. Where transport is concerned, we lend insight into the Meyer–Neldel compensation rule and discuss a thermally averaged Kubo–Greenwood formula as a means to estimate electrical conductivity and especially its temperature dependence. We close by showing how the optical gap of an amorphous semiconductor can be computationally engineered with the judicious use of Hellmann–Feynman forces (associated with a few defect states) using molecular dynamics simulations. These forces can be used to close or open an optical gap, and identify a structure with a prescribed gap. We use the approach with plane-wave density functional methods to identify a low-energy amorphous phase of silicon including several coordination defects, yet with a gap close to that of good quality a-Si models.

  12. Electrons and phonons in amorphous semiconductors

    NASA Astrophysics Data System (ADS)

    Prasai, Kiran; Biswas, Parthapratim; Drabold, D. A.

    2016-07-01

    The coupling between lattice vibrations and electrons is one of the central concepts of condensed matter physics. The subject has been deeply studied for crystalline materials, but far less so for amorphous and glassy materials, which are among the most important for applications. In this paper, we explore the electron-lattice coupling using current tools of a first-principles computer simulation. We choose three materials to illustrate the phenomena: amorphous silicon (a-Si), amorphous selenium (a-Se) and amorphous gallium nitride (a-GaN). In each case, we show that there is a strong correlation between the localization of electron states and the magnitude of thermally induced fluctuations in energy eigenvalues obtained from the density-functional theory (i.e. Kohn-Sham eigenvalues). We provide a heuristic theory to explain these observations. The case of a-GaN, a topologically disordered partly ionic insulator, is distinctive compared to the covalent amorphous examples. Next, we explore the consequences of changing the charge state of a system as a proxy for tracking photo-induced structural changes in the materials. Where transport is concerned, we lend insight into the Meyer-Neldel compensation rule and discuss a thermally averaged Kubo-Greenwood formula as a means to estimate electrical conductivity and especially its temperature dependence. We close by showing how the optical gap of an amorphous semiconductor can be computationally engineered with the judicious use of Hellmann-Feynman forces (associated with a few defect states) using molecular dynamics simulations. These forces can be used to close or open an optical gap, and identify a structure with a prescribed gap. We use the approach with plane-wave density functional methods to identify a low-energy amorphous phase of silicon including several coordination defects, yet with a gap close to that of good quality a-Si models.

  13. Amorphous Diamond MEMS and Sensors

    SciTech Connect

    SULLIVAN, JOHN P.; FRIEDMANN, THOMAS A.; ASHBY, CAROL I.; DE BOER, MAARTEN P.; SCHUBERT, W. KENT; SHUL, RANDY J.; HOHLFELDER, ROBERT J.; LAVAN, D.A.

    2002-06-01

    This report describes a new microsystems technology for the creation of microsensors and microelectromechanical systems (MEMS) using stress-free amorphous diamond (aD) films. Stress-free aD is a new material that has mechanical properties close to that of crystalline diamond, and the material is particularly promising for the development of high sensitivity microsensors and rugged and reliable MEMS. Some of the unique properties of aD include the ability to easily tailor film stress from compressive to slightly tensile, hardness and stiffness 80-90% that of crystalline diamond, very high wear resistance, a hydrophobic surface, extreme chemical inertness, chemical compatibility with silicon, controllable electrical conductivity from insulating to conducting, and biocompatibility. A variety of MEMS structures were fabricated from this material and evaluated. These structures included electrostatically-actuated comb drives, micro-tensile test structures, singly- and doubly-clamped beams, and friction and wear test structures. It was found that surface micromachined MEMS could be fabricated in this material easily and that the hydrophobic surface of the film enabled the release of structures without the need for special drying procedures or the use of applied hydrophobic coatings. Measurements using these structures revealed that aD has a Young's modulus of {approx}650 GPa, a tensile fracture strength of 8 GPa, and a fracture toughness of 8 MPa{center_dot}m {sup 1/2}. These results suggest that this material may be suitable in applications where stiction or wear is an issue. Flexural plate wave (FPW) microsensors were also fabricated from aD. These devices use membranes of aD as thin as {approx}100 nm. The performance of the aD FPW sensors was evaluated for the detection of volatile organic compounds using ethyl cellulose as the sensor coating. For comparable membrane thicknesses, the aD sensors showed better performance than silicon nitride based sensors. Greater than

  14. Amorphous Silicon Based Neutron Detector

    SciTech Connect

    Xu, Liwei

    2004-12-12

    Various large-scale neutron sources already build or to be constructed, are important for materials research and life science research. For all these neutron sources, neutron detectors are very important aspect. However, there is a lack of a high-performance and low-cost neutron beam monitor that provides time and temporal resolution. The objective of this SBIR Phase I research, collaboratively performed by Midwest Optoelectronics, LLC (MWOE), the University of Toledo (UT) and Oak Ridge National Laboratory (ORNL), is to demonstrate the feasibility for amorphous silicon based neutron beam monitors that are pixilated, reliable, durable, fully packaged, and fabricated with high yield using low-cost method. During the Phase I effort, work as been focused in the following areas: 1) Deposition of high quality, low-defect-density, low-stress a-Si films using very high frequency plasma enhanced chemical vapor deposition (VHF PECVD) at high deposition rate and with low device shunting; 2) Fabrication of Si/SiO2/metal/p/i/n/metal/n/i/p/metal/SiO2/ device for the detection of alpha particles which are daughter particles of neutrons through appropriate nuclear reactions; and 3) Testing of various devices fabricated for alpha and neutron detection; As the main results: · High quality, low-defect-density, low-stress a-Si films have been successfully deposited using VHF PECVD on various low-cost substrates; · Various single-junction and double junction detector devices have been fabricated; · The detector devices fabricated have been systematically tested and analyzed. · Some of the fabricated devices are found to successfully detect alpha particles. Further research is required to bring this Phase I work beyond the feasibility demonstration toward the final prototype devices. The success of this project will lead to a high-performance, low-cost, X-Y pixilated neutron beam monitor that could be used in all of the neutron facilities worldwide. In addition, the technologies

  15. Understanding Thermal Conductivity in Amorphous Materials

    NASA Astrophysics Data System (ADS)

    Kommandur, Sampath; Yee, Shannon

    2014-03-01

    Current energy technologies such as thermoelectrics, photovoltaics, and LEDs make extensive use of amorphous materials and are limited by heat transfer. Device improvements necessitate a better understanding of the thermal conductivity in amorphous materials. While there are basic theories that capture the trends in thermal conductivity of a select set of amorphous materials, a general framework is needed to explain the fundamental transport of heat in all amorphous materials. One empirical theory that has been successful at describing the thermal conductivity in some materials is the k-min model, however, assumptions in that model limit its generalizability. Another theory defines the existence of propagons, diffusons, and locons, which constitute vibrational modes that carry heat. Our work first presents a summary of literature on the thermal conductivity in amorphous materials and then compares those theories to a breadth of experimental data. Based upon those results, a generic model is proposed that is widely applicable with the ultimate goal of this work being to describe the temperature dependent thermal conductivity of polymers. -/abstract- Sampath Kommandur and Shannon K. Yee 21.1.1: Thermoelectric Phenomena, Materials, Devices, and Applications (GER

  16. SURVIVAL OF AMORPHOUS WATER ICE ON CENTAURS

    SciTech Connect

    Guilbert-Lepoutre, Aurelie

    2012-10-01

    Centaurs are believed to be Kuiper Belt objects in transition between Jupiter and Neptune before possibly becoming Jupiter family comets. Some indirect observational evidence is consistent with the presence of amorphous water ice in Centaurs. Some of them also display a cometary activity, probably triggered by the crystallization of the amorphous water ice, as suggested by Jewitt and this work. Indeed, we investigate the survival of amorphous water ice against crystallization, using a fully three-dimensional thermal evolution model. Simulations are performed for varying heliocentric distances and obliquities. They suggest that crystallization can be triggered as far as 16 AU, though amorphous ice can survive beyond 10 AU. The phase transition is an efficient source of outgassing up to 10-12 AU, which is broadly consistent with the observations of the active Centaurs. The most extreme case is 167P/CINEOS, which barely crystallizes in our simulations. However, amorphous ice can be preserved inside Centaurs in many heliocentric distance-obliquity combinations, below a {approx}5-10 m crystallized crust. We also find that outgassing due to crystallization cannot be sustained for a time longer than 10{sup 4}-10{sup 4} years, leading to the hypothesis that active Centaurs might have recently suffered from orbital changes. This could be supported by both observations (although limited) and dynamical studies.

  17. Synthesis method for amorphous metallic foam

    NASA Astrophysics Data System (ADS)

    Schroers, Jan; Veazey, Chris; Demetriou, Marios D.; Johnson, William L.

    2004-12-01

    A synthesis method for the production of amorphous metallic foam is introduced. This method utilizes the thermodynamic stability and thermoplastic formability of the supercooled liquid state to produce low-density amorphous metallic foams in dimensions that are not limited to the critical casting thickness. The method consists of three stages: the prefoaming stage, in which a large number of small bubbles are created in the equilibrium liquid under pressure; the quenching stage, in which the liquid prefoam is quenched to its amorphous state; the foam expansion stage, in which the amorphous prefoam is reheated to the supercooled liquid region and is processed under pressures substantially lower than those applied in the prefoaming step. Results from a dynamic model suggest that the foam expansion process is feasible, as the kinetics of bubble expansion in the supercooled liquid region are faster than the kinetics of crystallization. Within the proposed synthesis method, bulk amorphous foam products characterized by bubble volume fractions of as high as 85% are successfully produced.

  18. Amorphous metallic films in silicon metallization systems

    NASA Technical Reports Server (NTRS)

    So, F.; Kolawa, E.; Nicolet, M. A.

    1985-01-01

    Diffusion barrier research was focussed on lowering the chemical reactivity of amorphous thin films on silicon. An additional area of concern is the reaction with metal overlays such as aluminum, silver, and gold. Gold was included to allow for technology transfer to gallium arsenide PV cells. Amorphous tungsten nitride films have shown much promise. Stability to annealing temperatures of 700, 800, and 550 C were achieved for overlays of silver, gold, and aluminum, respectively. The lower results for aluminum were not surprising because there is an eutectic that can form at a lower temperature. It seems that titanium and zirconium will remove the nitrogen from a tungsten nitride amorphous film and render it unstable. Other variables of research interest were substrate bias and base pressure during sputtering.

  19. Phase transitions in biogenic amorphous calcium carbonate.

    PubMed

    Gong, Yutao U T; Killian, Christopher E; Olson, Ian C; Appathurai, Narayana P; Amasino, Audra L; Martin, Michael C; Holt, Liam J; Wilt, Fred H; Gilbert, P U P A

    2012-04-17

    Crystalline biominerals do not resemble faceted crystals. Current explanations for this property involve formation via amorphous phases. Using X-ray absorption near-edge structure (XANES) spectroscopy and photoelectron emission microscopy (PEEM), here we examine forming spicules in embryos of Strongylocentrotus purpuratus sea urchins, and observe a sequence of three mineral phases: hydrated amorphous calcium carbonate (ACC · H(2)O) → dehydrated amorphous calcium carbonate (ACC) → calcite. Unexpectedly, we find ACC · H(2)O-rich nanoparticles that persist after the surrounding mineral has dehydrated and crystallized. Protein matrix components occluded within the mineral must inhibit ACC · H(2)O dehydration. We devised an in vitro, also using XANES-PEEM, assay to identify spicule proteins that may play a role in stabilizing various mineral phases, and found that the most abundant occluded matrix protein in the sea urchin spicules, SM50, stabilizes ACC · H(2)O in vitro. PMID:22492931

  20. IUE observations of amorphous hot galaxies

    NASA Technical Reports Server (NTRS)

    Lamb, S. A.; Hjellming, M. S.; Gallagher, J. S., III; Hunter, D. A.

    1985-01-01

    Blue amorphous galaxies are star-forming, irregularlike systems which lack the spatially distinct OB stellar groups that are characteristic of most late-type galaxies. In order to better understand the nature of star-formation processes in these unusual galaxies, short-wavelength IUE spectra of the amorphous galaxies NGC 1705 and NGC 1800 have been obtained. It is found that NGC 1705 contains a normal mix of OB stars, which is consistent with the nearly constant recent star-formation rate inferred from new optical data. NGC 1800 is likely to have similar properties, and blue galaxies with amorphous structures thus do not show evidence for anomalies in stellar populations. The UV spectra of these galaxies and a variety of other hot extragalactic stellar systems in fact have similar characteristics, which suggests OB stellar populations are often homogeneous in their properties.

  1. Synthesis and photocurrent of amorphous boron nanowires.

    PubMed

    Ge, Liehui; Lei, Sidong; Hart, Amelia H C; Gao, Guanhui; Jafry, Huma; Vajtai, Robert; Ajayan, Pulickel M

    2014-08-22

    Although theoretically feasible, synthesis of boron nanostructures is challenging due to the highly reactive nature, high melting and boiling points of boron. We have developed a thermal vapor transfer approach to synthesizing amorphous boron nanowire using a solid boron source. The amorphous nature and chemical composition of boron nanowires were characterized by high resolution transmission electron microscopy, selected area electron diffraction, and electron energy loss spectroscopy. Optical properties and photoconduction of boron nanowires have not yet been reported. In our investigation, the amorphous boron nanowire showed much better optical and electrical properties than previously reported photo-response of crystalline boron nanobelts. When excited by a blue LED, the photo/dark current ratio (I/I₀) is 1.5 and time constants in the order of tens of seconds. I/I₀ is 1.17 using a green light. PMID:25061013

  2. Superior radiation tolerant materials: Amorphous silicon oxycarbide

    NASA Astrophysics Data System (ADS)

    Nastasi, Michael; Su, Qing; Price, Lloyd; Colón Santana, Juan A.; Chen, Tianyi; Balerio, Robert; Shao, Lin

    2015-06-01

    We studied the radiation tolerance of amorphous silicon oxycarbide (SiOC) alloys by combining ion irradiation, X-ray diffraction (XRD) and transmission electron microscopy (TEM). The amorphous SiOC alloys thin films were grown via co-sputtering from SiO2 and SiC (amorphous phase) targets either on a surface oxidized Si (100) substrate or on a sodium chloride substrate. By controlling the sputtering rate of each target, SiOC alloys with different compositions (1:2, 1:1, 2:1 ratios) were obtained. These alloys were irradiated by 100 keV He+ ions at both room temperature and 600 °C with damage levels ranging from 1 to 20 displacements per atom (dpa). TEM characterization shows no sign of crystallization, void formation or segregation in all irradiated samples. Our findings suggest that SiOC alloys are a class of promising radiation-tolerant materials.

  3. Enthalpy of crystallization of amorphous yttrium oxide

    SciTech Connect

    Reznitskii, L.A.

    1988-02-01

    Measurements have been made on the enthalpies of crystallization of amorphous Fe/sub 2/O/sub 3/ and Y/sub 3/Fe/sub 5/O/sub 12/ from amorphous Fe/sub 2/O/sub 3/ and Y/sub 2/O/sub 3/ as determined by the DSC method. The heat of crystallization for Y/sub 2/O/sub 3am/ does not make itself felt on the heating thermogram, in contrast to that for Fe/sub 2/O/sub 3/, evidently because it is spread out over a wide temperature range, so it is difficult to measure. One can combine thermochemical equations to calculate the enthalpy of crystallization for amorphous yttrium oxide as ..delta..H = -24.9 kJ/mole.

  4. The Phagocytosis and Toxicity of Amorphous Silica

    PubMed Central

    Costantini, Lindsey M.; Gilberti, Renée M.; Knecht, David A.

    2011-01-01

    Background Inhalation of crystalline silica is known to cause an inflammatory reaction and chronic exposure leads to lung fibrosis and can progress into the disease, silicosis. Cultured macrophages bind crystalline silica particles, phagocytose them, and rapidly undergo apoptotic and necrotic death. The mechanism by which particles are bound and internalized and the reason particles are toxic is unclear. Amorphous silica has been considered to be a less toxic form, but this view is controversial. We compared the uptake and toxicity of amorphous silica to crystalline silica. Methodology/Principal Findings Amorphous silica particles are phagocytosed by macrophage cells and a single internalized particle is capable of killing a cell. Fluorescent dextran is released from endo-lysosomes within two hours after silica treatment and Caspase-3 activation occurs within 4 hours. Interestingly, toxicity is specific to macrophage cell lines. Other cell types are resistant to silica particle toxicity even though they internalize the particles. The large and uniform size of the spherical, amorphous silica particles allowed us to monitor them during the uptake process. In mCherry-actin transfected macrophages, actin rings began to form 1-3 minutes after silica binding and the actin coat disassembled rapidly following particle internalization. Pre-loading cells with fluorescent dextran allowed us to visualize the fusion of phagosomes with endosomes during internalization. These markers provided two new ways to visualize and quantify particle internalization. At 37°C the rate of amorphous silica internalization was very rapid regardless of particle coating. However, at room temperature, opsonized silica is internalized much faster than non-opsonized silica. Conclusions/Significance Our results indicate that amorphous and crystalline silica are both phagocytosed and both toxic to mouse alveolar macrophage (MH-S) cells. The pathway leading to apoptosis appears to be similar in both

  5. Cooling of hot electrons in amorphous silicon

    SciTech Connect

    Vanderhaghen, R.; Hulin, D.; Cuzeau, S.; White, J.O.

    1997-07-01

    Measurements of the cooling rate of hot carriers in amorphous silicon are made with a two-pump, one-probe technique. The experiment is simulated with a rate-equation model describing the energy transfer between a population of hot carriers and the lattice. An energy transfer rate proportional to the temperature difference is found to be consistent with the experimental data while an energy transfer independent of the temperature difference is not. This contrasts with the situation in crystalline silicon. The measured cooling rates are sufficient to explain the difficulty in observing avalanche effects in amorphous silicon.

  6. Thermal conductivity of sputtered amorphous Ge films

    SciTech Connect

    Zhan, Tianzhuo; Xu, Yibin; Goto, Masahiro; Tanaka, Yoshihisa; Kato, Ryozo; Sasaki, Michiko; Kagawa, Yutaka

    2014-02-15

    We measured the thermal conductivity of amorphous Ge films prepared by magnetron sputtering. The thermal conductivity was significantly higher than the value predicted by the minimum thermal conductivity model and increased with deposition temperature. We found that variations in sound velocity and Ge film density were not the main factors in the high thermal conductivity. Fast Fourier transform patterns of transmission electron micrographs revealed that short-range order in the Ge films was responsible for their high thermal conductivity. The results provide experimental evidences to understand the underlying nature of the variation of phonon mean free path in amorphous solids.

  7. Production feature of soft magnetic amorphous alloys

    NASA Astrophysics Data System (ADS)

    Tyagunov, A. G.; Baryshev, E. E.; Shmakova, K. Yu

    2016-06-01

    Methods for making nanocrystalline alloys have been discussed. Temperature dependences of the surface tension (σ), electric resistivity (ρ), magnetic susceptibility (χ) and kinematic viscosity (ν) have been obtained. Comparison of the properties of amorphous ribbons obtained by the pilot and serial technologies has been conducted. Science-based technology of multi-component alloy smelting makes it possible to prepare equilibrium smelt, the structure of which has a significant effect on the properties of the amorphous ribbon before spinning and kinetics of its crystallization has been offered.

  8. Ion bombardment and disorder in amorphous silicon

    SciTech Connect

    Sidhu, L.S.; Gaspari, F.; Zukotynski, S.

    1997-07-01

    The effect of ion bombardment during growth on the structural and optical properties of amorphous silicon are presented. Two series of films were deposited under electrically grounded and positively biased substrate conditions. The biased samples displayed lower growth rates and increased hydrogen content relative to grounded counterparts. The film structure was examined using Raman spectroscopy. The transverse optic like phonon band position was used as a parameter to characterize network order. Biased samples displayed an increased order of the amorphous network relative to grounded samples. Furthermore, biased samples exhibited a larger optical gap. These results are correlated and attributed to reduced ion bombardment effects.

  9. Short range order in amorphous polycondensates

    SciTech Connect

    Lamers, C.; Richter, D.; Schweika, W.; Batoulis, J.; Sommer, K.; Cable, J.W.; Shapiro, S.M.

    1992-12-01

    The static coherent structure factors S(Q) of the polymer glass Bisphenol-A-Polycarbonate and its chemical variation Bisphenol-A- Polyctherkctone- both in differently deuterated versions- have been measured by spin polarized neutron scattering. The method of spin polarization analysis provided an experimental separation of coherent and incoherent scattering and a reliable intensity calibration. Results are compared to structure factors calculated for model structures which were obtained by ``amorphous cell`` computer simulations. In general reasonable agreement is found between experiment and simulation; however, certain discrepancies hint at an insufficient structural relaxation in the amorphous cell method. 15 refs, 1 fig, 1 tab.

  10. Amorphous Insulator Films With Controllable Properties

    NASA Technical Reports Server (NTRS)

    Alterovitz, Samuel A.; Warner, Joseph D.; Liu, David C.; Pouch, John J.

    1987-01-01

    In experiments described in report, amorphous hydrogenated carbon films grown at room temperature by low-frequency plasma deposition, using methane or butane gas. Films have unique array of useful properties; (a) adhere to wide variety of materials; (b) contain only carbon and hydrogen; (c) smooth and free of pinholes; (d) resistant to attack by moisture and chemicals; and (e) have high electric-breakdown strength and electrical resistivity. Two of optical properties and hardness of this film controlled by deposition conditions. Amorphous a-C:H and BN films used for hermetic sealing and protection of optical, electronic, magnetic, or delicate mechanical systems, and for semiconductor field dielectrics.

  11. New Amorphous Silicon Alloy Systems

    NASA Astrophysics Data System (ADS)

    Kapur, Mridula N.

    1990-01-01

    The properties of hydrogenated amorphous silicon (a-Si:H) have been modified by alloying with Al, Ga and S respectively. The Al and Ga alloys are in effect quaternary alloys as they were fabricated in a carbon-rich discharge. The alloys were prepared by the plasma assisted chemical vapor deposition (PACVD) method. This method has several advantages, the major one being the relatively low defect densities of the resulting materials. The PACVD system used to grow the alloy films was designed and constructed in the laboratory. It was first tested with known (a-Si:H and a-Si:As:H) materials. Thus, it was established that device quality alloy films could be grown with the home-made PACVD setup. The chemical composition of the alloys was characterized by secondary ion mass spectrometry (SIMS), and electron probe microanalysis (EPMA). The homogeneous nature of hydrogen distribution in the alloys was established by SIMS depth profile analysis. A quantitative analysis of the bulk elemental content was carried out by EPMA. The analysis indicated that the alloying element was incorporated in the films more efficiently at low input gas concentrations than at the higher concentrations. A topological model was proposed to explain the observed behavior. The optical energy gap of the alloys could be varied in the 0.90 to 1.92 eV range. The Al and Ga alloys were low band gap materials, whereas alloying with S had the effect of widening the energy gap. It was observed that although the Si-Al and Si-Ga alloys contained significant amounts of C and H, the magnitude of the energy gap was determined by the metallic component. The various trends in optical properties could be related to the binding characteristics of the respective alloy systems. A quantitative explanation of the results was provided by White's tight binding model. The dark conductivity-temperature dependence of the alloys was examined. A linear dependence was observed for the Al and Ga systems. Electronic conduction in

  12. Physical Properties Variation of Graphene and Multi Wall Carbon Nanotubes by Planetary Ball Mill and Heat Treatment

    NASA Astrophysics Data System (ADS)

    Jo, G.; Mahmudul Haque, A. K. M.; Kim, S.; Jeong, H.; Chung, H.

    2015-09-01

    The article reports the experimental study of graphene, multiwall carbon nanotubes and their composite where samples are made by applying dry grinding and wet grinding as well as heat treatment processes. The investigation information is recorded and compared by SEM analysis, EDS spectrum and density measurement which give the informative evidence. And finally the article tries to find the basic difference in physical properties of these samples.

  13. Controlling the number of walls in multi walled carbon nanotubes/alumina hybrid compound via ball milling of precipitate catalyst

    NASA Astrophysics Data System (ADS)

    Nosbi, Norlin; Akil, Hazizan Md

    2015-06-01

    This paper reports the influence of milling time on the structure and properties of the precipitate catalyst of multi walled carbon nanotubes (MWCNT)/alumina hybrid compound, produced through the chemical vapour deposition (CVD) process. For this purpose, light green precipitate consisted of aluminium, nickel(II) nitrate hexahydrate and sodium hydroxide mixture was placed in a planetary mill equipped with alumina vials using alumina balls at 300 rpm rotation speed for various milling time (5-15 h) prior to calcinations and CVD process. The compound was characterized using various techniques. Based on high-resolution transmission electron microscopy analysis, increasing the milling time up to 15 h decreased the diameter of MWCNT from 32.3 to 13.1 nm. It was noticed that the milling time had a significant effect on MWCNT wall thickness, whereby increasing the milling time from 0 to 15 h reduced the number of walls from 29 to 12. It was also interesting to note that the carbon content increased from 23.29 wt.% to 36.37 wt.% with increasing milling time.

  14. Amorphization and nanocrystallization of silcon under shock compression

    SciTech Connect

    Remington, B. A.; Wehrenberg, C. E.; Zhao, S.; Hahn, E. N.; Kad, B.; Bringa, E. M.; Meyers, M. A.

    2015-11-06

    High-power, short-duration, laser-driven, shock compression and recovery experiments on [001] silicon unveiled remarkable structural changes above a pressure threshold. Two distinct amorphous regions were identified: (a) a bulk amorphous layer close to the surface and (b) amorphous bands initially aligned with {111} slip planes. Further increase of the laser energy leads to the re-crystallization of amorphous silicon into nanocrystals with high concentration of nano-twins. This amorphization is produced by the combined effect of high magnitude hydrostatic and shear stresses under dynamic shock compression. Shock-induced defects play a very important role in the onset of amorphization. Calculations of the free energy changes with pressure and shear, using the Patel-Cohen methodology, are in agreement with the experimental results. Molecular dynamics simulation corroborates the amorphization, showing that it is initiated by the nucleation and propagation of partial dislocations. As a result, the nucleation of amorphization is analyzed qualitatively by classical nucleation theory.

  15. Inverted amorphous silicon solar cell utilizing cermet layers

    DOEpatents

    Hanak, Joseph J.

    1979-01-01

    An amorphous silicon solar cell incorporating a transparent high work function metal cermet incident to solar radiation and a thick film cermet contacting the amorphous silicon opposite to said incident surface.

  16. High resolution amorphous silicon radiation detectors

    DOEpatents

    Street, Robert A.; Kaplan, Selig N.; Perez-Mendez, Victor

    1992-01-01

    A radiation detector employing amorphous Si:H cells in an array with each detector cell having at least three contiguous layers (n type, intrinsic, p type), positioned between two electrodes to which a bias voltage is applied. An energy conversion layer atop the silicon cells intercepts incident radiation and converts radiation energy to light energy of a wavelength to which the silicon cells are responsive. A read-out device, positioned proximate to each detector element in an array allows each such element to be interrogated independently to determine whether radiation has been detected in that cell. The energy conversion material may be a layer of luminescent material having a columnar structure. In one embodiment a column of luminescent material detects the passage therethrough of radiation to be detected and directs a light beam signal to an adjacent a-Si:H film so that detection may be confined to one or more such cells in the array. One or both electrodes may have a comb structure, and the teeth of each electrode comb may be interdigitated for capacitance reduction. The amorphous Si:H film may be replaced by an amorphous Si:Ge:H film in which up to 40 percent of the amorphous material is Ge. Two dimensional arrays may be used in X-ray imaging, CT scanning, crystallography, high energy physics beam tracking, nuclear medicine cameras and autoradiography.

  17. High resolution amorphous silicon radiation detectors

    DOEpatents

    Street, R.A.; Kaplan, S.N.; Perez-Mendez, V.

    1992-05-26

    A radiation detector employing amorphous Si:H cells in an array with each detector cell having at least three contiguous layers (n-type, intrinsic, p-type), positioned between two electrodes to which a bias voltage is applied. An energy conversion layer atop the silicon cells intercepts incident radiation and converts radiation energy to light energy of a wavelength to which the silicon cells are responsive. A read-out device, positioned proximate to each detector element in an array allows each such element to be interrogated independently to determine whether radiation has been detected in that cell. The energy conversion material may be a layer of luminescent material having a columnar structure. In one embodiment a column of luminescent material detects the passage therethrough of radiation to be detected and directs a light beam signal to an adjacent a-Si:H film so that detection may be confined to one or more such cells in the array. One or both electrodes may have a comb structure, and the teeth of each electrode comb may be interdigitated for capacitance reduction. The amorphous Si:H film may be replaced by an amorphous Si:Ge:H film in which up to 40 percent of the amorphous material is Ge. Two dimensional arrays may be used in X-ray imaging, CT scanning, crystallography, high energy physics beam tracking, nuclear medicine cameras and autoradiography. 18 figs.

  18. Excess specific heat in evaporated amorphous silicon.

    PubMed

    Queen, D R; Liu, X; Karel, J; Metcalf, T H; Hellman, F

    2013-03-29

    The specific heat C of e-beam evaporated amorphous silicon (a-Si) thin films prepared at various growth temperatures T(S) and thicknesses t was measured from 2 to 300 K, along with sound velocity v, shear modulus G, density n(Si), and Raman spectra. Increasing T(S) results in a more ordered amorphous network with increases in n(Si), v, G, and a decrease in bond angle disorder. Below 20 K, an excess C is seen in films with less than full density where it is typical of an amorphous solid, with both a linear term characteristic of two-level systems (TLS) and an additional (non-Debye) T3 contribution. The excess C is found to be independent of the elastic properties but to depend strongly on density. The density dependence suggests that low energy glassy excitations can form in a-Si but only in microvoids or low density regions and are not intrinsic to the amorphous silicon network. A correlation is found between the density of TLS n0 and the excess T3 specific heat c(ex) suggesting that they have a common origin.

  19. Metal electrode for amorphous silicon solar cells

    DOEpatents

    Williams, Richard

    1983-01-01

    An amorphous silicon solar cell having an N-type region wherein the contact to the N-type region is composed of a material having a work function of about 3.7 electron volts or less. Suitable materials include strontium, barium and magnesium and rare earth metals such as gadolinium and yttrium.

  20. Transient amorphous calcium phosphate in forming enamel.

    PubMed

    Beniash, Elia; Metzler, Rebecca A; Lam, Raymond S K; Gilbert, P U P A

    2009-05-01

    Enamel, the hardest tissue in the body, begins as a three-dimensional network of nanometer size mineral particles, suspended in a protein gel. This mineral network serves as a template for mature enamel formation. To further understand the mechanisms of enamel formation we characterized the forming enamel mineral at an early secretory stage using X-ray absorption near-edge structure (XANES) spectromicroscopy, transmission electron microscopy (TEM), FTIR microspectroscopy and polarized light microscopy. We show that the newly formed enamel mineral is amorphous calcium phosphate (ACP), which eventually transforms into apatitic crystals. Interestingly, the size, shape and spatial organization of these amorphous mineral particles and older crystals are essentially the same, indicating that the mineral morphology and organization in enamel is determined prior to its crystallization. Mineralization via transient amorphous phases has been previously reported in chiton teeth, mollusk shells, echinoderm spicules and spines, and recent reports strongly suggest the presence of transient amorphous mineral in forming vertebrate bones. The present finding of transient ACP in murine tooth enamel suggests that this strategy might be universal. PMID:19217943

  1. 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.

  2. A rational synthesis of hierarchically porous, N-doped carbon from Mg-based MOFs: understanding the link between nitrogen content and oxygen reduction electrocatalysis.

    PubMed

    Eisenberg, David; Stroek, Wowa; Geels, Norbert J; Tanase, Stefania; Ferbinteanu, Marilena; Teat, Simon J; Mettraux, Pierre; Yan, Ning; Rothenberg, Gadi

    2016-07-27

    Controlled mixtures of novel Mg-based metal-organic frameworks (MOFs) were prepared, with H(+) or K(+) as counterions. A linear relation was found between synthesis pH and K/H ratio in the resultant mixture, establishing the tunability of the synthesis. Upon pyrolysis, these precursor mixtures yield nitrogen-doped, hierarchically porous carbons, which have good activity towards the oxygen reduction reaction (ORR) at pH 13. The nitrogen content varies significantly along the homologous carbon series (>400%, 1.3 at% to 5.7 at%), to a much greater extent than microstructural parameters such as surface area and graphitization. This allows us to isolate the positive correlation between nitrogen content and electrocatalytic oxygen reduction ORR activity in this class of metal-free, N-doped, porous carbons. PMID:27412725

  3. Amorphous silica-like carbon dioxide.

    PubMed

    Santoro, Mario; Gorelli, Federico A; Bini, Roberto; Ruocco, Giancarlo; Scandolo, Sandro; Crichton, Wilson A

    2006-06-15

    Among the group IV elements, only carbon forms stable double bonds with oxygen at ambient conditions. At variance with silica and germania, the non-molecular single-bonded crystalline form of carbon dioxide, phase V, only exists at high pressure. The amorphous forms of silica (a-SiO2) and germania (a-GeO2) are well known at ambient conditions; however, the amorphous, non-molecular form of CO2 has so far been described only as a result of first-principles simulations. Here we report the synthesis of an amorphous, silica-like form of carbon dioxide, a-CO2, which we call 'a-carbonia'. The compression of the molecular phase III of CO2 between 40 and 48 GPa at room temperature initiated the transformation to the non-molecular amorphous phase. Infrared spectra measured at temperatures up to 680 K show the progressive formation of C-O single bonds and the simultaneous disappearance of all molecular signatures. Furthermore, state-of-the-art Raman and synchrotron X-ray diffraction measurements on temperature-quenched samples confirm the amorphous character of the material. Comparison with vibrational and diffraction data for a-SiO2 and a-GeO2, as well as with the structure factor calculated for the a-CO2 sample obtained by first-principles molecular dynamics, shows that a-CO2 is structurally homologous to the other group IV dioxide glasses. We therefore conclude that the class of archetypal network-forming disordered systems, including a-SiO2, a-GeO2 and water, must be extended to include a-CO2. PMID:16778885

  4. Pressure-induced amorphous-to-amorphous configuration change in Ca-Al metallic glasses

    PubMed Central

    Lou, H. B.; Fang, Y. K.; Zeng, Q. S.; Lu, Y. H.; Wang, X. D.; Cao, Q. P.; Yang, K.; Yu, X. H.; Zheng, L.; Zhao, Y. D.; Chu, W. S.; Hu, T. D.; Wu, Z. Y.; Ahuja, R.; Jiang, J. Z.

    2012-01-01

    Pressure-induced amorphous-to-amorphous configuration changes in Ca-Al metallic glasses (MGs) were studied by performing in-situ room-temperature high-pressure x-ray diffraction up to about 40 GPa. Changes in compressibility at about 18 GPa, 15.5 GPa and 7.5 GPa during compression are detected in Ca80Al20, Ca72.7Al27.3, and Ca66.4Al33.6 MGs, respectively, whereas no clear change has been detected in the Ca50Al50 MG. The transfer of s electrons into d orbitals under pressure, reported for the pressure-induced phase transformations in pure polycrystalline Ca, is suggested to explain the observation of an amorphous-to-amorphous configuration change in this Ca-Al MG system. Results presented here show that the pressure induced amorphous-to-amorphous configuration is not limited to f electron-containing MGs. PMID:22530094

  5. 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.

  6. Defect-induced solid state amorphization of molecular crystals

    NASA Astrophysics Data System (ADS)

    Lei, Lei; Carvajal, Teresa; Koslowski, Marisol

    2012-04-01

    We investigate the process of mechanically induced amorphization in small molecule organic crystals under extensive deformation. In this work, we develop a model that describes the amorphization of molecular crystals, in which the plastic response is calculated with a phase field dislocation dynamics theory in four materials: acetaminophen, sucrose, γ-indomethacin, and aspirin. The model is able to predict the fraction of amorphous material generated in single crystals for a given applied stress. Our results show that γ-indomethacin and sucrose demonstrate large volume fractions of amorphous material after sufficient plastic deformation, while smaller amorphous volume fractions are predicted in acetaminophen and aspirin, in agreement with experimental observation.

  7. Atomic-scale disproportionation in amorphous silicon monoxide

    NASA Astrophysics Data System (ADS)

    Hirata, Akihiko; Kohara, Shinji; Asada, Toshihiro; Arao, Masazumi; Yogi, Chihiro; Imai, Hideto; Tan, Yongwen; Fujita, Takeshi; Chen, Mingwei

    2016-05-01

    Solid silicon monoxide is an amorphous material which has been commercialized for many functional applications. However, the amorphous structure of silicon monoxide is a long-standing question because of the uncommon valence state of silicon in the oxide. It has been deduced that amorphous silicon monoxide undergoes an unusual disproportionation by forming silicon- and silicon-dioxide-like regions. Nevertheless, the direct experimental observation is still missing. Here we report the amorphous structure characterized by angstrom-beam electron diffraction, supplemented by synchrotron X-ray scattering and computer simulations. In addition to the theoretically predicted amorphous silicon and silicon-dioxide clusters, suboxide-type tetrahedral coordinates are detected by angstrom-beam electron diffraction at silicon/silicon-dioxide interfaces, which provides compelling experimental evidence on the atomic-scale disproportionation of amorphous silicon monoxide. Eventually we develop a heterostructure model of the disproportionated silicon monoxide which well explains the distinctive structure and properties of the amorphous material.

  8. Amorphous-crystalline transition in thermoelectric NbO2

    NASA Astrophysics Data System (ADS)

    Music, Denis; Chen, Yen-Ting; Bliem, Pascal; Geyer, Richard W.

    2015-06-01

    Density functional theory was employed to design enhanced amorphous NbO2 thermoelectrics. The covalent-ionic nature of Nb-O bonding is identical in amorphous NbO2 and its crystalline counterpart. However, the Anderson localisation occurs in amorphous NbO2, which may affect the transport properties. We calculate a multifold increase in the absolute Seebeck coefficient for the amorphous state. These predictions were critically appraised by measuring the Seebeck coefficient of sputtered amorphous and crystalline NbO2 thin films with the identical short-range order. The first-order phase transition occurs at approximately 550 °C, but amorphous NbO2 possesses enhanced transport properties at all temperatures. Amorphous NbO2, reaching  -173 μV K-1, exhibits up to a 29% larger absolute Seebeck coefficient value, thereby validating the predictions.

  9. Atomic-scale disproportionation in amorphous silicon monoxide.

    PubMed

    Hirata, Akihiko; Kohara, Shinji; Asada, Toshihiro; Arao, Masazumi; Yogi, Chihiro; Imai, Hideto; Tan, Yongwen; Fujita, Takeshi; Chen, Mingwei

    2016-05-13

    Solid silicon monoxide is an amorphous material which has been commercialized for many functional applications. However, the amorphous structure of silicon monoxide is a long-standing question because of the uncommon valence state of silicon in the oxide. It has been deduced that amorphous silicon monoxide undergoes an unusual disproportionation by forming silicon- and silicon-dioxide-like regions. Nevertheless, the direct experimental observation is still missing. Here we report the amorphous structure characterized by angstrom-beam electron diffraction, supplemented by synchrotron X-ray scattering and computer simulations. In addition to the theoretically predicted amorphous silicon and silicon-dioxide clusters, suboxide-type tetrahedral coordinates are detected by angstrom-beam electron diffraction at silicon/silicon-dioxide interfaces, which provides compelling experimental evidence on the atomic-scale disproportionation of amorphous silicon monoxide. Eventually we develop a heterostructure model of the disproportionated silicon monoxide which well explains the distinctive structure and properties of the amorphous material.

  10. Characterization of Poly-Amorphous Indomethacin by Terahertz Spectroscopy

    NASA Astrophysics Data System (ADS)

    Otsuka, Makoto; Nishizawa, Jun-ichi; Fukura, Naomi; Sasaki, Tetsuo

    2012-09-01

    Since the stability of amorphous solids of pharmaceuticals differs depending on the method of preparation, there are several solid-state chemical structures in amorphous solids, which like poly-amorphous solids might have different characteristics the same as in crystalline solids. However, it is not easy to identify the differences in solid-state characteristics between amorphous solids using conventional analytical methods, such as powder X-ray diffraction analysis, since all of the poly-amorphous solids had similar halo X-ray diffraction patterns. However, terahertz spectroscopy can distinguish the amorphous solids of indomethacin with different physicochemical properties, and is expected to provide a rapid and non-destructive qualitative analysis for the solid materials, it would be useful for the qualitative evaluation of amorphous solids in the pharmaceutical industry.

  11. Characterization of Poly-Amorphous Indomethacin by Terahertz Spectroscopy

    NASA Astrophysics Data System (ADS)

    Otsuka, Makoto; Nishizawa, Jun-ichi; Fukura, Naomi; Sasaki, Tetsuo

    2012-05-01

    Since the stability of amorphous solids of pharmaceuticals differs depending on the method of preparation, there are several solid-state chemical structures in amorphous solids, which like poly-amorphous solids might have different characteristics the same as in crystalline solids. However, it is not easy to identify the differences in solid-state characteristics between amorphous solids using conventional analytical methods, such as powder X-ray diffraction analysis, since all of the poly-amorphous solids had similar halo X-ray diffraction patterns. However, terahertz spectroscopy can distinguish the amorphous solids of indomethacin with different physicochemical properties, and is expected to provide a rapid and non-destructive qualitative analysis for the solid materials, it would be useful for the qualitative evaluation of amorphous solids in the pharmaceutical industry.

  12. Atomic-scale disproportionation in amorphous silicon monoxide

    PubMed Central

    Hirata, Akihiko; Kohara, Shinji; Asada, Toshihiro; Arao, Masazumi; Yogi, Chihiro; Imai, Hideto; Tan, Yongwen; Fujita, Takeshi; Chen, Mingwei

    2016-01-01

    Solid silicon monoxide is an amorphous material which has been commercialized for many functional applications. However, the amorphous structure of silicon monoxide is a long-standing question because of the uncommon valence state of silicon in the oxide. It has been deduced that amorphous silicon monoxide undergoes an unusual disproportionation by forming silicon- and silicon-dioxide-like regions. Nevertheless, the direct experimental observation is still missing. Here we report the amorphous structure characterized by angstrom-beam electron diffraction, supplemented by synchrotron X-ray scattering and computer simulations. In addition to the theoretically predicted amorphous silicon and silicon-dioxide clusters, suboxide-type tetrahedral coordinates are detected by angstrom-beam electron diffraction at silicon/silicon-dioxide interfaces, which provides compelling experimental evidence on the atomic-scale disproportionation of amorphous silicon monoxide. Eventually we develop a heterostructure model of the disproportionated silicon monoxide which well explains the distinctive structure and properties of the amorphous material. PMID:27172815

  13. Annealing behavior of high permeability amorphous alloys

    SciTech Connect

    Rabenberg, L.

    1980-06-01

    Effects of low temperature annealing on the magnetic properties of the amorphous alloy Co/sub 71/ /sub 4/Fe/sub 4/ /sub 6/Si/sub 9/ /sub 6/B/sub 14/ /sub 4/ were investigated. Annealing this alloy below 400/sup 0/C results in magnetic hardening; annealing above 400/sup 0/C but below the crystallization temperature results in magnetic softening. Above the crystallization temperature the alloy hardens drastically and irreversibly. Conventional and high resolution transmission electron microscopy were used to show that the magnetic property changes at low temperatures occur while the alloy is truly amorphous. By imaging the magnetic microstructures, Lorentz electron microscopy has been able to detect the presence of microscopic inhomogeneities in this alloy. The low temperature annealing behavior of this alloy has been explained in terms of atomic pair ordering in the presence of the internal molecular field. Lorentz electron microscopy has been used to confirm this explanation.

  14. Thermoluminescence characteristics of hydrogenated amorphous zirconia

    NASA Astrophysics Data System (ADS)

    Montalvo, T. R.; Tenorio, L. O.; Nieto, J. A.; Salgado, M. B.; Estrada, A. M. S.; Furetta, C.

    2005-05-01

    This paper reports the experimental results concerning the thermoluminescent (TL) characteristics of hydrogenated amorphous zirconium oxide (a-Zr:H) powder prepared by the sol-gel method. The advantages of this method are the homogeneity and the purity of the gels associated with a relatively low sintering temperature. Hydrogenated amorphous powder was characterized by thermal analysis and X-ray diffraction. The main TL characteristics investigated were the TL response as a function of the absorbed dose, the reproducibility of the TL readings and the fading. The undoped a-Zr:H powder presents a TL glow curve with two peaks centered at 150 and 260 degrees C, respectively, after beta irradiation. The TL response a-Zr:H as a function of the absorbed dose showed a linear behavior over a wide range. The results presented open the possibility to use this material as a good TL dosimeter.

  15. Germanium detector passivated with hydrogenated amorphous germanium

    DOEpatents

    Hansen, William L.; Haller, Eugene E.

    1986-01-01

    Passivation of predominantly crystalline semiconductor devices (12) is provided for by a surface coating (21) of sputtered hydrogenated amorphous semiconductor material. Passivation of a radiation detector germanium diode, for example, is realized by sputtering a coating (21) of amorphous germanium onto the etched and quenched diode surface (11) in a low pressure atmosphere of hydrogen and argon. Unlike prior germanium diode semiconductor devices (12), which must be maintained in vacuum at cryogenic temperatures to avoid deterioration, a diode processed in the described manner may be stored in air at room temperature or otherwise exposed to a variety of environmental conditions. The coating (21) compensates for pre-existing undesirable surface states as well as protecting the semiconductor device (12) against future impregnation with impurities.

  16. Wear Resistant Amorphous and Nanocomposite Coatings

    SciTech Connect

    Racek, O

    2008-03-26

    Glass forming materials (critical cooling rate <10{sup 4}K.s{sup -1}) are promising for their high corrosion and wear resistance. During rapid cooling, the materials form an amorphous structure that transforms to nanocrystalline during a process of devitrification. High hardness (HV 1690) can be achieved through a controlled crystallization. Thermal spray process has been used to apply coatings, which preserves the amorphous/nanocomposite structure due to a high cooling rate of the feedstock particles during the impact on a substrate. Wear properties have been studied with respect to process conditions and feedstock material properties. Application specific properties such as sliding wear resistance have been correlated with laboratory tests based on instrumented indentation and scratch tests.

  17. Characterization of Amorphous Zinc Tin Oxide Semiconductors

    SciTech Connect

    Rajachidambaram, Jaana Saranya; Sanghavi, Shail P.; Nachimuthu, Ponnusamy; Shutthanandan, V.; Varga, Tamas; Flynn, Brendan T.; Thevuthasan, Suntharampillai; Herman, Gregory S.

    2012-06-12

    Amorphous zinc tin oxide (ZTO) was investigated to determine the effect of deposition and post annealing conditions on film structure, composition, surface contamination, and thin film transistor (TFT) device performance. X-ray diffraction results indicated that the ZTO films remain amorphous even after annealing to 600 °C. We found that the bulk Zn:Sn ratio of the sputter deposited films were slightly tin rich compared to the composition of the ceramic sputter target, and there was a significant depletion of zinc at the surface. X-ray photoelectron spectroscopy also indicated that residual surface contamination depended strongly on the sample post-annealing conditions where water, carbonate and hydroxyl species were absorbed to the surface. Electrical characterization of ZTO films, using TFT test structures, indicated that mobilities as high as 17 cm2/Vs could be obtained for depletion mode devices.

  18. Reversibility and criticality in amorphous solids

    PubMed Central

    Regev, Ido; Weber, John; Reichhardt, Charles; Dahmen, Karin A.; Lookman, Turab

    2015-01-01

    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 chaotic behaviour and why chaotic motion is not possible in pinned systems. 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. PMID:26564783

  19. Reversibility and criticality in amorphous solids

    DOE PAGES

    Regev, Ido; Weber, John; Reichhardt, Charles; Dahmen, Karin A.; Lookman, Turab

    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

  20. Reversibility and criticality in amorphous solids

    SciTech Connect

    Regev, Ido; Weber, John; Reichhardt, Charles; Dahmen, Karin A.; Lookman, Turab

    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 chaotic 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.

  1. Reversibility and criticality in amorphous solids.

    PubMed

    Regev, Ido; Weber, John; Reichhardt, Charles; Dahmen, Karin A; Lookman, Turab

    2015-01-01

    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 chaotic behaviour and why chaotic motion is not possible in pinned systems. 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. PMID:26564783

  2. Design Requirements for Amorphous Piezoelectric Polymers

    NASA Technical Reports Server (NTRS)

    Ounaies, Z.; Young, J. A.; Harrison, J. S.

    1999-01-01

    An overview of the piezoelectric activity in amorphous piezoelectric polymers is presented. The criteria required to render a polymer piezoelectric are discussed. Although piezoelectricity is a coupling between mechanical and electrical properties, most research has concentrated on the electrical properties of potentially piezoelectric polymers. In this work, we present comparative mechanical data as a function of temperature and offer a summary of polarization and electromechanical properties for each of the polymers considered.

  3. Synthesis of new amorphous metallic spin glasses

    DOEpatents

    Haushalter, R.C.

    1985-02-11

    Disclosed are: amorphous metallic precipitates having the formula (M/sub 1/)/sub a/(M/sub 2/)/sub b/ wherein M/sub 1/ is at least one transition metal, M/sub 2/ is at least one main group metal and the integers ''a'' and ''b'' provide stoichiometric balance; the precipitates having a degree of local order characteristic of chemical compounds from the precipitation process and useful electrical and mechanical properties.

  4. Synthesis of new amorphous metallic spin glasses

    DOEpatents

    Haushalter, Robert C.

    1988-01-01

    Amorphous metallic precipitates having the formula (M.sub.1).sub.a (M.sub.2).sub.b wherein M.sub.1 is at least one transition metal, M.sub.2 is at least one main group metal and the integers "a" and "b" provide stoichiometric balance; the precipitates having a degree of local order characteristic of chemical compounds from the precipitation process and useful electrical and mechanical properties.

  5. Synthesis of new amorphous metallic spin glasses

    DOEpatents

    Haushalter, Robert C.

    1986-01-01

    Amorphous metallic precipitates having the formula (M.sub.1).sub.a (M.sub.2).sub.b wherein M.sub.1 is at least one transition metal, M.sub.2 is at least one main group metal and the integers "a" and "b" provide stoichiometric balance; the precipitates having a degree of local order characteristic of chemical compounds from the precipitation process and useful electrical and mechanical properties.

  6. Multiple cell photoresponsive amorphous alloys and devices

    SciTech Connect

    Ovshinsky, S.R.; Adler, D.

    1990-01-02

    This patent describes an improved photoresponsive tandem multiple solar cell device. The device comprising: at least a first and second superimposed cell of various materials. The first cell being formed of a silicon alloy material. The second cell including an amorphous silicon alloy semiconductor cell body having an active photoresponsive region in which radiation can impinge to produce charge carriers, the amorphous cell body including at least one density of states reducing element. The element being fluorine. The amorphous cell body further including a band gap adjusting element therein at least in the photoresponsive region to enhance the radiation absorption thereof, the adjusting element being germanium: the second cell being a multi-layer body having deposited semiconductor layers of opposite (p and n) conductivity type; and the first cell being formed with the second cell in substantially direct Junction contact therebetween. The first and second cells designed to generate substantially matched currents from each cell from a light source directed through the first cell and into the second cell.

  7. Concurrent multiscale modeling of amorphous materials

    NASA Astrophysics Data System (ADS)

    Tan, Vincent

    2013-03-01

    An approach to multiscale modeling of amorphous materials is presented whereby atomistic scale domains coexist with continuum-like domains. The atomistic domains faithfully predict severe deformation while the continuum domains allow the computation to scale up the size of the model without incurring excessive computational costs associated with fully atomistic models and without the introduction of spurious forces across the boundary of atomistic and continuum-like domains. The material domain is firstly constructed as a tessellation of Amorphous Cells (AC). For regions of small deformation, the number of degrees of freedom is then reduced by computing the displacements of only the vertices of the ACs instead of the atoms within. This is achieved by determining, a priori, the atomistic displacements within such Pseudo Amorphous Cells associated with orthogonal deformation modes of the cell. Simulations of nanoscale polymer tribology using full molecular mechanics computation and our multiscale approach give almost identical prediction of indentation force and the strain contours of the polymer. We further demonstrate the capability of performing adaptive simulations during which domains that were discretized into cells revert to full atomistic domains when their strain attain a predetermined threshold. The authors would like to acknowledge the financial support given to this study by the Agency of Science, Technology and Research (ASTAR), Singapore (SERC Grant No. 092 137 0013).

  8. Phase transitions in biogenic amorphous calcium carbonate

    NASA Astrophysics Data System (ADS)

    Gong, Yutao

    Geological calcium carbonate exists in both crystalline phases and amorphous phases. Compared with crystalline calcium carbonate, such as calcite, aragonite and vaterite, the amorphous calcium carbonate (ACC) is unstable. Unlike geological calcium carbonate crystals, crystalline sea urchin spicules (99.9 wt % calcium carbonate and 0.1 wt % proteins) do not present facets. To explain this property, crystal formation via amorphous precursors was proposed in theory. And previous research reported experimental evidence of ACC on the surface of forming sea urchin spicules. By using X-ray absorption near-edge structure (XANES) spectroscopy and photoelectron emission microscopy (PEEM), we studied cross-sections of fresh sea urchin spicules at different stages (36h, 48h and 72h after fertilization) and observed the transition sequence of three mineral phases: hydrated ACC → dehydrated ACC → biogenic calcite. In addition, we unexpectedly found hydrated ACC nanoparticles that are surrounded by biogenic calcite. This observation indicates the dehydration from hydrated ACC to dehydrated ACC is inhibited, resulting in stabilization of hydrated ACC nanoparticles. We thought that the dehydration was inhibited by protein matrix components occluded within the biomineral, and we designed an in vitro assay to test the hypothesis. By utilizing XANES-PEEM, we found that SM50, the most abundant occluded matrix protein in sea urchin spicules, has the function to stabilize hydrated ACC in vitro.

  9. Amorphous molybdenum silicon superconducting thin films

    SciTech Connect

    Bosworth, D. Sahonta, S.-L.; Barber, Z. H.; Hadfield, R. H.

    2015-08-15

    Amorphous superconductors have become attractive candidate materials for superconducting nanowire single-photon detectors due to their ease of growth, homogeneity and competitive superconducting properties. To date the majority of devices have been fabricated using W{sub x}Si{sub 1−x}, though other amorphous superconductors such as molybdenum silicide (Mo{sub x}Si{sub 1−x}) offer increased transition temperature. This study focuses on the properties of MoSi thin films grown by magnetron sputtering. We examine how the composition and growth conditions affect film properties. For 100 nm film thickness, we report that the superconducting transition temperature (Tc) reaches a maximum of 7.6 K at a composition of Mo{sub 83}Si{sub 17}. The transition temperature and amorphous character can be improved by cooling of the substrate during growth which inhibits formation of a crystalline phase. X-ray diffraction and transmission electron microscopy studies confirm the absence of long range order. We observe that for a range of 6 common substrates (silicon, thermally oxidized silicon, R- and C-plane sapphire, x-plane lithium niobate and quartz), there is no variation in superconducting transition temperature, making MoSi an excellent candidate material for SNSPDs.

  10. Amorphous molybdenum silicon superconducting thin films

    NASA Astrophysics Data System (ADS)

    Bosworth, D.; Sahonta, S.-L.; Hadfield, R. H.; Barber, Z. H.

    2015-08-01

    Amorphous superconductors have become attractive candidate materials for superconducting nanowire single-photon detectors due to their ease of growth, homogeneity and competitive superconducting properties. To date the majority of devices have been fabricated using WxSi1-x, though other amorphous superconductors such as molybdenum silicide (MoxSi1-x) offer increased transition temperature. This study focuses on the properties of MoSi thin films grown by magnetron sputtering. We examine how the composition and growth conditions affect film properties. For 100 nm film thickness, we report that the superconducting transition temperature (Tc) reaches a maximum of 7.6 K at a composition of Mo83Si17. The transition temperature and amorphous character can be improved by cooling of the substrate during growth which inhibits formation of a crystalline phase. X-ray diffraction and transmission electron microscopy studies confirm the absence of long range order. We observe that for a range of 6 common substrates (silicon, thermally oxidized silicon, R- and C-plane sapphire, x-plane lithium niobate and quartz), there is no variation in superconducting transition temperature, making MoSi an excellent candidate material for SNSPDs.

  11. Preparation of bulk superhard B-C-N nanocomposite compact

    DOEpatents

    Zhao, Yusheng; He, Duanwei

    2011-05-10

    Bulk, superhard, B--C--N nanocomposite compacts were prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture at a pressure in a range of from about 15 GPa to about 25 GPa, and sintering the pressurized encapsulated ball-milled mixture at a temperature in a range of from about 1800-2500 K. The product bulk, superhard, nanocomposite compacts were well sintered compacts with nanocrystalline grains of at least one high-pressure phase of B--C--N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compacts had a measured Vicker's hardness in a range of from about 41 GPa to about 68 GPa.

  12. In vitro responses of bone-forming MC3T3-E1 pre-osteoblasts to biodegradable Mg-based bulk metallic glasses.

    PubMed

    Li, Haifei; He, Wei; Pang, Shujie; Liaw, Peter K; Zhang, Tao

    2016-11-01

    In light of the superior property profile of favorable biocompatibility, proper corrosion/degradation behavior and good mechanical properties, Mg-based bulk metallic glasses (BMGs) are considered as potential biodegradable biomaterials. In the present study, in vitro responses of bone-forming MC3T3-E1 pre-osteoblasts to Mg-Zn-Ca-Sr BMGs were studied in order to assess their feasibility to serve as orthopedic implants. The Mg-Zn-Ca-Sr BMGs were much more capable of supporting cell adhesion and spreading in comparison with crystalline AZ31B Mg alloy. The Mg-Zn-Ca-Sr BMG extracts showed no cytotoxicity to and slightly stimulated the proliferation of pre-osteoblasts. The cells cultured in 100% BMG extracts exhibited lower alkaline phosphatase activity as compared with that in negative control, which could be mainly ascribed to the inhibition of high concentrations of Zn ions on cell differentiation. With decreasing the extract concentration, the inhibitory effect was diminished and the 5% BMG extract exhibited slight stimulation in cell differentiation and mineralization. The high corrosion resistance of BMGs contributed to smaller environmental variations, compared with AZ31B alloy, thus lowering the unfavorable influences on cellular responses. A comparison among the biodegradable Mg-, Ca- and Sr-based BMGs for their biomedical applications is presented. PMID:27524063

  13. Characterizing Amorphous Silicates in Extraterrestrial Materials

    NASA Astrophysics Data System (ADS)

    Fu, X.; Wang, A.; Krawczynski, M. J.

    2015-12-01

    Amorphous silicates are common in extraterrestrial materials. They are seen in the matrix of carbonaceous chondrites as well as in planetary materials. Tagish Lake is one of the most primitive carbonaceous meteorites in which TEM and XRD analyses found evidence for poorly crystalline phyllosilicate-like species; Raman spectra revealed amorphous silicates with variable degree of polymerization and low crystallinity. On Mars, CheMin discovered amorphous phases in all analyzed samples, and poorly crystalline smectite in mudstone samples. These discoveries pose questions on the crystallinity of phyllosilicates found by remote sensing on Mars, which is directly relevant to aqueous alteration during geologic history of Mars. Our goal is to use spectroscopy to better characterize amorphous silicates. We use three approaches: (1) using silicate glasses synthesized with controlled chemistry to study the effects of silicate polymerization and (2) using phyllosilicates synthesized with controlled hydrothermal treatment to study the effect of crystallinity on vibrational spectroscopy, finally (3) to use the developed correlations in above two steps to study amorphous phases in meteorites, and those found in future missions to Mars. In the 1st step, silicate glasses were synthesized from pure oxides in a range of NBO/T ratios (from 0 to 4). Depending on the targeted NBO/T and composition of mixed oxides, temperatures for each experiment fell in a range from 1260 to 1520 °C, run for ~ 4 hrs. The melt was quenched in liquid N2 or water. Homogeneity of glass was checked under optical microscopy. Raman spectra were taken over 100 spots on small chips free of bubbles and crystals. We have observed that accompanying an increase of NBO/T, there is a strengthening and a position shift of the Raman peak near 1000 cm-1 (Si-Onon-bridging stretching mode), and the weakening of broad Raman peaks near 500 cm-1 (ring breathing mode) and 700cm-1 (Si-Obridging-Si mode). We are building the

  14. Infrared emission from hydrogenated amorphous carbon and amorphous carbon grains in the interstellar medium

    NASA Technical Reports Server (NTRS)

    Duley, W. W.; Jones, A. P.; Taylor, S. D.; Williams, D. A.

    1993-01-01

    The correlations deduced by Boulanger et al. (1990) from IRAS maps of the Chamaeleon, Taurus and Ursa Major molecular cloud complexes are interpreted in terms of the evolutionary hydrogenated amorphous carbon model of interstellar dust. In particular, regions of relatively strong 12-micron emission may be regions where recently accreted carbon is being converted by ambient UV to small PAHs in situ. Regions of weak 12-micron emission are probably quiescent regions where carbon has been annealed to amorphous carbon. Observational consequences of these inferences are briefly described.

  15. Formation of amorphous silicon by light ion damage

    SciTech Connect

    Shih, Y.C.

    1985-12-01

    Amorphization by implantation of boron ions (which is the lightest element generally used in I.C. fabrication processes) has been systematically studied for various temperatures, various voltages and various dose rates. Based on theoretical considerations and experimental results, a new amorphization model for light and intermediate mass ion damage is proposed consisting of two stages. The role of interstitial type point defects or clusters in amorphization is emphasized. Due to the higher mobility of interstitials out-diffusion to the surface particularly during amorphization with low energy can be significant. From a review of the idealized amorphous structure, diinterstitial-divacancy pairs are suggested to be the embryos of amorphous zones formed during room temperature implantation. The stacking fault loops found in specimens implanted with boron at room temperature are considered to be the origin of secondary defects formed during annealing.

  16. Amorphous silicon/polycrystalline thin film solar cells

    SciTech Connect

    Ullal, H.S.

    1991-03-13

    An improved photovoltaic solar cell is described including a p-type amorphous silicon layer, intrinsic amorphous silicon, and an n-type polycrystalline semiconductor such as cadmium sulfide, cadmium zinc sulfide, zinc selenide, gallium phosphide, and gallium nitride. The polycrystalline semiconductor has an energy bandgap greater than that of the amorphous silicon. The solar cell can be provided as a single-junction device or a multijunction device.

  17. Structure and dynamics of amorphous water ice.

    PubMed

    Laufer, D; Kochavi, E; Bar-Nun, A

    1987-12-15

    Further insight into the structure and dynamics of amorphous water ice, at low temperatures, was obtained by trapping in it Ar, Ne, H2, and D2. Ballistic water-vapor deposition results in the growth of smooth, approximately 1 x 0.2 micrometer2, ice needles. The amorphous ice seems to exist in at least two separate forms, at T < 85 K and at 85 < T < 136.8 K, and transform irreversibly from one form to the other through a series of temperature-dependent metastable states. The channels formed by the water hexagons in the ice are wide enough to allow the free penetration of H2 and D2 into the ice matrix even in the relatively compact cubic ice, resulting in H2-(D2-) to-ice ratios (by number) as high as 0.63. The larger Ar atoms can penetrate only into the wider channels of amorphous ice, and Ne is an intermediate case. Dynamic percolation behavior explains the emergence of Ar and Ne (but not H2 and D2) for the ice, upon warming, in small and big gas jets. The big jets, each containing approximately 5 x 10(10) atoms, break and propel the ice needles. Dynamic percolation also explains the collapse of the ice matrix under bombardment by Ar , at a pressure exceeding 2.6 dyn cm-2, and the burial of huge amounts of gas inside the collapsed matrix, up to an Ar-to-ice of 3.3 (by number). The experimental results could be relevant to comets, icy satellites, and icy grain mantles in dense interstellar clouds.

  18. Structure and dynamics of amorphous water ice

    NASA Technical Reports Server (NTRS)

    Laufer, D.; Kochavi, E.; Bar-Nun, A.; Owen, T. (Principal Investigator)

    1987-01-01

    Further insight into the structure and dynamics of amorphous water ice, at low temperatures, was obtained by trapping in it Ar, Ne, H2, and D2. Ballistic water-vapor deposition results in the growth of smooth, approximately 1 x 0.2 micrometer2, ice needles. The amorphous ice seems to exist in at least two separate forms, at T < 85 K and at 85 < T < 136.8 K, and transform irreversibly from one form to the other through a series of temperature-dependent metastable states. The channels formed by the water hexagons in the ice are wide enough to allow the free penetration of H2 and D2 into the ice matrix even in the relatively compact cubic ice, resulting in H2-(D2-) to-ice ratios (by number) as high as 0.63. The larger Ar atoms can penetrate only into the wider channels of amorphous ice, and Ne is an intermediate case. Dynamic percolation behavior explains the emergence of Ar and Ne (but not H2 and D2) for the ice, upon warming, in small and big gas jets. The big jets, each containing approximately 5 x 10(10) atoms, break and propel the ice needles. Dynamic percolation also explains the collapse of the ice matrix under bombardment by Ar , at a pressure exceeding 2.6 dyn cm-2, and the burial of huge amounts of gas inside the collapsed matrix, up to an Ar-to-ice of 3.3 (by number). The experimental results could be relevant to comets, icy satellites, and icy grain mantles in dense interstellar clouds.

  19. Medical imaging applications of amorphous silicon

    SciTech Connect

    Mireshghi, A.; Drewery, J.S.; Hong, W.S.; Jing, T.; Kaplan, S.N.; Lee, H.K.; Perez-Mendez, V.

    1994-07-01

    Two dimensional hydrogenated amorphous silicon (a-Si:H) pixel arrays are good candidates as flat-panel imagers for applications in medical imaging. Various performance characteristics of these imagers are reviewed and compared with currently used equipments. An important component in the a-Si:H imager is the scintillator screen. A new approach for fabrication of high resolution CsI(Tl) scintillator layers, appropriate for coupling to a-Si:H arrays, are presented. For nuclear medicine applications, a new a-Si:H based gamma camera is introduced and Monte Carlo simulation is used to evaluate its performance.

  20. Radiation resistance studies of amorphous silicon films

    NASA Technical Reports Server (NTRS)

    Woodyard, James R.; Payson, J. Scott

    1989-01-01

    Hydrogenated amorphous silicon thin films were irradiated with 2.00 MeV helium ions using fluences ranging from 1E11 to 1E15 cm(-2). The films were characterized using photothermal deflection spectroscopy and photoconductivity measurements. The investigations show that the radiation introduces sub-band-gap states 1.35 eV below the conduction band and the states increase supralinearly with fluence. Photoconductivity measurements suggest the density of states above the Fermi energy is not changing drastically with fluence.

  1. Mechanism for hydrogen diffusion in amorphous silicon

    SciTech Connect

    Biswas, R.; Li, Q.; Pan, B.C.; Yoon, Y.

    1998-01-01

    Tight-binding molecular-dynamics calculations reveal a mechanism for hydrogen diffusion in hydrogenated amorphous silicon. Hydrogen diffuses through the network by successively bonding with nearby silicons and breaking their Si{endash}Si bonds. The diffusing hydrogen carries with it a newly created dangling bond. These intermediate transporting states are densely populated in the network, have lower energies than H at the center of stretched Si{endash}Si bonds, and can play a crucial role in hydrogen diffusion. {copyright} {ital 1998} {ital The American Physical Society}

  2. Obstacles using amorphous materials for volume applications

    NASA Astrophysics Data System (ADS)

    Kiessling, Albert; Reininger, Thomas

    2012-10-01

    This contribution is especially focussed on the attempt to use amorphous or nanocrystalline metals in position sensor applications and to describe the difficulties and obstacles encountered in coherence with the development of appropriate industrial high volume series products in conjunction with the related quality requirements. The main motivation to do these investigations was to beat the generally known sensors especially silicon based Hall-sensors as well as AMR- and GMR-sensors - well known from mobile phones and electronic storage devices like hard discs and others - in terms of cost-effectiveness and functionality.

  3. Amorphous computing: examples, mathematics and theory.

    PubMed

    Stark, W Richard

    2013-01-01

    The cellular automata model was described by John von Neumann and his friends in the 1950s as a representation of information processing in multicellular tissue. With crystalline arrays of cells and synchronous activity, it missed the mark (Stark and Hughes, BioSystems 55:107-117, 2000). Recently, amorphous computing, a valid model for morphogenesis in multicellular information processing, has begun to fill the void. Through simple examples and elementary mathematics, this paper begins a computation theory for this important new direction. PMID:23946719

  4. Diffusion and ion mixing in amorphous alloys

    SciTech Connect

    Hahn, H.; Averback, R.S.; Ding, F.; Loxton, C.; Baker, J.

    1986-10-01

    Tracer impurity diffusion and ion beam mixing in amorphous (a-)Ni/sub 50/Zr/sub 50/ were measured. A correlation between the metallic radius of an impurity and its tracer diffusivity was observed; it is similar to that found in crystalline ..cap alpha..-Zr and ..cap alpha..-Ti. In addition, the temperature dependence of diffusion in a-NiZr exhibits Arrhenius behavior. Ion beam mixing of different impurities in a-NiZr correlates with tracer diffusivity at both high and low temperatures. At higher temperatures radiation enhanced diffusion (RED) was observed. The activation enthalpy of the RED diffusion coefficient is 0.3 eV/atom.

  5. Encoding of Memory in Sheared Amorphous Solids

    NASA Astrophysics Data System (ADS)

    Fiocco, Davide; Foffi, Giuseppe; Sastry, Srikanth

    2014-01-01

    We show that memory can be encoded in a model amorphous solid subjected to athermal oscillatory shear deformations, and in an analogous spin model with disordered interactions, sharing the feature of a deformable energy landscape. When these systems are subjected to oscillatory shear deformation, they retain memory of the deformation amplitude imposed in the training phase, when the amplitude is below a "localization" threshold. Remarkably, multiple persistent memories can be stored using such an athermal, noise-free, protocol. The possibility of such memory is shown to be linked to the presence of plastic deformations and associated limit cycles traversed by the system, which exhibit avalanche statistics also seen in related contexts.

  6. Self-Diffusion in Amorphous Silicon.

    PubMed

    Strauß, Florian; Dörrer, Lars; Geue, Thomas; Stahn, Jochen; Koutsioubas, Alexandros; Mattauch, Stefan; Schmidt, Harald

    2016-01-15

    The present Letter reports on self-diffusion in amorphous silicon. Experiments were done on ^{29}Si/^{nat}Si heterostructures using neutron reflectometry and secondary ion mass spectrometry. The diffusivities follow the Arrhenius law in the temperature range between 550 and 700 °C with an activation energy of (4.4±0.3)  eV. In comparison with single crystalline silicon the diffusivities are tremendously higher by 5 orders of magnitude at about 700 °C, which can be interpreted as the consequence of a high diffusion entropy. PMID:26824552

  7. Deuterium in crystalline and amorphous silicon

    SciTech Connect

    Borzi, R.; Ma, H.; Fedders, P.A.; Leopold, D.J.; Norberg, R.E.; Boyce, J.B.; Johnson, N.M.; Ready, S.E.; Walker, J.

    1997-07-01

    The authors report deuteron magnetic resonance (DMR) measurements on aged deuterium-implanted single crystal n-type silicon and comparisons with amorphous silicon spectra. The sample film was prepared six years ago by deuteration from a-D{sub 2} plasma and evaluated by a variety of experimental methods. Deuterium has been evolving with time and the present DMR signal shows a smaller deuteron population. A doublet from Si-D configurations along (111) has decreased more than have central molecular DMR components, which include 47 and 12 kHz FWHM gaussians. Transient DMR magnetization recoveries indicate spin lattice relaxation to para-D{sub 2} relaxation centers.

  8. Cyclic behaviors of amorphous shape memory polymers.

    PubMed

    Yu, Kai; Li, Hao; McClung, Amber J W; Tandon, Gyaneshwar P; Baur, Jeffery W; Qi, H Jerry

    2016-04-01

    Cyclic loading conditions are commonly encountered in the applications of shape memory polymers (SMPs), where the cyclic characteristics of the materials determine their performance during the service life, such as deformation resistance, shape recovery speed and shape recovery ratio. Recent studies indicate that in addition to the physical damage or some other irreversible softening effects, the viscoelastic nature could also be another possible reason for the degraded cyclic behavior of SMPs. In this paper, we explore in detail the influence of the viscoelastic properties on the cyclic tension and shape memory (SM) behavior of an epoxy based amorphous thermosetting polymer. Cyclic experiments were conducted first, which show that although the epoxy material does not have any visible damage or irreversible softening effect during deformation, it still exhibits obvious degradation in the cyclic tension and SM behaviors. A linear multi-branched model is utilized to assist in the prediction and understanding of the mechanical responses of amorphous SMPs. Parametric studies based on the applied model suggest that the shape memory performance can be improved by adjusting programming and recovery conditions, such as lowering the loading rate, increasing the programming temperature, and reducing the holding time. PMID:26924339

  9. Structural and Elastic Properties of Amorphous Silicon

    NASA Astrophysics Data System (ADS)

    Feldman, Joseph; Papaconstantopoulos, Dimitris; Bernstein, Noam; Mehl, Michael

    2003-03-01

    In this work we study the elastic and structural properties of amorphous silicon using the NRL tight-binding method (N. Bernstein, et al., Phys. Rev. B 62, 4477 (2000).). Using conjugate gradient energy minimization we have relaxed a 216 atom model. The amorphous-crystal energy difference is 0.017 Ryd/atom, similar to a calculation on a related model using the empirical Stillinger-Weber potential and twice the experimental value. The structure of the relaxed model is consistent with diffraction experiments as well as more indirect experimental results. The model is fully four-fold coordinated with an RMS bond angle deviation of only 11^rc, and is expanded 2% in volume with respect to the TB crystalline value. Using the method of homogeneous deformation we have found a relaxed shear modulus of ˜57 GPa (with an estimated 2% uncertainty due to anisotropy) and relaxed bulk modulus of 87.3 GPa, in very good agreement with a previous (ab initio) calculated value of 82.5 GPa (M. Durandurdu and D. A. Drabold, Phys. Rev. B 64, 014101 (2001).). We find that the distribution of relaxation displacements under shear is markedly skewed towards large values. Finally, we discuss the force constants and vacancy energy distributions for several models.

  10. Modeling of amorphous polyaniline emeraldine base.

    PubMed

    Canales, Manel; Curcó, David; Alemán, Carlos

    2010-08-01

    Amorphous polyaniline emeraldine base has been investigated using atomistic classical molecular dynamics simulations. Initially, different sets of force-field parameters, which differ in the atomic charges and/or the van der Waals parameters, were tested. The experimental density of polyaniline was satisfactorily reproduced using the following combination: (i) equilibrium bond lengths, equilibrium bond angles, and electrostatic charges derived from quantum mechanical calculations and (ii) van der Waals parameters extrapolated from GROMOS for all atoms with the exception of the CH pseudoparticles of the phenyl ring, which were taken from an anisotropic united atom potential. Next, this force field was used to investigate the structure of the polymer in the amorphous state, the trajectories performed for this purpose allowing accumulation of 750 ns. Analyses of the energies evidence that the interactions between one repeating unit containing an amine nitrogen atom and another unit with an imine nitrogen are favored with respect to those between two identical repeating units. This conclusion is also supported by quantum mechanical and quantum mechanical/molecular mechanics calculations. On the other hand, the partial radial distribution functions indicate that this material only exhibits short-range intramolecular correlation, which is in excellent agreement with experimental evidence.

  11. Atomic-Scale Imprinting into Amorphous Metals

    NASA Astrophysics Data System (ADS)

    Schwarz, Udo; Li, Rui; Simon, Georg; Kinser, Emely; Liu, Ze; Chen, Zheng; Zhou, Chao; Singer, Jonathan; Osuji, Chinedum; Schroers, Jan

    Nanoimprinting by thermoplastic forming (TPF) has attracted significant attention in recent years due to its promise of low-cost fabrication of nanostructured devices. Usually performed using polymers, amorphous metals have been identified as a material class that might be even better suited for nanoimprinting due to a combination of mechanical properties and processing ability. Commonly referred to as metallic glasses, their featureless atomic structure suggests that there may not be an intrinsic size limit to the material's ability to replicate a mold. To study this hypothesis, we demonstrate atomic-scale imprinting into amorphous metals by TPF under ambient conditions. Atomic step edges of a SrTiO3 (STO) single crystal used as mold were successfully imprinted into Pt-based bulk metallic glasses (BMGs) with high fidelity. Terraces on the BMG replicas possess atomic smoothness with sub-Angstrom roughness that is identical to the one measured on the STO mold. Systematic studies revealed that the quality of the replica depends on the loading rate during imprinting, that the same mold can be used multiple times without degradation of mold or replicas, and that the atomic-scale features on as-imprinted BMG surfaces has impressive long-term stability (months).

  12. Structural Characteristics of Synthetic Amorphous Calcium Carbonate

    SciTech Connect

    Michel, F. Marc; MacDonald, Jason; Feng, Jian; Phillips, Brian L.; Ehm, Lars; Tarabrella, Cathy; Parise, John B.; Reeder, Richard J.

    2008-08-06

    Amorphous calcium carbonate (ACC) is an important phase involved in calcification by a wide variety of invertebrate organisms and is of technological interest in the development of functional materials. Despite widespread scientific interest in this phase a full characterization of structure is lacking. This is mainly due to its metastability and difficulties in evaluating structure using conventional structure determination methods. Here we present new findings from the application of two techniques, pair distribution function analysis and nuclear magnetic resonance spectroscopy, which provide new insight to structural aspects of synthetic ACC. Several important results have emerged from this study of ACC formed in vitro using two common preparation methods: (1) ACC exhibits no structural coherence over distances > 15 {angstrom} and is truly amorphous; (2) most of the hydrogen in ACC is present as structural H{sub 2}O, about half of which undergoes restricted motion on the millisecond time scale near room temperature; (3) the short- and intermediate-range structure of ACC shows no distinct match to any known structure in the calcium carbonate system; and (4) most of the carbonate in ACC is monodentate making it distinctly different from monohydrocalcite. Although the structure of synthetic ACC is still not fully understood, the results presented provide an important baseline for future experiments evaluating biogenic ACC and samples containing certain additives that may play a role in stabilization of ACC, crystallization kinetics, and final polymorph selection.

  13. The future of amorphous silicon photovoltaic technology

    SciTech Connect

    Crandall, R; Luft, W

    1995-06-01

    Amorphous silicon modules are commercially available. They are the first truly commercial thin-film photovoltaic (PV) devices. Well-defined production processes over very large areas (>1 m{sup 2}) have been implemented. There are few environmental issues during manufacturing, deployment in the field, or with the eventual disposal of the modules. Manufacturing safety issues are well characterized and controllable. The highest measured initial efficiency to date is 13.7% for a small triple-stacked cell and the highest stabilized module efficiency is 10%. There is a consensus among researchers, that in order to achieve a 15% stabilized efficiency, a triple-junction amorphous silicon structure is required. Fundamental improvements in alloys are needed for higher efficiencies. This is being pursued through the DOE/NREL Thin-Film Partnership Program. Cost reductions through improved manufacturing processes are being pursued under the National Renewable Energy Laboratory/US Department of Energy (NREL/DOE)-sponsored research in manufacturing technology (PVMaT). Much of the work in designing a-Si devices is a result of trying to compensate for the Staebler-Wronski effect. Some new deposition techniques hold promise because they have produced materials with lower stabilized defect densities. However, none has yet produced a high efficiency device and shown it to be more stable than those from standard glow discharge deposited material.

  14. Cyclic behaviors of amorphous shape memory polymers.

    PubMed

    Yu, Kai; Li, Hao; McClung, Amber J W; Tandon, Gyaneshwar P; Baur, Jeffery W; Qi, H Jerry

    2016-04-01

    Cyclic loading conditions are commonly encountered in the applications of shape memory polymers (SMPs), where the cyclic characteristics of the materials determine their performance during the service life, such as deformation resistance, shape recovery speed and shape recovery ratio. Recent studies indicate that in addition to the physical damage or some other irreversible softening effects, the viscoelastic nature could also be another possible reason for the degraded cyclic behavior of SMPs. In this paper, we explore in detail the influence of the viscoelastic properties on the cyclic tension and shape memory (SM) behavior of an epoxy based amorphous thermosetting polymer. Cyclic experiments were conducted first, which show that although the epoxy material does not have any visible damage or irreversible softening effect during deformation, it still exhibits obvious degradation in the cyclic tension and SM behaviors. A linear multi-branched model is utilized to assist in the prediction and understanding of the mechanical responses of amorphous SMPs. Parametric studies based on the applied model suggest that the shape memory performance can be improved by adjusting programming and recovery conditions, such as lowering the loading rate, increasing the programming temperature, and reducing the holding time.

  15. CORROSION STUDY OF AMORPHOUS METAL RIBBONS

    SciTech Connect

    Lian, T; Day, S D; Farmer, J C

    2006-07-31

    Corrosion costs the Department of Defense billions of dollars every year, with an immense quantity of material in various structures undergoing corrosion. For example, in addition to fluid and seawater piping, ballast tanks, and propulsions systems, approximately 345 million square feet of structure aboard naval ships and crafts require costly corrosion control measures. The use of advanced corrosion-resistant materials to prevent the continuous degradation of this massive surface area would be extremely beneficial. The potential advantages of amorphous metals have been recognized for some time [Latanison 1985]. Iron-based corrosion-resistant, amorphous-metal coatings under development may prove important for maritime applications [Farmer et al. 2005]. Such materials could also be used to coat the entire outer surface of containers for the transportation and long-term storage of spent nuclear fuel, or to protect welds and heat affected zones, thereby preventing exposure to environments that might cause stress corrosion cracking [Farmer et al. 1991, 2000a, 2000b]. In the future, it may be possible to substitute such high-performance iron-based materials for more-expensive nickel-based alloys, thereby enabling cost savings in a wide variety of industrial applications. It should be noted that thermal-spray ceramic coatings have also been investigated for such applications [Haslam et al. 2005]. This report focuses on the corrosion resistance of iron-based melt-spun amorphous metal ribbons. Melt-Spun ribbon is made by rapid solidification--a stream of molten metal is dropped onto a spinning copper wheel, a process that enables the manufacture of amorphous metals which are unable to be manufactured by conventional cold or hot rolling techniques. The study of melt-spun ribbon allows quick evaluation of amorphous metals corrosion resistance. The melt-spun ribbons included in this study are DAR40, SAM7, and SAM8, SAM1X series, and SAM2X series. The SAM1X series ribbons have

  16. Quantifying Nanoscale Order in Amorphous Materials via Fluctuation Electron Microscopy

    ERIC Educational Resources Information Center

    Bogle, Stephanie Nicole

    2009-01-01

    Fluctuation electron microscopy (FEM) has been used to study the nanoscale order in various amorphous materials. The method is explicitly sensitive to 3- and 4-body atomic correlation functions in amorphous materials; this is sufficient to establish the existence of structural order on the nanoscale, even when the radial distribution function…

  17. LOW-TEMPERATURE CRYSTALLIZATION OF AMORPHOUS SILICATE IN ASTROPHYSICAL ENVIRONMENTS

    SciTech Connect

    Tanaka, Kyoko K.; Yamamoto, Tetsuo; Kimura, Hiroshi

    2010-07-01

    We construct a theoretical model for low-temperature crystallization of amorphous silicate grains induced by exothermic chemical reactions. As a first step, the model is applied to the annealing experiments, in which the samples are (1) amorphous silicate grains and (2) amorphous silicate grains covered with an amorphous carbon layer. We derive the activation energies of crystallization for amorphous silicate and amorphous carbon from the analysis of the experiments. Furthermore, we apply the model to the experiment of low-temperature crystallization of an amorphous silicate core covered with an amorphous carbon layer containing reactive molecules. We clarify the conditions of low-temperature crystallization due to exothermic chemical reactions. Next, we formulate the crystallization conditions so as to be applicable to astrophysical environments. We show that the present crystallization mechanism is characterized by two quantities: the stored energy density Q in a grain and the duration of the chemical reactions {tau}. The crystallization conditions are given by Q>Q{sub min} and {tau} < {tau}{sub cool} regardless of details of the reactions and grain structure, where {tau}{sub cool} is the cooling timescale of the grains heated by exothermic reactions, and Q{sub min} is minimum stored energy density determined by the activation energy of crystallization. Our results suggest that silicate crystallization occurs in wider astrophysical conditions than hitherto considered.

  18. Polarization effects in femtosecond laser induced amorphization of monocrystalline silicon

    NASA Astrophysics Data System (ADS)

    Bai, Feng; Li, Hong-Jin; Huang, Yuan-Yuan; Fan, Wen-Zhong; Pan, Huai-Hai; Wang, Zhuo; Wang, Cheng-Wei; Qian, Jing; Li, Yang-Bo; Zhao, Quan-Zhong

    2016-10-01

    We have used femtosecond laser pulses to ablate monocrystalline silicon wafer. Raman spectroscopy and X-ray diffraction analysis of ablation surface indicates horizontally polarized laser beam shows an enhancement in amorphization efficiency by a factor of 1.6-1.7 over the circularly polarized laser ablation. This demonstrates that one can tune the amorphization efficiency through the polarization of irradiation laser.

  19. Electrically conducting ternary amorphous fully oxidized materials and their application

    NASA Technical Reports Server (NTRS)

    Giauque, Pierre (Inventor); Nicolet, Marc (Inventor); Gasser, Stefan M. (Inventor); Kolawa, Elzbieta A. (Inventor); Cherry, Hillary (Inventor)

    2004-01-01

    Electrically active devices are formed using a special conducting material of the form Tm--Ox mixed with SiO2 where the materials are immiscible. The immiscible materials are forced together by using high energy process to form an amorphous phase of the two materials. The amorphous combination of the two materials is electrically conducting but forms an effective barrier.

  20. Pressure-induced transformations in amorphous silicon: A computational study

    SciTech Connect

    Garcez, K. M. S.; Antonelli, A.

    2014-02-14

    We study the transformations between amorphous phases of Si through molecular simulations using the environment dependent interatomic potential (EDIP) for Si. Our results show that upon pressure, the material undergoes a transformation from the low density amorphous (LDA) Si to the high density amorphous (HDA) Si. This transformation can be reversed by decompressing the material. This process, however, exhibits clear hysteresis, suggesting that the transformation LDA ↔ HDA is first-order like. The HDA phase is predominantly five-fold coordinated, whereas the LDA phase is the normal tetrahedrally bonded amorphous Si. The HDA phase at 400 K and 20 GPa was submitted to an isobaric annealing up to 800 K, resulting in a denser amorphous phase, which is structurally distinct from the HDA phase. Our results also show that the atomic volume and structure of this new amorphous phase are identical to those of the glass obtained by an isobaric quenching of the liquid in equilibrium at 2000 K and 20 GPa down to 400 K. The similarities between our results and those for amorphous ices suggest that this new phase is the very high density amorphous Si.

  1. Method for improving the stability of amorphous silicon

    DOEpatents

    Branz, Howard M.

    2004-03-30

    A method of producing a metastable degradation resistant amorphous hydrogenated silicon film is provided, which comprises the steps of growing a hydrogenated amorphous silicon film, the film having an exposed surface, illuminating the surface using an essentially blue or ultraviolet light to form high densities of a light induced defect near the surface, and etching the surface to remove the defect.

  2. Using Amorphous Phases in the Design of Structural Alloys

    NASA Astrophysics Data System (ADS)

    Schwarz, R. B.; Nash, P.

    1989-01-01

    The recent discovery that amorphous alloy powders can be prepared by mechanically alloying a mixture of pure crystalline intermetallics is opening new windows to the synthesis of engineering materials. Amorphous powders synthesized by mechanical alloying may find application in the design of structural alloys, high thermal conductivity alloys, and metal-matrix composites.

  3. Superlattice doped layers for amorphous silicon photovoltaic cells

    DOEpatents

    Arya, Rajeewa R.

    1988-01-12

    Superlattice doped layers for amorphous silicon photovoltaic cells comprise a plurality of first and second lattices of amorphous silicon alternatingly formed on one another. Each of the first lattices has a first optical bandgap and each of the second lattices has a second optical bandgap different from the first optical bandgap. A method of fabricating the superlattice doped layers also is disclosed.

  4. Amorphization and nanocrystallization of silcon under shock compression

    DOE PAGES

    Remington, B. A.; Wehrenberg, C. E.; Zhao, S.; Hahn, E. N.; Kad, B.; Bringa, E. M.; Meyers, M. A.

    2015-11-06

    High-power, short-duration, laser-driven, shock compression and recovery experiments on [001] silicon unveiled remarkable structural changes above a pressure threshold. Two distinct amorphous regions were identified: (a) a bulk amorphous layer close to the surface and (b) amorphous bands initially aligned with {111} slip planes. Further increase of the laser energy leads to the re-crystallization of amorphous silicon into nanocrystals with high concentration of nano-twins. This amorphization is produced by the combined effect of high magnitude hydrostatic and shear stresses under dynamic shock compression. Shock-induced defects play a very important role in the onset of amorphization. Calculations of the free energymore » changes with pressure and shear, using the Patel-Cohen methodology, are in agreement with the experimental results. Molecular dynamics simulation corroborates the amorphization, showing that it is initiated by the nucleation and propagation of partial dislocations. As a result, the nucleation of amorphization is analyzed qualitatively by classical nucleation theory.« less

  5. Fabrication and Characterization of Amorphous/Nanocrystalline Thin Film Composite

    NASA Astrophysics Data System (ADS)

    Newton, Benjamin S.

    Combining the absorption abilities of amorphous silicon and the electron transport capabilities of crystalline silicon would be a great advantage to not only solar cells but other semiconductor devices. In this work composite films were created using molecular beam epitaxy and electron beam deposition interchangeably as a method to create metallic precursors. Aluminum induced crystallization techniques were used to convert an amorphous silicon film with a capping layer of aluminum nanodots into a film composed of a mixture of amorphous silicon and nanocrystalline silicon. This layer was grown into the amorphous layer by cannibalizing a portion of the amorphous silicon material during the aluminum induced crystallization. Characterization was performed on films and metallic precursors utilizing SEM, TEM, ellipsometry and spectrophotometer.

  6. Direct-patterned optical waveguides on amorphous silicon films

    DOEpatents

    Vernon, Steve; Bond, Tiziana C.; Bond, Steven W.; Pocha, Michael D.; Hau-Riege, Stefan

    2005-08-02

    An optical waveguide structure is formed by embedding a core material within a medium of lower refractive index, i.e. the cladding. The optical index of refraction of amorphous silicon (a-Si) and polycrystalline silicon (p-Si), in the wavelength range between about 1.2 and about 1.6 micrometers, differ by up to about 20%, with the amorphous phase having the larger index. Spatially selective laser crystallization of amorphous silicon provides a mechanism for controlling the spatial variation of the refractive index and for surrounding the amorphous regions with crystalline material. In cases where an amorphous silicon film is interposed between layers of low refractive index, for example, a structure comprised of a SiO.sub.2 substrate, a Si film and an SiO.sub.2 film, the formation of guided wave structures is particularly simple.

  7. Parametrized dielectric functions of amorphous GeSn alloys

    NASA Astrophysics Data System (ADS)

    D'Costa, Vijay Richard; Wang, Wei; Schmidt, Daniel; Yeo, Yee-Chia

    2015-09-01

    We obtained the complex dielectric function of amorphous Ge1-xSnx (0 ≤ x ≤ 0.07) alloys using spectroscopic ellipsometry from 0.4 to 4.5 eV. Amorphous GeSn films were formed by room-temperature implantation of phosphorus into crystalline GeSn alloys grown by molecular beam epitaxy. The optical response of amorphous GeSn alloys is similar to amorphous Ge and can be parametrized using a Kramers-Kronig consistent Cody-Lorentz dispersion model. The parametric model was extended to account for the dielectric functions of amorphous Ge0.75Sn0.25 and Ge0.50Sn0.50 alloys from literature. The compositional dependence of band gap energy Eg and parameters associated with the Lorentzian oscillator have been determined. The behavior of these parameters with varying x can be understood in terms of the alloying effect of Sn on Ge.

  8. Atomistic simulation of damage accumulation and amorphization in Ge

    SciTech Connect

    Gomez-Selles, Jose L. Martin-Bragado, Ignacio; Claverie, Alain; Benistant, Francis

    2015-02-07

    Damage accumulation and amorphization mechanisms by means of ion implantation in Ge are studied using Kinetic Monte Carlo and Binary Collision Approximation techniques. Such mechanisms are investigated through different stages of damage accumulation taking place in the implantation process: from point defect generation and cluster formation up to full amorphization of Ge layers. We propose a damage concentration amorphization threshold for Ge of ∼1.3 × 10{sup 22} cm{sup −3} which is independent on the implantation conditions. Recombination energy barriers depending on amorphous pocket sizes are provided. This leads to an explanation of the reported distinct behavior of the damage generated by different ions. We have also observed that the dissolution of clusters plays an important role for relatively high temperatures and fluences. The model is able to explain and predict different damage generation regimes, amount of generated damage, and extension of amorphous layers in Ge for different ions and implantation conditions.

  9. Atomic structure of amorphous shear bands in boron carbide.

    PubMed

    Reddy, K Madhav; Liu, P; Hirata, A; Fujita, T; Chen, M W

    2013-01-01

    Amorphous shear bands are the main deformation and failure mode of super-hard boron carbide subjected to shock loading and high pressures at room temperature. Nevertheless, the formation mechanisms of the amorphous shear bands remain a long-standing scientific curiosity mainly because of the lack of experimental structure information of the disordered shear bands, comprising light elements of carbon and boron only. Here we report the atomic structure of the amorphous shear bands in boron carbide characterized by state-of-the-art aberration-corrected transmission electron microscopy. Distorted icosahedra, displaced from the crystalline matrix, were observed in nano-sized amorphous bands that produce dislocation-like local shear strains. These experimental results provide direct experimental evidence that the formation of amorphous shear bands in boron carbide results from the disassembly of the icosahedra, driven by shear stresses.

  10. Moringa coagulant as a stabilizer for amorphous solids: Part I.

    PubMed

    Bhende, Santosh; Jadhav, Namdeo

    2012-06-01

    Stabilization of amorphous state is a focal area for formulators to reap benefits related with solubility and consequently bioavailability of poorly soluble drugs. In the present work, an attempt has been made to explore the potential of moringa coagulant as an amorphous state stabilizer by investigating its role in stabilization of spray-dried (amorphous) ibuprofen, meloxicam and felodipine. Thermal studies like glass forming ability, glass transition temperature, hot stage microscopy and DSC were carried out for understanding thermodynamic stabilization of drugs. PXRD and dissolution studies were performed to support contribution of moringa coagulant. Studies showed that hydrogen bonding and electrostatic interactions between drug and moringa coagulant are responsible for amorphous state stabilization as explored by ATR-FTIR and molecular docking. Especially, H-bonding was found to be predominant mechanism for drug stabilization. Therein, arginine (basic amino acid in coagulant) exhibited various interactions and played important role in stabilization of aforesaid amorphous drugs. PMID:22359158

  11. Salt Fog Testing Iron-Based Amorphous Alloys

    SciTech Connect

    Rebak, Raul B.; Aprigliano, Louis F.; Day, S. Daniel; Farmer, Joseph C.

    2007-07-01

    Iron-based amorphous alloys are hard and highly corrosion resistant, which make them desirable for salt water and other applications. These alloys can be produced as powder and can be deposited as coatings on any surface that needs to be protected from the environment. It was of interest to examine the behavior of these amorphous alloys in the standard salt-fog testing ASTM B 117. Three different amorphous coating compositions were deposited on 316L SS coupons and exposed for many cycles of the salt fog test. Other common engineering alloys such as 1018 carbon steel, 316L SS and Hastelloy C-22 were also tested together with the amorphous coatings. Results show that amorphous coatings are resistant to rusting in salt fog. Partial devitrification may be responsible for isolated rust spots in one of the coatings. (authors)

  12. Amorphous molybdenum sulfides as hydrogen evolution catalysts.

    PubMed

    Morales-Guio, Carlos G; Hu, Xile

    2014-08-19

    Providing energy for a population projected to reach 9 billion people within the middle of this century is one of the most pressing societal issues. Burning fossil fuels at a rate and scale that satisfy our near-term demand will irreversibly damage the living environment. Among the various sources of alternative and CO2-emission-free energies, the sun is the only source that is capable of providing enough energy for the whole world. Sunlight energy, however, is intermittent and requires an efficient storage mechanism. Sunlight-driven water splitting to make hydrogen is widely considered as one of the most attractive methods for solar energy storage. Water splitting needs a hydrogen evolution catalyst to accelerate the rate of hydrogen production and to lower the energy loss in this process. Precious metals such as Pt are superior catalysts, but they are too expensive and scarce for large-scale applications. In this Account, we summarize our recent research on the preparation, characterization, and application of amorphous molybdenum sulfide catalysts for the hydrogen evolution reaction. The catalysts can be synthesized by electrochemical deposition under ambient conditions from readily available and inexpensive precursors. The catalytic activity is among the highest for nonprecious catalysts. For example, at a loading of 0.2 mg/cm(2), the optimal catalyst delivers a current density of 10 mA/cm(2) at an overpotential of 160 mV. The growth mechanism of the electrochemically deposited film catalysts was revealed by an electrochemical quartz microcrystal balance study. While different electrochemical deposition methods produce films with different initial compositions, the active catalysts are the same and are identified as a "MoS(2+x)" species. The activity of the film catalysts can be further promoted by divalent Fe, Co, and Ni ions, and the origins of the promotional effects have been probed. Highly active amorphous molybdenum sulfide particles can also be prepared

  13. Characteristics of amorphous kerogens fractionated from terrigenous sedimentary rocks

    NASA Astrophysics Data System (ADS)

    Suzuki, Noriyuki

    1984-02-01

    A preliminary attempt to fractionate amorphous kerogens from terrigenous bulk kerogen by a benzene-water two phase partition method under acidic condition was made. Microscopic observation revealed that amorphous kerogens and structured kerogens were fractionated effectively by this method. Characteristics of the amorphous and structured kerogens fractionated by this method were examined by some chemical analyses and compared with those of the bulk kerogen and humic acid isolated from the same rock sample (Haizume Formation, Pleistocene, Japan). The elemental and infrared (IR) analyses showed that the amorphous kerogen fraction had the highest atomic H/C ratio and the lowest atomic N/C ratio and was the richest in aliphatic structures and carbonyl and carboxyl functional groups. Quantities of fatty acids from the saponification products of each geopolymer were in agreement with the results of elemental and IR analyses. Distribution of the fatty acids was suggestive that more animal lipids participate in the formation of amorphous kerogens because of the abundance of relatively lower molecular weight fatty acids (such as C 16 and C 18 acids) in saponification products of amorphous kerogens. On the other hand, although the amorphous kerogen fraction tends to be rich in aliphatic structures compared with bulk kerogen of the same rock samples, van Krevelen plots of elemental compositions of kerogens from the core samples (Nishiyama Oil Field, Tertiary, Japan) reveal that the amorphous kerogen fraction is not necessarily characterized by markedly high atomic H/C ratio. This was attributed to the oxic environment of deposition and the abundance of biodegraded terrestrial amorphous organic matter in the amorphous kerogen fraction used in this work.

  14. 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.

  15. Theoretical studies of amorphous silicon and hydrogenated amorphous silicon with molecular dynamics simulations

    SciTech Connect

    Kwon, I.

    1991-12-20

    Amorphous silicon (a-Si) and hydrogenated amorphous silicon (a-Si:H) have been studied with molecular dynamics simulations. The structural, vibrational, and electronic properties of these materials have been studied with computer-generated structural models and compare well with experimental observations. The stability of a-si and a-Si:H have been studied with the aim of understanding microscopic mechanisms underlying light-induced degradation in a-Si:H (the Staebler-Wronski effect). With a view to understanding thin film growth processes, a-Si films have been generated with molecular dynamics simulations by simulating the deposition of Si-clusters on a Si(111) substrate. A new two- and three-body interatomic potential for Si-H interactions has been developed. The structural properties of a-Si:H networks are in good agreement with experimental measurements. The presence of H atoms reduces strain and disorder relative to networks without H.

  16. Nanostructural characterization of amorphous diamondlike carbon films

    SciTech Connect

    SIEGAL,MICHAEL P.; TALLANT,DAVID R.; MARTINEZ-MIRANDA,L.J.; BARBOUR,J. CHARLES; SIMPSON,REGINA L.; OVERMYER,DONALD L.

    2000-01-27

    Nanostructural characterization of amorphous diamondlike carbon (a-C) films grown on silicon using pulsed-laser deposition (PLD) is correlated to both growth energetic and film thickness. Raman spectroscopy and x-ray reflectivity probe both the topological nature of 3- and 4-fold coordinated carbon atom bonding and the topographical clustering of their distributions within a given film. In general, increasing the energetic of PLD growth results in films becoming more ``diamondlike'', i.e. increasing mass density and decreasing optical absorbance. However, these same properties decrease appreciably with thickness. The topology of carbon atom bonding is different for material near the substrate interface compared to material within the bulk portion of an a-C film. A simple model balancing the energy of residual stress and the free energies of resulting carbon topologies is proposed to provide an explanation of the evolution of topographical bonding clusters in a growing a-C film.

  17. Amorphous silicon-based microchannel plates

    NASA Astrophysics Data System (ADS)

    Franco, Andrea; Riesen, Yannick; Wyrsch, Nicolas; Dunand, Sylvain; Powolny, François; Jarron, Pierre; Ballif, Christophe

    2012-12-01

    Microchannel plates (MCP) based on hydrogenated amorphous silicon (a-Si:H) were recently introduced to overcome some of the limitations of crystalline silicon and glass MCP. The typical thickness of a-Si:H based MCPs (AMCP) ranges between 80 and 100 μm and the micromachining of the channels is realized by deep reactive ion etching (DRIE). Advantages and issues regarding the fabrication process are presented and discussed. Electron amplification is demonstrated and analyzed using Electron Beam Induced Current (EBIC) technique. The gain increases as a function of the bias voltage, limited to -340 V on account of high leakage currents across the structure. EBIC maps on 10° tilted samples confirm that the device active area extend to the entire channel opening. AMCP characterization with the electron beam shows gain saturation and signal quenching which depends on the effectiveness of the charge replenishment in the channel walls.

  18. Bulk amorphous steels based on Fe alloys

    DOEpatents

    Lu, ZhaoPing; Liu, Chain T.

    2006-05-30

    A bulk amorphous alloy has the approximate composition: Fe.sub.(100-a-b-c-d-e)Y.sub.aMn.sub.bT.sub.cM.sub.dX.sub.e wherein: T includes at least one of the group consisting of: Ni, Cu, Cr and Co; M includes at least one of the group consisting of W, Mo, Nb, Ta, Al and Ti; X includes at least one of the group consisting of Co, Ni and Cr; a is an atomic percentage, and a<5; b is an atomic percentage, and b.ltoreq.25; c is an atomic percentage, and c.ltoreq.25; d is an atomic percentage, and d.ltoreq.25; and e is an atomic percentage, and 5.ltoreq.e.ltoreq.30.

  19. Orientational fluctuations of amorphous nematogenic solids

    NASA Astrophysics Data System (ADS)

    Ye, Fangfu; Lu, Bing; Goldbart, Paul

    2012-02-01

    Amorphous nematogenic solids (ANS) are media comprising rod-like nematogens that have been randomly linked to form elastically deformable macroscopic networks. Classes of ANS include chemical nematogen gels (i.e., networks of small molecules) and liquid crystalline elastomers (built from crosslinked nematogen-containing macromolecules), as well as biophysical networks such as those composed of actin filaments. We use a method inspired by the cavity approach to construct a replica free energy for these random systems, and investigate the correlations of the thermal fluctuations of the orientational alignment of the nematogens at spatially separated points. We identify two qualitatively distinct regimes: (a) a weakly localized regime, in which the correlations decay exponentially with separation; and (b) a strongly localized regime, characterized by correlations that also decay but oscillate as they do.

  20. Ultrafast recombination and trapping in amorphous silicon

    NASA Astrophysics Data System (ADS)

    Esser, A.; Seibert, K.; Kurz, H.; Parsons, G. N.; Wang, C.; Davidson, B. N.; Lucovsky, G.; Nemanich, R. J.

    1990-02-01

    We have studied the time-resolved reflectivity and transmission changes induced by femtosecond laser pulses in hydrogenated and nonhydrogenated amorphous silicon thin films, a-Si:H and a-Si, respectively. By varying the pump power, and hence the photoexcited free-carrier densities, by several orders of magnitude, a quadratic, nonradiative recombination process has been identified that controls the density of free carriers on a picosecond time scale for excitation levels above 5×1018 cm-3 in a-Si:H and above 5×1019 cm-3 in a-Si. At lower free-carrier densities, the reflectivity transients display the dynamics expected from a trapping mechanism. We suggest that the process that dominates for the higher free-carrier densities may result from Auger recombination but with a dependence on the carrier density that is different from that which has been observed in crystalline semiconductors where k selection prevails.

  1. Polarization Stability of Amorphous Piezoelectric Polyimides

    NASA Technical Reports Server (NTRS)

    Park, C.; Ounaies, Z.; Su, J.; Smith, J. G., Jr.; Harrison, J. S.

    2000-01-01

    Amorphous polyimides containing polar functional groups have been synthesized and investigated for potential use as high temperature piezoelectric sensors. The thermal stability of the piezoelectric effect of one polyimide was evaluated as a function of various curing and poling conditions under dynamic and static thermal stimuli. First, the polymer samples were thermally cycled under strain by systematically increasing the maximum temperature from 50 C to 200 C while the piezoelectric strain coefficient was being measured. Second, the samples were isothermally aged at an elevated temperature in air, and the isothermal decay of the remanent polarization was measured at room temperature as a function of time. Both conventional and corona poling methods were evaluated. This material exhibited good thermal stability of the piezoelectric properties up to 100 C.

  2. Breakdown of continuum elasticity in amorphous solids

    NASA Astrophysics Data System (ADS)

    Lerner, Edan; DeGiuli, Eric; Düring, Gustavo; Wyart, Matthieu

    We show numerically that the response of simple amorphous solids (elastic networks and particle packings) to a local force dipole is characterized by a lengthscale $\\ell_c$ that diverges as unjamming is approached as $\\ell_c \\sim (z - 2d)^{-1/2}$, where $z \\ge 2d$ is the mean coordination, and $d$ is the spatial dimension, at odds with previous numerical claims. We also show how the magnitude of the lengthscale $\\ell_c$ is amplified by the presence of internal stresses in the disordered solid. Our data suggests a divergence of $\\ell_c\\sim (p_c-p)^{-1/4}$ with proximity to a critical internal stress $p_c$ at which soft elastic modes become unstable.

  3. Evidence for Valence Alternation in Amorphous Selenium

    NASA Astrophysics Data System (ADS)

    Xiaodong, Zhang; Drabold, D. A.

    1998-05-01

    A molecular-dynamics simulation has been carried out for amorphous selenium. The simulation used 64 atoms as well as 216 atoms in a constant volume simple cubic cell. The pair correlation function g(r) and structure factors S(Q) were computed and compared with experimental and previous theoretical data. The coordination number is exactly 2 in both 64 atoms and 216 atoms model. In 64 atoms model, only 1 intimate valence alternation pair (IVAP) type defect was produced. The majority defect types are IVAP and valence alternation pair (VAP) in 216 atoms model. The electronic density function of state and the localization of the electronic state also manisfest some characternistic of VAP defect type. The results give a theoretical evidence for valence alternation in a-Se.

  4. Buckling instability in amorphous carbon films

    NASA Astrophysics Data System (ADS)

    Zhu, X. D.; Narumi, K.; Naramoto, H.

    2007-06-01

    In this paper, we report the buckling instability in amorphous carbon films on mirror-polished sapphire (0001) wafers deposited by ion beam assisted deposition at various growth temperatures. For the films deposited at 150 °C, many interesting stress relief patterns are found, which include networks, blisters, sinusoidal patterns with π-shape, and highly ordered sinusoidal waves on a large scale. Starting at irregular buckling in the centre, the latter propagate towards the outer buckling region. The maximum length of these ordered patterns reaches 396 µm with a height of ~500 nm and a wavelength of ~8.2 µm. However, the length decreases dramatically to 70 µm as the deposition temperature is increased to 550 °C. The delamination of the film appears instead of sinusoidal waves with a further increase of the deposition temperature. This experimental observation is correlated with the theoretic work of Crosby (1999 Phys. Rev. E 59 R2542).

  5. Amorphous materials molded IR lens progress report

    NASA Astrophysics Data System (ADS)

    Hilton, A. R., Sr.; McCord, James; Timm, Ronald; Le Blanc, R. A.

    2008-04-01

    Amorphous Materials began in 2000 a joint program with Lockheed Martin in Orlando to develop molding technology required to produce infrared lenses from chalcogenide glasses. Preliminary results were reported at this SPIE meeting by Amy Graham1 in 2003. The program ended in 2004. Since that time, AMI has concentrated on improving results from two low softening glasses, Amtir 4&5. Both glasses have been fully characterized and antireflection coatings have been developed for each. Lenses have been molded from both glasses, from Amtir 6 and from C1 Core glass. A Zygo unit is used to evaluate the results of each molded lens as a guide to improving the molding process. Expansion into a larger building has provided room for five production molding units. Molded lens sizes have ranged from 8 mm to 136 mm in diameter. Recent results will be presented

  6. Short range atomic migration in amorphous silicon

    NASA Astrophysics Data System (ADS)

    Strauß, F.; Jerliu, B.; Geue, T.; Stahn, J.; Schmidt, H.

    2016-05-01

    Experiments on self-diffusion in amorphous silicon between 400 and 500 °C are presented, which were carried out by neutron reflectometry in combination with 29Si/natSi isotope multilayers. Short range diffusion is detected on a length scale of about 2 nm, while long range diffusion is absent. Diffusivities are in the order of 10-19-10-20 m2/s and decrease with increasing annealing time, reaching an undetectable low value for long annealing times. This behavior is strongly correlated to structural relaxation and can be explained as a result of point defect annihilation. Diffusivities for short annealing times of 60 s follow the Arrhenius law with an activation enthalpy of (0.74 ± 0.21) eV, which is interpreted as the activation enthalpy of Si migration.

  7. Enthalpy of formation of amorphous silica

    SciTech Connect

    Klyuchnikov, V.A.; Voronkov, M.G.; Landa, L.M.; Pepekin, V.I.; Tikhenko, T.M.; Shvets, G.N.; Popov, V.T.

    1987-07-01

    In calculating the formation heat of organosilicon compounds from the results of their combustion heat on oxygen it is necessary to have a reliable value of the standard formation heat of hydrated silica. This paper, in trying to assess this property, examines the following factors: the character of the surface, the structure and specific concentration of surface silicon hydroxide groups, and the energy of its wetting with water. Combustion experiments are carried out and described. It is concluded that the formation heat of amorphous silica is not a constant value and is determined by the character of its surface and degree of hydration. For this reason, in the combustion of organosilicon compounds, the formation heat of silica should be determined experimentally.

  8. Lithium transport through nanosized amorphous silicon layers.

    PubMed

    Hüger, Erwin; Dörrer, Lars; Rahn, Johanna; Panzner, Tobias; Stahn, Jochen; Lilienkamp, Gerhard; Schmidt, Harald

    2013-03-13

    Lithium migration in nanostructured electrode materials is important for an understanding and improvement of high energy density lithium batteries. An approach to measure lithium transport through nanometer thin layers of relevant electrochemical materials is presented using amorphous silicon as a model system. A multilayer consisting of a repetition of five [(6)LiNbO3(15 nm)/Si (10 nm)/(nat)LiNbO3 (15 nm)/Si (10 nm)] units is used for analysis, where LiNbO3 is a Li tracer reservoir. It is shown that the change of the relative (6)Li/(7)Li isotope fraction in the LiNbO3 layers by lithium diffusion through the nanosized silicon layers can be monitored nondestructively by neutron reflectometry. The results can be used to calculate transport parameters.

  9. Structural relaxation of vacancies in amorphous silicon

    SciTech Connect

    Kim, E.; Lee, Y.H.; Chen, C.; Pang, T.

    1997-07-01

    The authors have studied the structural relaxation of vacancies in amorphous silicon (a-Si) using a tight-binding molecular-dynamics method. The most significant difference between vacancies in a-Si and those in crystalline silicon (c-Si) is that the deep gap states do not show up in a-Si. This difference is explained through the unusual behavior of the structural relaxation near the vacancies in a-Si, which enhances the sp{sup 2} + p bonding near the band edges. They have also observed that the vacancies do not migrate below 450 K although some of them can still be annihilated, particularly at high defect density due to large structural relaxation.

  10. How does an amorphous surface influence molecular binding?--ovocleidin-17 and amorphous calcium carbonate.

    PubMed

    Freeman, Colin L; Harding, John H; Quigley, David; Rodger, P Mark

    2015-07-14

    Atomistic molecular dynamics simulations of dehydrated amorphous calcium carbonate interacting with the protein ovocleidin-17 are presented. These simulations demonstrate that the amorphisation of the calcium carbonate surface removes water structure from the surface. This reduction of structure allows the protein to bind with many residues, unlike on crystalline surfaces where binding is strongest when only a few residues are attached to the surface. Basic residues are observed to dominate the binding interactions. The implications for protein control over crystallisation are discussed.

  11. Castable Amorphous Metal Mirrors and Mirror Assemblies

    NASA Technical Reports Server (NTRS)

    Hofmann, Douglas C.; Davis, Gregory L.; Agnes, Gregory S.; Shapiro, Andrew A.

    2013-01-01

    A revolutionary way to produce a mirror and mirror assembly is to cast the entire part at once from a metal alloy that combines all of the desired features into the final part: optical smoothness, curvature, flexures, tabs, isogrids, low CTE, and toughness. In this work, it has been demonstrated that castable mirrors are possible using bulk metallic glasses (BMGs, also called amorphous metals) and BMG matrix composites (BMGMCs). These novel alloys have all of the desired mechanical and thermal properties to fabricate an entire mirror assembly without machining, bonding, brazing, welding, or epoxy. BMGs are multi-component metal alloys that have been cooled in such a manner as to avoid crystallization leading to an amorphous (non-crystalline) microstructure. This lack of crystal structure and the fact that these alloys are glasses, leads to a wide assortment of mechanical and thermal properties that are unlike those observed in crystalline metals. Among these are high yield strength, carbide-like hardness, low melting temperatures (making them castable like aluminum), a thermoplastic processing region (for improving smoothness), low stiffness, high strength-to-weight ratios, relatively low CTE, density similar to titanium alloys, high elasticity and ultra-smooth cast parts (as low as 0.2-nm surface roughness has been demonstrated in cast BMGs). BMGMCs are composite alloys that consist of a BMG matrix with crystalline dendrites embedded throughout. BMGMCs are used to overcome the typically brittle failure observed in monolithic BMGs by adding a soft phase that arrests the formation of cracks in the BMG matrix. In some cases, BMGMCs offer superior castability, toughness, and fatigue resistance, if not as good a surface finish as BMGs. This work has demonstrated that BMGs and BMGMCs can be cast into prototype mirrors and mirror assemblies without difficulty.

  12. Anomalous hopping conduction in nanocrystalline/amorphous composites and amorphous semiconductor thin films

    NASA Astrophysics Data System (ADS)

    Kakalios, James; Bodurtha, Kent

    Composite nanostructured materials consisting of nanocrystals (nc) embedded within a thin film amorphous matrix can exhibit novel opto-electronic properties. Composite films are synthesized in a dual-chamber co-deposition PECVD system capable of producing nanocrystals of material A and embedding then within a thin film matrix of material B. Electronic conduction in composite thin films of hydrogenated amorphous silicon (a-Si:H) containing nc-germanium or nc-silicon inclusions, as well as in undoped a-Si:H, does not follow an Arrhenius temperature dependence, but rather is better described by an anomalous hopping expression (exp[-(To/T)3/4) , as determined from the ``reduced activation energy'' proposed by Zabrodskii and Shlimak. This temperature dependence has been observed in other thin film resistive materials, such as ultra-thin disordered films of Ag, Bi, Pb and Pd; carbon-black polymer composites; and weakly coupled Au and ZnO quantum dot arrays. There is presently no accepted theoretical understanding of this expression. The concept of a mobility edge, accepted for over four decades, appears to not be necessary to account for charge transport in amorphous semiconductors. Supported by NSF-DMR and the Minnesota Nano Center.

  13. Amorphous Calcium Carbonate Based-Microparticles for Peptide Pulmonary Delivery.

    PubMed

    Tewes, Frederic; Gobbo, Oliviero L; Ehrhardt, Carsten; Healy, Anne Marie

    2016-01-20

    Amorphous calcium carbonate (ACC) is known to interact with proteins, for example, in biogenic ACC, to form stable amorphous phases. The control of amorphous/crystalline and inorganic/organic ratios in inhalable calcium carbonate microparticles may enable particle properties to be adapted to suit the requirements of dry powders for pulmonary delivery by oral inhalation. For example, an amorphous phase can immobilize and stabilize polypeptides in their native structure and amorphous and crystalline phases have different mechanical properties. Therefore, inhalable composite microparticles made of inorganic (i.e., calcium carbonate and calcium formate) and organic (i.e., hyaluronan (HA)) amorphous and crystalline phases were investigated for peptide and protein pulmonary aerosol delivery. The crystalline/amorphous ratio and polymorphic form of the inorganic component was altered by changing the microparticle drying rate and by changing the ammonium carbonate and HA initial concentration. The bioactivity of the model peptide, salmon calcitonin (sCT), coprocessed with alpha-1-antitrypsin (AAT), a model protein with peptidase inhibitor activity, was maintained during processing and the microparticles had excellent aerodynamic properties, making them suitable for pulmonary aerosol delivery. The bioavailability of sCT after aerosol delivery as sCT and AAT-loaded composite microparticles to rats was 4-times higher than that of sCT solution.

  14. Amorphous Calcium Carbonate Based-Microparticles for Peptide Pulmonary Delivery.

    PubMed

    Tewes, Frederic; Gobbo, Oliviero L; Ehrhardt, Carsten; Healy, Anne Marie

    2016-01-20

    Amorphous calcium carbonate (ACC) is known to interact with proteins, for example, in biogenic ACC, to form stable amorphous phases. The control of amorphous/crystalline and inorganic/organic ratios in inhalable calcium carbonate microparticles may enable particle properties to be adapted to suit the requirements of dry powders for pulmonary delivery by oral inhalation. For example, an amorphous phase can immobilize and stabilize polypeptides in their native structure and amorphous and crystalline phases have different mechanical properties. Therefore, inhalable composite microparticles made of inorganic (i.e., calcium carbonate and calcium formate) and organic (i.e., hyaluronan (HA)) amorphous and crystalline phases were investigated for peptide and protein pulmonary aerosol delivery. The crystalline/amorphous ratio and polymorphic form of the inorganic component was altered by changing the microparticle drying rate and by changing the ammonium carbonate and HA initial concentration. The bioactivity of the model peptide, salmon calcitonin (sCT), coprocessed with alpha-1-antitrypsin (AAT), a model protein with peptidase inhibitor activity, was maintained during processing and the microparticles had excellent aerodynamic properties, making them suitable for pulmonary aerosol delivery. The bioavailability of sCT after aerosol delivery as sCT and AAT-loaded composite microparticles to rats was 4-times higher than that of sCT solution. PMID:26692360

  15. Rate of H2 formation on amorphous grains

    NASA Technical Reports Server (NTRS)

    Smoluchowski, R.

    1981-01-01

    The rate of formation of molecular hydrogen from hydrogen atoms adsorbed on amorphous grains taken to represent interstellar dust grains is analyzed. Following a brief review of the structure and thermodynamics of amorphous grains and the evidence that interstellar grains are indeed amorphous, consideration is given to the mechanism of formation of H2 molecules by the impact of H atoms on grains with adsorbed H atoms, and it is concluded that on amorphous grains, molecule formation will only occur if H atoms are adsorbed within a distance on the order of 10 A of each other. Rates of H2 formation on single crystal and polycrystalline grains are then calculated and compared with those for amorphous grains, and it is shown that, except for certain temperatures and high H atom densities, the rates of H2 formation on polycrystalline and amorphous grains are up to a few orders of magnitude lower than on single crystals. The results suggest that amorphous grains will lead to H2 clouds with irregular and sharply delineated features in contrast to the more uniform clouds formed on crystalline grains.

  16. Preparation and electrochemical properties of Co-Si 3N 4 nanocomposites

    NASA Astrophysics Data System (ADS)

    Yao, S. M.; Xi, K.; Li, G. R.; Gao, X. P.

    Cobalt nanoparticles on an amorphous Si 3N 4 matrix were synthesized by direct ball-milling of Co and Si 3N 4 powders for an improvement of their electrochemical performance. The microstructure, morphology and chemical state of the ball-milled Co-Si 3N 4 composites are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The electrochemical performance of Co-Si 3N 4 composites was investigated by galvanostatic charge-discharge process and cyclic voltammetry (CV) technique. It is found that metallic Co nanoparticles of 10-20 nm in size are highly dispersed on the amorphous inactive Si 3N 4 matrix after the ball-milling. The composite with a Co/Si molar ratio of 2/1 shows the optimized electrochemical performance, including discharge capacity and cycle stability. The formation of Co nanoparticles with a good reaction activity is responsible for the discharge capacity of the composites. The reversible faradic reaction between Co and β-Co(OH) 2 is dominant for ball-milled Co-Si 3N 4 composite. The surface modification of the hydrogen storage PrMg 12-Ni composites using Co-Si 3N 4 composites can enhance the initial discharge capacity based on the hydrogen electrochemical oxidation and Co redox reaction.

  17. Health hazards due to the inhalation of amorphous silica.

    PubMed

    Merget, R; Bauer, T; Küpper, H U; Philippou, S; Bauer, H D; Breitstadt, R; Bruening, T

    2002-01-01

    Occupational exposure to crystalline silica dust is associated with an increased risk for pulmonary diseases such as silicosis, tuberculosis, chronic bronchitis, chronic obstructive pulmonary disease (COPD) and lung cancer. This review summarizes the current knowledge about the health effects of amorphous (non-crystalline) forms of silica. The major problem in the assessment of health effects of amorphous silica is its contamination with crystalline silica. This applies particularly to well-documented pneumoconiosis among diatomaceous earth workers. Intentionally manufactured synthetic amorphous silicas are without contamination of crystalline silica. These synthetic forms may be classified as (1) wet process silica, (2) pyrogenic ("thermal" or "fumed") silica, and (3) chemically or physically modified silica. According to the different physicochemical properties, the major classes of synthetic amorphous silica are used in a variety of products, e.g. as fillers in the rubber industry, in tyre compounds, as free-flow and anti-caking agents in powder materials, and as liquid carriers, particularly in the manufacture of animal feed and agrochemicals; other uses are found in toothpaste additives, paints, silicon rubber, insulation material, liquid systems in coatings, adhesives, printing inks, plastisol car undercoats, and cosmetics. Animal inhalation studies with intentionally manufactured synthetic amorphous silica showed at least partially reversible inflammation, granuloma formation and emphysema, but no progressive fibrosis of the lungs. Epidemiological studies do not support the hypothesis that amorphous silicas have any relevant potential to induce fibrosis in workers with high occupational exposure to these substances, although one study disclosed four cases with silicosis among subjects exposed to apparently non-contaminated amorphous silica. Since the data have been limited, a risk of chronic bronchitis, COPD or emphysema cannot be excluded. There is no study

  18. Dissolution and analysis of amorphous silica in marine sediments.

    USGS Publications Warehouse

    Eggimann, D.W.; Manheim, F. T.; Betzer, P.R.

    1980-01-01

    The analytical estimation of amorphous silica in selected Atlantic and Antarctic Ocean sediments, the U.S.G.S. standard marine mud (MAG-1), A.A.P.G. clays, and samples from cultures of a marine diatom, Hemidiscus, has been examined. Our values for amorphous silica-rich circum-Antarctic sediments are equal to or greater than literature values, whereas our values for a set of amorphous silica-poor sediments from a transect of the N. Atlantic at 11oN, after appropriate correction for silica released from clays, are significantly lower than previous estimates from the same region. -from Authors

  19. The 'depletion layer' of amorphous p-n junctions

    NASA Technical Reports Server (NTRS)

    Von Roos, O.

    1981-01-01

    It is shown that within reasonable approximations for the density of state distribution within the mobility gap of a:Si, a one-to-one correspondence exists between the electric field distribution in the transition region of an amorphous p-n junction and that in the depletion layer of a crystalline p-n junction. Thus it is inferred that the depletion layer approximation which leads to a parabolic potential distribution within the depletion layer of crystalline junctions also constitutes a fair approximation in the case of amorphous junctions. This fact greatly simplifies an analysis of solid-state electronic devices based on amorphous material (i.e., solar cells).

  20. Amorphous photonic crystals with only short-range order.

    PubMed

    Shi, Lei; Zhang, Yafeng; Dong, Biqin; Zhan, Tianrong; Liu, Xiaohan; Zi, Jian

    2013-10-01

    Distinct from conventional photonic crystals with both short- and long-range order, amorphous photonic crystals that possess only short-range order show interesting optical responses owing to their unique structural features. Amorphous photonic crystals exhibit unique light scattering and transport, which lead to a variety of interesting phenomena such as isotropic photonic bandgaps or pseudogaps, noniridescent structural colors, and light localization. Recent experimental and theoretical advances in the study of amorphous photonic crystals are summarized, focusing on their unique optical properties, artificial fabrication, bionspiration, and potential applications.