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

Deibler, Lisa Anne; Brown, Arthur; Puskar, Joseph D.

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grainmore » growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.« less

On a Fast and Accurate In Situ Measuring Strategy for Recrystallization Kinetics and Its Application to an Al-Fe-Si Alloy

NASA Astrophysics Data System (ADS)

Kühbach, Markus; Brüggemann, Thiemo; Molodov, Konstantin D.; Gottstein, Günter

2015-03-01

In the current study, we detail a novel in situ X-ray diffraction-based bulk measurement technique, which allows for the continuous tracking of primary recrystallization kinetics. The approach is based on measuring the diffracted intensity that is correlated with the evolution of the volume fraction of particular texture components during annealing of a sample within a texture goniometer. The method is applied in an experimental study on a cold-rolled industrial Al-Fe-Si alloy. For comparison purposes, the macrotexture and the hardness evolution were monitored ex situ along isothermal and nonisothermal annealing. These measurements were then contrasted to the in situ obtained growth kinetics of recrystallizing grains in beta-fiber deformation and cube orientation. The results showed clearly that this method can be reliably utilized for the characterization of recrystallization kinetics in an industrial context.

Disclination mediated dynamic recrystallization in metals at low temperature.

PubMed

Aramfard, Mohammad; Deng, Chuang

2015-09-16

Recrystallization is one of the most important physical phenomena in condensed matter that has been utilized for materials processing for thousands of years in human history. It is generally believed that recrystallization is thermally activated and a minimum temperature must be achieved for the necessary atomic mechanisms to occur. Here, using atomistic simulations, we report a new mechanism of dynamic recrystallization that can operate at temperature as low as T = 10 K in metals during deformation. In contrast to previously proposed dislocation-based models, this mechanism relies on the generation of disclination quadrupoles, which are special defects that form during deformation when the grain boundary migration is restricted by structural defects such as triple junctions, cracks or obstacles. This mechanism offers an alternative explanation for the grain refinement in metals during severe plastic deformation at cryogenic temperature and may suggest a new method to tailor the microstructure in general crystalline materials.

Disclination mediated dynamic recrystallization in metals at low temperature

PubMed Central

Aramfard, Mohammad; Deng, Chuang

2015-01-01

Recrystallization is one of the most important physical phenomena in condensed matter that has been utilized for materials processing for thousands of years in human history. It is generally believed that recrystallization is thermally activated and a minimum temperature must be achieved for the necessary atomic mechanisms to occur. Here, using atomistic simulations, we report a new mechanism of dynamic recrystallization that can operate at temperature as low as T = 10 K in metals during deformation. In contrast to previously proposed dislocation-based models, this mechanism relies on the generation of disclination quadrupoles, which are special defects that form during deformation when the grain boundary migration is restricted by structural defects such as triple junctions, cracks or obstacles. This mechanism offers an alternative explanation for the grain refinement in metals during severe plastic deformation at cryogenic temperature and may suggest a new method to tailor the microstructure in general crystalline materials. PMID:26374603

Cryogenic strength improvement by utilizing room-temperature deformation twinning in a partially recrystallized VCrMnFeCoNi high-entropy alloy

PubMed Central

Jo, Y. H.; Jung, S.; Choi, W. M.; Sohn, S. S.; Kim, H. S.; Lee, B. J.; Kim, N. J.; Lee, S.

2017-01-01

The excellent cryogenic tensile properties of the CrMnFeCoNi alloy are generally caused by deformation twinning, which is difficult to achieve at room temperature because of insufficient stress for twinning. Here, we induced twinning at room temperature to improve the cryogenic tensile properties of the CrMnFeCoNi alloy. Considering grain size effects on the critical stress for twinning, twins were readily formed in the coarse microstructure by cold rolling without grain refinement by hot rolling. These twins were retained by partial recrystallization and played an important role in improving strength, allowing yield strengths approaching 1 GPa. The persistent elongation up to 46% as well as the tensile strength of 1.3 GPa are attributed to additional twinning in both recrystallized and non-recrystallization regions. Our results demonstrate that non-recrystallized grains, which are generally avoided in conventional alloys because of their deleterious effect on ductility, can be useful in achieving high-strength high-entropy alloys. PMID:28604656

Scanning transmission electron microscopy analysis of Ge(O)/(graphitic carbon nitride) nanocomposite powder

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

Kawasaki, Masahiro; Sompetch, Kanganit; Sarakonsri, Thapanee, E-mail: tsarakonsri@gmail.com

2015-12-15

Analytical electron microscopy has revealed the structure of particles that were synthesized by chemical reaction of GeO{sub 2} with NaBH{sub 4} in the basic solution including graphitic carbon nitride (g-C{sub 3}N{sub 4}) powders. The g-C{sub 3}N{sub 4} was arranged by recrystallization of melamine at 600 °C under N{sub 2} gas atmosphere. The samples were dried at 60 °C or 180 °C for 4 h. The g-C{sub 3}N{sub 4} was observed as lamellae of several ten nm or less in size and had an amorphous-like structure with a distorted lattice in an area as small as a few hundred pm inmore » size. The reaction product was Ge(O) particles as fine as several nm in size and composed of Ge and O atoms. Most of the particles must be of GeO{sub 2−x} with the amorphous-like structure that has also a distorted lattice in an area of a few hundred pm in size. In the sample dried at 60 °C, the particles were found to be dispersed in a wide area on the g-C{sub 3}N{sub 4} lamella. It is hard to recognize those particles in TEM images. The particles in the sample dried at 180 °C became larger and were easily observed as isolated lumps. Hence, these powders can be regarded as GeO{sub 2}/g-C{sub 3}N{sub 4} or Ge/GeO{sub 2}/g-C{sub 3}N{sub 4} nanocomposites, and expected to be applicable to anode materials for high energy Li-ion batteries due to Ge catalysis effect, accordingly. - Graphical abstract: STEM analysis of Ge(O)/(graphitic carbon nitride) nanocomposite powder. - Highlights: • Graphitic (g)-C{sub 3}N{sub 4} powder was prepared at 600 °C by recrystallization of melamine. • Ge(O) was prepared by chemical reaction in a solution including the g-C{sub 3}N{sub 4} powders. • The products can be regarded as GeO{sub 2}/g-C{sub 3}N{sub 4} or Ge/GeO{sub 2}/g-C{sub 3}N{sub 4} nanocomposites. • GeO{sub 2} was amorphous several-nm particles and g-C{sub 3}N{sub 4} was amorphous lamella of several 10 nm in size. • We expect them to be applicable for high energy Li-ion battery anode materials.« less

Fabrication of graphite/epoxy cases for orbit insertion motors

NASA Technical Reports Server (NTRS)

Schmidt, W. W.

1973-01-01

The fabrication procedures are described for filament-wound rocket motor cases, approximately 26.25 inches long by 25.50 inches diameter, utilizing graphite fibers. The process utilized prepreg tape which consists of Fortafil 4-R fibers in the E-759 epoxy resin matrix. This fabrication effect demonstrated an ability to fabricate high quality graphite/epoxy rocket motor cases in the 26.25 inch by 25.50 inch size range.

Solid dispersion of acetaminophen and poly(ethylene oxide) prepared by hot-melt mixing.

PubMed

Yang, Min; Wang, Peng; Huang, Chien-Yueh; Ku, M Sherry; Liu, Huiju; Gogos, Costas

2010-08-16

In this study, a model drug, acetaminophen (APAP), was melt mixed with poly(ethylene oxide) (PEO) using a Brabender mixer. APAP was found to recrystallize upon cooling to room temperature for all the drug loadings investigated. Higher drug loading leads to faster recrystallization rate. However, the morphology of the recrystallized drug crystals is identical in samples with different drug loadings and does not change with the storage time. To adjust the drug's dissolution rate, nanoclay Cloisite 15A and 30B were added into the binary mixture. The presence of either of the nanoclay dramatically accelerates the drug's recrystallization rate and slows down the drug's releasing rate. The drop of the releasing rate is mainly due to the decrease of wettability, as supported by the contact angle data. Data analysis of the dissolution results suggests that the addition of nanoclays changes the drug's release mechanism from erosion dominant to diffusion dominant. This study suggests that nanoclays may be utilized to tailor the drug's releasing rate and to improve the dosage form's stability by dramatically shortening the lengthy recrystallization process. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Filament-wound graphite/epoxy rocket motor case

NASA Technical Reports Server (NTRS)

Humphrey, W. D.; Schmidt, W. W.

1972-01-01

The fabrication procedures are described for a filament-wound rocket motor case, approximately 56 cm long x 71 cm diameter, utilizing high tensile strength graphite fibers. The process utilized Fiberite Hy-E-1330B prepreg tape which consists of Courtaulds HTS fibers in a temperature-sensitive epoxy matrix. This fabrication effort, with resultant design, material and process recommendations, substantiates the manufacturing feasibility of graphite/epoxy rocket motor cases in the 56 cm x 71 cm size range.

Experiments and modeling to characterize microstructure and hardness in 304L

DOE PAGES

Deibler, Lisa Anne; Brown, Arthur; Puskar, Joseph D.

2017-01-12

Drawn 304L stainless steel tubing was subjected to 42 different annealing heat treatments with the goal of initializing a microstructural model to select a heat treatment to soften the tubing from a hardness of 305 Knoop to 225–275 Knoop. The amount of recrystallization and grain size caused by 18 heat treatments were analyzed via optical microscopy and image analysis, revealing the full range of recrystallization from 0 to 100%. The formation of carbides during the longer duration and higher-temperature heat treatments was monitored via transmission electron microscope evaluation. The experimental results informed a model which includes recovery, recrystallization, and grainmore » growth to predict microstructure and hardness. After initialization of the model, it was able to predict hardness with a R 2 value of 0.95 and recrystallization with an R 2 value of 0.99. As a result, the model was then utilized in the design and testing of a heat treatment to soften the tubing.« less

Composite Magnetite and Protein Containing CaCO3 Crystals. External Manipulation and Vaterite → Calcite Recrystallization-Mediated Release Performance.

PubMed

Sergeeva, Alena; Sergeev, Roman; Lengert, Ekaterina; Zakharevich, Andrey; Parakhonskiy, Bogdan; Gorin, Dmitry; Sergeev, Sergey; Volodkin, Dmitry

2015-09-30

Biocompatibility and high loading capacity of mesoporous CaCO3 vaterite crystals give an option to utilize the polycrystals for a wide range of (bio)applications. Formation and transformations of calcium carbonate polymorphs have been studied for decades, aimed at both basic and applied research interests. Here, composite multilayer-coated calcium carbonate polycrystals containing Fe3O4 magnetite nanoparticles and model protein lysozyme are fabricated. The structure of the composite polycrystals and vaterite → calcite recrystallization kinetics are studied. The recrystallization results in release of both loaded protein and Fe3O4 nanoparticles (magnetic manipulation is thus lost). Fe3O4 nanoparticles enhance the recrystallization that can be induced by reduction of the local pH with citric acid and reduction of the polycrystal crystallinity. Oppositely, the layer-by-layer assembled poly(allylamine hydrochloride)/poly(sodium styrenesulfonate) polyelectrolyte coating significantly inhibits the vaterite → calcite recrystallization (from hours to days) most likely due to suppression of the ion exchange giving an option to easily tune the release kinetics for a wide time scale, for example, for prolonged release. Moreover, the recrystallization of the coated crystals results in formulation of multilayer capsules keeping the feature of external manipulation. This study can help to design multifunctional microstructures with tailor-made characteristics for loading and controlled release as well as for external manipulation.

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

Chuang, Chihpin; Singh, Dileep; Kenesei, Peter

The size and morphology of the graphite particles play a crucial role in determining various mechanical and thermal properties of cast iron. In the present study, we utilized high-energy synchrotron X-ray tomography to perform quantitative 3D-characterization of the distribution of graphite particles in high-strength compacted graphite iron (CGI). The size, shape, and spatial connectivity of graphite were examined. The analysis reveals that the compacted graphite can grow with a coral-tree-like morphology and span several hundred microns in the iron matrix.

AC induction field heating of graphite foam

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

Klett, James W.; Rios, Orlando; Kisner, Roger

A magneto-energy apparatus includes an electromagnetic field source for generating a time-varying electromagnetic field. A graphite foam conductor is disposed within the electromagnetic field. The graphite foam when exposed to the time-varying electromagnetic field conducts an induced electric current, the electric current heating the graphite foam. An energy conversion device utilizes heat energy from the heated graphite foam to perform a heat energy consuming function. A device for heating a fluid and a method of converting energy are also disclosed.

Graphite fiber reinforced structure for supporting machine tools

DOEpatents

Knight, Jr., Charles E.; Kovach, Louis; Hurst, John S.

1978-01-01

Machine tools utilized in precision machine operations require tool support structures which exhibit minimal deflection, thermal expansion and vibration characteristics. The tool support structure of the present invention is a graphite fiber reinforced composite in which layers of the graphite fibers or yarn are disposed in a 0/90.degree. pattern and bonded together with an epoxy resin. The finished composite possesses a low coefficient of thermal expansion and a substantially greater elastic modulus, stiffness-to-weight ratio, and damping factor than a conventional steel tool support utilized in similar machining operations.

Rheology, microstructure and crystallographic preferred orientation of matrix containing a dispersed second phase: Insight from experimentally deformed ice

NASA Astrophysics Data System (ADS)

Cyprych, Daria; Piazolo, Sandra; Wilson, Christopher J. L.; Luzin, Vladimir; Prior, David J.

2016-09-01

We utilize in situ neutron diffraction to continuously track the average grain size and crystal preferred orientation (CPO) development in ice, during uniaxial compression of two-phase and pure ice samples. Two-phase samples are composed of ice matrix and 20 vol.% of second phases of two types: (1) rheologically soft, platy graphite, and (2) rigid, rhomb-shaped calcite. The samples were tested at 10 °C below the ice melting point, ambient pressures, and two strain rates (1 ×10-5 and 2.5 ×10-6 s-1), to 10 and 20% strain. The final CPO in the ice matrix, where second phases are present, is significantly weaker, and ice grain size is smaller than in an ice-only sample. The microstructural and rheological data point to dislocation creep as the dominant deformation regime. The evolution and final strength of the CPO in ice depend on the efficiency of the recrystallization processes, namely grain boundary migration and nucleation. These processes are markedly influenced by the strength, shape, and grain size of the second phase. In addition, CPO development in ice is further accentuated by strain partitioning into the soft second phase, and the transfer of stress onto the rigid second phase.

User-independent EBSD parameters to study the progress of recovery and recrystallization in Cu-Zn alloy during in situ heating.

PubMed

Sharma, N K; Shekhar, S

2016-12-01

Microstructural evolution of cold-rolled Cu-5%Zn alloy during in situ heating inside field-emission scanning electron microscope was utilized to obtain user-independent parameters in order to trace the progress of static recovery and recrystallization. Electron back-scattered diffraction (EBSD)-based orientation imaging microscopy was used to obtain micrographs at various stages of in situ heating. It is shown that unlike the pre-existing methods, additional EBSD-based parameter can be used to trace the progress of recovery and recrystallization, which is not dependent on user input and hence less prone to error. True strain of 0.3 was imposed during cold rolling of alloy sample. Rolled sample was subjected to in situ heating from room temperature to 500°C (∼0.58 Tm) with soaking time of 10 min, at each of the intermediate temperatures viz. 100, 200, 300, 400 and 450°C. After reaching 500°C, the sample was kept at this temperature for a maximum duration of around 15 h. The sample showed clear signs of recovery for temperature up to 450°C, and at 500°C, recrystallization started to take place. Recrystallization kinetics was moderate, and full recrystallization was achieved in approximately 120 min. We found that EBSD parameter, namely, band contrast intensity can be used as an extra handle to map out the progress of recrystallization occurring in the sample. By contrast, mean angular deviation can be used to understand the evolution of recovery in samples. The parameters mentioned in the current study, unlike other pre-existing methods, can also be used for mapping local microstructural transformations due to recovery and recrystallization. We discuss the benefits and limitations in using these additional handles in understanding the changes taking place in the material during in situ heating. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Development, manufacturing, and test of graphite-epoxy composite spoilers for flight service on 737 transport aircraft

NASA Technical Reports Server (NTRS)

Stoecklin, R. L.

1976-01-01

A total of 114 spoiler units were fabricated in a production shop environment, utilizing three graphite epoxy material systems. Production planning paper was generated for each spoiler unit to completely document each production step of each spoiler unit. The graphite epoxy skins were laid up on production tooling using both mechanical and hand layup techniques. Inspection techniques utilized MRB type assessment in the abscence of quality requirements. Each completed spoiler was subjected to ultrasonic inspection utilizing a multicolor recording system that documented each inspection result. In addition, one static test spoiler was sectioned after the test to examine the adhesive filleting to the honeycomb core. Visual examination of the cured adhesives showed excellent results.

SUMMARY TECHNICAL REPORT FOR THE PERIOD JANUARY 1, 1961-MARCH 31, 1961

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

Burgett, R. ed

1961-05-01

Uranium and TBP Recovery from Waste Solvent. Laboratory and pilot-scale tests were carried out which demonstrated (1) that uranium in waste solvent can be removed by slurrying the solvent with activated charcoal, filtering the slurry, and washing the slurry with water and 3% Na/sub 2/CO/sub 3/ and (2) that TBP can be recovered from the waste solvent by splitting the solvent with HCl and distilling the TBP-rich phase. Improvement of Green Salt Quality. Denitration of ammonium uranyl trinitrate yielded a light, finely divided form of gamma -UO/ sub 3/ with a surface area higher than that of conventional batch potmore » powder; however, its reactivity in reduction and hydrofluorination tests was only moderately higher in comparison. Oxidation-reduction cycles were found to increase the reactivity of UO/sub 2/ toward hydrofluorination. The properties of various UO/sub 2/ samples were determined and correlated with the preparative methods used. Dehydration of Winlo Green Salt. About 27 tons of Winlo green salt was successfully dehydrated to a water content of -0.04% in a hydrofluorination reactor bank in the Green Salt Plant. Recovery of Uranium from MgF/sub 2/ Slag. A process for continuously digesting MgF/sub 2/ slag for uranium recovery was successfully tested on a plant scale. In this process, a water slurry of slag is transferred at a fixed rate and reacted with HCl, and the controlled feed rate reduces the hydrogen concentration. Graphite Liner for Bomb Reduction of Green Salt. An evaluation was made on machined graphite as a replacement for jolt-packed MgF/sub 2/ presently used to line reduction vessels for uranium metal production. Best results were obtained with a onepiece graphite liner fitted inside a steel vessel with an annulus of MgF/sub 2/ between liner and pot. Effects of Feed Material on Ingot Chemical Purity and Yields. The effects of various types of uranium feed stock on the chemical purity and yield of ingots were studied. The following results were obtained: (1) The H content was higher in ingots cast from melts contairing more derby material, (2) the O, N, and C contents of samples from ingot tops were signiicantly lower than those from ingot bottoms, (3) the crude ingot yields were lowest for pigots, briquettes, and heat-shocked grade III derbies, (4) pigots were deleterious to ingot chemical purity, (5) degreased drip crops and dingot extrnsion scrap were deleterious to core-to-good-core yield. Alpha Annealing of Uranium. The effect of a high alpha temperature anneal on the structure and growin index of beta heat treated uranium was evaluated. It was found that longer alpha annealing times gave greater recrystallization and that higher temperatures gave more rapid recrystallization. Delays of up to 6 months between beta heat treatment and alpha anneal did not affect either the recrystallization or the growth index. Billet Drilling. A LeBlond-Carlstedt Rapid Borer was tested as a urarium billet drilling machine and found to give satisfactory results, although some tool breakage occurred. (D.L.C.)« less

Infrared signal generation from AC induction field heating of graphite foam

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

Klett, James W.; Rios, Orlando

A magneto-energy apparatus includes an electromagnetic field source for generating a time-varying electromagnetic field. A graphite foam conductor is disposed within the electromagnetic field. The graphite foam when exposed to the time-varying electromagnetic field conducts an induced electric current, the electric current heating the graphite foam to produce light. An energy conversion device utilizes light energy from the heated graphite foam to perform a light energy consuming function. A device for producing light and a method of converting energy are also disclosed.

Physical stability and recrystallization kinetics of amorphous ibipinabant drug product by fourier transform raman spectroscopy.

PubMed

Sinclair, Wayne; Leane, Michael; Clarke, Graham; Dennis, Andrew; Tobyn, Mike; Timmins, Peter

2011-11-01

The solid-state physical stability and recrystallization kinetics during storage stability are described for an amorphous solid dispersed drug substance, ibipinabant, at a low concentration (1.0%, w/w) in a solid oral dosage form (tablet). The recrystallization behavior of the amorphous ibipinabant-polyvinylpyrrolidone solid dispersion in the tablet product was characterized by Fourier transform (FT) Raman spectroscopy. A partial least-square analysis used for multivariate calibration based on Raman spectra was developed and validated to detect less than 5% (w/w) of the crystalline form (equivalent to less than 0.05% of the total mass of the tablet). The method provided reliable and highly accurate predictive crystallinity assessments after exposure to a variety of stability storage conditions. It was determined that exposure to moisture had a significant impact on the crystallinity of amorphous ibipinabant. The information provided by the method has potential utility for predictive physical stability assessments. Dissolution testing demonstrated that the predicted crystallinity had a direct correlation with this physical property of the drug product. Recrystallization kinetics was measured using FT Raman spectroscopy for the solid dispersion from the tablet product stored at controlled temperature and relative humidity. The measurements were evaluated by application of the Johnson-Mehl-Avrami (JMA) kinetic model to determine recrystallization rate constants and Avrami exponent (n = 2). The analysis showed that the JMA equation could describe the process very well, and indicated that the recrystallization kinetics observed was a two-step process with an induction period (nucleation) followed by rod-like crystal growth. Copyright © 2011 Wiley-Liss, Inc.

Fire test method for graphite fiber reinforced plastics

NASA Technical Reports Server (NTRS)

Bowles, K. J.

1980-01-01

A potential problem in the use of graphite fiber reinforced resin matrix composites is the dispersal of graphite fibers during accidential fires. Airborne, electrically conductive fibers originating from the burning composites could enter and cause shorting in electrical equipment located in surrounding areas. A test method for assessing the burning characteristics of graphite fiber reinforced composites and the effectiveness of the composites in retaining the graphite fibers has been developed. The method utilizes a modified rate of heat release apparatus. The equipment and the testing procedure are described. The application of the test method to the assessment of composite materials is illustrated for two resin matrix/graphite composite systems.

New high-temperature flame-resistant resin matrix for RP/C

NASA Technical Reports Server (NTRS)

Kourtides, D. A.

1981-01-01

The processing parameters of graphite composites utilizing graphite fabric and epoxy or other advanced thermoset and thermoplastic resins as matrices are discussed. The evaluated properties include anaerobic char yield, limiting oxygen index, smoke evolution, moisture absorption, and high-temperature mechanical properties. It is shown that graphite composites having the highest char yield exhibit optimum fire-resistant properties.

GAP Peptide Synthesis via Design of New GAP Protecting Group: An Fmoc/tBu Synthesis of Thymopentin Free from Polymers, Chromatography and Recrystallization

PubMed Central

Seifert, Cole W.; Paniagua, Armando; White, Gabrielle A.; Cai, Lucy

2016-01-01

A novel method for Fmoc/tBu solution-phase peptide synthesis and the development of a new benzyl-type GAP protecting group is reported. This new GAP protecting group is utilized in place of a polymer support, facilitating C→N Fmoc peptide synthesis without chromatography, recrystallization, or polymer supports. The GAP group can be added and removed in high yield, and was used to synthesize over 1 gram of the immunostimulant, thymopentin, in high overall yield (83%) and purity (99%). PMID:28663711

Fire test method for graphite fiber reinforced plastics

NASA Technical Reports Server (NTRS)

Bowles, K. J.

1980-01-01

A potential problem in the use of graphite fiber reinforced resin matrix composites is the dispersal of graphite fibers during accidental fires. Airborne, electrically conductive fibers originating from the burning composites could enter and cause shorting in electrical equipment located in surrounding areas. A test method for assessing the burning characteristics of graphite fiber reinforced composites and the effectiveness of the composites in retaining the graphite fibers has been developed. The method utilizes a modified Ohio State University Rate of Heat Release apparatus. The equipment and the testing procedure are described. The application of the test method to the assessment of composite materials is illustrated for two resin matrix/graphite composite systems.

Carbon Materials Research

DTIC Science & Technology

2006-08-01

carbon would be highly oriented pyrolytic graphite ( HOPG ), which is formed by depositing one atom at a time on a surface utilizing the pyrolysis of a... of the crystallites, and baking to 2800 K produces a polycrystalline graphite part that has high strength and conductivity. To make isotropic...pitch fibers) or flexible (Graphoil®), as well as anisotropic ( HOPG ) or isotropic ( polycrystalline graphite ). In addition, porosity, lubricity

Graphite Recycling from Spent Lithium-Ion Batteries.

PubMed

Rothermel, Sergej; Evertz, Marco; Kasnatscheew, Johannes; Qi, Xin; Grützke, Martin; Winter, Martin; Nowak, Sascha

2016-12-20

The present work reports on challenges in utilization of spent lithium-ion batteries (LIBs)-an increasingly important aspect associated with a significantly rising demand for electric vehicles (EVs). In this context, the feasibility of anode recycling in combination with three different electrolyte extraction concepts is investigated. The first method is based on a thermal treatment of graphite without electrolyte recovery. The second method additionally utilizes a subcritical carbon-dioxide (subcritical CO 2 )-assisted electrolyte extraction prior to thermal treatment. And the final investigated approach uses supercritical carbon dioxide (scCO 2 ) as extractant, subsequently followed by the thermal treatment. It is demonstrated that the best performance of recycled graphite anodes can be achieved when electrolyte extraction is performed using subcritical CO 2 . Comparative studies reveal that, in the best case, the electrochemical performance of recycled graphite exceeds the benchmark consisting of a newly synthesized graphite anode. As essential efforts towards electrolyte extraction and cathode recycling have been made in the past, the electrochemical behavior of recycled graphite, demonstrating the best performance, is investigated in combination with a recycled LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Design, fabrication and test of graphite/epoxy metering truss structure components, phase 3

NASA Technical Reports Server (NTRS)

1974-01-01

The design, materials, tooling, manufacturing processes, quality control, test procedures, and results associated with the fabrication and test of graphite/epoxy metering truss structure components exhibiting a near zero coefficient of thermal expansion are described. Analytical methods were utilized, with the aid of a computer program, to define the most efficient laminate configurations in terms of thermal behavior and structural requirements. This was followed by an extensive material characterization and selection program, conducted for several graphite/graphite/hybrid laminate systems to obtain experimental data in support of the analytical predictions. Mechanical property tests as well as the coefficient of thermal expansion tests were run on each laminate under study, the results of which were used as the selection criteria for the single most promising laminate. Further coefficient of thermal expansion measurement was successfully performed on three subcomponent tubes utilizing the selected laminate.

Molecular dynamics study of the melting of a supported 887-atom Pd decahedron.

PubMed

Schebarchov, D; Hendy, S C; Polak, W

2009-04-08

We employ classical molecular dynamics simulations to investigate the melting behaviour of a decahedral Pd(887) cluster on a single layer of graphite (graphene). The interaction between Pd atoms is modelled with an embedded-atom potential, while the adhesion of Pd atoms to the substrate is approximated with a Lennard-Jones potential. We find that the decahedral structure persists at temperatures close to the melting point, but that just below the melting transition, the cluster accommodates to the substrate by means of complete melting and then recrystallization into an fcc structure. These structural changes are in qualitative agreement with recently proposed models, and they verify the existence of an energy barrier preventing softly deposited clusters from 'wetting' the substrate at temperatures below the melting point.

FennoFlakes: a project for identifying flake graphite ores in the Fennoscandian shield and utilizing graphite in different applications

NASA Astrophysics Data System (ADS)

Palosaari, Jenny; Eklund, O.; Raunio, S.; Lindfors, T.; Latonen, R.-M.; Peltonen, J.; Smått, J.-H.; Kauppila, J.; Lund, S.; Sjöberg-Eerola, P.; Blomqvist, R.; Marmo, J.

2016-04-01

Natural graphite is a strategic mineral, since the European Commission stated (Report on critical raw materials for the EU (2014)) that graphite is one of the 20 most critical materials for the European Union. The EU consumed 13% of all flake graphite in the world but produced only 3%, which stresses the demand of the material. Flake graphite, which is a flaky version of graphite, forms under high metamorphic conditions. Flake graphite is important in different applications like batteries, carbon brushes, heat sinks etc. Graphene (a single layer of graphite) can be produced from graphite and is commonly used in many nanotechnological applications, e.g. in electronics and sensors. The steps to obtain pure graphene from graphite ore include fragmentation, flotation and exfoliation, which can be cumbersome and resulting in damaging the graphene layers. We have started a project named FennoFlakes, which is a co-operation between geologists and chemists to fill the whole value chain from graphite to graphene: 1. Exploration of graphite ores (geological and geophysical methods). 2. Petrological and geochemical analyses on the ores. 3. Development of fragmentation methods for graphite ores. 4. Chemical exfoliation of the enriched flake graphite to separate flake graphite into single and multilayer graphene. 5. Test the quality of the produced material in several high-end applications with totally environmental friendly and disposable material combinations. Preliminary results show that flake graphite in high metamorphic areas has better qualities compared to synthetic graphite produced in laboratories.

Creep-Rupture Behavior and Recrystallization in HR6W and Haynes Alloy 230 Cold-Bent Boiler Tubing for Ultrasupercritical (USC) Steam Boiler Applications

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

Shingledecker, John P

2007-01-01

Creep-rupture experiments were conducted on HR6W and Haynes 230, candidate Ultrasupercritical (USC) alloys, tubes to evaluate the effects of cold-work and recrystallization during high-temperature service. These creep tests were performed by internally pressurizing cold-bent boiler tubes at 775 C for times up to 8000 hours. The bends were fabricated with cold-work levels beyond the current ASME Boiler and Pressure Vessel (ASME B&PV) Code Section I limits for austenitic stainless steels. Destructive metallographic evaluation of the crept tube bends was used to determine the effects of cold-work and the degree of recrystallization. The metallographic analysis combined with an evaluation of themore » creep and rupture data suggest that solid-solution strengthened nickel-based alloys can be fabricated for high-temperature service at USC conditions utilizing levels of cold-work higher than the current allowed levels for austenitic stainless steels.« less

REACTOR HAVING NaK-UO$sub 2$ SLURRY HELICALLY POSITIONED IN A GRAPHITE MODERATOR

DOEpatents

Rodin, M.B.; Carter, J.C.

1962-05-15

A reactor utilizing 20% enriched uranium consists of a central graphite island in cylindrical form, with a spiral coil of tubing fitting against the central island. An external graphite moderator is placed around the central island and coil. A slurry of uranium dioxide dispersed in alkali metal passes through the coil to transfer heat externally to the reactor. There are also conventional controls for regulating the nuclear reaction. (AEC)

Evolution of microstructure, texture and inhibitor along the processing route for grain-oriented electrical steels using strip casting

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

Liu, Hai-Tao, E-mail: liuht@ral.neu.edu.cn; Institute of Research of Iron and Steel, Shasteel, Zhangjiagang 215625, Jiangsu; Yao, Sheng-Jie

2015-08-15

In the present work, a regular grade GO sheet was produced successively by strip casting, hot rolling, normalizing annealing, two-stage cold rolling with intermediate annealing, primary recrystallization annealing, secondary recrystallization annealing and purification. The aim of this paper was to characterize the evolution of microstructure, texture and inhibitor along the new processing route by comprehensive utilization of optical microscopy, X-ray diffraction and transmission electron microscopy. It was found that a fine microstructure with the ferrite grain size range of 7–12 μm could be obtained in the primary recrystallization annealed sheet though a very coarse microstructure was produced in the initialmore » as-cast strip. The main finding was that the “texture memory” effect on Goss texture started on the through-thickness intermediate annealed strip after first cold rolling, which was not similar to the “texture memory” effect on Goss texture starting on the surface layers of the hot rolled strip in the conventional production route. As a result, the origin of Goss nuclei capable of secondary recrystallization lied in the grains already presented in Goss orientation in the intermediate annealed strip after first cold rolling. Another finding was that fine and dispersive inhibitors (mainly AlN) were easy to be produced in the primary recrystallization microstructure due to the initial rapid solidification during strip casting and the subsequent rapid cooling, and the very high temperature reheating usually used before hot rolling in the conventional production route could be avoided. - Highlights: • A regular grade grain-oriented electrical steel was produced. • Evolution of microstructure, texture and inhibitor was characterized. • Origin of Goss nuclei lied in the intermediate annealed strip. • A fine primary recrystallization microstructure could be produced. • Effective inhibitors were easy to be obtained in the new processing route.« less

Nanostructured carbon films with oriented graphitic planes

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

Teo, E. H. T.; Kalish, R.; Kulik, J.

2011-03-21

Nanostructured carbon films with oriented graphitic planes can be deposited by applying energetic carbon bombardment. The present work shows the possibility of structuring graphitic planes perpendicular to the substrate in following two distinct ways: (i) applying sufficiently large carbon energies for deposition at room temperature (E>10 keV), (ii) utilizing much lower energies for deposition at elevated substrate temperatures (T>200 deg. C). High resolution transmission electron microscopy is used to probe the graphitic planes. The alignment achieved at elevated temperatures does not depend on the deposition angle. The data provides insight into the mechanisms leading to the growth of oriented graphiticmore » planes under different conditions.« less

Direct growth of aligned graphitic nanoribbons from a DNA template by chemical vapour deposition.

PubMed

Sokolov, Anatoliy N; Yap, Fung Ling; Liu, Nan; Kim, Kwanpyo; Ci, Lijie; Johnson, Olasupo B; Wang, Huiliang; Vosgueritchian, Michael; Koh, Ai Leen; Chen, Jihua; Park, Jinseong; Bao, Zhenan

2013-01-01

Graphene, laterally confined within narrow ribbons, exhibits a bandgap and is envisioned as a next-generation material for high-performance electronics. To take advantage of this phenomenon, there is a critical need to develop methodologies that result in graphene ribbons <10 nm in width. Here we report the use of metal salts infused within stretched DNA as catalysts to grow nanoscopic graphitic nanoribbons. The nanoribbons are termed graphitic as they have been determined to consist of regions of sp(2) and sp(3) character. The nanoscopic graphitic nanoribbons are micrometres in length, <10 nm in width, and take on the shape of the DNA template. The DNA strand is converted to a graphitic nanoribbon by utilizing chemical vapour deposition conditions. Depending on the growth conditions, metallic or semiconducting graphitic nanoribbons are formed. Improvements in the growth method have potential to lead to bottom-up synthesis of pristine single-layer graphene nanoribbons.

Ice Recrystallization Inhibiting Polymers Enable Glycerol-Free Cryopreservation of Micro-organisms.

PubMed

Hasan, Muhammad; Fayter, Alice E R; Gibson, Matthew I

2018-06-22

All modern molecular biology and microbiology is underpinned not only by the tools to handle and manipulate microorganisms, but also those to store, bank and transport them. Glycerol is the current gold-standard cryoprotectant but it is intrinsically toxic to most micro-organisms: only a fraction of cells survive freezing and the presence of glycerol can impact down-stream applications and assays. Extremophile organisms survive repeated freeze/thaw cycles by producing antifreeze proteins which are potent ice recrystallization inhibitors. Here we introduce a new concept for the storage/transport of micro-organisms by using ice recrystallization inhibiting poly(vinyl alcohol) in tandem with poly(ethylene glycol). This cryopreserving formulation is shown to result in a 4-fold increase in E. coli yield post-thaw, compared to glycerol, utilizing lower concentrations, with successful cryopreservation at just 1.1 weight percent of additive. The mechanism of protection is demonstrated to be linked to inhibiting ice recrystallization (by comparison to a recombinant antifreeze protein) but also to the significantly lower toxicity of the polymers compared to glycerol. Optimized formulations are presented and shown to be broadly applicable to the cryopreservation of a panel of Gram negative, Gram positive and Mycobacteria strains. This represents a step-change in how micro-organisms will be stored by the design of new macromolecular ice growth inhibitors; it should enable a transition from traditional solvent-based to macromolecular microbiology storage methods.

GRAPHITE PRODUCTION UTILIZING URANYL NITRATE HEXAHYDRATE CATALYST

DOEpatents

Sheinberg, H.; Armstrong, J.R.; Schell, D.H.

1964-03-10

ABS>The graphitizing of a mixture composed of furfuryl alcohol binder and uranyl nitrate hexahydrate hardener and the subsequent curing, baking, and graphitizing with pressure being initially applied prior to curing are described. The pressure step may be carried out by extrusion, methyl cellulose being added to the mixture before the completion of extrusion. Uranium oxide may be added to the graphitizable mixture prior to the heating and pressure steps. The graphitizable mixture may consist of discrete layers of different compositions. (AEC)

Geological constraints on detecting the earliest life on Earth: a perspective from the Early Archaean (older than 3.7 Gyr) of southwest Greenland

PubMed Central

Fedo, Christopher M; Whitehouse, Martin J; Kamber, Balz S

2006-01-01

At greater than 3.7 Gyr, Earth's oldest known supracrustal rocks, comprised dominantly of mafic igneous with less common sedimentary units including banded iron formation (BIF), are exposed in southwest Greenland. Regionally, they were intruded by younger tonalites, and then both were intensely dynamothermally metamorphosed to granulite facies (the highest pressures and temperatures generally encountered in the Earth's crust during metamorphism) in the Archaean and subsequently at lower grades until about 1500 Myr ago. Claims for the first preserved life on Earth have been based on the occurrence of greater than 3.8 Gyr isotopically light C occurring as graphite inclusions within apatite crystals from a 5 m thick purported BIF on the island of Akilia. Detailed geologic mapping and observations there indicate that the banding, first claimed to be depositional, is clearly deformational in origin. Furthermore, the mineralogy of the supposed BIF, being dominated by pyroxene, amphibole and quartz, is unlike well-known BIF from the Isua Greenstone Belt (IGB), but resembles enclosing mafic and ultramafic igneous rocks modified by metasomatism and repeated metamorphic recrystallization. This scenario parsimoniously links the geology, whole-rock geochemistry, 2.7 Gyr single crystal zircon ages in the unit, an approximately 1500 Myr age for apatites that lack any graphite, non-MIF sulphur isotopes in the unit and an inconclusive Fe isotope signature. Although both putative body fossils and carbon-12 enriched isotopes in graphite described at Isua are better explained by abiotic processes, more fruitful targets for examining the earliest stages in the emergence of life remain within greater than 3.7 Gyr IGB, which preserves BIF and other rocks that unambiguously formed at Earth's surface. PMID:16754603

Tip-induced local strain on Mo S 2 / graphite detected by inelastic electron tunneling spectroscopy

DOE PAGES

Ko, Wonhee; Hus, Saban M.; Li, Xufan; ...

2018-03-02

We report the detection of tip-induced local strain applied to the monolayer MoS 2 grown on a graphite substrate by scanning tunneling microscope. Monolayer MoS 2 behaves as both mechanical and tunneling barriers that prevent the tip from contacting the graphite while maintaining the tunneling current. Inelastic tunneling electron spectroscopy (IETS) is utilized to probe the phonon modes in graphite. As the tip pushes the sample, IETS reveals a continuous phonon softening in graphite, corroborated by a downward shift of the phonon energy as calculated by density-functional theory. Finally, our results demonstrate a way to apply local mechanical strain andmore » simultaneously detect the induced change in phonon modes by unitizing IETS with two-dimensional materials as a tunneling barrier.« less

Tip-induced local strain on Mo S 2 / graphite detected by inelastic electron tunneling spectroscopy

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

Ko, Wonhee; Hus, Saban M.; Li, Xufan

We report the detection of tip-induced local strain applied to the monolayer MoS 2 grown on a graphite substrate by scanning tunneling microscope. Monolayer MoS 2 behaves as both mechanical and tunneling barriers that prevent the tip from contacting the graphite while maintaining the tunneling current. Inelastic tunneling electron spectroscopy (IETS) is utilized to probe the phonon modes in graphite. As the tip pushes the sample, IETS reveals a continuous phonon softening in graphite, corroborated by a downward shift of the phonon energy as calculated by density-functional theory. Finally, our results demonstrate a way to apply local mechanical strain andmore » simultaneously detect the induced change in phonon modes by unitizing IETS with two-dimensional materials as a tunneling barrier.« less

Tip-induced local strain on Mo S2/graphite detected by inelastic electron tunneling spectroscopy

NASA Astrophysics Data System (ADS)

Ko, Wonhee; Hus, Saban M.; Li, Xufan; Berlijn, Tom; Nguyen, Giang D.; Xiao, Kai; Li, An-Ping

2018-03-01

We report the detection of tip-induced local strain applied to the monolayer Mo S2 grown on a graphite substrate by scanning tunneling microscope. Monolayer Mo S2 behaves as both mechanical and tunneling barriers that prevent the tip from contacting the graphite while maintaining the tunneling current. Inelastic tunneling electron spectroscopy (IETS) is utilized to probe the phonon modes in graphite. As the tip pushes the sample, IETS reveals a continuous phonon softening in graphite, corroborated by a downward shift of the phonon energy as calculated by density-functional theory. Our results demonstrate a way to apply local mechanical strain and simultaneously detect the induced change in phonon modes by unitizing IETS with two-dimensional materials as a tunneling barrier.

Novel 1.5 GPa-strength with 50%-ductility by transformation-induced plasticity of non-recrystallized austenite in duplex steels.

PubMed

Sohn, Seok Su; Song, Hyejin; Jo, Min Chul; Song, Taejin; Kim, Hyoung Seop; Lee, Sunghak

2017-04-28

Needs for steel designs of ultra-high strength and excellent ductility have been an important issue in worldwide automotive industries to achieve energy conservation, improvement of safety, and crashworthiness qualities. Because of various drawbacks in existing 1.5-GPa-grade steels, new development of formable cold-rolled ultra-high-strength steels is essentially needed. Here we show a plausible method to achieve ultra-high strengths of 1.0~1.5 GPa together with excellent ductility above 50% by actively utilizing non-recrystallization region and TRansformation-Induced Plasticity (TRIP) mechanism in a cold-rolled and annealed Fe-Mn-Al-C-based steel. We adopt a duplex microstructure composed of austenite and ultra-fine ferrite in order to overcome low-yield-strength characteristics of austenite. Persistent elongation up to 50% as well as ultra-high yield strength over 1.4 GPa are attributed to well-balanced mechanical stability of non-crystallized austenite with critical strain for TRIP. Our results demonstrate how the non-recrystallized austenite can be a metamorphosis in 1.5-GPa-grade steel sheet design.

Modeling the Flow Behavior, Recrystallization, and Crystallographic Texture in Hot-Deformed Fe-30 Wt Pct Ni Austenite

NASA Astrophysics Data System (ADS)

Abbod, M. F.; Sellars, C. M.; Cizek, P.; Linkens, D. A.; Mahfouf, M.

2007-10-01

The present work describes a hybrid modeling approach developed for predicting the flow behavior, recrystallization characteristics, and crystallographic texture evolution in a Fe-30 wt pct Ni austenitic model alloy subjected to hot plane strain compression. A series of compression tests were performed at temperatures between 850 °C and 1050 °C and strain rates between 0.1 and 10 s-1. The evolution of grain structure, crystallographic texture, and dislocation substructure was characterized in detail for a deformation temperature of 950 °C and strain rates of 0.1 and 10 s-1, using electron backscatter diffraction and transmission electron microscopy. The hybrid modeling method utilizes a combination of empirical, physically-based, and neuro-fuzzy models. The flow stress is described as a function of the applied variables of strain rate and temperature using an empirical model. The recrystallization behavior is predicted from the measured microstructural state variables of internal dislocation density, subgrain size, and misorientation between subgrains using a physically-based model. The texture evolution is modeled using artificial neural networks.

Titanium Nitride: An Oxidizable Coating for the High-Temperature Protection of Graphite

NASA Technical Reports Server (NTRS)

Wakelyn, N. T.

1961-01-01

A titanium nitride coating for graphite, prepared by deposition process, protected test specimens for 60 seconds the vapors in a supersonic ceramic-heated air jet with a stagnation temperature of approximately 2,250 K. For the same test conditions, coated specimens showed no damage to the graphite body for the 60-second test, whereas uncoated specimens were very severely damaged after 20 seconds and were destroyed toward the end of the test. A discussion of the coating of these graphite specimens and of some of the conditions necessary for the utilization of oxidizable substances as oxidation-protective coatings for bodies facing high convective heat transfer in the atmosphere is presented.

Performance Properties of Graphite Reinforced Composites with Advanced Resin Matrices

NASA Technical Reports Server (NTRS)

Kourtides, Demetrius A.

1980-01-01

This article looks at the effect of different resin matrices on thermal and mechanical properties of graphite composites, and relates the thermal and flammability properties to the anaerobic char yield of the resins. The processing parameters of graphite composites utilizing graphite fabric and epoxy or other advanced resins as matrices are presented. Thermoset resin matrices studied were: aminecured polyfunctional glycidyl aminetype epoxy (baseline), phenolicnovolac resin based on condensation of dihydroxymethyl-xylene and phenol cured with hexamine, two types of polydismaleimide resins, phenolic resin, and benzyl resin. The thermoplastic matrices studied were polyethersulfone and polyphenylenesulfone. Properties evaluated in the study included anaerobic char yield, limiting oxygen index, smoke evolution, moisture absorption, and mechanical properties at elevated temperatures including tensile, compressive, and short-beam shear strengths. Generally, it was determined that graphite composites with the highest char yield exhibited optimum fire-resistant properties.

Graphite fiber reinforced thermoplastic resins

NASA Technical Reports Server (NTRS)

Novak, R. C.

1975-01-01

Mechanical properties of neat resin samples and graphite fiber reinforced samples of thermoplastic resins were characterized with particular emphasis directed to the effects of environmental exposure (humidity, temperature and ultraviolet radiation). Tensile, flexural, interlaminar shear, creep and impact strengths were measured for polysulfone, polyarylsulfone and a state-of-the-art epoxy resin samples. In general, the thermoplastic resins exhibited environmental degradation resistance equal to or superior to the reference epoxy resin. Demonstration of the utility and quality of a graphite/thermoplastic resin system was accomplished by successfully thermoforming a simulated compressor blade and a fan exit guide vane.

Development of graphite/copper composites utilizing engineered interfaces. M.S. Thesis Final Report

NASA Technical Reports Server (NTRS)

Devincent, Sandra M.

1991-01-01

In situ measurements of graphite/copper alloy contact angles were made using the sessile drop method. The interfacial energy values obtained from these measurements were then applied to a model for the fiber matrix interfacial debonding phenomenon found in graphite/copper composites. The formation obtained from the sessile drop tests led to the development of a copper alloy that suitably wets graphite. Characterization of graphite/copper alloy interfaces subjected to elevated temperatures was conducted using Scanning Electron Microscopy, Energy Dispersive Spectroscopy, Auger Electron Spectroscopy, and X Ray Diffraction analyses. These analyses indicated that during sessile drop tests conducted at 1130 C for 1 hour, copper alloys containing greater than 0.98 at pct chromium form continuous reaction layers of approx. 10 microns in thickness. The reaction layers are adherent to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 deg or less. X ray diffraction results indicate that the reaction layer is Cr3C2.

Critical Heat Flux in Pool Boiling on Metal-Graphite Composite Surfaces

NASA Technical Reports Server (NTRS)

Zhang, Nengli; Yang, Wen-Jei; Chao, David F.; Chao, David F. (Technical Monitor)

2000-01-01

A study is conducted on high heat-flux pool boiling of pentane on micro-configured composite surfaces. The boiling surfaces are copper-graphite (Cu-Gr) and aluminum-graphite (Al-Gr) composites with a fiber volume concentration of 50%. The micro-graphite fibers embedded in the matrix contribute to a substantial enhancement in boiling heat-transfer performance. Correlation equations are obtained for both the isolated and coalesced bubble regimes, utilizing a mathematical model based on a metal-graphite, two-tier configuration with the aid of experimental data. A new model to predict the critical heat flux (CHF) on the composites is proposed to explain the fundamental aspects of the boiling phenomena. Three different factors affecting the CHF are considered in the model. Two of them are expected to become the main agents driving vapor volume detachment under microgravity conditions, using the metal-graphite composite surfaces as the heating surface and using liquids with an unusual Marangoni effect as the working fluid.

Roll-to-Roll Laser-Printed Graphene-Graphitic Carbon Electrodes for High-Performance Supercapacitors.

PubMed

Kang, Sangmin; Lim, Kyungmi; Park, Hyeokjun; Park, Jong Bo; Park, Seong Chae; Cho, Sung-Pyo; Kang, Kisuk; Hong, Byung Hee

2018-01-10

Carbon electrodes including graphene and thin graphite films have been utilized for various energy and sensor applications, where the patterning of electrodes is essentially included. Laser scribing in a DVD writer and inkjet printing were used to pattern the graphene-like materials, but the size and speed of fabrication has been limited for practical applications. In this work, we devise a simple strategy to use conventional laser-printer toner materials as precursors for graphitic carbon electrodes. The toner was laser-printed on metal foils, followed by thermal annealing in hydrogen environment, finally resulting in the patterned thin graphitic carbon or graphene electrodes for supercapacitors. The electrochemical cells made of the graphene-graphitic carbon electrodes show remarkably higher energy and power performance compared to conventional supercapacitors. Furthermore, considering the simplicity and scalability of roll-to-roll (R2R) electrode patterning processes, the proposed method would enable cheaper and larger-scale synthesis and patterning of graphene-graphitic carbon electrodes for various energy applications in the future.

Microstructure effects on the recrystallization of low-symmetry alpha-uranium

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

McCabe, Rodney James; Richards, Andrew Walter; Coughlin, Daniel Robert

2015-10-01

We employ electron backscatter diffraction (EBSD) to investigate microstructural evolution of uranium during recrystallization. To understand the relationship between microstructure and recrystallization, we use measures of intra-granular misorientation within grains and near grain boundaries in both deformed (non-recrystallized) uranium and recrystallizing uranium. The data show that the level of intra-granular misorientation depends on crystallographic orientation. However, contrary to expectation, this relationship does not significantly affect the recrystallization texture. Rather, the analysis suggests that recrystallization nucleation occurs along high angle grain boundaries in the deformed microstructure. Specifically, we show that the nucleation of recrystallized grains correlates well with the spatially heterogeneousmore » distribution of high angle boundaries. Due to the inhomogeneous distribution of high angle boundaries, the recrystallized microstructure after long times exhibits clustered distributions of small and large grains. Twin boundaries do not appear to act as recrystallization nucleation sites.« less

A Rate-Theory-Phase-Field Model of Irradiation-Induced Recrystallization in UMo Nuclear Fuels

NASA Astrophysics Data System (ADS)

Hu, Shenyang; Joshi, Vineet; Lavender, Curt A.

2017-12-01

In this work, we developed a recrystallization model to study the effect of microstructures and radiation conditions on recrystallization kinetics in UMo fuels. The model integrates the rate theory of intragranular gas bubble and interstitial loop evolutions and a phase-field model of recrystallization zone evolution. A first passage method is employed to describe one-dimensional diffusion of interstitials with a diffusivity value several orders of magnitude larger than that of fission gas xenons. With the model, the effect of grain sizes on recrystallization kinetics is simulated. The results show that (1) recrystallization in large grains starts earlier than that in small grains, (2) the recrystallization kinetics (recrystallization volume fraction) decrease as the grain size increases, (3) the predicted recrystallization kinetics are consistent with the experimental results, and (4) the recrystallization kinetics can be described by the modified Avrami equation, but the parameters of the Avrami equation strongly depend on the grain size.

Size Controllable, Transparent, and Flexible 2D Silver Meshes Using Recrystallized Ice Crystals as Templates.

PubMed

Wu, Shuwang; Li, Linhai; Xue, Han; Liu, Kai; Fan, Qingrui; Bai, Guoying; Wang, Jianjun

2017-10-24

Ice templates have been widely utilized for the preparation of porous materials due to the obvious advantages, such as environmentally benign and applicable to a wide range of materials. However, it remains a challenge to have controlled pore size as well as dimension of the prepared porous materials with the conventional ice template, since it often employs the kinetically not-stable growing ice crystals as the template. For example, there is no report so far for the preparation of 2D metal meshes with tunable pore size based on the ice template, although facile and eco-friendly prepared metal meshes are highly desirable for wearable electronics. Here, we report the preparation of 2D silver meshes with tunable mesh size employing recrystallized ice crystals as templates. Ice recrystallization is a kinetically stable process; therefore, the grain size of recrystallized ice crystals can be easily tuned, e.g., by adding different salts and changing the annealing temperature. Consequently, the size and line width of silver meshes obtained after freeze-drying can be easily adjusted, which in turn varied the conductivity of the obtained 2D silver film. Moreover, the silver meshes are transparent and display stable conductivity after the repeated stretching and bending. It can be envisioned that this approach for the preparation of 2D conducting films is of practical importance for wearable electronics. Moreover, this study provides a generic approach for the fabrication of 2D meshes with a controllable pore size.

Graphite tail powder and liquid biofertilizer as trace elements source for ground nut

NASA Astrophysics Data System (ADS)

Hindersah, Reginawanti; Setiawati, M. Rochimi; Fitriatin, B. Natalie; Suryatama, Pujawati; Asmiran, Priyanka; Panatarani, Camellia; Joni, I. Made

2018-02-01

Utilization of graphite tail waste from the mineral beneficiation processing is very important since it contain significant amount of essential minerals which are necessary for plant growth. These mineral are required in biochemical processes and mainly play an important role as cofactor in enzymatic reaction. The objective of this research is to investigate the performance of graphite tail on supporting plant growth and yield of ground nut (Arachishypogeae L.). A field experiment has been performed to test the performance of mixed graphite tail and reduced organic matter dose. The graphite tail size were reduced to various sieved size, -80 mesh, -100 mesh and -200 mesh. The experiment was setup in randomized block design with 4 treatments and 6 replications for each treatment, while the control plot is received without graphite tail. The results demonstrated that reduced organic matter along with -200 mesh tail has potentially decreased plant height at the end of vegetative growth stage, in contrast for to -80 mesh tail amendment increased individual fresh plant biomass. Statistically, there was no change of plant nodule, individual shoot fresh and dry weight, root nodule, number of pod following any mesh of graphite tail amendment. Reducing organic matter while adding graphite tail of 5% did not change bean weight in all plot. In contrast, reduced organic matter along with 80-mesh graphite tail amendment improved the nut yield per plot. This experiment suggests that graphite tail, mainly -80 mesh graphite tail can be possibly used in legume production.

Graphite for the nuclear industry

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

Burchell, T.D.; Fuller, E.L.; Romanoski, G.R.

Graphite finds applications in both fission and fusion reactors. Fission reactors harness the energy liberated when heavy elements, such as uranium or plutonium, fragment or fission''. Reactors of this type have existed for nearly 50 years. The first nuclear fission reactor, Chicago Pile No. 1, was constructed of graphite under a football stand at Stagg Field, University of Chicago. Fusion energy devices will produce power by utilizing the energy produced when isotopes of the element hydrogen are fused together to form helium, the same reaction that powers our sun. The role of graphite is very different in these two reactormore » systems. Here we summarize the function of the graphite in fission and fusion reactors, detailing the reasons for their selection and discussing some of the challenges associated with their application in nuclear fission and fusion reactors. 10 refs., 15 figs., 1 tab.« less

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

Woltornist, Steven J.; Carrillo, Jan-Michael Y.; Xu, Thomas O.

The unique electrical, thermal, and mechanical properties of graphene make it a perfect candidate for applications in graphene/graphite based polymer composites, yet challenges due to the lack of solubility of pristine graphene/graphite in water and common organic solvents have limited its practical utilization. In this paper, we report a scalable and environmentally friendly technique to form water-in-oil type emulsions stabilized by overlapping pristine graphene sheets, enabling the synthesis of open cell foams containing a continuous graphitic network. Our approach utilizes the insolubility of graphene/graphite in both water and organic solvents and so does not require oxidation, reduction, surfactants, high boilingmore » solvents, chemical functionalization, or the input of large amounts of mechanical energy or heat. At the heart of our technique is the strong attraction of graphene to high-energy oil and water interfaces. This allows for the creation of stable water-in-oil emulsions with controlled droplet size and overlapping graphene sheets playing the role of surfactant by covering the droplet surface and stabilizing the interfaces with a thin graphitic skin. Finally, these emulsions are used as templates for the synthesis of open cell foams with densities below 0.35 g/cm 3 that exhibit remarkable mechanical and electrical properties including compressive moduli up to ~100 MPa, compressive strengths of over 8.3 MPa (1200 psi), and bulk conductivities approaching 7 S/m.« less

Polymer/Pristine graphene based composites: from emulsions to strong, electrically conducting foams

DOE PAGES

Woltornist, Steven J.; Carrillo, Jan-Michael Y.; Xu, Thomas O.; ...

2015-01-21

The unique electrical, thermal, and mechanical properties of graphene make it a perfect candidate for applications in graphene/graphite based polymer composites, yet challenges due to the lack of solubility of pristine graphene/graphite in water and common organic solvents have limited its practical utilization. In this paper, we report a scalable and environmentally friendly technique to form water-in-oil type emulsions stabilized by overlapping pristine graphene sheets, enabling the synthesis of open cell foams containing a continuous graphitic network. Our approach utilizes the insolubility of graphene/graphite in both water and organic solvents and so does not require oxidation, reduction, surfactants, high boilingmore » solvents, chemical functionalization, or the input of large amounts of mechanical energy or heat. At the heart of our technique is the strong attraction of graphene to high-energy oil and water interfaces. This allows for the creation of stable water-in-oil emulsions with controlled droplet size and overlapping graphene sheets playing the role of surfactant by covering the droplet surface and stabilizing the interfaces with a thin graphitic skin. Finally, these emulsions are used as templates for the synthesis of open cell foams with densities below 0.35 g/cm 3 that exhibit remarkable mechanical and electrical properties including compressive moduli up to ~100 MPa, compressive strengths of over 8.3 MPa (1200 psi), and bulk conductivities approaching 7 S/m.« less

Quartz grainsize evolution during dynamic recrystallization across a natural shear zone boundary

NASA Astrophysics Data System (ADS)

Xia, Haoran; Platt, John P.

2018-04-01

Although it is widely accepted that grainsize reduction by dynamic recrystallization can lead to strain localization, the details of the grainsize evolution during dynamic recrystallization remain unclear. We investigated the bulge size and grainsizes of quartz at approximately the initiation and the completion stages of bulging recrystallization across the upper boundary of a 500 m thick mylonite zone above the Vincent fault in the San Gabriel Mountains, southern California. Within uncertainty, the average bulge size of quartz, 4.7 ± 1.5 μm, is the same as the recrystallized grainsize, 4.5 ± 1.5 μm, at the incipient stage of dynamic recrystallization, and also the same within uncertainties as the recrystallized grainsize when dynamic recrystallization is largely complete, 4.7 ± 1.3 μm. These observations indicate that the recrystallized grainsize is controlled by the nucleation process and does not change afterwards. It is also consistent with the experimental finding that the quartz recrystallized grainsize paleopiezometer is independent of temperature.

Susceptibility of Goethite to Fe2+-Catalyzed Recrystallization over Time.

PubMed

Joshi, Prachi; Fantle, Matthew S; Larese-Casanova, Philip; Gorski, Christopher A

2017-10-17

Recent work has shown that iron oxides, such as goethite and hematite, may recrystallize in the presence of aqueous Fe 2+ under anoxic conditions. This process, referred to as Fe 2+ -catalyzed recrystallization, can influence water quality by causing the incorporation/release of environmental contaminants and biological nutrients. Accounting for the effects of Fe 2+ -catalyzed recrystallization on water quality requires knowing the time scale over which recrystallization occurs. Here, we tested the hypothesis that nanoparticulate goethite becomes less susceptible to Fe 2+ -catalyzed recrystallization over time. We set up two batches of reactors in which 55 Fe 2+ tracer was added at two different time points and tracked the 55 Fe partitioning in the aqueous and goethite phases over 60 days. Less 55 Fe uptake occurred between 30 and 60 days than between 0 and 30 days, suggesting goethite recrystallization slowed with time. Fitting the data with a box model indicated that 17% of the goethite recrystallized after 30 days of reaction, and an additional 2% recrystallized between 30 and 60 days. The decreasing susceptibility of goethite to recrystallize as it reacted with aqueous Fe 2+ suggested that recrystallization is likely only an important process over short time scales.

The Recrystallization Behavior of Unalloyed Mg and a Mg-Al Alloy

NASA Astrophysics Data System (ADS)

Murphy, Aeriel D.; Allison, John E.

2018-02-01

The static recrystallization behavior of pure Mg and Mg-4Al was characterized over a range of annealing temperatures. The electron backscatter diffraction grain orientation spread technique was used to quantify the level of recrystallization at various annealing times. Recrystallization kinetics were characterized using the Johnson-Mehl-Avrami-Kolmogorov (JMAK) relationship and it was found that two sequential annealing stages exist. Stage 1 involves heterogeneous nucleation of recrystallization in regions with a high stored energy, including twins and grain boundaries, and can be represented by an Avrami exponent of n 1 ranging from 0.35 to 0.6. During Stage 2, recrystallization occurred predominately in the interior of deformed grains with incomplete recrystallization generally observed even at annealing times in excess of two weeks. The second recrystallization stage exhibited a much lower Avrami exponent, n 2, ranging from 0.02 to 0.2. Increasing the starting grain size in the pure Mg condition led to a significant delay in recrystallization. The addition of Al had a minimal effect on the recrystallization kinetics of Mg.

Determination of grain boundary mobility during recrystallization by statistical evaluation of electron backscatter diffraction measurements

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

Basu, I., E-mail: basu@imm.rwth-aachen.de; Chen, M.; Loeck, M.

One of the key aspects influencing microstructural design pathways in metallic systems is grain boundary motion. The present work introduces a method by means of which direct measurement of grain boundary mobility vs. misorientation dependence is made possible. The technique utilizes datasets acquired by means of serial electron backscatter diffraction (EBSD) measurements. The experimental EBSD measurements are collectively analyzed, whereby datasets were used to obtain grain boundary mobility and grain aspect ratio with respect to grain boundary misorientation. The proposed method is further validated using cellular automata (CA) simulations. Single crystal aluminium was cold rolled and scratched in order tomore » nucleate random orientations. Subsequent annealing at 300 °C resulted in grains growing, in the direction normal to the scratch, into a single deformed orientation. Growth selection was observed, wherein the boundaries with misorientations close to Σ7 CSL orientation relationship (38° 〈111〉) migrated considerably faster. The obtained boundary mobility distribution exhibited a non-monotonic behavior with a maximum corresponding to misorientation of 38° ± 2° about 〈111〉 axes ± 4°, which was 10–100 times higher than the mobility values of random high angle boundaries. Correlation with the grain aspect ratio values indicated a strong growth anisotropy displayed by the fast growing grains. The observations have been discussed in terms of the influence of grain boundary character on grain boundary motion during recrystallization. - Highlights: • Statistical microstructure method to measure grain boundary mobility during recrystallization • Method implementation independent of material or crystal structure • Mobility of the Σ7 boundaries in 5N Al was calculated as 4.7 × 10{sup –8} m{sup 4}/J ⋅ s. • Pronounced growth selection in the recrystallizing nuclei in Al • Boundary mobility values during recrystallization 2–3 orders of magnitude larger vis-à-vis curvature driven motion.« less

Carbon fiber manufacturing via plasma technology

DOEpatents

Paulauskas, Felix L.; Yarborough, Kenneth D.; Meek, Thomas T.

2002-01-01

The disclosed invention introduces a novel method of manufacturing carbon and/or graphite fibers that avoids the high costs associated with conventional carbonization processes. The method of the present invention avoids these costs by utilizing plasma technology in connection with electromagnetic radiation to produce carbon and/or graphite fibers from fully or partially stabilized carbon fiber precursors. In general, the stabilized or partially stabilized carbon fiber precursors are placed under slight tension, in an oxygen-free atmosphere, and carbonized using a plasma and electromagnetic radiation having a power input which is increased as the fibers become more carbonized and progress towards a final carbon or graphite product. In an additional step, the final carbon or graphite product may be surface treated with an oxygen-plasma treatment to enhance adhesion to matrix materials.

Recrystallization of polycrystalline silicon

NASA Technical Reports Server (NTRS)

Lall, C.; Kulkarni, S. B.; Graham, C. D., Jr.; Pope, D. P.

1981-01-01

Optical metallography is used to investigate the recrystallization properties of polycrystalline semiconductor-grade silicon. It is found that polycrystalline silicon recrystallizes at 1380 C in relatively short times, provided that the prior deformation is greater than 30%. For a prior deformation of about 40%, the recrystallization process is essentially complete in about 30 minutes. Silicon recrystallizes at a substantially slower rate than metals at equivalent homologous temperatures. The recrystallized grain size is insensitive to the amount of prestrain for strains in the range of 10-50%.

Controlling the Surface Chemistry of Graphite by Engineered Self-Assembled Peptides

PubMed Central

Khatayevich, Dmitriy; So, Christopher R.; Hayamizu, Yuhei; Gresswell, Carolyn; Sarikaya, Mehmet

2012-01-01

The systematic control over surface chemistry is a long-standing challenge in biomedical and nanotechnological applications for graphitic materials. As a novel approach, we utilize graphite-binding dodecapeptides that self-assemble into dense domains to form monolayer thick long-range ordered films on graphite. Specifically, the peptides are rationally designed through their amino acid sequences to predictably display hydrophilic and hydrophobic characteristics while maintaining their self-assembly capabilities on the solid substrate. The peptides are observed to maintain a high tolerance for sequence modification, allowing the control over surface chemistry via their amino acid sequence. Furthermore, through a single step co-assembly of two different designed peptides, we predictably and precisely tune the wettability of the resulting functionalized graphite surfaces from 44 to 83 degrees. The modular molecular structures and predictable behavior of short peptides demonstrated here give rise to a novel platform for functionalizing graphitic materials that offers numerous advantages, including non-invasive modification of the substrate, bio-compatible processing in an aqueous environment, and simple fusion with other functional biological molecules. PMID:22428620

Study of Graphite/Epoxy Composites for Material Flaw Criticality.

DTIC Science & Technology

1980-11-01

criticality of disbonds with two-dimensional planforms located in laminated graphite/epoxy composites has been examined. Linear elastic fracture...mechanics approach, semi-empirical growth laws and methods of stress analysis based on a modified laminated plate theory have been studied for assessing...growth rates of disbonds in a transverse shear environ- ment. Elastic stability analysis has been utilized for laminates with disbonds subjected to in

High temperature resin matrix composites for aerospace structures

NASA Technical Reports Server (NTRS)

Davis, J. G., Jr.

1980-01-01

Accomplishments and the outlook for graphite-polyimide composite structures are briefly outlined. Laminates, skin-stiffened and honeycomb sandwich panels, chopped fiber moldings, and structural components were fabricated with Celion/LARC-160 and Celion/PMR-15 composite materials. Interlaminar shear and flexure strength data obtained on as-fabricated specimens and specimens that were exposed for 125 hours at 589 K indicate that epoxy sized and polyimide sized Celion graphite fibers exhibit essentially the same behavior in a PMR-15 matrix composite. Analyses and tests of graphite-polyimide compression and shear panels indicate that utilization in moderately loaded applications offers the potential for achieving a 30 to 50 percent reduction in structural mass compared to conventional aluminum panels. Data on effects of moisture, temperature, thermal cycling, and shuttle fluids on mechanical properties indicate that both LARC-160 and PMR-15 are suitable matrix materials for a graphite-polyimide aft body flap. No technical road blocks to building a graphite-polyimide composite aft body flap are identified.

A Fluorinated Ether Electrolyte Enabled High Performance Prelithiated Graphite/Sulfur Batteries

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

Chen, Shuru; Yu, Zhaoxin; Gordin, Mikhail L.

Lithium/sulfur (Li/S) batteries have attracted great attention as a promising energy storage technology, but so far their practical applications are greatly hindered by issues of polysulfide shuttling and unstable lithium/electrolyte interface. To address these issues, a feasible strategy is to construct a rechargeable prelithiated graphite/sulfur batteries. In this study, a fluorinated ether of bis(2,2,2-trifluoroethyl) ether (BTFE) was reported to blend with 1,3-dioxolane (DOL) for making a multifunctional electrolyte of 1.0 M LiTFSI DOL/BTFE (1:1, v/v) to enable high performance prelithiated graphite/S batteries. First, the electrolyte significantly reduces polysulfide solubility to suppress the deleterious polysulfide shuttling and thus improves capacity retentionmore » of sulfur cathodes. Second, thanks to the low viscosity and good wettability, the fluorinated electrolyte dramatically enhances the reaction kinetics and sulfur utilization of high-areal-loading sulfur cathodes. More importantly, this electrolyte forms a stable solid-electrolyte interphase (SEI) layer on graphite surface and thus enables remarkable cyclability of graphite anodes. Lastly, by coupling prelithiated graphite anodes with sulfur cathodes with high areal capacity of ~3 mAh cm -2, we demonstrate prelithiated graphite/sulfur batteries that show high sulfur-specific capacity of ~1000 mAh g -1 and an excellent capacity retention of >65% after 450 cycles at C/10.« less

A Fluorinated Ether Electrolyte Enabled High Performance Prelithiated Graphite/Sulfur Batteries

DOE PAGES

Chen, Shuru; Yu, Zhaoxin; Gordin, Mikhail L.; ...

2017-02-03

Lithium/sulfur (Li/S) batteries have attracted great attention as a promising energy storage technology, but so far their practical applications are greatly hindered by issues of polysulfide shuttling and unstable lithium/electrolyte interface. To address these issues, a feasible strategy is to construct a rechargeable prelithiated graphite/sulfur batteries. In this study, a fluorinated ether of bis(2,2,2-trifluoroethyl) ether (BTFE) was reported to blend with 1,3-dioxolane (DOL) for making a multifunctional electrolyte of 1.0 M LiTFSI DOL/BTFE (1:1, v/v) to enable high performance prelithiated graphite/S batteries. First, the electrolyte significantly reduces polysulfide solubility to suppress the deleterious polysulfide shuttling and thus improves capacity retentionmore » of sulfur cathodes. Second, thanks to the low viscosity and good wettability, the fluorinated electrolyte dramatically enhances the reaction kinetics and sulfur utilization of high-areal-loading sulfur cathodes. More importantly, this electrolyte forms a stable solid-electrolyte interphase (SEI) layer on graphite surface and thus enables remarkable cyclability of graphite anodes. Lastly, by coupling prelithiated graphite anodes with sulfur cathodes with high areal capacity of ~3 mAh cm -2, we demonstrate prelithiated graphite/sulfur batteries that show high sulfur-specific capacity of ~1000 mAh g -1 and an excellent capacity retention of >65% after 450 cycles at C/10.« less

Eddy current inspection of graphite fiber components

NASA Technical Reports Server (NTRS)

Workman, G. L.; Bryson, C. C.

1990-01-01

The recognition of defects in materials properties still presents a number of problems for nondestructive testing in aerospace systems. This project attempts to utilize current capabilities in eddy current instrumentation, artificial intelligence, and robotics in order to provide insight into defining geometrical aspects of flaws in composite materials which are capable of being evaluated using eddy current inspection techniques. The unique capabilities of E-probes and horseshoe probes for inspecting probes for inspecting graphite fiber materials were evaluated and appear to hold great promise once the technology development matures. The initial results are described of modeling eddy current interactions with certain flaws in graphite fiber samples.

Lithium-ion capacitors using carbide-derived carbon as the positive electrode - A comparison of cells with graphite and Li4Ti5O12 as the negative electrode

NASA Astrophysics Data System (ADS)

Rauhala, Taina; Leis, Jaan; Kallio, Tanja; Vuorilehto, Kai

2016-11-01

The use of carbide-derived carbon (CDC) as the positive electrode material for lithium-ion capacitors (LICs) is investigated. CDC based LIC cells are studied utilizing two different negative electrode materials: graphite and lithium titanate Li4Ti5O12 (LTO). The graphite electrodes are prelithiated before assembling the LICs, and LTO containing cells are studied with and without prelithiation. The rate capability and cycle life stability during 1000 cycles are evaluated by galvanostatic cycling at current densities of 0.4-4 mA cm-2. The CDC shows a specific capacitance of 120 F g-1 in the organic lithium-containing electrolyte, and the LICs demonstrate a good stability over 1000 charge-discharge cycles. The choice of the negative electrode is found to have an effect on the utilization of the CDC positive electrode during cycling and on the specific energy of the device. The graphite/CDC cell delivers a maximum specific discharge energy of 90 Wh kg-1 based on the total mass of active material in the cell. Both the prelithiated and non-prelithiated LTO/CDC cells show a specific energy of around 30 Wh kg-1.

Acoustic emission evaluation of reinforced concrete bridge beam with graphite composite laminate

NASA Astrophysics Data System (ADS)

Johnson, Dan E.; Shen, H. Warren; Finlayson, Richard D.

2001-07-01

A test was recently conducted on August 1, 2000 at the FHwA Non-Destructive Evaluation Validation Center, sponsored by The New York State DOT, to evaluate a graphite composite laminate as an effective form of retrofit for reinforced concrete bridge beam. One portion of this testing utilized Acoustic Emission Monitoring for Evaluation of the beam under test. Loading was applied to this beam using a two-point loading scheme at FHwA's facility. This load was applied in several incremental loadings until the failure of the graphite composite laminate took place. Each loading culminated by either visual crack location or large audible emissions from the beam. Between tests external cracks were located visually and highlighted and the graphite epoxy was checked for delamination. Acoustic Emission data was collected to locate cracking areas of the structure during the loading cycles. To collect this Acoustic Emission data, FHwA and NYSDOT utilized a Local Area Monitor, an Acoustic Emission instrument developed in a cooperative effort between FHwA and Physical Acoustics Corporation. Eight Acoustic Emission sensors were attached to the structure, with four on each side, in a symmetrical fashion. As testing progressed and culminated with beam failure, Acoustic Emission data was gathered and correlated against time and test load. This paper will discuss the analysis of this test data.

Graphene nanosheets preparation using magnetic nanoparticle assisted liquid phase exfoliation of graphite: The coupled effect of ultrasound and wedging nanoparticles.

PubMed

Hadi, Alireza; Zahirifar, Jafar; Karimi-Sabet, Javad; Dastbaz, Abolfazl

2018-06-01

This study aims to investigate a novel technique to improve the yield of liquid phase exfoliation of graphite to graphene sheets. The method is based on the utilization of magnetic Fe 3 O 4 nanoparticles as "particle wedge" to facilitate delamination of graphitic layers. Strong shear forces resulted from the collision of Fe 3 O 4 particles with graphite particles, and intense ultrasonic waves lead to enhanced exfoliation of graphite. High quality of graphene sheets along with the ease of Fe 3 O 4 particle separation from graphene solution which arises from the magnetic nature of Fe 3 O 4 nanoparticles are the unique features of this approach. Initial graphite flakes and produced graphene sheets were characterized by various methods including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy, atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Zeta potential analysis. Moreover, the effect of process factors comprising initial graphite concentration, Fe 3 O 4 nanoparticles concentration, sonication time, and sonication power were investigated. Results revealed that graphene preparation yield and the number of layers could be manipulated by the presence of magnetic nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

A STATE-VARIABLE APPROACH FOR PREDICTING THE TIME REQUIRED FOR 50% RECRYSTALLIZATION

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

M. STOUT; ET AL

2000-08-01

It is important to be able to model the recrystallization kinetics in aluminum alloys during hot deformation. The industrial relevant process of hot rolling is an example of where the knowledge of whether or not a material recrystallizes is critical to making a product with the correct properties. Classically, the equations that describe the kinetics of recrystallization predict the time to 50% recrystallization. These equations are largely empirical; they are based on the free energy for recrystallization, a Zener-Holloman parameter, and have several adjustable exponents to fit the equation to engineering data. We have modified this form of classical theorymore » replacing the Zener-Hollomon parameter with a deformation energy increment, a free energy available to drive recrystallization. The advantage of this formulation is that the deformation energy increment is calculated based on the previously determined temperature and strain-rate sensitivity of the constitutive response. We modeled the constitutive response of the AA5182 aluminum using a state variable approach, the value of the state variable is a function of the temperature and strain-rate history of deformation. Thus, the recrystallization kinetics is a function of only the state variable and free energy for recrystallization. There are no adjustable exponents as in classical theory. Using this approach combined with engineering recrystallization data we have been able to predict the kinetics of recrystallization in AA5182 as a function of deformation strain rate and temperature.« less

Development of re-crystallized W-1.1%TiC with enhanced room-temperature ductility and radiation performance

NASA Astrophysics Data System (ADS)

Kurishita, H.; Matsuo, S.; Arakawa, H.; Sakamoto, T.; Kobayashi, S.; Nakai, K.; Takida, T.; Kato, M.; Kawai, M.; Yoshida, N.

2010-03-01

Ultra-fine grained (UFG) W-TiC compacts fabricated by powder metallurgical methods utilizing mechanical alloying (MA) are very promising for use in irradiation environments. However, the assurance of room-temperature ductility and enhancement in surface resistances to low-energy hydrogen irradiation are unsettled issues. As an approach to solution to these, microstructural modification by hot plastic working has been applied to UFG W-TiC processed by MA in a purified Ar or H 2 atmosphere and hot isostatic pressing (HIP). Hot plastically worked compacts have been subjected to 3-point bend tests at room temperature and TEM microstructural examinations. It is found that the microstructural modification allows us to convert UFG W-1.1%TiC to compacts exhibiting a very high fracture strength and appreciable ductility at room temperature. The compacts of W-1.1%TiC/Ar (MA atmosphere: Ar) and W-1.1%TiC/H 2 (MA atmosphere: H 2) exhibit re-crystallized structures with approximately 0.5 and 1.5 μm in grain size, respectively. It is shown that the enhancement of fracture resistance by microstructural modifications is attributed to significant strengthening of weak grain boundaries in the re-crystallized state. As a result the modified compacts exhibit superior surface resistance to low-energy deuteron irradiation.

Inhibition of Ice Growth and Recrystallization by Zirconium Acetate and Zirconium Acetate Hydroxide

PubMed Central

Mizrahy, Ortal; Bar-Dolev, Maya; Guy, Shlomit; Braslavsky, Ido

2013-01-01

The control over ice crystal growth, melting, and shaping is important in a variety of fields, including cell and food preservation and ice templating for the production of composite materials. Control over ice growth remains a challenge in industry, and the demand for new cryoprotectants is high. Naturally occurring cryoprotectants, such as antifreeze proteins (AFPs), present one solution for modulating ice crystal growth; however, the production of AFPs is expensive and inefficient. These obstacles can be overcome by identifying synthetic substitutes with similar AFP properties. Zirconium acetate (ZRA) was recently found to induce the formation of hexagonal cavities in materials prepared by ice templating. Here, we continue this line of study and examine the effects of ZRA and a related compound, zirconium acetate hydroxide (ZRAH), on ice growth, shaping, and recrystallization. We found that the growth rate of ice crystals was significantly reduced in the presence of ZRA and ZRAH, and that solutions containing these compounds display a small degree of thermal hysteresis, depending on the solution pH. The compounds were found to inhibit recrystallization in a manner similar to that observed in the presence of AFPs. The favorable properties of ZRA and ZRAH suggest tremendous potential utility in industrial applications. PMID:23555701

Non-destructive and three-dimensional measurement of local strain development during tensile deformation in an aluminium alloy

NASA Astrophysics Data System (ADS)

Kobayashi, M.; Miura, H.; Toda, H.

2015-08-01

Anisotropy of mechanical responses depending on crystallographic orientation causes inhomogeneous deformation on the mesoscopic scale (grain size scale). Investigation of the local plastic strain development is important for discussing recrystallization mechanisms, because the sites with higher local plastic strain may act as potential nucleation sites for recrystallization. Recently, high-resolution X-ray tomography, which is non-destructive inspection method, has been utilized for observation of the materials structure. In synchrotron radiation X-ray tomography, more than 10,000 microstructural features, like precipitates, dispersions, compounds and hydrogen pores, can be observed in aluminium alloys. We have proposed employing these microstructural features as marker gauges to measure local strains, and then have developed a method to calculate the three-dimensional strain distribution by tracking the microstructural features. In this study, we report the development of local plastic strain as a function of the grain microstructure in an aluminium alloy by means of this three-dimensional strain measurement technique. Strongly heterogeneous strain development was observed during tensile loading to 30%. In other words, some parts of the sample deform little whereas another deforms a lot. However, strain in the whole specimen was keeping harmony. Comparing the microstructure with the strain concentration that is obtained by this method has a potential to reveal potential nucleation sites of recrystallization.

Mesoscale model for fission-induced recrystallization in U-7Mo alloy

DOE PAGES

Liang, Linyun; Mei, Zhi -Gang; Kim, Yeon Soo; ...

2016-08-09

A mesoscale model is developed by integrating the rate theory and phase-field models and is used to study the fission-induced recrystallization in U-7Mo alloy. The rate theory model is used to predict the dislocation density and the recrystallization nuclei density due to irradiation. The predicted fission rate and temperature dependences of the dislocation density are in good agreement with experimental measurements. This information is used as input for the multiphase phase-field model to investigate the fission-induced recrystallization kinetics. The simulated recrystallization volume fraction and bubble induced swelling agree well with experimental data. The effects of the fission rate, initial grainmore » size, and grain morphology on the recrystallization kinetics are discussed based on an analysis of recrystallization growth rate using the modified Avrami equation. Here, we conclude that the initial microstructure of the U-Mo fuels, especially the grain size, can be used to effectively control the rate of fission-induced recrystallization and therefore swelling.« less

Microstructure and critical strain of dynamic recrystallization of 6082 aluminum alloy in thermal deformation

NASA Astrophysics Data System (ADS)

Ren, W. W.; Xu, C. G.; Chen, X. L.; Qin, S. X.

2018-05-01

Using high temperature compression experiments, true stress true strain curve of 6082 aluminium alloy were obtained at the temperature 460°C-560°C and the strain rate 0.01 s-1-10 s-1. The effects of deformation temperature and strain rate on the microstructure are investigated; (‑∂lnθ/∂ε) ‑ ε curves are plotted based on σ-ε curve. Critical strains of dynamic recrystallization of 6082 aluminium alloy model were obtained. The results showed lower strain rates were beneficial to increase the volume fraction of recrystallization, the average recrystallized grain size was coarse; High strain rates are beneficial to refine average grain size, the volume fraction of dynamic recrystallized grain is less than that by using low strain rates. High temperature reduced the dislocation density and provided less driving force for recrystallization so that coarse grains remained. Dynamic recrystallization critical strain model and thermal experiment results can effectively predict recrystallization critical point of 6082 aluminium alloy during thermal deformation.

Effects of homogenization treatment on recrystallization behavior of 7150 aluminum sheet during post-rolling annealing

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

Guo, Zhanying; Department of Applied Science, University of Québec at Chicoutimi, Saguenay, QC G7H 2B1; Zhao, Gang

2016-04-15

The effects of two homogenization treatments applied to the direct chill (DC) cast billet on the recrystallization behavior in 7150 aluminum alloy during post-rolling annealing have been investigated using the electron backscatter diffraction (EBSD) technique. Following hot and cold rolling to the sheet, measured orientation maps, the recrystallization fraction and grain size, the misorientation angle and the subgrain size were used to characterize the recovery and recrystallization processes at different annealing temperatures. The results were compared between the conventional one-step homogenization and the new two-step homogenization, with the first step being pretreated at 250 °C. Al{sub 3}Zr dispersoids with highermore » densities and smaller sizes were obtained after the two-step homogenization, which strongly retarded subgrain/grain boundary mobility and inhibited recrystallization. Compared with the conventional one-step homogenized samples, a significantly lower recrystallized fraction and a smaller recrystallized grain size were obtained under all annealing conditions after cold rolling in the two-step homogenized samples. - Highlights: • Effects of two homogenization treatments on recrystallization in 7150 Al sheets • Quantitative study on the recrystallization evolution during post-rolling annealing • Al{sub 3}Zr dispersoids with higher densities and smaller sizes after two-step treatment • Higher recrystallization resistance of 7150 sheets with two-step homogenization.« less

On the Coupling between Recrystallization and Precipitation Following Hot Deformation in a γ-γ' Nickel-Based Superalloy

NASA Astrophysics Data System (ADS)

Seret, Anthony; Moussa, Charbel; Bernacki, Marc; Bozzolo, Nathalie

2018-06-01

Postdynamic recrystallization and γ' precipitation during cooling from γ' supersolvus temperature after hot compression were studied in the AD730 (AD730 is a trademark of Aubert et Duval Company in Paris, France) γ-γ' nickel-based superalloy. Emphasis was on not only both phenomena as distinct mechanisms but also on their mutual influence in terms of physical mechanisms. The growth of γ' precipitates is hastened in the unrecrystallized grains compared to the recrystallized ones. This could possibly be attributed to the higher dislocation content acting as high-diffusivity paths. Postdynamic recrystallization is not prevented by Smith-Zener pinning of the recrystallization front by the γ' precipitates. Instead, the recrystallization front dissolves γ' precipitates, which then reprecipitate discontinuously or continuously and coherently with the surrounding γ matrix in the recrystallized grains.

Preparation, Characterization and Utilization of Electrodes Coated with Polymeric Networks Formed by Gamma Radiation Crosslinking.

DTIC Science & Technology

1987-04-01

polymers such as poly[ diallyl dimethyl ammonium chloride] , poly [vinylbenzyl trimethyl ammonium chloride], poly[styrene sulfonic acid , sodium salt] and...poly[acrylic acid ], which would ordinarily dissolve from the electrode surface in aqueous solution unless crosslinked into a network, and several...Irradiation on a Water-Soluble Polymer: DDAC 8 E. Electrochemistry of DDAC Networks on Platinum and Graphite 10 F. Poly [acrylic acid ] Films on Graphite

Process for producing metal compounds from graphite oxide

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

2000-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen This intermediary product can be flier processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Process for Producing Metal Compounds from Graphite Oxide

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

2000-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon. metal. chloride. and oxygen This intermediary product can be flier processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon. metal carbonate. and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide: b) in an inert environment to produce metal oxide on carbon substrate: c) in a reducing environment. to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

The Determination of Trace Metals in Saline Waters and Biological Tissues Using the Heated Graphite Atomizer

NASA Technical Reports Server (NTRS)

Segar, D. A.

1971-01-01

A selective, volatalization technique utilizing the heated graphite atomizer atomic absorption technique has been developed for the analysis of iron in sea water. A similar technique may be used to determine vanadium, copper, nickel and cobalt in saline waters when their concentrations are higher than those normally encountered'in unpolluted sea waters. A preliminary solvent extraction using ammonium pyrolidine dithiocarbamate and methyl iso-butyl ketone permits the determination of a number of elements including iron, copper, zinc, nickel, cobalt and lead in sea water. The heated graphite atomized technique has also been applied to the determination of a range of trace transition elements in marine plant and animal tissues.

Influence of Fe(2+)-catalysed iron oxide recrystallization on metal cycling.

PubMed

Latta, Drew E; Gorski, Christopher A; Scherer, Michelle M

2012-12-01

Recent work has indicated that iron (oxyhydr-)oxides are capable of structurally incorporating and releasing metals and nutrients as a result of Fe2+-induced iron oxide recrystallization. In the present paper, we briefly review the current literature examining the mechanisms by which iron oxides recrystallize and summarize how recrystallization affects metal incorporation and release. We also provide new experimental evidence for the Fe2+-induced release of structural manganese from manganese-doped goethite. Currently, the exact mechanism(s) for Fe2+-induced recrystallization remain elusive, although they are likely to be both oxide-and metal-dependent. We conclude by discussing some future research directions for Fe2+-catalysed iron oxide recrystallization.

Negative Temperature Dependence of Recrystallized Grain Size: Formulation and Experimental Confirmation on Copper

PubMed Central

Elmasry, Mohamed; Liu, Fan; Jiang, Yao; Mao, Ze Ning; Liu, Ying; Wang, Jing Tao

2017-01-01

The catalyzing effect on nucleation of recrystallization from existing grains resulting from previous lower temperature deformation is analyzed, analogous to the size effect of foreign nucleus in heterogeneous nucleation. Analytical formulation of the effective nucleation site for recrystallization leads to a negative temperature dependence of recrystallized grain size of metals. Non-isochronal annealing—where annealing time is set just enough for the completion of recrystallization at different temperatures—is conducted on pure copper after severe plastic deformation. More homogeneous and smaller grains are obtained at higher annealing temperature. The good fit between analytical and experimental results unveils the intrinsic feature of this negative temperature dependence of recrystallized grain size. PMID:28772676

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

Liang, Linyun; Mei, Zhi -Gang; Kim, Yeon Soo

A mesoscale model is developed by integrating the rate theory and phase-field models and is used to study the fission-induced recrystallization in U-7Mo alloy. The rate theory model is used to predict the dislocation density and the recrystallization nuclei density due to irradiation. The predicted fission rate and temperature dependences of the dislocation density are in good agreement with experimental measurements. This information is used as input for the multiphase phase-field model to investigate the fission-induced recrystallization kinetics. The simulated recrystallization volume fraction and bubble induced swelling agree well with experimental data. The effects of the fission rate, initial grainmore » size, and grain morphology on the recrystallization kinetics are discussed based on an analysis of recrystallization growth rate using the modified Avrami equation. Here, we conclude that the initial microstructure of the U-Mo fuels, especially the grain size, can be used to effectively control the rate of fission-induced recrystallization and therefore swelling.« less

Adaptive characterization of recrystallization kinetics in IF steel by electron backscatter diffraction.

PubMed

Kim, Dong-Kyu; Park, Won-Woong; Lee, Ho Won; Kang, Seong-Hoon; Im, Yong-Taek

2013-12-01

In this study, a rigorous methodology for quantifying recrystallization kinetics by electron backscatter diffraction is proposed in order to reduce errors associated with the operator's skill. An adaptive criterion to determine adjustable grain orientation spread depending on the recrystallization stage is proposed to better identify the recrystallized grains in the partially recrystallized microstructure. The proposed method was applied in characterizing the microstructure evolution during annealing of interstitial-free steel cold rolled to low and high true strain levels of 0.7 and 1.6, respectively. The recrystallization kinetics determined by the proposed method was found to be consistent with the standard method of Vickers microhardness. The application of the proposed method to the overall recrystallization stages showed that it can be used for the rigorous characterization of progressive microstructure evolution, especially for the severely deformed material. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Modeling the Controlled Recrystallization of Particle-Containing Aluminum Alloys

NASA Astrophysics Data System (ADS)

Adam, Khaled; Root, Jameson M.; Long, Zhengdong; Field, David P.

2017-01-01

The recrystallized fraction for AA7050 during the solution heat treatment is highly dependent upon the history of deformation during thermomechanical processing. In this work, a state variable model was developed to predict the recrystallization volume fraction as a function of processing parameters. Particle stimulated nucleation (PSN) was observed as a dominant mechanism of recrystallization in AA7050. The mesoscale Monte Carlo Potts model was used to simulate the evolved microstructure during static recrystallization with the given recrystallization fraction determined already by the state variable model for AA7050 alloy. The spatial inhomogeneity of nucleation is obtained from the measurement of the actual second-phase particle distribution in the matrix identified using backscattered electron (BSE) imaging. The state variable model showed good fit with the experimental results, and the simulated microstructures were quantitatively comparable to the experimental results for the PSN recrystallized microstructure of 7050 aluminum alloy. It was also found that the volume fraction of recrystallization did not proceed as dictated by the Avrami equation in this alloy because of the presence of the growth inhibitors.

Through-thickness recrystallization characteristics of a laminated AA3xxx–AA6xxx aluminum alloy system

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

Liao, L.H., E-mail: l2liao@uwaterloo.ca; Jin, H.; Gallerneault, M.

2015-03-15

The through-thickness annealing behavior of a laminated AA3xxx–AA6xxx alloy system at 300 °C has been studied by scanning electron microscopy, electron backscatter diffraction analysis, electron probe micro-analysis, differential scanning calorimetry, and hardness measurement. Results show that the recrystallization process starts at the interface region between the AA3xxx (clad) and AA6xxx (core) layers. Subsequently, the recrystallization process front progresses into the core layer, while the clad layer is the last region to recrystallize. It is also found that precipitation precedes recrystallization in the entire laminate at the investigated temperature. The preferential onset of recrystallization at the interface region is attributed tomore » the net driving pressure being the highest in this region. The factors that lead to such enhanced net driving pressure are (a) deformation incompatibility between the two alloy layers, (b) lower solute content of the interface, which also leads to lower volume fraction of precipitates, and (c) an accelerated rate of precipitate coarsening due to the presence of a higher density of dislocations. The gradual progress of recrystallization from the interface towards the core layer is dictated by precipitate coarsening and the dependence of its rate on the density of deformation-induced dislocations. The lower driving pressure due to lower work hardening capacity, high solute drag pressure due to Mn, and additional Zener drag from precipitates that form due to solute redistribution during annealing explain the late initiation of recrystallization in the clad layer. - Highlights: • The through-thickness recrystallization of a laminated system is investigated. • The early onset of recrystallization at the interface is discussed. • The effects of precipitation and coarsening on recrystallization are analyzed.« less

Multi-walled Carbon Nanotubes/Graphite Nanosheets Modified Glassy Carbon Electrode for the Simultaneous Determination of Acetaminophen and Dopamine.

PubMed

Zhang, Susu; He, Ping; Zhang, Guangli; Lei, Wen; He, Huichao

2015-01-01

Graphite nanosheets prepared by thermal expansion and successive sonication were utilized for the construction of a multi-walled carbon nanotubes/graphite nanosheets based amperometric sensing platform to simultaneously determine acetaminophen and dopamine in the presence of ascorbic acid in physiological conditions. The synergistic effect of multi-walled carbon nanotubes and graphite nanosheets catalyzed the electrooxidation of acetaminophen and dopamine, leading to a remarkable potential difference up to 200 mV. The as-prepared modified electrode exhibited linear responses to acetaminophen and dopamine in the concentration ranges of 2.0 × 10(-6) - 2.4 × 10(-4) M (R = 0.999) and 2.0 × 10(-6) - 2.0 × 10(-4) M (R = 0.998), respectively. The detection limits were down to 2.3 × 10(-7) M for acetaminophen and 3.5 × 10(-7) M for dopamine (S/N = 3). Based on the simple preparation and prominent electrochemical properties, the obtained multi-walled carbon nanotubes/graphite nanosheets modified electrode would be a good candidate for the determination of acetaminophen and dopamine without the interference of ascorbic acid.

Electrode systems for in situ vitrification

DOEpatents

Buelt, James L.; Carter, John G.; Eschbach, Eugene A.; FitzPatrick, Vincent F.; Koehmstedt, Paul L.; Morgan, William C.; Oma, Kenton H.; Timmerman, Craig L.

1990-01-01

An electrode comprising a molybdenum rod is received within a conductive collar formed of graphite. The molybdenum rod and the graphite collar may be physically joined at the bottom. A pair of such electrodes are placed in soil containing buried waste material and an electric current is passed therebetween for vitrifying the soil. The graphite collar enhances the thermal conductivity of the combination, bringing heat to the surface, and preventing formation of a cold cap of material above the ground surface. The annulus between the molybdenum rod electrode and the graphite collar is suitably filled with a conductive ceramic powder that sinters upon the molybdenum rod, protecting the same from oxidation as graphite material is consumed, or a metal powder which liquefies at operating temperatures. The center of the molybdenum rod, used with a collar of separately, can be hollow and filled with a powdered metal, such as copper, which liquefies at operating temperatures. Connection to electrodes can be provided below ground level to avoid open circuit due to electrode deterioration, or sacrificial electrodes may be employed when operation is started. Outboard electrodes cna be utilized to square up a vitrified area.

Dielectric properties of novel polyurethane-PZT-graphite foam composites

NASA Astrophysics Data System (ADS)

Tolvanen, Jarkko; Hannu, Jari; Nelo, Mikko; Juuti, Jari; Jantunen, Heli

2016-09-01

Flexible foam composite materials offer multiple benefits to future electronic applications as the rapid development of the electronics industry requires smaller, more efficient, and lighter materials to further develop foldable and wearable applications. The aims of this work were to examine the electrical properties of three- and four-phase novel foam composites in different conditions, find the optimal mixture for four-phase foam composites, and study the combined effects of lead zirconate titanate (PZT) and graphite fillers. The flexible and highly compressible foams were prepared in a room-temperature mixing process using polyurethane, PZT, and graphite components as well as their combinations, in which air acted as one phase. In three-phase foams the amount of PZT varied between 20 and 80 wt% and the amount of graphite, between 1 and 15 wt%. The four-phase foams were formed by adding 40 wt% of PZT while the amount of graphite ranged between 1 and 15 wt%. The presented results and materials could be utilized to develop new flexible and soft sensor applications by means of material technology.

Genesis of base-metal sulfide deposits, Alabama Piedmont: Final report for the 1985-1986 SOMED (School of Mines and Energy Development) project year

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

Lesher, C.M.

1987-03-18

The best characterized massive sulfide deposit in the Northern Alabama Piedmont is the Stone Hill deposit, one of several small Fe-Cu-Zn deposits and prospects associated with metasedimentary and metavolcanic rocks of the Ashland Supergroup. The Fe-Cu-Zn sulfide mineralization in the Stone Hill district is hosted by thin felsic schist horizons within the Ketchepedrakee amphibolite, along the contact between metasediments of the Mad Indian and Poe Bridge Mountain Groups. Associated lithologies include garnetites, tremolite-chlorite rocks, and oxide facies iron-formations. The mineralized felsic schists and garnetites are of very limited stratigraphic extent, generally occur within the interpreted upper part of the amphibolite,more » and normally exhibit gradational contacts with enclosing amphibolites. The mineralized felsic schists contain enigmatic grains and polycrystalline aggregates of quartz +- feldspar +- amphibole +- mica that probably represent boudinaged quartz-feldspar segregations, but it is impossible to completely preclude an origin as recrystallized clastic sedimentary particles, recrystallized and deformed igneous phenocrysts, or cataclastic particles. Multivariate statistical analyses and mass balance calculations suggest that the mineralized felsic schists and garnetites are hydrothermally-altered, metamorphosed equivalents of the amphibolites, consistent with the field relationships. Interpretation of the Ketchepedrakee amphibolite as an ocean floor basalt, the mineralized felsic schists and garnetites as hydrothermally-altered variants, and the enclosing graphitic and garnetiferous schists as flysch-type sediments suggests that the rocks of the Stone Hill district were deposited along a rifted continental margin. The close association of mineralization and hydrothermal alteration indicates that a proximal volcanogenic model is most appropriate for the massive sulfide deposits in this area.« less

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

Hu, Shenyang; Joshi, Vineet; Lavender, Curt A.

Experiments showed that recrystallization dramatically speeds up the gas bubble swelling kinetics in metallic UMo fuels. In this work a recrystallization model is developed to study the effect of microstructures and radiation conditions on recrystallization kinetics. The model integrates the rate theory of intra-granular gas bubble and interstitial loop evolution and a phase field model of recrystallization zone evolution. A fast passage method is employed to describe one dimensional diffusion of interstitials which have diffusivity several order magnitude larger than that of the fission gas Xe. With the model, the effect of grain sizes on recrystallization kinetics is simulated.

Web-structured graphitic carbon fiber felt as an interlayer for rechargeable lithium-sulfur batteries with highly improved cycling performance

NASA Astrophysics Data System (ADS)

Lee, Dong Kyu; Ahn, Chi Won; Jeon, Hwan-Jin

2017-08-01

Graphitic carbon fiber felt (GCFF) with a crystalline graphitic carbon structure was facilely prepared by a combination of electrospinning and graphitization (2800 °C heat treatment) and was used as an interlayer between the cathode and separator in Li-S batteries. This GCFF interlayer trapped the polysulfides on the cathode side and increased the utilization of sulfur by suppressing the shuttle phenomenon. Also, the GCFF was shown to be able to act as an upper current collector to reduce the charge-transfer resistance owing to the high crystallinity of the graphitic carbon fibers. The sulfur cathode with the GCFF interlayer showed a high specific initial discharge capacity of 1280.14 mAh g-1 and excellent cycling stability (1004.62 mAh g-1 after 100 cycles) at 0.2 C. Also, an image of the glass fiber (GF) separator on the anode side confirmed the presence of an SEI after 200 cycles, which apparently resulted from stable Li deposition on the Li metal because of the low or medium concentration of sulfur in the electrolyte solution. Our observations should contribute to elucidating the key features of complex three-dimensional carbon fabrics with crystalline graphitic structures that allow them, when inserted as interlayers, to markedly improve the performance of rechargeable batteries.

Stable mineral recrystallization in low temperature aqueous systems: A critical review

NASA Astrophysics Data System (ADS)

Gorski, Christopher A.; Fantle, Matthew S.

2017-02-01

Minerals may undergo recrystallization reactions in low temperature (<100 °C) aqueous systems, during which they exchange isotopes and trace elements with the dissolved reservoir without undergoing overt structural, bulk compositional, or morphological changes. These interfacial reactions, which are often referred to in the literature as "atom exchange" and herein as "stable mineral recrystallization", have important implications for the use of isotopic and elemental proxies to interpret past temperatures, oxidation states, and aqueous chemistries on Earth. The reactions are also significant for modern environments, including engineered systems, as they imply that mineral lattices may be substantially more open to exchanging toxic elements and radionuclides with coexisting solutions than previously thought. To date, observations of stable mineral recrystallization are distributed among several disciplines, and no work has attempted to review their findings comprehensively. Accordingly, this review article presents laboratory evidence for stable mineral recrystallization, describes data collection and interpretation strategies, summarizes similar recrystallization systematics observed in multiple studies, explores the potential occurrence of stable mineral recrystallization in natural systems, and discusses possible mechanisms by which stable mineral recrystallization occurs. The review focuses primarily on carbonates, sulfates, and iron oxides because these minerals have been studied most extensively to date. The review concludes by presenting key questions that should be addressed in this field to further understand and account for stable mineral recrystallization in natural and engineered aqueous systems at low temperatures.

Static Recrystallization Behavior of Z12CN13 Martensite Stainless Steel

NASA Astrophysics Data System (ADS)

Luo, Min; Zhou, Bing; Li, Rong-bin; Xu, Chun; Guo, Yan-hui

2017-09-01

In order to increase the hot workability and provide proper hot forming parameters of forging Z12CN13 martensite stainless steel for the simulation and production, the static recrystallization behavior has been studied by double-pass hot compression tests. The effects of deformation temperature, strain rate and inter-pass time on the static recrystallization fraction by the 2% offset method are extensively studied. The results indicate that increasing the inter-pass time and the deformation temperature as well as strain rate appropriately can increase the fraction of static recrystallization. At the temperature of 1050-1150 °C, inter-pass time of 30-100 s and strain rate of 0.1-5 s-1, the static recrystallization behavior is obvious. In addition, the kinetics of static recrystallization behavior of Z12CN13 steel has been established and the activation energy of static recrystallization is 173.030 kJ/mol. The substructure and precipitates have been studied by TEM. The results reveal that the nucleation mode is bulging at grain boundary. Undissolved precipitates such as MoNi3 and Fe3C have a retarding effect on the recrystallization kinetics. The effect is weaker than the accelerating effect of deformation temperature.

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

Liang, Linyun; Mei, Zhi-Gang; Yacout, Abdellatif M.

We have developed a mesoscale phase-field model for studying the effect of recrystallization on the gas-bubble-driven swelling in irradiated U-Mo alloy fuel. The model can simulate the microstructural evolution of the intergranular gas bubbles on the grain boundaries as well as the recrystallization process. Our simulation results show that the intergranular gas-bubble-induced fuel swelling exhibits two stages: slow swelling kinetics before recrystallization and rapid swelling kinetics with recrystallization. We observe that the recrystallization can significantly expedite the formation and growth of gas bubbles at high fission densities. The reason is that the recrystallization process increases the nucleation probability of gasmore » bubbles and reduces the diffusion time of fission gases from grain interior to grain boundaries by increasing the grain boundary area and decreasing the diffusion distance. The simulated gas bubble shape, size distribution, and density on the grain boundaries are consistent with experimental measurements. We investigate the effect of the recrystallization on the gas-bubble-driven fuel swelling in UMo through varying the initial grain size and grain aspect ratio. We conclude that the initial microstructure of fuel, such as grain size and grain aspect ratio, can be used to effectively control the recrystallization and therefore reduce the swelling in U-Mo fuel.« less

Ion-specific ice recrystallization provides a facile approach for the fabrication of porous materials

NASA Astrophysics Data System (ADS)

Wu, Shuwang; Zhu, Chongqin; He, Zhiyuan; Xue, Han; Fan, Qingrui; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-05-01

Ice recrystallization is of great importance to both fundamental research and practical applications, however understanding and controlling ice recrystallization processes remains challenging. Here, we report the discovery of an ion-specific effect on ice recrystallization. By simply changing the initial type and concentration of ions in an aqueous solution, the size of ice grains after recrystallization can be tuned from 27.4+/-4.1 to 277.5+/-30.9 μm. Molecular dynamics simulations show that the ability of the ion to be incorporated into the ice phase plays a key role in the ultimate size of the ice grains after recrystallization. Moreover, by using recrystallized ice crystals as templates, 2D and 3D porous networks with tuneable pore sizes could be prepared from various materials, for example, NaBr, collagen, quantum dots, silver and polystyrene colloids. These porous materials are suitable for a wide range of applications, for example, in organic electronics, catalysis and bioengineering.

Microstructural evolution and rheology of quartz in a mid-crustal shear zone

NASA Astrophysics Data System (ADS)

Rahl, Jeffrey M.; Skemer, Philip

2016-06-01

We present microstructural and crystallographic preferred orientation (CPO) data on quartz deformed in the middle crust to explore the interaction and feedback between dynamic recrystallization, deformation processes, and CPO evolution. The sample investigated here is a moderately deformed quartz-rich mylonite from the Blue Ridge in Virginia. We have created high-resolution crystallographic orientation maps using electron backscatter diffraction (EBSD) of 51 isolated quartz porphyroclasts with recrystallized grain fractions ranging from 10 to 100%. Recrystallized grains are internally undeformed and display crystallographic orientations dispersed around the orientation of the associated parent porphyroclast. We document a systematic decrease in fabric intensity with recrystallization, suggesting that progressive deformation of the recrystallized domains involves processes that can weaken a pre-existing CPO. Relationships between recrystallization fraction and shear strain suggest that complete microstructural re-equilibration requires strains in excess of γ = 5. Variation in the degree of recrystallization implies that strain was accumulated heterogeneously, and that a steady-state microstructure and rheology were not achieved.

Ion-specific ice recrystallization provides a facile approach for the fabrication of porous materials

PubMed Central

Wu, Shuwang; Zhu, Chongqin; He, Zhiyuan; Xue, Han; Fan, Qingrui; Song, Yanlin; Francisco, Joseph S.; Zeng, Xiao Cheng; Wang, Jianjun

2017-01-01

Ice recrystallization is of great importance to both fundamental research and practical applications, however understanding and controlling ice recrystallization processes remains challenging. Here, we report the discovery of an ion-specific effect on ice recrystallization. By simply changing the initial type and concentration of ions in an aqueous solution, the size of ice grains after recrystallization can be tuned from 27.4±4.1 to 277.5±30.9 μm. Molecular dynamics simulations show that the ability of the ion to be incorporated into the ice phase plays a key role in the ultimate size of the ice grains after recrystallization. Moreover, by using recrystallized ice crystals as templates, 2D and 3D porous networks with tuneable pore sizes could be prepared from various materials, for example, NaBr, collagen, quantum dots, silver and polystyrene colloids. These porous materials are suitable for a wide range of applications, for example, in organic electronics, catalysis and bioengineering. PMID:28462937

Ion-specific ice recrystallization provides a facile approach for the fabrication of porous materials.

PubMed

Wu, Shuwang; Zhu, Chongqin; He, Zhiyuan; Xue, Han; Fan, Qingrui; Song, Yanlin; Francisco, Joseph S; Zeng, Xiao Cheng; Wang, Jianjun

2017-05-02

Ice recrystallization is of great importance to both fundamental research and practical applications, however understanding and controlling ice recrystallization processes remains challenging. Here, we report the discovery of an ion-specific effect on ice recrystallization. By simply changing the initial type and concentration of ions in an aqueous solution, the size of ice grains after recrystallization can be tuned from 27.4±4.1 to 277.5±30.9 μm. Molecular dynamics simulations show that the ability of the ion to be incorporated into the ice phase plays a key role in the ultimate size of the ice grains after recrystallization. Moreover, by using recrystallized ice crystals as templates, 2D and 3D porous networks with tuneable pore sizes could be prepared from various materials, for example, NaBr, collagen, quantum dots, silver and polystyrene colloids. These porous materials are suitable for a wide range of applications, for example, in organic electronics, catalysis and bioengineering.

Modifications in the AA5083 Johnson-Cook Material Model for Use in Friction Stir Welding Computational Analyses

NASA Astrophysics Data System (ADS)

Grujicic, M.; Pandurangan, B.; Yen, C.-F.; Cheeseman, B. A.

2012-11-01

Johnson-Cook strength material model is frequently used in finite-element analyses of various manufacturing processes involving plastic deformation of metallic materials. The main attraction to this model arises from its mathematical simplicity and its ability to capture the first-order metal-working effects (e.g., those associated with the influence of plastic deformation, rate of deformation, and the attendant temperature). However, this model displays serious shortcomings when used in the engineering analyses of various hot-working processes (i.e., those utilizing temperatures higher than the material recrystallization temperature). These shortcomings are related to the fact that microstructural changes involving: (i) irreversible decrease in the dislocation density due to the operation of annealing/recrystallization processes; (ii) increase in grain-size due to high-temperature exposure; and (iii) dynamic-recrystallization-induced grain refinement are not accounted for by the model. In this study, an attempt is made to combine the basic physical-metallurgy principles with the associated kinetics relations to properly modify the Johnson-Cook material model, so that the model can be used in the analyses of metal hot-working and joining processes. The model is next used to help establish relationships between process parameters, material microstructure and properties in friction stir welding welds of AA5083 (a non-age-hardenable, solid-solution strengthened, strain-hardened/stabilized Al-Mg-Mn alloy).

Spatial distribution of quartz recrystallization microstructures across the Aar massif (Swiss Central Alps)

NASA Astrophysics Data System (ADS)

Peters, M.; Herwegh, M.

2012-04-01

In the Aar massif, main foliation and major deformation structures were developed during NW-SE compression associated with the Alpine orogeny (Steck 1968). To be precise, shearing at the brittle to ductile transition may have initiated at different stages between 22-20 Ma and 14-12 Ma, followed by purely brittle deformation at around 10 Ma (Rolland et al. 2009). In light of the onset of dynamic recrystallization in quartz, Bambauer et al. (2009) defined a quartz recrystallization isograd in the northern part of the Aar massif. To the south, the grain size of recrystallized grains increases due to an increase of metamorphic temperatures from N to S. The aim of the current project is to carry out quantitative analysis on changes of the dynamic and static recrystallization behavior of quartz. Across the Aar massif, two general types of microstructures have to be discriminated: (i) weakly to moderately deformed host rocks and (ii) intensely deformed mylonites to ultramylonites out of high strain shear zones. In (i), volume fraction and size of recrystallized quartz grains increase towards the S showing grain size changes from around 5 µm up to ca. 200 µm. Southern microstructures are characterized by complete recrystallization. In terms of recrystallization processes, a transition from bulging recrystallization in the N to subgrain rotation recrystallization in the S occurs. Such a change in dynamic recrystallization processes combined with a grain size increase points towards reduced differential stresses with increasing temperature. This temperature gradient is also corroborated by a switch in the active glide systems in quartz from basal to rhomb dominated glide. In contrast to the granitic host rocks, the mylonites and ultramylonites (ii) show smaller recrystallized grain sizes due to enhanced strain rates. However, they also reveal a general increase of recrystallized grain sizes from N to S. In the S, microstructures from (i) and (ii) show equidimensional grains with 120° triple junctions and straight grain boundaries. Such microstructures are typical for static annealing. For that reason, we propose a post-deformational temperature pulse mainly affecting the southern part of the Aar massif. This annealing stage might correlate with the fluid pulse between 12-10 Ma suggested by Challandes et al. (2008). We will present constraints on the grade of deformation based on grain size data and CPO analyses, supporting the hypothesis that various deformation stages are well preserved in statically recrystallized structures.

Thermal neutron streaming effects and WIMS analysis of the Penn State subcritical graphite pile

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

Feltus, M.A.; Zediak, C.S.; Jester, W.A.

1997-12-01

This analysis was performed on the Pennsylvania State University (PSU) subcritical reactor to find more accurate values for such nuclear parameters as the thermal fuel utilization factor, thermal diffusion length in the graphite, migration area, k{sub eff}, etc. The analysis involved using the Winfrith Integrated Multigroup Scheme (WIMS) code as well as various hand calculations to find and compare those parameters. The data found in this analysis will be used by future students in the Penn State laboratory courses.

Progressive fracture of fiber composites

NASA Technical Reports Server (NTRS)

Irvin, T. B.; Ginty, C. A.

1983-01-01

Refined models and procedures are described for determining progressive composite fracture in graphite/epoxy angleplied laminates. Lewis Research Center capabilities are utilized including the Real Time Ultrasonic C Scan (RUSCAN) experimental facility and the Composite Durability Structural Analysis (CODSTRAN) computer code. The CODSTRAN computer code is used to predict the fracture progression based on composite mechanics, finite element stress analysis, and fracture criteria modules. The RUSCAN facility, CODSTRAN computer code, and scanning electron microscope are used to determine durability and identify failure mechanisms in graphite/epoxy composites.

CNTs grown on nanoporous carbon from zeolitic imidazolate frameworks for supercapacitors.

PubMed

Kim, Jeonghun; Young, Christine; Lee, Jaewoo; Park, Min-Sik; Shahabuddin, Mohammed; Yamauchi, Yusuke; Kim, Jung Ho

2016-10-27

Carbon nanotubes (CNT) grown on nanoporous carbon (NPC), which yields coexisting amorphous and graphitic nanoarchitectures, have been prepared on a large scale from zeolitic imidazolate framework (ZIF) by introducing bimetallic ions (Co 2+ and Zn 2+ ). Interestingly, the hybrid Co/Zn-ZIF-derived NPC showed rich graphitic CNTs on the surface. This NPC was utilized for a coin-type supercapacitor cell with an aqueous electrolyte, which showed enhanced retention at high current density and good stability over 10 000 cycles.

Fabrication and physical testing of graphite composite panels utilizing woven graphite fabric with current and advanced state-of-the-art resin systems

NASA Technical Reports Server (NTRS)

Lee, S. C. S.

1979-01-01

Three weaves were evaluated; a balanced plain weave, a balanced 8-harness satin weave, and a semiunidirectional crowfoot satin weave. The current state-of-the-art resin system selected was Fiberite's 934 Epoxy; the advanced resin systems evaluated were Phenolic, Phenolic/Novolac, Benzyl and Bismaleimide. The panels were fabricated for testing on NASA/Ames Research Center's Composites Modification Program. Room temperature mechanical tests only were performed by Hitco; the results are presented.

Manufacturing methods of a composite cell case for a Ni-Cd battery

NASA Technical Reports Server (NTRS)

Bauer, J. L.

1979-01-01

Basic manufacturing method refinements for using graphite epoxy material for a nickel cadmium battery cell case were performed to demonstrate production feasibility. The various facets of production scale-up, i.e., process and tooling development, together with material and process control, were integrated into a comprehensive manufacturing process that assures production reproducibility and product uniformity. Test results substantiate that a battery cell case produced from graphite epoxy pre-impregnated material, utilizing the internal pressure bag fabrication method, is feasible.

Analytical techniques and instrumentation, a compilation

NASA Technical Reports Server (NTRS)

1974-01-01

Procedures for conducting materials tests and structural analyses of aerospace components are presented as a part of the NASA technology utilization program. Some of the subjects discussed are as follows: (1) failures in cryogenic tank insulation, (2) friction characteristics of graphite and graphite-metal combinations, (3) evaluation of polymeric products in thermal-vacuum environment, (4) erosion of metals by multiple impacts with water, (5) mass loading effects on vibrated ring and shell structures, (6) nonlinear damping in structures, and (7) method for estimating reliability of randomly excited structures.

Solvent Selection for Recrystallization: An Undergraduate Organic Experiment.

ERIC Educational Resources Information Center

Baumann, Jacob B.

1979-01-01

This experiment develops the students' ability to carry out a simple recrystallization effectively, and demonstrates how a solvent may be selected or rejected for the recrystallization of a specific organic compound. (Author/BB)

On the use of copper-based substrates for YBCO coated conductors

NASA Astrophysics Data System (ADS)

Vannozzi, A.; Fabbri, F.; Augieri, A.; Angrisani Armenio, A.; Galluzzi, V.; Mancini, A.; Rizzo, F.; Rufoloni, A.; Padilla, J. A.; Xuriguera, E.; De Felicis, D.; Bemporad, E.; Celentano, G.

2014-05-01

It is well known that the recrystallization texture of heavily cold-rolled pure copper is almost completely cubic. However, one of the main drawbacks concerning the use of pure copper cube-textured substrates for YBCO coated conductor is the reduced secondary recrystallization temperature. The onset of secondary recrystallization (i.e., the occurrence of abnormal grains with unpredictable orientation) in pure copper substrate was observed within the typical temperature range required for buffer layer and YBCO processing (600-850 °C). To avoid the formation of abnormal grains the effect of both grain size adjustment (GSA) and recrystallization annealing was analyzed. The combined use of a small initial grain size and a recrystallization two-step annealing (TSA) drastically reduced the presence of abnormal grains in pure copper tapes. Another way to overcome the limitation imposed by the formation of abnormal grains is to deposit a buffer layer at temperatures where secondary recrystallization does not occur. For example, La2Zr2O7 (LZO) film with a high degree of epitaxy was grown by metal-organic decomposition (MOD) at 1000 °C on pure copper substrate. In several samples the substrate underwent secondary recrystallization. Our experiments indicate that the motion of grain boundaries occurring during secondary recrystallization process does not affect the quality of LZO film.

Effect of Sn Micro-alloying on Recrystallization Nucleation and Growth Processes of Ferritic Stainless Steels

NASA Astrophysics Data System (ADS)

He, Tong; Bai, Yang; Liu, Xiuting; Guo, Dan; Liu, Yandong

2018-04-01

We investigated the effect of Sn micro-alloying on recrystallization nucleation and growth processes of ferritic stainless steels. The as-received hot rolled sheets were cold rolled up to 80% reduction and then annealed at 740-880 °C for 5 min. The cold rolling and recrystallization microstructures and micro-textures of Sn-containing and Sn-free ferritic stainless steels were all determined by electron backscatter diffraction. Our Results show that Sn micro-alloying has important effects on recrystallization nucleation and growth processes of ferritic stainless steels. Sn micro-alloying conduces to grain fragmentation in the deformation band, more fragmented grains are existed in Sn-containing cold rolled sheets, which provides more sites for recrystallization nucleation. Sn micro-alloying also promotes recrystallization process and inhibits the growth of recrystallized grains. The recrystallization nucleation and growth mechanism of Sn-containing and Sn-free ferritic stainless steels are both characterized by orientation nucleation and selective growth, but Sn micro-alloying promotes the formation of γ-oriented grains. Furthermore, Sn micro-alloying contributes to the formation of Σ13b CSL boundaries and homogeneous γ-fiber texture. Combining the results of microstructure and micro-texture, the formability of Sn-containing ferritic stainless steels will be improved to some extent.

Space structures concepts and materials

NASA Technical Reports Server (NTRS)

Nowitzky, A. M.; Supan, E. C.

1988-01-01

An extension is preseted of the evaluation of graphite/aluminum metal matrix composites (MMC) for space structures application. A tubular DWG graphite/aluminum truss assembly was fabricated having the structural integrity and thermal stability needed for space application. DWG is a proprietary thin ply continuous graphite reinforced aluminum composite. The truss end fittings were constructed using the discontinuous ceramic particulate reinforced MMC DWAl 20 (trademark). Thermal stability was incorporated in the truss by utilizing high stiffness, negative coefficient of thermal expansion (CTE) P100 graphite fibers in a 6061 aluminum matrix, crossplied to provide minimized CTE in the assembled truss. Tube CTE was designed to be slightly negative to offset the effects of the end fitting and sleeve, CTE values of which are approx. 1/2 that of aluminum. In the design of the truss configuration, the CTE contribution of each component was evaluated to establish the component dimension and layup configuration required to provide a net zero CTE in the subassemblies which would then translate to a zero CTE for the entire truss bay produced.

Design, fabrication, and test of a graphite/epoxy metering truss. [as applied to the LST

NASA Technical Reports Server (NTRS)

Oken, S.; Skoumal, D. E.

1975-01-01

A graphite/epoxy metering truss as applied to the large space telescope was investigated. A full-scale truss was designed, fabricated and tested. Tests included static limit loadings, a modal survey and thermal-vacuum distortion evaluation. The most critical requirement was the demonstration of the dimensional stability provided by the graphite/epoxy truss concept. Crucial to the attainment of this objective was the ability to make very sophisticated thermal growth measurements which was provided by a seven beam laser interferometer. The design of the basic truss elements were tuned to provide the high degree of dimensional stability and stiffness required by the truss. The struts and spider assembly were fabricated with Fiberite's AS/934 and HMS/934 broadgoods. The rings utilized T300 graphite fabricate with the same materials. The predicted performance of the truss was developed using the NASTRAN program. These results showed conformance with the critical stiffness and thermal distortion requirements and correlated well with the test results.

Mechanism of secondary recrystallization of Goss grains in grain-oriented electrical steel

NASA Astrophysics Data System (ADS)

Hayakawa, Yasuyuki

2017-12-01

Since its invention by Goss in 1934, grain-oriented (GO) electrical steel has been widely used as a core material in transformers. GO exhibits a grain size of over several millimeters attained by secondary recrystallization during high-temperature final batch annealing. In addition to the unusually large grain size, the crystal direction in the rolling direction is aligned with <001>, which is the easy magnetization axis of α-iron. Secondary recrystallization is the phenomenon in which a certain very small number of {110}<001> (Goss) grains grow selectively (about one in 106 primary grains) at the expense of many other primary recrystallized grains. The question of why the Goss orientation is exclusively selected during secondary recrystallization has long been a main research subject in this field. The general criterion for secondary recrystallization is a small and uniform primary grain size, which is achieved through the inhibition of normal grain growth by fine precipitates called inhibitors. This paper describes several conceivable mechanisms of secondary recrystallization of Goss grains mainly based on the selective growth model.

Mechanism of secondary recrystallization of Goss grains in grain-oriented electrical steel

PubMed Central

Hayakawa, Yasuyuki

2017-01-01

Abstract Since its invention by Goss in 1934, grain-oriented (GO) electrical steel has been widely used as a core material in transformers. GO exhibits a grain size of over several millimeters attained by secondary recrystallization during high-temperature final batch annealing. In addition to the unusually large grain size, the crystal direction in the rolling direction is aligned with <001>, which is the easy magnetization axis of α-iron. Secondary recrystallization is the phenomenon in which a certain very small number of {110}<001> (Goss) grains grow selectively (about one in 106 primary grains) at the expense of many other primary recrystallized grains. The question of why the Goss orientation is exclusively selected during secondary recrystallization has long been a main research subject in this field. The general criterion for secondary recrystallization is a small and uniform primary grain size, which is achieved through the inhibition of normal grain growth by fine precipitates called inhibitors. This paper describes several conceivable mechanisms of secondary recrystallization of Goss grains mainly based on the selective growth model. PMID:28804524

Investigating the principles of recrystallization from glyceride melts.

PubMed

Windbergs, Maike; Strachan, Clare J; Kleinebudde, Peter

2009-01-01

Different lipids were melted and resolidified as model systems to gain deeper insight into the principles of recrystallization processes in lipid-based dosage forms. Solid-state characterization was performed on the samples with differential scanning calorimetry and X-ray powder diffraction. Several recrystallization processes could be identified during storage of the lipid layers. Pure triglycerides that generally crystallize to the metastable alpha-form from the melt followed by a recrystallization process to the stable beta-form with time showed a chain-length-dependent behavior during storage. With increasing chain length, the recrystallization to the stable beta-form was decelerated. Partial glycerides exhibited a more complex recrystallization behavior due to the fact that these substances are less homogenous. Mixtures of a long-chain triglyceride and a partial glyceride showed evidence of some interaction between the two components as the partial glyceride hindered the recrystallization of the triglyceride to the stable beta-form. In addition, the extent of this phenomenon depended on the amount of partial glyceride in the mixture. Based on these results, changes in solid dosage forms based on glycerides during processing and storage can be better understood.

Mechanism of secondary recrystallization of Goss grains in grain-oriented electrical steel.

PubMed

Hayakawa, Yasuyuki

2017-01-01

Since its invention by Goss in 1934, grain-oriented (GO) electrical steel has been widely used as a core material in transformers. GO exhibits a grain size of over several millimeters attained by secondary recrystallization during high-temperature final batch annealing. In addition to the unusually large grain size, the crystal direction in the rolling direction is aligned with <001>, which is the easy magnetization axis of α-iron. Secondary recrystallization is the phenomenon in which a certain very small number of {110}<001> (Goss) grains grow selectively (about one in 10 6 primary grains) at the expense of many other primary recrystallized grains. The question of why the Goss orientation is exclusively selected during secondary recrystallization has long been a main research subject in this field. The general criterion for secondary recrystallization is a small and uniform primary grain size, which is achieved through the inhibition of normal grain growth by fine precipitates called inhibitors. This paper describes several conceivable mechanisms of secondary recrystallization of Goss grains mainly based on the selective growth model.

A superhard, quenchable carbon polymorph formed by the room-temperature compression of graphite (Invited)

NASA Astrophysics Data System (ADS)

Wang, Y.; Kiefer, B.; Lee, K. K.

2010-12-01

As one of the revolutionary inventions of the 20th century, synthetic diamond has had a large impact on industry and on scientific research. However, the necessities of high pressures, high temperatures and a metal catalyst during the manufacturing of synthetic diamond make it energy consuming thus limits its availability and use. Here, we report on the synthesis of a superhard non-diamond material resulting from the compression of graphite above ~20 GPa at room temperature without the utilization of metal catalysts. The final product includes a nano-sized phase of carbon that is recoverable at ambient conditions. Furthermore, the ring cracks left on the diamond anvils suggest that the hardness of this post-graphite phase is at least comparable to that of diamond. We use high-resolution synchrotron x-ray diffraction and micro-Raman spectroscopy to monitor the structural transformation in graphite under high pressure and room temperature and find the transition to be sluggish. The possible crystal structure of the new, quenchable phase will be discussed and the time-dependent formation of this superhard post-graphite carbon will be addressed and compared to first-principle predictions.

Hot Deformation and Dynamic Recrystallization Behavior of the Cu-Cr-Zr-Y Alloy

NASA Astrophysics Data System (ADS)

Zhang, Yi; Huili, Sun; Volinsky, Alex A.; Tian, Baohong; Chai, Zhe; Liu, Ping; Liu, Yong

2016-03-01

To study the workability and to optimize the hot deformation processing parameters of the Cu-Cr-Zr-Y alloy, the strain hardening effect and dynamic softening behavior of the Cu-Cr-Zr-Y alloy were investigated. The flow stress increases with the strain rate and stress decreases with deformation temperature. The critical conditions, including the critical strain and stress for the occurrence of dynamic recrystallization, were determined based on the alloy strain hardening rate. The critical stress related to the onset of dynamic recrystallization decreases with temperature. The evolution of DRX microstructure strongly depends on the deformation temperature and the strain rate. Dynamic recrystallization appears at high temperatures and low strain rates. The addition of Y can refine the grain and effectively accelerate dynamic recrystallization. Dislocation generation and multiplication are the main hot deformation mechanisms for the alloy. The deformation temperature increase and the strain rate decrease can promote dynamic recrystallization of the alloy.

Effect of controlling recrystallization from the melt on the residual stress and structural properties of the Silica-clad Ge core fiber

NASA Astrophysics Data System (ADS)

Zhao, Ziwen; Cheng, Xueli; He, Ting; Xue, Fei; Zhang, Wei; Chen, Na; Wen, Jianxiang; Zeng, Xianglong; Wang, Tingyun

2017-09-01

Effect of controlling recrystallization from the melt (1000 °C) on the residual stress and structural properties of a Ge core fiber via molten core drawing (MCD) method is investigated. Ge core fibers is investigated using Raman spectroscopy, scanning electron microscope (SEM), and X-ray diffraction (XRD). Compared with the as-drawn Ge fiber, the Raman peak of the recrystallized Ge fiber shift from 300 cm-1 to 300.6 cm-1 and full width at half maximum (FWHM) decreased from 5.36 cm-1 to 4.48 cm-1. The Ge crystal grains which sizes are of 200-600 nm were formed during the process of recrystallization; the XRD peak of (1 1 1) plane is observed after recrystallization. These results show that controlling recrystallization allows the release of the thermal stress, and improvement of the crystal quality of Ge core.

Microstructure heterogeneity after the ECAP process and its influence on recrystallization in aluminium

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

Wronski, S., E-mail: wronski@fis.agh.edu.pl; Tarasiuk, J., E-mail: tarasiuk@ftj.agh.edu.pl; Bacroix, B., E-mail: brigitte.bacroix@univ-paris13.fr

The main purpose of the present work is to describe the qualitative and quantitative behaviours of aluminium during high strain plastic deformation and the effect of deformation on the subsequent recrystallization process. An Electron Backscatter Diffraction analysis of aluminium after the Equal channel angular pressing (ECAP) and recrystallization process is presented. In order to do this, several topological maps are measured for samples processed by 4 and 8 passes and recrystallized. The processing was conducted with route C. For all samples, distributions of grain size, misorientation, image quality factor (IQ) and texture were preceded and then analysed in some detail.more » - Highlights: ► Describe the microstructure fragmentation in aluminum. ► High strain plastic deformation and effect of deformation on recrystallization. ► The microstructure fragmentation and its influence on recrystallization. ► Image quality factor and misorientation characteristics are examined using EBSD.« less

Evaluation of co-cokes from bituminous coal with vacuum resid or decant oil, and evaluation of anthracites, as precursors to graphite

NASA Astrophysics Data System (ADS)

Nyathi, Mhlwazi S.

2011-12-01

Graphite is utilized as a neutron moderator and structural component in some nuclear reactor designs. During the reactor operaction the structure of graphite is damaged by collision with fast neutrons. Graphite's resistance to this damage determines its lifetime in the reactor. On neutron irradiation, isotropic or near-isotropic graphite experiences less structural damage than anisotropic graphite. The degree of anisotropy in a graphite artifact is dependent on the structure of its precursor coke. Currently, there exist concerns over a short supply of traditional precursor coke, primarily due to a steadily increasing price of petroleum. The main goal of this study was to study the anisotropic and isotropic properties of graphitized co-cokes and anthracites as a way of investigating the possibility of synthesizing isotropic or near-isotropic graphite from co-cokes and anthracites. Demonstrating the ability to form isotropic or near-isotropic graphite would mean that co-cokes and anthracites have a potential use as filler material in the synthesis of nuclear graphite. The approach used to control the co-coke structure was to vary the reaction conditions. Co-cokes were produced by coking 4:1 blends of vacuum resid/coal and decant oil/coal at temperatures of 465 and 500 °C for reaction times of 12 and 18 hours under autogenous pressure. Co-cokes obtained were calcined at 1420 °C and graphitized at 3000 °C for 24 hours. Optical microscopy, X-ray diffraction, temperature-programmed oxidation and Raman spectroscopy were used to characterize the products. It was found that higher reaction temperature (500 °C) or shorter reaction time (12 hours) leads to an increase in co-coke structural disorder and an increase in the amount of mosaic carbon at the expense of textural components that are necessary for the formation of anisotropic structure, namely, domains and flow domains. Characterization of graphitized co-cokes showed that the quality, as expressed by the degree of graphitization and crystallite dimensions, of the final product is dependent on the nature of the precursor co-coke. The methodology for studying anthracites was to select two anthracites on basis of rank, PSOC1515 being semi-anthracite and DECS21 anthracite. The selected anthracites were graphitized, in both native and demineralized states, under the same conditions as co-cokes. Products obtained from DECS21 showed higher degrees of graphitization and larger crystallite dimensions than products obtained from PSOC1515. Demineralization of anthracites served to increase the degree of graphitization, indicating that the minerals contained in these anthracites have no graphitization-enhancing ability. A larger crystallite length for products obtained from native versions, compared to demineralized versions, was attributed to a formation and decomposition of a silicon carbide during graphitization of native versions. In order to examine the anisotropic and isotropic properties, nuclear-grade graphite samples obtained from Oak Ridge National Laboratory (ORNL) and commercial graphite purchased from Fluka were characterized under similar conditions as graphitized co-cokes and anthracites. These samples served as representatives of "two extremes", with ORNL samples being the isotropic end and commercial graphite being the anisotropic end. Through evaluating relationships between structural parameters, it was observed that graphitized co-cokes are situated, structurally, somewhere between the "two extremes", whereas graphitized anthracites are closer to the anisotropic end. Basically, co-cokes have a better potential than anthracites to transform to isotropic or near-isotropic graphite upon graphitization. By co-coking vacuum resid/coal instead of decant oil/coal or using 500 °C instead of 465 °C, a shift away from commercial graphite towards ORNL samples was attained. Graphitizing a semi-anthracite or demineralizing anthracites before graphitization also caused a shift towards ORNL samples.

Multi-Scale Modeling of a Graphite-Epoxy-Nanotube System

NASA Technical Reports Server (NTRS)

Frankland, S. J. V.; Riddick, J. C.; Gates, T. S.

2005-01-01

A multi-scale method is utilized to determine some of the constitutive properties of a three component graphite-epoxy-nanotube system. This system is of interest because carbon nanotubes have been proposed as stiffening and toughening agents in the interlaminar regions of carbon fiber/epoxy laminates. The multi-scale method uses molecular dynamics simulation and equivalent-continuum modeling to compute three of the elastic constants of the graphite-epoxy-nanotube system: C11, C22, and C33. The 1-direction is along the nanotube axis, and the graphene sheets lie in the 1-2 plane. It was found that the C11 is only 4% larger than the C22. The nanotube therefore does have a small, but positive effect on the constitutive properties in the interlaminar region.

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

NASA Technical Reports Server (NTRS)

Hung, Ching-Chen (Inventor)

1999-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a percursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Elemental Metals or Oxides Distributed on a Carbon Substrate or Self-Supported and the Manufacturing Process Using Graphite Oxide as Template

NASA Technical Reports Server (NTRS)

Hung, Ching-Cheh (Inventor)

1999-01-01

A process for providing elemental metals or metal oxides distributed on a carbon substrate or self-supported utilizing graphite oxide as a precursor. The graphite oxide is exposed to one or more metal chlorides to form an intermediary product comprising carbon, metal, chloride, and oxygen. This intermediary product can be further processed by direct exposure to carbonate-solutions to form a second intermediary product comprising carbon, metal carbonate, and oxygen. Either intermediary product may be further processed: a) in air to produce metal oxide; b) in an inert environment to produce metal oxide on carbon substrate; c) in a reducing environment to produce elemental metal distributed on carbon substrate. The product generally takes the shape of the carbon precursor.

Enhanced and selective optical trapping in a slot-graphite photonic crystal.

PubMed

Krishnan, Aravind; Huang, Ningfeng; Wu, Shao-Hua; Martínez, Luis Javier; Povinelli, Michelle L

2016-10-03

Applicability of optical trapping tools for nanomanipulation is limited by the available laser power and trap efficiency. We utilized the strong confinement of light in a slot-graphite photonic crystal to develop high-efficiency parallel trapping over a large area. The stiffness is 35 times higher than our previously demonstrated on-chip, near field traps. We demonstrate the ability to trap both dielectric and metallic particles of sub-micron size. We find that the growth kinetics of nanoparticle arrays on the slot-graphite template depends on particle size. This difference is exploited to selectively trap one type of particle out of a binary colloidal mixture, creating an efficient optical sieve. This technique has rich potential for analysis, diagnostics, and enrichment and sorting of microscopic entities.

Strain induced grain boundary migration effects on grain growth of an austenitic stainless steel during static and metadynamic recrystallization

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

Paggi, A., E-mail: alpaggi@tenaris.com; Angella, G.; Donnini, R.

Static and metadynamic recrystallization of an AISI 304L austenitic stainless steel was investigated at 1100 °C and 10{sup −} {sup 2} s{sup −} {sup 1} strain rate. The kinetics of recrystallization was determined through double hit compression tests. Two strain levels were selected for the first compression hit: ε{sub f} = 0.15 for static recrystallization (SRX) and 0.25 for metadynamic recrystallization (MDRX). Both the as-deformed and the recrystallized microstructures were investigated through optical microscopy and electron back-scattered diffraction (EBSD) technique. During deformation, strain induced grain boundary migration appeared to be significant, producing a square-like grain boundary structure aligned along themore » directions of the maximum shear stresses in compression. EBSD analysis revealed to be as a fundamental technique that the dislocation density was distributed heterogeneously in the deformed grains. Grain growth driven by surface energy reduction was also investigated, finding that it was too slow to explain the experimental data. Based on microstructural results, it was concluded that saturation of the nucleation sites occurred in the first stages of recrystallization, while grain growth driven by strain induced grain boundary migration (SIGBM) dominated the subsequent stages. - Highlights: • Recrystallization behavior of a stainless steel was investigated at 1100 °C. • EBSD revealed that the dislocation density distribution was heterogeneous during deformation. • Saturation of nucleation sites occurred in the first stages of recrystallization. • Strain induced grain boundary migration (SIGBM) effects were significant. • Grain growth driven by SIGBM dominated the subsequent stages.« less

Titanium concentration in quartz as a record of multiple deformation mechanisms in an extensional shear zone

NASA Astrophysics Data System (ADS)

Nachlas, William O.; Whitney, Donna L.; Teyssier, Christian; Bagley, Brian; Mulch, Andreas

2014-04-01

Results of high precision analysis of Ti concentration ([Ti]) in quartz representing different recrystallization microstructures in a suite of progressively deformed quartzite mylonites show the effect of recrystallization on distribution of Ti in quartz. Petrographic observations and ion microprobe analysis reveals three texturally and geochemically distinct quartz microstructures in mylonites: (1) cores of recrystallized quartz ribbons preserve the highest [Ti] and are interpreted to have recrystallized via grain boundary migration recrystallization, (2) recrystallized rims and grain margins preserve a lower and more variable [Ti] and are interpreted to reflect the combined influence of subgrain rotation and bulging recrystallization, and (3) neocrystallized quartz precipitated in dilatancy sites has low (˜1 ppm) [Ti], reflecting the Ti content of the syndeformational fluid. Muscovite in nonmylonitic quartzite (at the base of the sampling traverse) is compositionally zoned, whereas muscovite in mylonitic quartzite shows a progressive decreasing in zoning in higher strain samples. Three-dimensional phase distribution mapping using X-ray computed tomography analysis of rock hand samples reveals that Ti-bearing accessory phases are less abundant and more dispersed in higher strained mylonites compared to nonmylonitic quartzite. This study demonstrates the influence of dynamic recrystallization on Ti substitution in quartz and evaluates the Ti buffering capacity of aqueous fluids (meteoric versus metamorphic/magmatic) as well as the distribution and reactivity of Ti-bearing accessory phases in a deforming quartzite. Results of this study suggest that Ti-in-quartz thermobarometry of deformed quartz is a sensitive technique for resolving the multistage history of quartz deformation and recrystallization in crustal shear zones.

An Ultrahigh Capacity Graphite/Li 2S Battery with Holey-Li 2S Nanoarchitectures

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

Ye, Fangmin; Noh, Hyungjun; Lee, Hongkyung

The pairing of high-capacity Li 2S cathode (1166 mAh g -1) and lithium-free anode (LFA) provides an unparalleled potential in developing safe and energy-dense next-generation secondary batteries. However, the low utilization of the Li 2S cathode and the lack of electrolytes compatible to both electrodes are impeding the development. Here, a novel graphite/Li 2S battery system, which features a self-assembled, holey-Li 2S nanoarchitecture and a stable solid electrolyte interface (SEI) on the graphite electrode, is reported. The holey structure on Li 2S is beneficial in decomposing Li 2S at the first charging process due to the enhanced Li ion extractionmore » and transfer from the Li 2S to the electrolyte. In addition, the concentrated dioxolane (DOL)-rich electrolyte designed lowers the irreversible capacity loss for SEI formation. By using the combined strategies, the graphite/holey-Li 2S battery delivers an ultrahigh discharge capacity of 810 mAh g -1 at 0.1 C (based on the mass of Li 2S) and of 714 mAh g -1 at 0.2 C. Moreover, it exhibits a reversible capacity of 300 mAh g -1 after a record lifecycle of 600 cycles at 1 C. These results suggest the great potential of the designed LFA/holey-Li 2S batteries for practical use.« less

An Ultrahigh Capacity Graphite/Li 2S Battery with Holey-Li 2S Nanoarchitectures

DOE PAGES

Ye, Fangmin; Noh, Hyungjun; Lee, Hongkyung; ...

2018-05-07

The pairing of high-capacity Li 2S cathode (1166 mAh g -1) and lithium-free anode (LFA) provides an unparalleled potential in developing safe and energy-dense next-generation secondary batteries. However, the low utilization of the Li 2S cathode and the lack of electrolytes compatible to both electrodes are impeding the development. Here, a novel graphite/Li 2S battery system, which features a self-assembled, holey-Li 2S nanoarchitecture and a stable solid electrolyte interface (SEI) on the graphite electrode, is reported. The holey structure on Li 2S is beneficial in decomposing Li 2S at the first charging process due to the enhanced Li ion extractionmore » and transfer from the Li 2S to the electrolyte. In addition, the concentrated dioxolane (DOL)-rich electrolyte designed lowers the irreversible capacity loss for SEI formation. By using the combined strategies, the graphite/holey-Li 2S battery delivers an ultrahigh discharge capacity of 810 mAh g -1 at 0.1 C (based on the mass of Li 2S) and of 714 mAh g -1 at 0.2 C. Moreover, it exhibits a reversible capacity of 300 mAh g -1 after a record lifecycle of 600 cycles at 1 C. These results suggest the great potential of the designed LFA/holey-Li 2S batteries for practical use.« less

Dynamic recrystallization in friction surfaced austenitic stainless steel coatings

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

Puli, Ramesh, E-mail: rameshpuli2000@gmail.com; Janaki Ram, G.D.

2012-12-15

Friction surfacing involves complex thermo-mechanical phenomena. In this study, the nature of dynamic recrystallization in friction surfaced austenitic stainless steel AISI 316L coatings was investigated using electron backscattered diffraction and transmission electron microscopy. The results show that the alloy 316L undergoes discontinuous dynamic recrystallization under conditions of moderate Zener-Hollomon parameter during friction surfacing. - Highlights: Black-Right-Pointing-Pointer Dynamic recrystallization in alloy 316L friction surfaced coatings is examined. Black-Right-Pointing-Pointer Friction surfacing leads to discontinuous dynamic recrystallization in alloy 316L. Black-Right-Pointing-Pointer Strain rates in friction surfacing exceed 400 s{sup -1}. Black-Right-Pointing-Pointer Estimated grain size matches well with experimental observations in 316L coatings.

Gelatinization and freeze-concentration effects on recrystallization in corn and potato starch gels.

PubMed

Ronda, Felicidad; Roos, Yrjö H

2008-04-07

Freeze-concentration of starch gels was controlled by temperature and gelatinization with glucose and lactose. The aim of the study was to evaluate the effects of freezing temperature and gel composition on starch recrystallization behaviour of corn and potato starch gels (water content 70%, w/w) in water or glucose or lactose (10%, w/w) solutions. Starch gels were obtained by heating in differential scanning calorimetry (DSC). Samples of starch gels were frozen at -10 degrees C, -20 degrees C and -30 degrees C for 24h and, after thawing, stored at +2 degrees C for 0, 1, 2, 4 and 8 days. The extent of starch recrystallization was taken from the enthalpy of melting of the recrystallized starch by DSC. Freezing temperatures, glucose, lactose and the origin of the starch affected the recrystallization behaviour greatly. The recrystallization of amorphous starch during storage was enhanced by freeze-concentration of gels at temperatures above T'(m). Molecular mobility was enhanced by unfrozen water and consequently molecular rearrangements for nucleation could take place. Further storage at a higher temperature enhanced the growth and the maturation of crystals. In particular, glucose decreased the T'(m) of the gels and consequently lower freezing temperatures were needed to reduce enhanced recrystallization during storage. Freeze-concentration temperatures also showed a significant effect on the size and the perfection of crystals formed in starch recrystallization.

Ultrasonic Determination Of Recrystallization

NASA Technical Reports Server (NTRS)

Generazio, Edward R.

1988-01-01

State of recrystallization identified. Measurement of ultrasonic attenuation shows promise as means of detecting recrystallization in metal. Technique applicable to real-time acoustic monitoring of thermomechanical treatments. Starting with work-hardened material, one ultrasonically determines effect of annealing, using correlation between ultrasonic attenuation and temperature.

A texture-component Avrami model for predicting recrystallization textures, kinetics and grain size

NASA Astrophysics Data System (ADS)

Raabe, Dierk

2007-03-01

The study presents an analytical model for predicting crystallographic textures and the final grain size during primary static recrystallization of metals using texture components. The kinetics is formulated as a matrix variant of the Johnson-Mehl-Avrami-Kolmogorov equation. The matrix form is required since the kinetic and crystallographic evolution of the microstructure is described in terms of a limited set of growing (recrystallizing) and swept (deformed) texture components. The number of components required (5-10) defines the order of the matrix since the kinetic coupling occurs between all recrystallizing and all deformed components. Each such couple is characterized by corresponding values for the nucleation energy and grain boundary mobility. The values of these parameters can be obtained by analytical or numerical coarse graining according to a renormalization scheme which replaces many individual grains which grow via recrystallization in a deformed texture component by a single equivalent recrystallization texture component or by fitting to experimental data. Each deformed component is further characterized by an average stored deformation energy. Each element of the kinetic matrix, reflecting one of the possible couplings between a deformed and a recrystallizing texture component, is then derived in each time step by a set of two differential equations. The first equation describes the thermally activated nucleation and growth processes for the expanded (free) volume for a particular couple of a deformed and a recrystallizing texture component and the second equation is used for calculating the constrained (real) volume for that couple which corrects the free volume for those portions of the deformation component which were already swept. The new method is particularly developed for the fast and physically based process simulation of recrystallization textures with respect to processing. The present paper introduces the method and applies it to the primary recrystallization of low carbon steels.

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

PubMed

Yang, Jiao; Grey, Kristin; Doney, John

2010-01-15

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

Manufacturing methods of a composite cell case for a Ni-Cd battery

NASA Technical Reports Server (NTRS)

Bauer, J. L.; Bogner, R. S.; Lowe, E. P.; Orlowski, E.

1979-01-01

Graphite epoxy material for a nickel cadmium battery cell case has been evaluated and determined to perform in the simulated environment of the battery. The basic manufacturing method requires refinement to demonstrate production feasibility. The various facets of production scale-up, i.e., process and tooling development together with material and process control, have been integrated into a comprehensive manufacturing process that assures production reproducibility and product uniformity. Test results substantiate that a battery cell case produced from graphite epoxy pre-impregnated material utilizing internal pressure bag fabrication method is feasible.

EXPERIMENTAL LIQUID METAL FUEL REACTOR

DOEpatents

Happell, J.J.; Thomas, G.R.; Denise, R.P.; Bunts, J.L. Jr.

1962-01-23

A liquid metal fuel nuclear fission reactor is designed in which the fissionable material is dissolved or suspended in a liquid metal moderator and coolant. The liquid suspension flows into a chamber in which a critical amount of fissionable material is obtained. The fluid leaves the chamber and the heat of fission is extracted for power or other utilization. The improvement is in the support arrangement for a segrnented graphite core to permit dif ferential thermal expansion, effective sealing between main and blanket liquid metal flows, and avoidance of excessive stress development in the graphite segments. (AEC)

Development of a Scanning Microscale Fast Neutron Irradiation Platform for Examining the Correlation Between Local Neutron Damage and Graphite Microstructure

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

Pinhero, Patrick; Windes, William

2015-03-10

The fast particle radiation damage effect of graphite, a main material in current and future nuclear reactors, has significant influence on the utilization of this material in fission and fusion plants. Atoms on graphite crystals can be easily replaced or dislocated by fast protons and result in interstitials and vacancies. The currently accepted model indicates that after most of the interstitials recombine with vacancies, surviving interstitials form clusters and furthermore gather to create loops with each other between layers. Meanwhile, surviving vacancies and interstitials form dislocation loops on the layers. The growth of these inserted layers cause the dimensional increase,more » i.e. swelling, of graphite. Interstitial and vacancy dislocation loops have been reported and they can easily been observed by electron microscope. However, observation of the intermediate atom clusters becomes is paramount in helping prove this model. We utilize fast protons generated from the University of Missouri Research Reactor (MURR) cyclotron to irradiate highly- oriented pyrolytic graphite (HOPG) as target for this research. Post-irradiation examination (PIE) of dosed targets with high-resolution transmission electron microscopy (HRTEM) has permit observation and analysis of clusters and dislocation loops to support the proposed theory. Another part of the research is to validate M.I. Heggie’s Ruck and Tuck model, which introduced graphite layers may fold under fast particle irradiation. Again, we employed microscopy to image irradiated specimens to determine how the extent of Ruck and Tuck by calculating the number of folds as a function of dose. Our most significant accomplishment is the invention of a novel class of high-intensity pure beta-emitters for long-term lightweight batteries. We have filed four invention disclosure records based on the research conducted in this project. These batteries are lightweight because they consist of carbon and tritium and can be fabricated to conform to many geometric shapes. In addition, we have published eight peer-reviewed American Nuclear Society (ANS) transactions, and presented our findings at ANS National Meetings, and several universities.« less

Pairing Heterocyclic Cations with closo-Icosahedral Borane and Carborane Anions, II: Benchtop Alternative Synthetic Methodologies for Binary Triazolium and Tetrazolium Salts with Significant Water Solubility (POSTPRINT)

DTIC Science & Technology

2012-01-01

interesting property, eutectic melting-point depression. Recrystallization of ternary salts 12–14 was not attempted because of a concern that a cation... recrystallization solvent mixture for these powders, and while some individual successes resulted, a general efficient solvent system for all salt...product recrystallizations could not be found. So, rather than recrystallizing each individual adduct, spectroscopic examination of the amorphous solids was

Effect of the Rate of Hot Compressive Deformation on the Kinetics of Dynamic and Static Recrystallization of Novel Medium-Carbon Medium-Alloy Steel

NASA Astrophysics Data System (ADS)

Khlusova, E. I.; Zisman, A. A.; Knyazyuk, T. V.; Novoskol'tsev, N. N.

2018-03-01

Dynamic and static recrystallization occurring under hot deformation at a rate of 1 and 100 sec - 1 in high-strength medium-carbon wear-resistant steels developed at CRISM "Prometey" for die forming of parts of driven elements of tillage machines is studied. The critical strain of dynamic recrystallization and the threshold temperatures and times of finish of static recrystallization are determined for the studied deformation rates at various temperatures.

Ultrasonic determination of recrystallization

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1986-01-01

Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and colume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.

Controlling conductivity of asphalt concrete with graphite.

DOT National Transportation Integrated Search

2014-08-01

Electrically conductive asphalt concrete has a huge potential for various multifunctional applications such as : self-healing, self-sensing, and deicing. In order to utilize the full spectrum of applications of electrically conductive : asphalt compo...

Simple, Green, and High-Yield Production of Boron-Based Nanostructures with Diverse Morphologies by Dissolution and Recrystallization of Layered Magnesium Diboride Crystals in Water.

PubMed

Gunda, Harini; Das, Saroj Kumar; Jasuja, Kabeer

2018-04-05

Layered metal diborides that contain metal atoms sandwiched between boron honeycomb planes offer a rich opportunity to access graphenic forms of boron. We recently demonstrated that magnesium diboride (MgB 2 ) could be exfoliated by ultrasonication in water to yield boron-based nanosheets. However, knowledge of the fate of metal boride crystals in aqueous phases is still in its incipient stages. This work presents our preliminary findings on the discovery that MgB 2 crystals can undergo dissolution in water under ambient conditions to result in precursors (prenucleation clusters) that, upon aging, undergo nonclassical crystallization preferentially growing in lateral directions by two-dimensional (2D) oriented attachment. We show that this recrystallization can be utilized as an avenue to obtain a high yield (≈92 %) of boron-based nanostructures, including nanodots, nanograins, nanoflakes, and nanosheets. These nanostructures comprise boron honeycomb planes chemically modified with hydride and oxy functional groups, which results in an overall negative charge on their surfaces. This ability of MgB 2 crystals to yield prenucleation clusters that can self-seed to form nanostructures comprising chemically modified boron honeycomb planes presents a new facet to the physicochemical interaction of MgB 2 with water. These findings also open newer avenues to obtain boron-based nanostructures with tunable morphologies by varying the chemical milieu during recrystallization. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Deformation Characteristics and Recrystallization Response of a 9310 Steel Alloy

NASA Astrophysics Data System (ADS)

Snyder, David; Chen, Edward Y.; Chen, Charlie C.; Tin, Sammy

2013-01-01

The flow behavior and recrystallization response of a 9310 steel alloy deformed in the ferrite temperature range were studied in this work. Samples were compressed under various conditions of strain (0.6, 0.8 and multi-axial), strain rate (10-4 seconds-1 to 10-1 seconds-1) and temperature [811 K to 1033 K (538 °C to 760 °C)] using a Gleeble thermo-mechanical simulator. Deformation was characterized by both qualitative and quantitative means, using standard microscopy, electron backscatter diffraction (EBSD) analysis and flow stress modeling. The results indicate that deformation is primarily accommodated through dynamic recovery in sub-grain formation. EBSD analysis shows a continuous increase in sub-grain boundary misorientation with increasing strain, ultimately producing recrystallized grains from the sub-grains at high strains. This suggests that a sub-grain rotation recrystallization mechanism predominates in this temperature range. Analyses of the results reveal a decreasing mean dynamically recrystallized grain size with increasing Zener-Hollomon parameter, and an increasing recrystallized fraction with increasing strain.

Glass-Transition Temperature of the β-Relaxation as the Major Predictive Parameter for Recrystallization of Neat Amorphous Drugs.

PubMed

Kissi, Eric Ofosu; Grohganz, Holger; Löbmann, Korbinian; Ruggiero, Michael T; Zeitler, J Axel; Rades, Thomas

2018-03-15

Recrystallization of amorphous drugs is currently limiting the simple approach to improve solubility and bioavailability of poorly water-soluble drugs by amorphization of a crystalline form of the drug. In view of this, molecular mobility, α-relaxation and β-relaxation processes with the associated transition temperatures T gα and T gβ , was investigated using dynamic mechanical analysis (DMA). The correlation between the transition temperatures and the onset of recrystallization for nine amorphous drugs, stored under dry conditions at a temperature of 296 K, was determined. From the results obtained, T gα does not correlate with the onset of recrystallization under the experimental storage conditions. However, a clear correlation between T gβ and the onset of recrystallization was observed. It is shown that at storage temperature below T gβ , amorphous nifedipine retains its amorphous form. On the basis of the correlation, an empirical correlation is proposed for predicting the onset of recrystallization for drugs stored at 0% RH and 296 K.

The deformation record of olivine in mylonitic peridotites from the Finero Complex, Ivrea Zone: Separate deformation cycles during exhumation

NASA Astrophysics Data System (ADS)

Matysiak, Agnes K.; Trepmann, Claudia A.

2015-12-01

Mylonitic peridotites from the Finero complex are investigated to detect characteristic olivine microfabrics that can resolve separate deformation cycles at different metamorphic conditions. The heterogeneous olivine microstructures are characterized by deformed porphyroclasts surrounded by varying amounts of recrystallized grains. A well-developed but only locally preserved foam structure is present in recrystallized grain aggregates. This indicates an early stage of dynamic recrystallization and subsequent recovery and recrystallization at quasi-static stress conditions, where the strain energy was reduced such that a reduction in surface energy controlled grain boundary migration. Ultramylonites record a renewed stage of localized deformation and recrystallization by a second generation of recrystallized grains that do not show a foam structure. This second generation of recrystallized grains as well as sutured grain and kink band boundaries of porphyroclasts indicate that these microstructures developed during a stage of localized deformation after development of the foam structure. The heterogeneity of the microfabrics is interpreted to represent several (at least two) cycles of localized deformation separated by a marked hiatus with quasi-static recrystallization and recovery and eventually grain growth. The second deformation cycle did not only result in reactivation of preexisting shear zones but instead also locally affected the host rock that was not deformed in the first stage. Such stress cycles can result from sudden increases in differential stress imposed by seismic events, i.e., high stress-loading rates, during exhumation of the Finero complex.

Experimental and Modeling Characterization of PETN Mobilization Mechanisms During Recrystallization at Ambient Conditions

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

Burnham, A K; Gee, R; Maiti, A

2005-11-03

Experimental measurements suggest that pentaerythritoltetranitrate (PETN) undergoes changes at the molecular level that cause macroscopic changes in the overall PETN powder characteristics over time. These changes have been attributed to the high molecular mobility of PETN, but the underlying mechanism(s) responsible for this redistribution are still uncertain. Two basic approaches have been implemented in the past year to provide insight into the nature of these underlying mechanisms. The first approach is of an experimental nature, utilizing both AFM and evaporation measurements, which address both surface mobility and evaporation. These data include AFM measurements performed at LLNL and evaporation rate measurementsmore » performed at Texas Tech. These results are compared to earlier vapor pressure measurements performed at SNL, and estimates of recrystallization time frames are given. The second approach utilizes first-principle calculations and simulations that will be used to compare directly to those experimental quantities measured. We are developing an accurate intermolecular potential for PETN, which via kinetic Monte Carlo (KMC) simulations would mimic real crystallite shapes. Once the basic theory is in place for the growth of single crystallites, we will be in a position to investigate realistic grain coarsening phenomena in multi-crystallite simulations. This will also enable us to study how to control the morphological evolution, e.g., through thermal cycling, or through the action of custom additives and impurities.« less

Kinetics of solvent supported tubule formation of Lotus (Nelumbo nucifera) wax on highly oriented pyrolytic graphite (HOPG) investigated by atomic force microscopy

PubMed Central

Koch, Kerstin; Barthlott, Wilhelm; Wandelt, Klaus

2018-01-01

The time dependence of the formation of lotus wax tubules after recrystallization from various chloroform-based solutions on an HOPG surface at room temperature was studied by atomic force microscopy (magnetic AC mode) taking series of consecutive images of the formation process. The growth of the tubules oriented in an upright fashion follows a sequential rodlet→ring→tubule behavior. The influence of a number of factors, e.g., different wax concentration in chloroform, the additional presence of water, or salts [(NH4)2SO4, NH4NO3] or a mixture of salt/water in the solution on the growth rate and orientation of the tubules is also investigated. Different wax concentrations were found to have no effect on the growth rate or the orientation of tubules in none of the solutions. The presence of water, however, considerably increased the growth rate of tubule formation, while the presence of salt was again found to have no effect on growth rate or orientation of tubules. PMID:29515959

Camphor-mediated synthesis of carbon nanoparticles, graphitic shell encapsulated carbon nanocubes and carbon dots for bioimaging

PubMed Central

Oza, Goldie; Ravichandran, M.; Merupo, Victor-Ishrayelu; Shinde, Sachin; Mewada, Ashmi; Ramirez, Jose Tapia; Velumani, S.; Sharon, Madhuri; Sharon, Maheshwar

2016-01-01

A green method for an efficient synthesis of water-soluble carbon nanoparticles (CNPs), graphitic shell encapsulated carbon nanocubes (CNCs), Carbon dots (CDs) using Camphor (Cinnamomum camphora) is demonstrated. Here, we describe a competent molecular fusion and fission route for step-wise synthesis of CDs. Camphor on acidification and carbonization forms CNPs, which on alkaline hydrolysis form CNCs that are encapsulated by thick graphitic layers and on further reduction by sodium borohydride yielded CDs. Though excitation wavelength dependent photoluminescence is observed in all the three carbon nanostructures, CDs possess enhanced photoluminescent properties due to more defective carbonaceous structures. The surface hydroxyl and carboxyl functional groups make them water soluble in nature. They possess excellent photostability, higher quantum yield, increased absorption, decreased cytotoxicity and hence can be utilized as a proficient bio imaging agent. PMID:26905737

Camphor-mediated synthesis of carbon nanoparticles, graphitic shell encapsulated carbon nanocubes and carbon dots for bioimaging

NASA Astrophysics Data System (ADS)

Oza, Goldie; Ravichandran, M.; Merupo, Victor-Ishrayelu; Shinde, Sachin; Mewada, Ashmi; Ramirez, Jose Tapia; Velumani, S.; Sharon, Madhuri; Sharon, Maheshwar

2016-02-01

A green method for an efficient synthesis of water-soluble carbon nanoparticles (CNPs), graphitic shell encapsulated carbon nanocubes (CNCs), Carbon dots (CDs) using Camphor (Cinnamomum camphora) is demonstrated. Here, we describe a competent molecular fusion and fission route for step-wise synthesis of CDs. Camphor on acidification and carbonization forms CNPs, which on alkaline hydrolysis form CNCs that are encapsulated by thick graphitic layers and on further reduction by sodium borohydride yielded CDs. Though excitation wavelength dependent photoluminescence is observed in all the three carbon nanostructures, CDs possess enhanced photoluminescent properties due to more defective carbonaceous structures. The surface hydroxyl and carboxyl functional groups make them water soluble in nature. They possess excellent photostability, higher quantum yield, increased absorption, decreased cytotoxicity and hence can be utilized as a proficient bio imaging agent.

Lifetime experimental study of graphite cathode for relativistic backward wave oscillator

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

Wu, Ping; Science and Technology on High Power Microwave Laboratory, Northwest Institute of Nuclear Technology, Xi'an 710024; Sun, Jun

2016-07-21

Graphite cathodes are widely used due to their good emission properties, especially their long lifetime. Some previous papers have researched their lifetime under certain conditions and uncovered some important phenomena. This paper is dedicated to research the lifetime of the graphite cathode under higher power. In the lifetime test, the voltage and current amplitudes are about 970 kV and 9.7 kA, respectively. The repetition rate is 20 Hz. An X-band relativistic backward wave oscillator is used to generate high power microwave by utilizing the electron beam energy. The experimental results demonstrate that the emission property of the graphite cathode remains quite stable duringmore » 10{sup 5} pulses, despite some slight deteriorations regarding the beam and microwave parameters. The macroscopic morphology change of the cathode blade due to material evaporation is observed by a laser microscope. The mass loss of the graphite cathode is about 60 μg/C. Meanwhile, the observation by a scanning electron microscope uncovers that the original numerous flaky micro-structures are totally replaced by a relatively smooth surface at the mid region of the cathode blade and a large number of new micro-protrusions at the blade edges during the lifetime test.« less

DNA Origami Reorganizes upon Interaction with Graphite: Implications for High-Resolution DNA Directed Protein Patterning

PubMed Central

Rahman, Masudur; Neff, David; Green, Nathaniel; Norton, Michael L.

2016-01-01

Although there is a long history of the study of the interaction of DNA with carbon surfaces, limited information exists regarding the interaction of complex DNA-based nanostructures with the important material graphite, which is closely related to graphene. In view of the capacity of DNA to direct the assembly of proteins and optical and electronic nanoparticles, the potential for combining DNA-based materials with graphite, which is an ultra-flat, conductive carbon substrate, requires evaluation. A series of imaging studies utilizing Atomic Force Microscopy has been applied in order to provide a unified picture of this important interaction of structured DNA and graphite. For the test structure examined, we observe a rapid destabilization of the complex DNA origami structure, consistent with a strong interaction of single-stranded DNA with the carbon surface. This destabilizing interaction can be obscured by an intentional or unintentional primary intervening layer of single-stranded DNA. Because the interaction of origami with graphite is not completely dissociative, and because the frustrated, expanded structure is relatively stable over time in solution, it is demonstrated that organized structures of pairs of the model protein streptavidin can be produced on carbon surfaces using DNA origami as the directing material. PMID:28335324

Proton irradiated graphite grades for a long baseline neutrino facility experiment

NASA Astrophysics Data System (ADS)

Simos, N.; Nocera, P.; Zhong, Z.; Zwaska, R.; Mokhov, N.; Misek, J.; Ammigan, K.; Hurh, P.; Kotsina, Z.

2017-07-01

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) four graphite grades were irradiated with protons in the energy range of 140-180 MeV, to peak fluence of ˜6.1 ×1020 p /cm2 and irradiation temperatures between 120 - 200 °C . The test array included POCO ZXF-5Q, Toyo-Tanso IG 430, Carbone-Lorraine 2020 and SGL R7650 grades of graphite. Irradiation was performed at the Brookhaven Linear Isotope Producer. Postirradiation analyses were performed with the objective of (a) comparing their response under the postulated irradiation conditions to guide a graphite grade selection for use as a pion target and (b) understanding changes in physical and mechanical properties as well as microstructure that occurred as a result of the achieved fluence and in particular at this low-temperature regime where pion graphite targets are expected to operate. A further goal of the postirradiation evaluation was to establish a proton-neutron correlation damage on graphite that will allow for the use of a wealth of available neutron-based damage data in proton-based studies and applications. Macroscopic postirradiation analyses as well as energy dispersive x-ray diffraction of 200 KeV x rays at the NSLS synchrotron of Brookhaven National Laboratory were employed. The macroscopic analyses revealed differences in the physical and strength properties of the four grades with behavior however under proton irradiation that qualitatively agrees with that reported for graphite under neutrons for the same low temperature regime and in particular the increase of thermal expansion, strength and Young's modulus. The proton fluence level of ˜1020 cm-2 where strength reaches a maximum before it begins to decrease at higher fluences has been identified and it agrees with neutron-induced changes. X-ray diffraction analyses of the proton irradiated graphite revealed for the first time the similarity in microstructural graphite behavior to that under neutron irradiation and the agreement between the fluence threshold of ˜5 ×1020 cm-2 where the graphite lattice undergoes a dramatic change. The confirmed similarity in behavior and agreement in threshold fluences for proton and neutron irradiation effects on graphite reported for the first time in this study will enable the safe utilization of the wealth of neutron irradiation data on graphite that extends to much higher fluences and different temperature regimes by the proton accelerator community searching for multi-MW graphite targets.

Proton irradiated graphite grades for a long baseline neutrino facility experiment

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

Simos, N.; Nocera, P.; Zhong, Z.

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) four graphite grades were irradiated with protons in the energy range of 140–180 MeV, to peak fluence of ~6.1×10 20 p/cm 2 and irradiation temperatures between 120–200 °C. The test array included POCO ZXF-5Q, Toyo-Tanso IG 430, Carbone-Lorraine 2020 and SGL R7650 grades of graphite. Irradiation was performed at the Brookhaven Linear Isotope Producer. Postirradiation analyses were performed with the objective of (a) comparing their response under the postulated irradiation conditions to guide a graphite grade selection for use asmore » a pion target and (b) understanding changes in physical and mechanical properties as well as microstructure that occurred as a result of the achieved fluence and in particular at this low-temperature regime where pion graphite targets are expected to operate. A further goal of the postirradiation evaluation was to establish a proton-neutron correlation damage on graphite that will allow for the use of a wealth of available neutron-based damage data in proton-based studies and applications. Macroscopic postirradiation analyses as well as energy dispersive x-ray diffraction of 200 KeV x rays at the NSLS synchrotron of Brookhaven National Laboratory were employed. The macroscopic analyses revealed differences in the physical and strength properties of the four grades with behavior however under proton irradiation that qualitatively agrees with that reported for graphite under neutrons for the same low temperature regime and in particular the increase of thermal expansion, strength and Young’s modulus. The proton fluence level of ~10 20 cm -2 where strength reaches a maximum before it begins to decrease at higher fluences has been identified and it agrees with neutron-induced changes. X-ray diffraction analyses of the proton irradiated graphite revealed for the first time the similarity in microstructural graphite behavior to that under neutron irradiation and the agreement between the fluence threshold of ~5×10 20 cm -2 where the graphite lattice undergoes a dramatic change. The confirmed similarity in behavior and agreement in threshold fluences for proton and neutron irradiation effects on graphite reported for the first time in this study will enable the safe utilization of the wealth of neutron irradiation data on graphite that extends to much higher fluences and different temperature regimes by the proton accelerator community searching for multi-MW graphite targets.« less

Proton irradiated graphite grades for a long baseline neutrino facility experiment

DOE PAGES

Simos, N.; Nocera, P.; Zhong, Z.; ...

2017-07-24

In search of a low-Z pion production target for the Long Baseline Neutrino Facility (LBNF) of the Deep Underground Neutrino Experiment (DUNE) four graphite grades were irradiated with protons in the energy range of 140–180 MeV, to peak fluence of ~6.1×10 20 p/cm 2 and irradiation temperatures between 120–200 °C. The test array included POCO ZXF-5Q, Toyo-Tanso IG 430, Carbone-Lorraine 2020 and SGL R7650 grades of graphite. Irradiation was performed at the Brookhaven Linear Isotope Producer. Postirradiation analyses were performed with the objective of (a) comparing their response under the postulated irradiation conditions to guide a graphite grade selection for use asmore » a pion target and (b) understanding changes in physical and mechanical properties as well as microstructure that occurred as a result of the achieved fluence and in particular at this low-temperature regime where pion graphite targets are expected to operate. A further goal of the postirradiation evaluation was to establish a proton-neutron correlation damage on graphite that will allow for the use of a wealth of available neutron-based damage data in proton-based studies and applications. Macroscopic postirradiation analyses as well as energy dispersive x-ray diffraction of 200 KeV x rays at the NSLS synchrotron of Brookhaven National Laboratory were employed. The macroscopic analyses revealed differences in the physical and strength properties of the four grades with behavior however under proton irradiation that qualitatively agrees with that reported for graphite under neutrons for the same low temperature regime and in particular the increase of thermal expansion, strength and Young’s modulus. The proton fluence level of ~10 20 cm -2 where strength reaches a maximum before it begins to decrease at higher fluences has been identified and it agrees with neutron-induced changes. X-ray diffraction analyses of the proton irradiated graphite revealed for the first time the similarity in microstructural graphite behavior to that under neutron irradiation and the agreement between the fluence threshold of ~5×10 20 cm -2 where the graphite lattice undergoes a dramatic change. The confirmed similarity in behavior and agreement in threshold fluences for proton and neutron irradiation effects on graphite reported for the first time in this study will enable the safe utilization of the wealth of neutron irradiation data on graphite that extends to much higher fluences and different temperature regimes by the proton accelerator community searching for multi-MW graphite targets.« less

Matrix recrystallization for MALDI-MS imaging of maize lipids at high-spatial resolution

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

Duenas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Furthermore, using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution.

Matrix recrystallization for MALDI-MS imaging of maize lipids at high-spatial resolution

DOE PAGES

Duenas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

2016-06-27

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Furthermore, using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution.

Matrix Recrystallization for MALDI-MS Imaging of Maize Lipids at High-Spatial Resolution

NASA Astrophysics Data System (ADS)

Dueñas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

2016-09-01

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution.

Correlation buildup during recrystallization in three-dimensional dusty plasma clusters

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

Schella, André; Mulsow, Matthias; Melzer, André

2014-05-15

The recrystallization process of finite three-dimensional dust clouds after laser heating is studied experimentally. The time-dependent Coulomb coupling parameter is presented, showing that the recrystallization starts with an exponential cooling phase where cooling is slower than damping by the neutral gas friction. At later times, the coupling parameter oscillates into equilibrium. It is found that a large fraction of cluster states after recrystallization experiments is in metastable states. The temporal evolution of the correlation buildup shows that correlation occurs on even slower time scale than cooling.

Matrix Recrystallization for MALDI-MS Imaging of Maize Lipids at High-Spatial Resolution.

PubMed

Dueñas, Maria Emilia; Carlucci, Laura; Lee, Young Jin

2016-09-01

Matrix recrystallization is optimized and applied to improve lipid ion signals in maize embryos and leaves. A systematic study was performed varying solvent and incubation time. During this study, unexpected side reactions were found when methanol was used as a recrystallization solvent, resulting in the formation of a methyl ester of phosphatidic acid. Using an optimum recrystallization condition with isopropanol, there is no apparent delocalization demonstrated with a transmission electron microscopy (TEM) pattern and maize leaf images obtained at 10 μm spatial resolution. Graphical Abstract ᅟ.

Ultrasonic attenuation measurements determine onset, degree, and completion of recrystallization

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1988-01-01

Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and volume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.

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

Zhang, Y. B.; Budai, J. D.; Tischler, J. Z.

How boundaries surrounding recrystallization grains migrate through the 3D network of dislocation boundaries in deformed crystalline materials is unknown and critical for the resulting recrystallized crystalline materials. Furthermore, by using X-ray Laue diffraction microscopy, we show for the first time the migration pattern of a typical recrystallization boundary through a well-characterized deformation matrix. The data provide a unique possibility to investigate effects of both boundary misorientation and plane normal on the migration, information which cannot be accessed with any other techniques. Our results show that neither of these two parameters can explain the observed migration behavior. Instead we suggest thatmore » the subdivision of the deformed microstructure ahead of the boundary plays the dominant role. Our experimental observations challenge the assumptions of existing recrystallization theories, and set the stage for determination of mobilities of recrystallization boundaries.« less

Grain Boundary Evolution of Cold-Rolled FePd Alloy during Recrystallization at Disordering Temperature

PubMed Central

Lin, Hung-Pin; Chen, Delphic; Kuo, Jui-Chao

2015-01-01

In this study, the grain boundary character and texture of 50% and 90% cold-rolled FePd alloy was investigated during recrystallization at 700 °C. Electron backscatter diffraction (EBSD) measurements were performed on the rolling direction to normal direction section. Kernel average misorientation (KAM) calculated from EBSD measurements was employed to determine the recrystallization fraction. The Avrami exponent n of recrystallization is 1.9 and 4.9 for 50% and 90% cold rolling, respectively. The new formation of texture reveals random texture during the recrystallization process. As annealing time increased, the number of high angle boundary (HAGB) and coincidence site lattice (CSL) increased with consumption of low angle boundary (LAGB). In addition, possible transformations between different grain boundaries are observed here.

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

Wang, Kun; Bannister, Mark E.; Meyer, Fred W.

Here, in a magnetic fusion energy (MFE) device, the plasma-facing materials (PFMs) will be subjected to tremendous fluxes of ions, heat, and neutrons. The response of PFMs to the fusion environment is still not well defined. Tungsten metal is the present candidate of choice for PFM applications such as the divertor in ITER. However, tungsten's microstructure will evolve in service, possibly to include recrystallization. How tungsten's response to plasma exposure evolves with changes in microstructure is presently unknown. In this work, we have exposed hot-worked and recrystallized tungsten to an 80 eV helium ion beam at a temperature of 900more » °C to fluences of 2 × 10 23 or 20 × 10 23 He/m 2. This resulted in a faceted surface structure at the lower fluence or short but well-developed nanofuzz structure at the higher fluence. There was little difference in the hot-rolled or recrystallized material's near-surface (≤50 nm) bubbles at either fluence. At higher fluence and deeper depth, the bubble populations of the hot-rolled and recrystallized were different, the recrystallized being larger and deeper. This may explain previous high-fluence results showing pronounced differences in recrystallized material. The deeper penetration in recrystallized material also implies that grain boundaries are traps, rather than high-diffusivity paths.« less

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

DOE PAGES

Aydogan, E.; El-Atwani, O.; Takajo, S.; ...

2018-02-09

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

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

Aydogan, E.; El-Atwani, O.; Takajo, S.

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less

Recrystallization and grain growth behavior of rolled tungsten under VDE-like short pulse high heat flux loads

NASA Astrophysics Data System (ADS)

Yuan, Y.; Greuner, H.; Böswirth, B.; Krieger, K.; Luo, G.-N.; Xu, H. Y.; Fu, B. Q.; Li, M.; Liu, W.

2013-02-01

Short pulse heat loads expected for vertical displacement events (VDEs) in ITER were applied in the high heat flux (HHF) test facility GLADIS at IPP-Garching onto samples of rolled W. Pulsed neutral beams with the central heat flux of 23 MW/m2 were applied for 0.5, 1.0 and 1.5 s, respectively. Rapid recrystallization of the adiabatically loaded 3 mm thick samples was observed when the pulse duration was up to 1.0 s. Grains grew markedly following recrystallization with increasing pulse length. The recrystallization temperature and temperature dependence of the recrystallized grain size were also investigated. The results showed that the recrystallization temperature of the W grade was around 2480 °C under the applied heat loading condition, which was nearly 1150 °C higher than the conventional recrystallization temperature, and the grains were much finer. A linear relationship between the logarithm of average grain size (ln d) and the inverse of maximum surface temperature (1/Tmax) was found and accordingly the activation energy for grain growth in temperature evolution up to Tmax in 1.5 s of the short pulse HHF load was deduced to be 4.1 eV. This provided an effective clue to predict the structure evolution under short pulse HHF loads.

Compression failure mechanisms of composite structures

NASA Technical Reports Server (NTRS)

Hahn, H. T.; Sohi, M.; Moon, S.

1986-01-01

An experimental and analytical study was conducted to delineate the compression failure mechanisms of composite structures. The present report summarizes further results on kink band formation in unidirectional composites. In order to assess the compressive strengths and failure modes of fibers them selves, a fiber bundle was embedded in epoxy casting and tested in compression. A total of six different fibers were used together with two resins of different stiffnesses. The failure of highly anisotropic fibers such as Kevlar 49 and P-75 graphite was due to kinking of fibrils. However, the remaining fibers--T300 and T700 graphite, E-glass, and alumina--failed by localized microbuckling. Compressive strengths of the latter group of fibers were not fully utilized in their respective composite. In addition, acoustic emission monitoring revealed that fiber-matrix debonding did not occur gradually but suddenly at final failure. The kink band formation in unidirectional composites under compression was studied analytically and through microscopy. The material combinations selected include seven graphite/epoxy composites, two graphite/thermoplastic resin composites, one Kevlar 49/epoxy composite and one S-glass/epoxy composite.

Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries

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

Wang , Jing; Bao, Wurigumula; Ma, Lu

2015-11-09

Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide–nickel–graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx/Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stickmore » well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx/Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials.« less

Scalable Preparation of Ternary Hierarchical Silicon Oxide-Nickel-Graphite Composites for Lithium-Ion Batteries.

PubMed

Wang, Jing; Bao, Wurigumula; Ma, Lu; Tan, Guoqiang; Su, Yuefeng; Chen, Shi; Wu, Feng; Lu, Jun; Amine, Khalil

2015-12-07

Silicon monoxide is a promising anode candidate because of its high theoretical capacity and good cycle performance. To solve the problems associated with this material, including large volume changes during charge-discharge processes, we report a ternary hierarchical silicon oxide-nickel-graphite composite prepared by a facile two-step ball-milling method. The composite consists of nano-Si dispersed silicon oxides embedded in nano-Ni/graphite matrices (Si@SiOx /Ni/graphite). In the composite, crystalline nano-Si particles are generated by the mechanochemical reduction of SiO by ball milling with Ni. These nano-Si dispersed oxides have abundant electrochemical activity and can provide high Li-ion storage capacity. Furthermore, the milled nano-Ni/graphite matrices stick well to active materials and interconnect to form a crosslinked framework, which functions as an electrical highway and a mechanical backbone so that all silicon oxide particles become electrochemically active. Owing to these advanced structural and electrochemical characteristics, the composite enhances the utilization efficiency of SiO, accommodates its large volume expansion upon cycling, and has good ionic and electronic conductivity. The composite electrodes thus exhibit substantial improvements in electrochemical performance. This ternary hierarchical Si@SiOx /Ni/graphite composite is a promising candidate anode material for high-energy lithium-ion batteries. Additionally, the mechanochemical ball-milling method is low cost and easy to reproduce, indicating potential for the commercial production of the composite materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Automatic twin vessel recrystallizer. Effective purification of acetaminophen by successive automatic recrystallization and absolute determination of purity by DSC.

PubMed

Nara, Osamu

2011-01-24

I describe an interchangeable twin vessel (J, N) automatic glass recrystallizer that eliminates the time-consuming recovery and recycling of crystals for repeated recrystallization. The sample goes in the dissolution vessel J containing a magnetic stir-bar K; J is clamped to the upper joint H of recrystallizer body D. Empty crystallization vessel N is clamped to the lower joint M. Pure solvent is delivered to the dissolution vessel and the crystallization vessel via the head of the condenser A. Crystallization vessel is heated (P). The dissolution reservoir is stirred and heated by the solvent vapor (F). Continuous outflow of filtrate E out of J keeps N at a stable boiling temperature. This results in efficient dissolution, evaporation and separation of pure crystals Q. Pure solvent in the dissolution reservoir is recovered by suction. Empty dissolution and crystallization vessels are detached. Stirrer magnet is transferred to the crystallization vessel and the role of the vessels are then reversed. Evacuating mother liquor out of the upper twin vessel, the apparatus unit is ready for the next automatic recrystallization by refilling twin vessels with pure solvent. We show successive automatic recrystallization of acetaminophen from diethyl ether obtaining acetaminophen of higher melting temperatures than USP and JP reference standards by 8× automatic recrystallization, 96% yield at each stage. Also, I demonstrate a novel approach to the determination of absolute purity by combining the successive automatic recrystallization with differential scanning calorimetry (DSC) measurement requiring no reference standards. This involves the measurement of the criterial melting temperature T(0) corresponding to the 100% pure material and quantitative ΔT in DSC based on the van't Hoff law of melting point depression. The purity of six commercial acetaminophen samples and reference standards and an eight times recrystallized product evaluated were 98.8 mol%, 97.9 mol%, 99.1 mol%, 98.3 mol%, 98.4 mol%, 98.5 mol% and 99.3 mol% respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

The risk of recrystallization: changes to the toxicity and morphology of pyrimethamine.

PubMed

Perold, Zak; Caira, Mino R; Brits, Marius

2014-01-01

Pyrimethamine, an anti-malarial agent known to exhibit solid state polymorphism, may be purified by means of recrystallization. Recrystallization may alter the solid state chemistry of pharmaceuticals, which may impact the toxicity and/or manufacturability thereof. We evaluated the risks associated with the recrystallization of pyrimethamine. Pyrimethamine was recrystallized using several organic solvents. X-ray diffraction, thermal analysis, infra-red spectroscopy, microscopy, flowability -, solubility and dissolution testing as well as computational work were employed to evaluate the recrystallized products. A toxic solvatomorph of pyrimethamine (Pyr-MeOH) was found to be the product from methanol recrystallization. The elucidation of - and the elaboration on the unique characteristics of Pyr-MeOH provides the pharmaceutical industry with several means to identify Pyr-MeOH and to distinguish it from the pharmaceutically preferred anhydrous form (Pyr). Thermal methods of analysis found that the toxicity of Pyr-MeOH may be reversed by overcoming a desolvation activation energy of 148 kJ/mol. In addition it was found that recrystallization altered the morphology of Pyr. Angle of repose and tapped density determinations identified that the different morphologies of Pyr displayed differences in powder flow and compressibility behaviour and In Silico calculations were successful in rendering morphologies resembling that found experimentally. We present a solvatomorph of pyrimethamine and provide several characteristic means to identify this unwanted toxic form and quantified the energy required to overcome its toxicity. In addition we describe that Pyr may present in different morphologies and show how it may impact the manufacturability thereof.

Development of a Muon Rotating Target for J-PARC/MUSE

NASA Astrophysics Data System (ADS)

Makimura, Shunsuke; Kobayashi, Yasuo; Miyake, Yasuhiro; Kawamura, Naritoshi; Strasser, Patrick; Koda, Akihiro; Shimomura, Koichiro; Fujimori, Hiroshi; Nishiyama, Kusuo; Kato, Mineo; Kojima, Kenji; Higemoto, Wataru; Ito, Takashi; Shimizu, Ryou; Kadono, Ryosuke

At the J-PARC muon science facility (J-PARC/MUSE), a graphite target with a thickness of 20 mm has been used in vacuum to obtain an intense pulsed muon beam from the RCS 3-GeV proton beam [1], [2]. In the current design, the target frame is constructed using copper with a stainless steel tube embedded for water cooling. The energy deposited by the proton beam at 1 MW is evaluated to be 3.3 kW on the graphite target and 600 W on the copper frame by a Monte-Carlo simulation code, PHITS [3]. Graphite materials are known to lose their crystal structure and can be shrunk under intense proton beam irradiation. Consequently, the lifetime of the muon target is essentially determined by the radiation damage in graphite, and is evaluated to be half a year [4]. Hence, we are planning to distribute the radiation damage by rotating a graphite wheel. Although the lifetime of graphite in this case will be more than 10 years, the design of the bearing must be carefully considered. Because the bearing in JPARC/MUSE is utilized in vacuum, under high radiation, and at high temperature, an inorganic and solid lubricant must be applied to the bearing. Simultaneously, the temperature of the bearing must also be decreased to extend the lifetime. In 2009, a mock-up of the Muon Rotating Target, which could heat up and rotate a graphite wheel, was fabricated. Then several tests were started to select the lubricant and to determine the structure of the Muon Rotating Target, the control system and so on. In this report, the present status of the Muon Rotating Target for J-PARC/MUSE, especially the development of a rotation system in vacuum, is described.

Analysis of Particle-Stimulated Nucleation (PSN)-Dominated Recrystallization for Hot-Rolled 7050 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Adam, Khaled F.; Long, Zhengdong; Field, David P.

2017-04-01

In 7xxx series aluminum alloys, the constituent large and small second-phase particles present during deformation process. The fraction and spatial distribution of these second-phase particles significantly influence the recrystallized structure, kinetics, and texture in the subsequent treatment. In the present work, the Monte Carlo Potts model was used to model particle-stimulated nucleation (PSN)-dominated recrystallization and grain growth in high-strength aluminum alloy 7050. The driving force for recrystallization is deformation-induced stored energy, which is also strongly affected by the coarse particle distribution. The actual microstructure and particle distribution of hot-rolled plate were used as an initial point for modeling of recrystallization during the subsequent solution heat treatment. Measurements from bright-field TEM images were performed to enhance qualitative interpretations of the developed microstructure. The influence of texture inhomogeneity has been demonstrated from a theoretical point of view using pole figures. Additionally, in situ annealing measurements in SEM were performed to track the orientational and microstructural changes and to provide experimental support for the recrystallization mechanism of PSN in AA7050.

Facile synthesis of hollow zeolite microspheres through dissolution–recrystallization procedure in the presence of organosilanes

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

Tao, Haixiang; Ren, Jiawen; Liu, Xiaohui

2013-04-15

Hollow zeolite microspheres have been hydrothermally synthesized in the presence of organosilanes via a dissolution–recrystallization procedure. In the presence of organosilanes, zeolite particles with a core/shell structure formed at the first stage of hydrothermal treatment, then the core was consumed and recrystallized into zeolite framework to form the hollow structure during the second hydrothermal process. The influence of organosilanes was discussed, and a related dissolution–recrystallization mechanism was proposed. In addition, the hollow zeolite microspheres exhibited an obvious advantage in catalytic reactions compared to conventional ZSM-5 catalysts, such as in the alkylation of toluene with benzyl chloride. - Graphical abstract: Hollowmore » zeolite spheres with aggregated zeolite nanocrystals were synthesized via a dissolution–recrystallization procedure in the presence of organosiline. Highlights: ► Hollow zeolite spheres with aggregated zeolite nanocrystals were synthesized via a dissolution–recrystallization procedure. ► Organosilane influences both the morphology and hollow structure of zeolite spheres. ► Hollow zeolite spheres showed an excellent catalytic performance in alkylation of toluene with benzyl chloride.« less

A fluorescent graphitic carbon nitride nanosheet biosensor for highly sensitive, label-free detection of alkaline phosphatase.

PubMed

Xiang, Mei-Hao; Liu, Jin-Wen; Li, Na; Tang, Hao; Yu, Ru-Qin; Jiang, Jian-Hui

2016-02-28

Graphitic C3N4 (g-C3N4) nanosheets provide an attractive option for bioprobes and bioimaging applications. Utilizing highly fluorescent and water-dispersible ultrathin g-C3N4 nanosheets, a highly sensitive, selective and label-free biosensor has been developed for ALP detection for the first time. The developed approach utilizes a natural substrate of ALP in biological systems and thus affords very high catalytic efficiency. This novel biosensor is demonstrated to enable quantitative analysis of ALP in a wide range from 0.1 to 1000 U L(-1) with a low detection limit of 0.08 U L(-1), which is among the most sensitive assays for ALP. It is expected that the developed method may provide a low-cost, convenient, rapid and highly sensitive platform for ALP-based clinical diagnostics and biomedical applications.

Effect of Prestraining of Recrystallization Temperature and Mechanical Properties of Commercial, Sintered, Wrought Molybdenum

NASA Technical Reports Server (NTRS)

Dike, Kenneth C; Long, Roger A

1953-01-01

Given three presumably identical lots of commercial, sintered, wrought molybdenum, the 1-hour recrystallization temperature of one lot remained above 2900 F by limiting the amount of effective restraining to 35 percent or less. Different recrystallization temperatures were obtained in various atmospheres, the highest in argon and the lowest in hydrogen. Metal thus fabricated and then stress-relieved possessed an ultimate tensile strength at room temperature within 10 percent of metal swaged 99 percent and also possessed equivalent ductility. At 1800 F, equivalent strength and ductility was obtained irrespective of the amount of swaging over the range of 10 to 99 percent. The amount of swaging greatly influenced the recrystallized grain size but the difference in grain size is not the major controlling factor which determines whether recrystallized molybdenum is ductile or brittle at room temperature.

Optimum rolling ratio for obtaining {001}<110> recrystallization texture in Ti-Nb-Al biomedical shape memory alloy.

PubMed

Inamura, T; Shimizu, R; Kim, H Y; Miyazaki, S; Hosoda, H

2016-04-01

The rolling rate (r) dependence of textures was investigated in the Ti-26Nb-3Al (mol%) alloy to reveal the conditions required to form the {001}<110> recrystallization texture, which is a desirable orientation for the β-titanium shape memory alloy. {001}<110> was the dominant cold-rolling texture when r=90% and it was transferred to the recrystallization texture without forming {112}<110>, which is detrimental for the isotropic mechanical properties of the rolled sheet. A further increase in r resulted in the formation of {112}<110> in both rolling and recrystallization textures. Therefore, r should be controlled to form only the {001}<110> rolling texture, because the {112}<110> texture can overwhelm the {001}<110> texture during recrystallization. Copyright © 2016 Elsevier B.V. All rights reserved.

Mineralogy of chondritic interplanetary dust particle impact residues from LDEF

NASA Technical Reports Server (NTRS)

Barrett, R. A.; Zolensky, M. E.; Bernhard, R.

1993-01-01

A detailed structural and compositional analysis of several impactor residues was performed utilizing transmission electron microscopy, energy dispersive spectroscopy, and electron diffraction. Residues from the interior of several craters in gold surfaces were removed with a tungsten needle, mounted in EMBED-812 epoxy, and ultramicrotomed. The presence in these residues of equilibrated ferromagnesian minerals, recrystallization textures, glass, and melted metal and sulfide bodies decorating grain boundaries is indicative of varying degrees of shock metamorphism in all impact residues we have characterized.

Mixed polyvalent-monovalent metal coating for carbon-graphite fibers

NASA Technical Reports Server (NTRS)

Harper-Tervet, J.; Tervet, F. W.; Humphrey, M. F. (Inventor)

1982-01-01

An improved coating of gasification catalyst for carbon-graphite fibers is provided comprising a mixture of a polyvalent metal such as calcium and a monovalent metal such as lithium. The addition of lithium provides a lighter coating and a more flexible coating when applied to a coating of a carboxyl containing resin such as polyacrylic acid since it reduces the crosslink density. Furthermore, the presence of lithium provides a glass-like substance during combustion which holds the fiber together resulting in slow, even combustion with much reduced evolution of conductive fragments. The coated fibers are utilized as fiber reinforcement for composites.

Humidifier for fuel cell using high conductivity carbon foam

DOEpatents

Klett, James W.; Stinton, David P.

2006-12-12

A method and apparatus of supplying humid air to a fuel cell is disclosed. The extremely high thermal conductivity of some graphite foams lends itself to enhance significantly the ability to humidify supply air for a fuel cell. By utilizing a high conductivity pitch-derived graphite foam, thermal conductivity being as high as 187 W/m.dot.K, the heat from the heat source is more efficiently transferred to the water for evaporation, thus the system does not cool significantly due to the evaporation of the water and, consequently, the air reaches a higher humidity ratio.

Effect of starting microstructure on helium plasma-materials interaction in tungsten

DOE PAGES

Wang, Kun; Bannister, Mark E.; Meyer, Fred W.; ...

2016-11-24

Here, in a magnetic fusion energy (MFE) device, the plasma-facing materials (PFMs) will be subjected to tremendous fluxes of ions, heat, and neutrons. The response of PFMs to the fusion environment is still not well defined. Tungsten metal is the present candidate of choice for PFM applications such as the divertor in ITER. However, tungsten's microstructure will evolve in service, possibly to include recrystallization. How tungsten's response to plasma exposure evolves with changes in microstructure is presently unknown. In this work, we have exposed hot-worked and recrystallized tungsten to an 80 eV helium ion beam at a temperature of 900more » °C to fluences of 2 × 10 23 or 20 × 10 23 He/m 2. This resulted in a faceted surface structure at the lower fluence or short but well-developed nanofuzz structure at the higher fluence. There was little difference in the hot-rolled or recrystallized material's near-surface (≤50 nm) bubbles at either fluence. At higher fluence and deeper depth, the bubble populations of the hot-rolled and recrystallized were different, the recrystallized being larger and deeper. This may explain previous high-fluence results showing pronounced differences in recrystallized material. The deeper penetration in recrystallized material also implies that grain boundaries are traps, rather than high-diffusivity paths.« less

Effect of strain on evolution of dynamic recrystallization in Nb-1 wt%Zr-0.1 wt%C alloy at 1500 and 1600 °C

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

Behera, A.N.

Uniaxial compression tests were carried out on Nb-1 wt%Zr-0.1 wt%C alloy at temperature of 1500 and 1600 °C and strain rate of 0.1 s{sup −1} to study the evolution of dynamic recrystallization with strain. Electron back scatter diffraction was used to quantify the microstructural evolution. Nb-1Zr-0.1C alloy showed a necklace structure at a strain of 0.9 when deformed at 1500 °C and at strain of 0.6 when deformed at 1600 °C, both at strain rate of 0.1 s{sup −1}. This suggested the occurrence of dynamic recrystallization. At 1500 °C and strain of 0.9 the local average misorientation and the grainmore » orientation spread was low confirming the presence of dynamic recrystallization at this deformation condition. At both 1500 and 1600 °C and all measured strains the recrystallized grains had a strong fiber component of <001>. - Highlights: • Necklace formation of dynamically recrystallized grains occurred at strain of 0.6 and 0.9 for 1500 and 1600 °C, respectively. • Equiaxed microstructures were seen with increase in strain for both 1500 and 1600 °C. • At large strains the predominant recrystallized texture evolved to <001> pole.« less

Low temperature simulation of subliming boundary layer flow in Jupiter atmosphere

NASA Technical Reports Server (NTRS)

Chen, C. J.

1976-01-01

A low-temperature approximate simulation for the sublimation of a graphite heat shield under Jovian entry conditions is studied. A set of algebraic equations is derived to approximate the governing equation and boundary conditions, based on order-of-magnitude analysis. Characteristic quantities such as the wall temperature and the subliming velocity are predicted. Similarity parameters that are needed to simulate the most dominant phenomena of the Jovian entry flow are also given. An approximate simulation of the sublimation of the graphite heat shield is performed with an air-dry-ice model. The simulation with the air-dry-ice model may be carried out experimentally at a lower temperature of 3000 to 6000 K instead of the entry temperature of 14,000 K. The rate of graphite sublimation predicted by the present algebraic approximation agrees to the order of magnitude with extrapolated data. The limitations of the simulation method and its utility are discussed.

Graphene Nanobubbles Produced by Water Splitting.

PubMed

An, Hongjie; Tan, Beng Hau; Moo, James Guo Sheng; Liu, Sheng; Pumera, Martin; Ohl, Claus-Dieter

2017-05-10

Graphene nanobubbles are of significant interest due to their ability to trap mesoscopic volumes of gas for various applications in nanoscale engineering. However, conventional protocols to produce such bubbles are relatively elaborate and require specialized equipment to subject graphite samples to high temperatures or pressures. Here, we demonstrate the formation of graphene nanobubbles between layers of highly oriented pyrolytic graphite (HOPG) with electrolysis. Although this process can also lead to the formation of gaseous surface nanobubbles on top of the substrate, the two types of bubbles can easily be distinguished using atomic force microscopy. We estimated the Young's modulus, internal pressure, and the thickness of the top membrane of the graphene nanobubbles. The hydrogen storage capacity can reach ∼5 wt % for a graphene nanobubble with a membrane that is four layers thick. The simplicity of our protocol paves the way for such graphitic nanobubbles to be utilized for energy storage and industrial applications on a wide scale.

Study of Improved Aluminum Materials for Vehicular Armor

DTIC Science & Technology

1977-04-07

and along cell walls. Dislocations generated during deformation cf the 17 -------------- recrystallized structure interacted with the grain...unrecrystallized (HR) 7475 plate containing dislocations within subgrains and along cell walls. Hot rolling the recrystallized structure at 750OF produced...a structure after solution heat treatment that consisted of elongated recrystallized grains containing polygonized cells . This structure developed

Orogen-scale along-strike continuity in quartz recrystallization microstructures adjacent to the Main Central Thrust: implications for deformation temperatures, strain rates and flow stresses

NASA Astrophysics Data System (ADS)

Law, Richard

2015-04-01

Traced for ~ 1500 km along the foreland edge of the Himalaya from NW India to Bhutan published reports indicate a remarkable along-strike continuity of quartz recrystallization microstructures in the footwall and hanging wall to the Main Central Thrust (MCT). Recrystallization in Lesser Himalayan Series (LHS) rocks in the footwall to the MCT is dominated by grain boundary bulging (BLG) microstructures, while recrystallization in Greater Himalayan Series (GHS) rocks in the hanging wall is dominated by grain boundary migration microstructures that traced structurally upwards transition in to the anatectic core of the GHS. In foreland-positioned high-strain rocks adjacent to the MCT recrystallization is dominated by subgrain rotation (SGR) with transitional BLG-SGR and SGR-GBM microstructures being recorded at structural distances of up to a few hundred meters below and above the MCT, respectively. Correlation with available information on temperatures of metamorphism indicated by mineral phase equilibria and RSCM data suggests that recrystallization in the structural zones dominated by BLG, SGR and GBM occurred at temperatures of ~ 350-450, 450-550 and 550- > 650 °C, respectively. It should be kept in mind, however, that these temperatures are likely to be 'close-to-peak' temperatures of metamorphism, whereas penetrative shearing and recrystallization may have continued during cooling. The dominance of SGR along the more foreland-positioned exposures of the MCT intuitively suggests that shearing occurred under a relatively restricted range of deformation temperatures and strain rates. Plotting the 'close-to-peak' 450-500 °C temperatures of metamorphism indicated for SGR-dominated rocks located at up to a few hundred meters below/above the MCT on the quartz recrystallization map developed by Stipp et al. (2002) indicates 'ball-park' strain rates of ~ 10-13 to 10-10 sec-1. However, only strain rates slower than 10-12 sec-1 on the MCT are likely to be compatible with know convergence rates between the Indian and Asian plates. If shearing continued during retrograde cooling while remaining in the SGR field, then the recrystallization map suggests that a significant drop in deformation temperature (> ~75-100 °C) would result in a decrease in strain rate. In general, however, the presence of a single recrystallization microstructure traced over a large (regional scale) distance does not necessarily mean that deformation temperature (or strain rate) remains constant but could, for example, indicate that spatial variations in deformation temperature are compensated for by changes in strain rate, with grain-scale deformation remaining within a particular recrystallization regime. Constant stress conditions plot along a straight line in the 1/T versus log strain rate space used in the quartz recrystallization mechanism map. This suggests that the observed along-strike consistency of SGR-dominated recrystallization microstructures may indicate near to constant stress boundary conditions (albeit with varying temperatures and strain rates) prevailing along what are now the more foreland-positioned exposures of the MCT. Extrapolation of the Hirth et al. (2001) flow law suggests a flow stress of ~ 30-50 MPa based on the deformation temperatures and strain rates inferred for foreland-positioned exposures of the MCT, in agreement with flow stresses estimated from recrystallized quartz grain size data.

Reinforcement of the Cube texture during recrystallization of a 1050 aluminum alloy partially recrystallized and 10% cold-rolled

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

Wang Wei; Helbert, Anne-Laure, E-mail: anne-laure.helbert@u-psud.fr; Baudin, Thierry

In high purity Aluminum, very strong {l_brace}100{r_brace}<001> recrystallization texture is developed after 98% cold rolling and annealing at 500 Degree-Sign C. On the contrary, in Aluminum alloys of commercial purity, the Cube component hardly exceeds 30% after complete recrystallization. Parameters controlling Cube orientation development are mainly the solute dragging due to impurities in solid solution and the stored deformation energy. In the present study, besides the 85% cold rolling, two extra annealings and a slight cold rolling are introduced in the processing route to increase the Cube volume fraction. The Cube development was analyzed by X-ray diffraction and Electron BackScatteredmore » Diffraction (EBSD). The nucleation and growth mechanisms responsible for the large Cube growth were investigated using FEG/EBSD in-situ heating experiments. Continuous recrystallization was observed in Cube oriented grains and competed with SIBM (Strain Induced Boundary Migration) mechanism. This latter was favored by the stored energy gap introduced during the additional cold-rolling between the Cube grains and their neighbors. Finally, a Cube volume fraction of 65% was reached after final recrystallization. - Highlights: Black-Right-Pointing-Pointer EBSD in-situ heating experiments of aluminum alloy of commercial purity. Black-Right-Pointing-Pointer A 10% cold-rolling after a partial recrystallization improved Cube nucleation and growth. Black-Right-Pointing-Pointer Annealing before cold-rolling limited the solute drag effect and permitted a large Cube growth. Black-Right-Pointing-Pointer Cube development is enhanced by continuous recrystallization of Cube sub-grains. Black-Right-Pointing-Pointer The preferential Cube growth occurs by SIBM of small Cube grains.« less

Microstructure Characterization and Stress Corrosion Evaluation of Autogenous and Hybrid Friction Stir Welded Al-Cu-Li 2195 Alloy

NASA Technical Reports Server (NTRS)

Li, Zhixian; Arbegast, William J.; Meletis, Efstathios I.

1997-01-01

Friction stir welding process is being evaluated for application on the Al-Cu-Li 2195 Super-Light Weight External Tank of the Space Transportation System. In the present investigation Al-Cu-Li 2195 plates were joined by autogenous friction stir welding (FSW) and hybrid FSW (friction stir welding over existing variable polarity plasma arc weld). Optical microscopy and transmission electron microscopy (TEM) were utilized to characterize microstructures of the weldments processed by both welding methods. TEM observations of autogenous FSW coupons in the center section of the dynamically-recrystallized zone showed an equiaxed recrystallized microstructure with an average grain size of approx. 3.8 microns. No T(sub 1), precipitates were present in the above-mentioned zone. Instead, T(sub B) and alpha precipitates were found in this zone with a lower population. Alternate immersion, anodic polarization, constant load, and slow strain tests were carried out to evaluate the general corrosion and stress-corrosion properties of autogenous and hybrid FSW prepared coupons. The experimental results will be discussed.

Sustainable Strategy Utilizing Biomass: Visible-Light-Mediated Synthesis of γ-Valerolactone

EPA Science Inventory

A novel sustainable approach to valued γ-valerolactone is described that exploits visible light mediated conversion of biomass-derived levulinic acid using a bimetallic catalyst on graphitic carbon nitride, AgPd@g-C3N4.

Combined Effect of Heating Rate and Microalloying Elements on Recrystallization During Annealing of Dual-Phase Steels

NASA Astrophysics Data System (ADS)

Bellavoine, Marion; Dumont, Myriam; Drillet, Josée; Hébert, Véronique; Maugis, Philippe

2018-05-01

Adjusting ferrite recrystallization kinetics during annealing is a way to control the final microstructure and thus the mechanical properties of advanced cold-rolled high-strength steels. Two strategies are commonly used for this purpose: adjusting heating rates and/or adding microalloying elements. The present work investigates the effect of heating rate and microalloying elements Ti, Nb, and Mo on recrystallization kinetics during annealing in various cold-rolled Dual-Phase steel grades. The use of combined experimental and modeling approaches allows a deeper understanding of the separate influence of heating rate and the addition of microalloying elements. The comparative effect of Ti, Nb, and Mo as solute elements and as precipitates on ferrite recrystallization is also clarified. It is shown that solute drag has the largest delaying effect on recrystallization in the present case and that the order of solute drag effectiveness of microalloying elements is Nb > Mo > Ti.

Combined Effect of Heating Rate and Microalloying Elements on Recrystallization During Annealing of Dual-Phase Steels

NASA Astrophysics Data System (ADS)

Bellavoine, Marion; Dumont, Myriam; Drillet, Josée; Hébert, Véronique; Maugis, Philippe

2018-07-01

Adjusting ferrite recrystallization kinetics during annealing is a way to control the final microstructure and thus the mechanical properties of advanced cold-rolled high-strength steels. Two strategies are commonly used for this purpose: adjusting heating rates and/or adding microalloying elements. The present work investigates the effect of heating rate and microalloying elements Ti, Nb, and Mo on recrystallization kinetics during annealing in various cold-rolled Dual-Phase steel grades. The use of combined experimental and modeling approaches allows a deeper understanding of the separate influence of heating rate and the addition of microalloying elements. The comparative effect of Ti, Nb, and Mo as solute elements and as precipitates on ferrite recrystallization is also clarified. It is shown that solute drag has the largest delaying effect on recrystallization in the present case and that the order of solute drag effectiveness of microalloying elements is Nb > Mo > Ti.

Recrystallization kinetics of warm-rolled tungsten in the temperature range 1150-1350 °C

NASA Astrophysics Data System (ADS)

Alfonso, A.; Juul Jensen, D.; Luo, G.-N.; Pantleon, W.

2014-12-01

Pure tungsten is a potential candidate material for the plasma-facing first wall and the divertor of fusion reactors. Both parts have to withstand high temperatures during service. This will alter the microstructure of the material by recovery, recrystallization and grain growth and will cause degradation in material properties as a loss in mechanical strength and embrittlement. The thermal stability of a pure tungsten plate warm-rolled to 67% thickness reduction was investigated by long-term isothermal annealing in the temperature range between 1150 °C and 1350 °C up to 2200 h. Changes in the mechanical properties during annealing are quantified by Vickers hardness measurements. They are described concisely by classical kinetic models for recovery and recrystallization. The observed time spans for recrystallization and the obtained value for the activation energy of the recrystallization process indicate a sufficient thermal stability of the tungsten plate during operation below 1075 °C.

Boundary migration in a 3D deformed microstructure inside an opaque sample

DOE PAGES

Zhang, Y. B.; Budai, J. D.; Tischler, J. Z.; ...

2017-06-30

How boundaries surrounding recrystallization grains migrate through the 3D network of dislocation boundaries in deformed crystalline materials is unknown and critical for the resulting recrystallized crystalline materials. Furthermore, by using X-ray Laue diffraction microscopy, we show for the first time the migration pattern of a typical recrystallization boundary through a well-characterized deformation matrix. The data provide a unique possibility to investigate effects of both boundary misorientation and plane normal on the migration, information which cannot be accessed with any other techniques. Our results show that neither of these two parameters can explain the observed migration behavior. Instead we suggest thatmore » the subdivision of the deformed microstructure ahead of the boundary plays the dominant role. Our experimental observations challenge the assumptions of existing recrystallization theories, and set the stage for determination of mobilities of recrystallization boundaries.« less

Improvement of seawater salt quality by hydro-extraction and re-crystallization methods

NASA Astrophysics Data System (ADS)

Sumada, K.; Dewati, R.; Suprihatin

2018-01-01

Indonesia is one of the salt producing countries that use sea water as a source of raw materials, the quality of salt produced is influenced by the quality of sea water. The resulting average salt quality contains 85-90% NaCl. The Indonesian National Standard (SNI) for human salt’s consumption sodium chloride content is 94.7 % (dry base) and for industrial salt 98,5 %. In this study developed the re-crystallization without chemical and hydro-extraction method. The objective of this research to choose the best methods based on efficiency. The results showed that re-crystallization method can produce salt with NaCl content 99,21%, while hydro-extraction method content 99,34 % NaCl. The salt produced through both methods can be used as a consumption and industrial salt, Hydro-extraction method is more efficient than re-crystallization method because re-crystallization method requires heat energy.

Diffusion-Controlled Recrystallization of Water Sorbed into Poly(meth)acrylates Revealed by Variable-Temperature Mid-Infrared Spectroscopy and Molecular Dynamics Simulation.

PubMed

Yasoshima, Nobuhiro; Fukuoka, Mizuki; Kitano, Hiromi; Kagaya, Shigehiro; Ishiyama, Tatsuya; Gemmei-Ide, Makoto

2017-05-18

Recrystallization behaviors of water sorbed into four poly(meth)acrylates, poly(2-methoxyethyl acrylate), poly(tetrahydrofurfuryl acrylate), poly(methyl acrylate), and poly(methyl methacrylate), are investigated by variable-temperature mid-infrared (VT-MIR) spectroscopy and molecular dynamics (MD) simulation. VT-MIR spectra demonstrate that recrystallization temperatures of water sorbed into the polymers are positively correlated with their glass-transition temperatures reported previously. The present MD simulation shows that a lower-limit temperature of the diffusion for the sorbed water and the glass-transition temperatures of the polymers also have a positive correlation, indicating that the recrystallization is controlled by diffusion mechanism rather than reorientation mechanism. Detailed molecular processes of not only recrystallization during rewarming but also crystallization during cooling and hydrogen-bonding states of water in the polymers are systematically analyzed and discussed.

Cellular monotectic model solidification

NASA Technical Reports Server (NTRS)

Kaukler, William F.

1987-01-01

Succinonitrile (sn) was purified to a superior level using a fractional recrystallization method. The melting point of the best twice recrystallized sn was not raised by following with double distillation. This was tested using differential scanning calorimetry. The peak shape on melting also proved that double distillation after double recrystallization did not improve the quality. Stability and phase diagrams for succinonitrile and glycerol are presented.

Effect of one-step recrystallization on the grain boundary evolution of CoCrFeMnNi high entropy alloy and its subsystems.

PubMed

Chen, Bo-Ru; Yeh, An-Chou; Yeh, Jien-Wei

2016-02-29

In this study, the grain boundary evolution of equiatomic CoCrFeMnNi, CoCrFeNi, and FeCoNi alloys after one-step recrystallization were investigated. The special boundary fraction and twin density of these alloys were evaluated by electron backscatter diffraction analysis. Among the three alloys tested, FeCoNi exhibited the highest special boundary fraction and twin density after one-step recrystallization. The special boundary increment after one-step recrystallization was mainly affected by grain boundary velocity, while twin density was mainly affected by average grain boundary energy and twin boundary energy.

Effect of Scandium on the Interaction of Concurrent Precipitation and Recrystallization in Commercial AA3003 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Tu, Yiyou; Qian, Huan; Zhou, Xuefeng; Jiang, Jianqing

2014-04-01

In the current study, the effect of Sc addition on the interaction of concurrent precipitation and recrystallization in commercial AA3003 aluminum alloy was investigated using optical microscopy, scanning electron microscopy, and transmission electron microscopy. In case of AA3003 alloy, which was cold rolled to a true strain of 2.20 and heated at a heating rate of 150 K/s, the onset of precipitation and ending of recrystallization are signified by the critical temperature, T C ~740 K (467 °C). There is a change in the shape of the recrystallized grains from pancake-like to equiaxed shape, as the annealing temperature increases greater than T C. In case of AA3003 alloy microalloyed with 0.4 wt pct of Sc, the high no. density precipitation of coherent Al3Sc precipitates always occurs before recrystallization because of the small nucleation barrier and high rate of decomposition. This leads to extremely coarse pancake-like recrystallization grains with high fraction of low-angle grain boundaries in the entire annealing temperature range, even at a high brazing temperature of 883 K (610 °C).

Incorporation of Eu(III) into Calcite under Recrystallization conditions.

PubMed

Hellebrandt, S E; Hofmann, S; Jordan, N; Barkleit, A; Schmidt, M

2016-09-13

The interaction of calcite with trivalent europium under recrystallization conditions was studied on the molecular level using site-selective time-resolved laser fluorescence spectroscopy (TRLFS). We conducted batch studies with a reaction time from seven days up to three years with three calcite powders, which differed in their specific surface area, recrystallization rates and impurities content. With increase of the recrystallization rate incorporation of Eu(3+) occurs faster and its speciation comes to be dominated by one species with its excitation maximum at 578.8 nm, so far not identified during previous investigations of this process under growth and phase transformation conditions. A long lifetime of 3750 μs demonstrates complete loss of hydration, consequently Eu must have been incorporated into the bulk crystal. The results show a strong dependence of the incorporation kinetics on the recrystallization rate of the different calcites. Furthermore the investigation of the effect of different background electrolytes (NaCl and KCl) demonstrate that the incorporation process under recrystallization conditions strongly depends on the availability of Na(+). These findings emphasize the different retention potential of calcite as a primary and secondary mineral e.g. in a nuclear waste disposal site.

Incorporation of Eu(III) into Calcite under Recrystallization conditions

PubMed Central

Hellebrandt, S. E.; Hofmann, S.; Jordan, N.; Barkleit, A.; Schmidt, M.

2016-01-01

The interaction of calcite with trivalent europium under recrystallization conditions was studied on the molecular level using site-selective time-resolved laser fluorescence spectroscopy (TRLFS). We conducted batch studies with a reaction time from seven days up to three years with three calcite powders, which differed in their specific surface area, recrystallization rates and impurities content. With increase of the recrystallization rate incorporation of Eu3+ occurs faster and its speciation comes to be dominated by one species with its excitation maximum at 578.8 nm, so far not identified during previous investigations of this process under growth and phase transformation conditions. A long lifetime of 3750 μs demonstrates complete loss of hydration, consequently Eu must have been incorporated into the bulk crystal. The results show a strong dependence of the incorporation kinetics on the recrystallization rate of the different calcites. Furthermore the investigation of the effect of different background electrolytes (NaCl and KCl) demonstrate that the incorporation process under recrystallization conditions strongly depends on the availability of Na+. These findings emphasize the different retention potential of calcite as a primary and secondary mineral e.g. in a nuclear waste disposal site. PMID:27618958

Anisotropic Morphological Changes in Goethite during Fe(2+)-Catalyzed Recrystallization.

PubMed

Joshi, Prachi; Gorski, Christopher A

2016-07-19

When goethite is exposed to aqueous Fe(2+), rapid and extensive Fe atom exchange can occur between solid-phase Fe(3+) and aqueous Fe(2+) in a process referred to as Fe(2+)-catalyzed recrystallization. This process can lead to the structural incorporation or release of trace elements, which has important implications for contaminant remediation and nutrient biogeochemical cycling. Prior work found that the process did not cause major changes to the goethite structure or morphology. Here, we further investigated if and how goethite morphology and aggregation behavior changed temporally during Fe(2+)-catalyzed recrystallization. On the basis of existing literature, we hypothesized that Fe(2+)-catalyzed recrystallization of goethite would not result in changes to individual particle morphology or interparticle interactions. To test this, we reacted nanoparticulate goethite with aqueous Fe(2+) at pH 7.5 over 30 days and used transmission electron microscopy (TEM), cryogenic TEM, and (55)Fe as an isotope tracer to observe changes in particle dimensions, aggregation, and isotopic composition over time. Over the course of 30 days, the goethite particles substantially recrystallized, and the particle dimensions changed anisotropically, resulting in a preferential increase in the mean particle width. The temporal changes in goethite morphology could not be completely explained by a single mineral-transformation mechanism but rather indicated that multiple transformation mechanisms occurred concurrently. Collectively, these results demonstrate that the morphology of goethite nanoparticles does change during recrystallization, which is an important step toward identifying the driving force(s) of recrystallization.

Photocatalytic CH activation and oxidative esterification using Pd@g-C3N4

EPA Science Inventory

Graphitic carbon nitride supported palladium nanoparticles, Pd@g-C3N4, have been synthesized and utilized for the direct oxidative esterification of alcohols using atmospheric oxygen as a co-oxidant via photocatalytic CH activation.

The microwave-assisted ionic liquid nanocomposite synthesis: platinum nanoparticles on graphene and the application on hydrogenation of styrene

PubMed Central

2013-01-01

The microwave-assisted nanocomposite synthesis of metal nanoparticles on graphene or graphite oxide was introduced in this research. With microwave assistance, the Pt nanoparticles on graphene/graphite oxide were successfully produced in the ionic liquid of 2-hydroxyethanaminium formate [HOCH2CH2NH3][HCO2]. On graphene/graphite oxide, the sizes of Pt nanoparticles were about 5 to 30 nm from transmitted electron microscopy (TEM) results. The crystalline Pt structures were examined by X-ray diffraction (XRD). Since hydrogenation of styrene is one of the important well-known chemical reactions, herein, we demonstrated then the catalytic hydrogenation capability of the Pt nanoparticles on graphene/graphite oxide for the nanocomposite to compare with that of the commercial catalysts (Pt/C and Pd/C, 10 wt.% metal catalysts on activated carbon from Strem chemicals, Inc.). The conversions with the Pt nanoparticles on graphene are >99% from styrene to ethyl benzene at 100°C and under 140 psi H2 atmosphere. However, ethyl cyclohexane could be found as a side product at 100°C and under 1,520 psi H2 atmosphere utilizing the same nanocomposite catalyst. PMID:24103100

Modeling the microstructural changes during hot tandem rolling of AA5 XXX aluminum alloys: Part I. Microstructural evolution

NASA Astrophysics Data System (ADS)

Wells, M. A.; Samarasekera, I. V.; Brimacombe, J. K.; Hawbolt, E. B.; Lloyd, D. J.

1998-06-01

A comprehensive mathematical model of the hot tandem rolling process for aluminum alloys has been developed. Reflecting the complex thermomechanical and microstructural changes effected in the alloys during rolling, the model incorporated heat flow, plastic deformation, kinetics of static recrystallization, final recrystallized grain size, and texture evolution. The results of this microstructural engineering study, combining computer modeling, laboratory tests, and industrial measurements, are presented in three parts. In this Part I, laboratory measurements of static recrystallization kinetics and final recrystallized grain size are described for AA5182 and AA5052 aluminum alloys and expressed quantitatively by semiempirical equations. In Part II, laboratory measurements of the texture evolution during static recrystallization are described for each of the alloys and expressed mathematically using a modified form of the Avrami equation. Finally, Part III of this article describes the development of an overall mathematical model for an industrial aluminum hot tandem rolling process which incorporates the microstructure and texture equations developed and the model validation using industrial data. The laboratory measurements for the microstructural evolution were carried out using industrially rolled material and a state-of-the-art plane strain compression tester at Alcan International. Each sample was given a single deformation and heat treated in a salt bath at 400 °C for various lengths of time to effect different levels of recrystallization in the samples. The range of hot-working conditions used for the laboratory study was chosen to represent conditions typically seen in industrial aluminum hot tandem rolling processes, i.e., deformation temperatures of 350 °C to 500 °C, strain rates of 0.5 to 100 seconds and total strains of 0.5 to 2.0. The semiempirical equations developed indicated that both the recrystallization kinetics and the final recrystallized grain size were dependent on the deformation history of the material i.e., total strain and Zener-Hollomon parameter ( Z), where Z = dot \\varepsilon exp left( {{Q_{def} }/{RT_{def }}} right) and time at the recrystallization temperature.

Activity of slip in amphibolite facies, fine-grained recrystallized quartz aggregates: high differential stress during high-T creep of quartz?

NASA Astrophysics Data System (ADS)

Viegas, G.; Menegon, L. M.; Archanjo, C. J.

2016-12-01

Quartz axis fabrics are a valuable tool to investigate strain partitioning/distribution in both naturally- and experimentally deformed quartz. Previous works have shown that slip dominates at high temperatures (> 600º C) and water-rich, commonly sub-magmatic conditions, typically associated with large grain sizes and grain boundary migration microstructures. In the Pernambuco shear zone, sheared quartz veins from a protomylonitic granitoid formed during the main amphibolite facies event constrained at mid-crustal conditions (550-600ºC, 5 kbar). The veins contain heterogeneously-deformed primary quartz grains, which typically form both flattened and elongated ribbons as well as more equant porphyroclasts surrounded by aggregates of fine-grained (ca. 20 µm) recrystallized aggregates. Recrystallized quartz with the same fine grain size may also occur in intracrystalline bands within the porphyroclasts. Chessboard extinction is widely observed in the porphyroclasts, and subgrain boundaries are either parallel or normal to the (0001) direction, suggesting slip on both basal and prismatic planes during recrystallization. Crystallographic preferred orientations (CPOs) of porphyroclasts (≥ 100 µm) show maxima of (0001) axes subparallel to Z and X, suggesting coeval glide along both basal and prism planes during shearing. In the recrystallized aggregates, fabric strength tends to become weaker, but still records glide along and directions. These preliminary results suggest that naturally deformed quartz veins record coeval activity of and slip during dynamic recrystallization under amphibolite facies conditions. The microstructure suggests that the CPO of the fine-grained aggregates is host-controlled and results from dominant subgrain rotation recrystallization. To our knowledge, activity of slip in fine-grained recrystallized aggregates has never been reported before. Thus, these preliminary results call into question the general view that slip is expected to be active only during dominant high-T grain boundary migration in the lower crust. In our samples, a fine grain size of dynamically recrystallized quartz associated with slip might indicate high differential stress/strain rates during high-T viscous creep along the Pernambuco shear zone.

Process for utilizing low-cost graphite substrates for polycrystalline solar cells

NASA Technical Reports Server (NTRS)

Chu, T. L. (Inventor)

1978-01-01

Low cost polycrystalline silicon solar cells supported on substrates were prepared by depositing successive layers of polycrystalline silicon containing appropriate dopants over supporting substrates of a member selected from the group consisting of metallurgical grade polycrystalline silicon, graphite and steel coated with a diffusion barrier of silica, borosilicate, phosphosilicate, or mixtures thereof such that p-n junction devices were formed which effectively convert solar energy to electrical energy. To improve the conversion efficiency of the polycrystalline silicon solar cells, the crystallite size in the silicon was substantially increased by melting and solidifying a base layer of polycrystalline silicon before depositing the layers which form the p-n junction.

Monte Carlo modeling of recrystallization processes in α-uranium

DOE PAGES

Steiner, M. A.; McCabe, R. J.; Garlea, E.; ...

2017-08-01

In this study, starting with electron backscattered diffraction (EBSD) data obtained from a warm clock-rolled α-uranium deformation microstructure, a Potts Monte Carlo model was used to simulate static site-saturated recrystallization while testing a number of different conditions for the assignment of recrystallized nuclei within the microstructure. The simulations support observations that recrystallized nuclei within α-uranium form preferentially on non-twin high-angle grain boundary sites at 450 °C, and demonstrate that the most likely nucleation sites on these boundaries can be identified by the surrounding degree of Kernel Average Misorientation (KAM), which may be considered as a proxy for the local geometricallymore » necessary dislocation (GND) density.« less

Dynamic Recrystallization Behavior of Zr-1Sn-0.3Nb Alloy During Hot Rolling Process

NASA Astrophysics Data System (ADS)

Zhao, Siyu; Liu, Huiqun; Lin, Gaoyong; Jiang, Yilan; Xun, Jian

2017-11-01

Zirconium alloys are advanced materials with properties that are greatly affected by their crystalline structure. To investigate this, sheets of Zr-1Sn-0.3Nb alloy were hot rolled with different reductions (10%, 30%, 50%, and 60%) at 1023 K and 1073 K to investigate the alloy's dynamic recrystallization behavior. Recrystallization kinetics was observed via electron backscattering diffraction and transmission electron microscopy, and the results were compared with estimates based on the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation. The values of the JMAK exponent n and k increased with the rolling temperature. The estimates and microstructural observations of dynamic recrystallization (DRX) kinetics were in good agreement.

Characterization of thermoplastic polyimide NEW-TPI

NASA Technical Reports Server (NTRS)

Hou, T. H.; Reddy, R. M.

1991-01-01

Thermal and rheological properties of a commercial thermoplastic polyimide, NEW-TPI, were characterized. The as-received material possesses initially a transient crystallite form with a bimodal distribution in peak melting temperatures. After the meltings of the initial crystallite structures, the sample can be recrystallized by various thermal treatments. A bimodal or single-modal melting peak distribution is formed for annealing temperatures below or above 360 C, respectively. The recrystallized crystallinities are all transient in nature. The polymers are unable to be recrystallized after being subjected to elevated temperature annealing above 450 C. The recrystallization mechanism was postulated, and a simple kinetics model was found to describe the behavior satisfactorily under conditions of prolonged thermal annealing.

Effect of one-step recrystallization on the grain boundary evolution of CoCrFeMnNi high entropy alloy and its subsystems

PubMed Central

Chen, Bo-Ru; Yeh, An-Chou; Yeh, Jien-Wei

2016-01-01

In this study, the grain boundary evolution of equiatomic CoCrFeMnNi, CoCrFeNi, and FeCoNi alloys after one-step recrystallization were investigated. The special boundary fraction and twin density of these alloys were evaluated by electron backscatter diffraction analysis. Among the three alloys tested, FeCoNi exhibited the highest special boundary fraction and twin density after one-step recrystallization. The special boundary increment after one-step recrystallization was mainly affected by grain boundary velocity, while twin density was mainly affected by average grain boundary energy and twin boundary energy. PMID:26923713

The Nuclear Cryogenic Propulsion Stage

NASA Technical Reports Server (NTRS)

Houts, Michael G.; Kim, Tony; Emrich, William J.; Hickman, Robert R.; Broadway, Jeramie W.; Gerrish, Harold P.; Belvin, Anthony D.; Borowski, Stanley K.; Scott, John H.

2014-01-01

Nuclear Thermal Propulsion (NTP) development efforts in the United States have demonstrated the technical viability and performance potential of NTP systems. For example, Project Rover (1955 - 1973) completed 22 high power rocket reactor tests. Peak performances included operating at an average hydrogen exhaust temperature of 2550 K and a peak fuel power density of 5200 MW/m3 (Pewee test), operating at a thrust of 930 kN (Phoebus-2A test), and operating for 62.7 minutes in a single burn (NRX-A6 test). Results from Project Rover indicated that an NTP system with a high thrust-to-weight ratio and a specific impulse greater than 900 s would be feasible. Excellent results were also obtained by the former Soviet Union. Although historical programs had promising results, many factors would affect the development of a 21st century nuclear thermal rocket (NTR). Test facilities built in the US during Project Rover no longer exist. However, advances in analytical techniques, the ability to utilize or adapt existing facilities and infrastructure, and the ability to develop a limited number of new test facilities may enable affordable development, qualification, and utilization of a Nuclear Cryogenic Propulsion Stage (NCPS). Bead-loaded graphite fuel was utilized throughout the Rover/NERVA program, and coated graphite composite fuel (tested in the Nuclear Furnace) and cermet fuel both show potential for even higher performance than that demonstrated in the Rover/NERVA engine tests.. NASA's NCPS project was initiated in October, 2011, with the goal of assessing the affordability and viability of an NCPS. FY 2014 activities are focused on fabrication and test (non-nuclear) of both coated graphite composite fuel elements and cermet fuel elements. Additional activities include developing a pre-conceptual design of the NCPS stage and evaluating affordable strategies for NCPS development, qualification, and utilization. NCPS stage designs are focused on supporting human Mars missions. The NCPS is being designed to readily integrate with the Space Launch System (SLS). A wide range of strategies for enabling affordable NCPS development, qualification, and utilization should be considered. These include multiple test and demonstration strategies (both ground and in-space), multiple potential test sites, and multiple engine designs. Two potential NCPS fuels are currently under consideration - coated graphite composite fuel and tungsten cermet fuel. During 2014 a representative, partial length (approximately 16") coated graphite composite fuel element with prototypic depleted uranium loading is being fabricated at Oak Ridge National Laboratory (ORNL). In addition, a representative, partial length (approximately 16") cermet fuel element with prototypic depleted uranium loading is being fabricated at Marshall Space Flight Center (MSFC). During the development process small samples (approximately 3" length) will be tested in the Compact Fuel Element Environmental Tester (CFEET) at high temperature (approximately 2800 K) in a hydrogen environment to help ensure that basic fuel design and manufacturing process are adequate and have been performed correctly. Once designs and processes have been developed, longer fuel element segments will be fabricated and tested in the Nuclear Thermal Rocket Element Environmental Simulator (NTREE) at high temperature (approximately 2800 K) and in flowing hydrogen.

Sustainable pathway to furanics from biomass via heterogeneous organo-catalysis

EPA Science Inventory

An organic sulfonated graphitic carbon nitride is synthesized and its application has been demonstrated inthe conversion of carbohydrates into furanics and related value-added products. The most importantfeature of the material is the stability and acidity, which could be utilize...

The effect of precipitation on the evolution of recrystallization textures in an AA 8011 aluminum alloy sheet

NASA Astrophysics Data System (ADS)

Ryu, Jong-Ho; Lee, Yoon-Soo; Lee, Dong Nyung

2001-06-01

The texture of an AA 8011 aluminum alloy sheet cold rolled by 95% showed a typical β-fiber, which runs from the copper orientation [C={112}<111>] over S [{123}<634>] to brass [B={011}<112>]. The development of annealing textures depended on annealing temperatures due to the interaction between precipitation and recrystallization. Upon annealing at a low temperature of 275°C, precipitation took place before recrystallization. This led to a weak recrystallization texture consisting of {011}<122>, {001˜<100>, and {hk0}<001>, among which the {011}<122> orientation developed near large FeAl3 particles as the main orientation and the cube [{001}<100>] orientation originating from the matrix was relatively weak. After annealing at 350 and 500°C, a strong cube texture developed along with a weak {011}<122> orientation. When the cube orientation developed, the copper orientation disappeared most rapidly. These results were discussed based on the interaction between precipitation and recrystallization.

Microstructure evolution and texture development of hot form-quench (HFQ) AZ31 twin roll cast (TRC) magnesium alloy

NASA Astrophysics Data System (ADS)

Alias, J.; Zhou, X.; Das, Sanjeev; El-Fakir, Omer; Thompson, G. E.

2017-12-01

The present study on the microstructure evolution of hot form-quench (HFQ) AZ31 twin roll cast magnesium alloy attempt to provide an understanding on the grain structure and heterogeneous intermetallic phase formation in the alloy and texture development following the HFQ process. Grain recrystallization and partial dissolution of eutectic β-Mg17Al12 phase particles were occurred during the solution heat treatment at 450°C, leaving the alloy consists of recrystallized grains and discontinuous or random β-Mg17Al12 phase particles distribution with small volume fraction. The particles act as effective nucleation sites for new grains during recrystallization and variation of recrystallization occurrence contributed to texture alteration. The partial or full β-Mg17Al12 phase dissolution following the HFQ induces void formation that act as fracture nucleation site and the corresponding texture alteration in the recrystallized grains led to poor formability in TRC alloy.

Dynamic moisture sorption characteristics of enzyme-resistant recrystallized cassava starch.

PubMed

Mutungi, Christopher; Schuldt, Stefan; Onyango, Calvin; Schneider, Yvonne; Jaros, Doris; Rohm, Harald

2011-03-14

The interaction of moisture with enzyme-resistant recrystallized starch, prepared by heat-moisture treatment of debranched acid-modified or debranched non-acid-modified cassava starch, was investigated in comparison with the native granules. Crystallinities of the powdered products were estimated by X-ray diffraction. Moisture sorption was determined using dynamic vapor sorption analyzer and data fitted to various models. Percent crystallinities of native starch (NS), non-acid-modified recrystallized starch (NAMRS), and acid-modified recrystallized starch (AMRS) were 39.7, 51.9, and 56.1%, respectively. In a(w) below 0.8, sorption decreased in the order NS > NAMRS > AMRS in line with increasing sample crystallinities but did not follow this crystallinity dependence at higher a(w) because of condensation and polymer dissolution effects. Adsorbed moisture became internally absorbed in NS but not in NAMRS and AMRS, which might explain the high resistance of the recrystallized starches to digestion because enzyme and starch cannot approach each other over fairly sufficient surface at the molecular level.

Recrystallization texture in nickel heavily deformed by accumulative roll bonding

NASA Astrophysics Data System (ADS)

Mishin, O. V.; Zhang, Y. B.; Godfrey, A.

2017-07-01

The recrystallization behavior of Ni processed by accumulative roll bonding to a total accumulated von Mises strain of 4.8 has been examined, and analyzed with respect to heterogeneity in the deformation microstructure. The regions near the bonding interface are found to be more refined and contain particle deformation zones around fragments of the steel wire brush used to prepare the surface for bonding. Sample-scale gradients are also observed, manifested as differences between the subsurface, intermediate and central layers, where the distributions of texture components are different. These heterogeneities affect the progress of recrystallization. While the subsurface and near-interface regions typically contain lower frequencies of cube-oriented grains than anywhere else in the sample, a strong cube texture forms in the sample during recrystallization, attributed to both a high nucleation rate and fast growth rate of cube-oriented grains. The observations highlight the sensitivity of recrystallization to heterogeneity in the deformation microstructure and demonstrate the importance of characterizing this heterogeneity over several length scales.

Photoacoustic Imaging.

DTIC Science & Technology

1983-12-01

recrystallization is currently an active area of research. Much effort has been made to grow large grain polysilicon with grain sizes of 100 microns from fine grain... polysilicon using laser recrystallization. The recrystallization process is inherently traumatic, producing large changes in temperature in short...temperature distribution above as the source term in the acoustic field equation, we ol fain r where B1)jwP) The general solution to this equation is given by

A quasi-in-situ EBSD observation of the transformation from rolling texture to recrystallization texture in V-4Cr-4Ti alloy

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

Peng, Lixia

Recrystallization texture evolution of rolled V-4Cr-4Ti alloy has been investigated by quasi-in-situ EBSD (electron back-scattering diffraction) method. Concurrently, the precipitates were characterized by SEM (Scanning Electron Microscopy). It was found that both the initial rolling textures and the distribution of the precipitates affected the formation of the recrystallization texture. It was revealed that the texture transformations of (558) 〈110〉 + (665) 〈110〉 to (334) 〈483〉 + (665) 〈1 1 2.4〉 were possibly attributed to the selective drag induced by the sparsely dispersed Ti-rich precipitates. While the densely distributed Ti-rich precipitates were responsible for the randomized recrystallization texture. Finally, when themore » precipitates were absent, the orientation changes from (112) 〈110〉 and (558) 〈110〉 to (111) 〈112〉 and (001) <110> to (001) <520> were observed. - Highlights: • Micro recrystallization texture evolution in V-4Cr-4Ti alloys is reported for the first time. • The volume fraction of Ti-rich precipitates has significant effect on the recrystallization texture evolution. • The dissolution of the Ti-rich precipitates above 1100 °C induces the strengthening of (111) <112> texture.« less

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

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

Taendl, J., E-mail: johannes.taendl@tugraz.atl; Nambu, S.; Orthacker, A.

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr)more » precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.« less

A Comparative Study on the Static Recrystallization Behavior of Cold-Rolled Mg-3Al-1Zn Alloy Stimulated by Electropulse Treatment and Conventional Heat Treatment

NASA Astrophysics Data System (ADS)

Li, Xiaopei; Li, Xiaohui; Kure-Chu, Song-Zhu; Tang, Guoyi

2017-12-01

Cold-rolled AZ31 Mg alloy strips, with a reduction of 33 pct, were subjected to electropulse treatment (EPT) and conventional heat treatment (HT) to evaluate the respective influences of electropulses and temperature on the recrystallization behavior of AZ31. The highest measured temperature during the EPT (543 K) was used in HT. The electron backscattered diffraction results demonstrated that the EPT-stimulated recrystallization was completed within 8 seconds, whereas for HT, recrystallization was still far from completion even after 240 seconds. It was found that both the nucleation and grain growth of these two processes were totally different. In the EPT samples, nucleation tended to occur preferentially near extension twin boundaries and grain boundaries by continuous recrystallization, whereas in the HT samples, nucleation occurred mainly by grain boundaries bulging via discontinuous recrystallization. As grain growth proceeded, the texture intensities of the EPT samples decreased gradually and finally evolved into an obvious transverse-direction-split texture. This is likely attributable to the impact of electropulses on the boundary energy and the contribution of nonbasal dislocations; however, the basal-type textures of the HT samples were notably strengthened, which is associated with a 30 deg〈0001〉 orientation with respect to the deformed texture.

A Comparative Study on the Static Recrystallization Behavior of Cold-Rolled Mg-3Al-1Zn Alloy Stimulated by Electropulse Treatment and Conventional Heat Treatment

NASA Astrophysics Data System (ADS)

Li, Xiaopei; Li, Xiaohui; Kure-Chu, Song-Zhu; Tang, Guoyi

2018-02-01

Cold-rolled AZ31 Mg alloy strips, with a reduction of 33 pct, were subjected to electropulse treatment (EPT) and conventional heat treatment (HT) to evaluate the respective influences of electropulses and temperature on the recrystallization behavior of AZ31. The highest measured temperature during the EPT (543 K) was used in HT. The electron backscattered diffraction results demonstrated that the EPT-stimulated recrystallization was completed within 8 seconds, whereas for HT, recrystallization was still far from completion even after 240 seconds. It was found that both the nucleation and grain growth of these two processes were totally different. In the EPT samples, nucleation tended to occur preferentially near extension twin boundaries and grain boundaries by continuous recrystallization, whereas in the HT samples, nucleation occurred mainly by grain boundaries bulging via discontinuous recrystallization. As grain growth proceeded, the texture intensities of the EPT samples decreased gradually and finally evolved into an obvious transverse-direction-split texture. This is likely attributable to the impact of electropulses on the boundary energy and the contribution of nonbasal dislocations; however, the basal-type textures of the HT samples were notably strengthened, which is associated with a 30 deg〈0001〉 orientation with respect to the deformed texture.

Cube texture formation during the early stages of recrystallization of Al-1%wt.Mn and AA1050 aluminium alloys

NASA Astrophysics Data System (ADS)

Miszczyk, M. M.; Paul, H.

2015-08-01

The cube texture formation during primary recrystallization was analysed in plane strain deformed samples of a commercial AA1050 alloy and an Al-1%wt.Mn model alloy single crystal of the Goss{110}<001> orientation. The textures were measured with the use of X-ray diffraction and scanning electron microscopy equipped with an electron backscattered diffraction facility. After recrystallization of the Al-1%wt.Mn single crystal, the texture of the recrystallized grains was dominated by four variants of the S{123}<634> orientation. The cube grains were only sporadically detected by the SEM/EBSD system. Nevertheless, an increased density of <111> poles corresponding to the cube orientation was observed. The latter was connected with the superposition of four variants of the S{123}<634> orientation. This indicates that the cube texture after the recrystallization was a ‘compromise texture’. In the case of the recrystallized AA1050 alloy, the strong cube texture results from both the increased density of the particular <111> poles of the four variants of the S orientation and the ∼40°(∼< 111>)-type rotation. The first mechanism transforms the Sdef-oriented areas into Srex ones, whereas the second the near S-oriented, as-deformed areas into near cube-oriented grains.

Influence of Heating Rate on Ferrite Recrystallization and Austenite Formation in Cold-Rolled Microalloyed Dual-Phase Steels

NASA Astrophysics Data System (ADS)

Philippot, C.; Bellavoine, M.; Dumont, M.; Hoummada, K.; Drillet, J.; Hebert, V.; Maugis, P.

2018-01-01

Compared with other dual-phase (DP) steels, initial microstructures of cold-rolled martensite-ferrite have scarcely been investigated, even though they represent a promising industrial alternative to conventional ferrite-pearlite cold-rolled microstructures. In this study, the influence of the heating rate (over the range of 1 to 10 K/s) on the development of microstructures in a microalloyed DP steel is investigated; this includes the tempering of martensite, precipitation of microalloying elements, recrystallization, and austenite formation. This study points out the influence of the degree of ferrite recrystallization prior to the austenite formation, as well as the importance of the cementite distribution. A low heating rate giving a high degree of recrystallization, leads to the formation of coarse austenite grains that are homogenously distributed in the ferrite matrix. However, a high heating rate leading to a low recrystallization degree, results in a banded-like structure with small austenite grains surrounded by large ferrite grains. A combined approach, involving relevant multiscale microstructural characterization and modeling to rationalize the effect of the coupled processes, highlights the role of the cold-worked initial microstructure, here a martensite-ferrite mixture: recrystallization and austenite formation commence in the former martensite islands before extending in the rest of the material.

Investigation of the Atypical Glass Transition and Recrystallization Behavior of Amorphous Prazosin Salts

PubMed Central

Kumar, Lokesh; Popat, Dharmesh; Bansal, Arvind K.

2011-01-01

This manuscript studied the effect of counterion on the glass transition and recrystallization behavior of amorphous salts of prazosin. Three amorphous salts of prazosin, namely, prazosin hydrochloride, prazosin mesylate and prazosin tosylate were prepared by spray drying, and characterized by optical-polarized microscopy, differential scanning calorimetry and powder X-ray diffraction. Modulated differential scanning calorimetry was used to determine the glass transition and recrystallization temperature of amorphous salts. Glass transition of amorphous salts followed the order: prazosin mesylate > prazosin tosylate ∼ prazosin hydrochloride. Amorphous prazosin mesylate and prazosin tosylate showed glass transition, followed by recrystallization. In contrast, amorphous prazosin hydrochloride showed glass transition and recrystallization simultaneously. Density Functional Theory, however, suggested the expected order of glass transition as prazosin hydrochloride > prazosin mesylate > prazosin tosylate. The counterintuitive observation of amorphous prazosin hydrochloride having lower glass transition was explained in terms of its lower activation energy (206.1 kJ/mol) for molecular mobility at Tg, compared to that for amorphous prazosin mesylate (448.5 kJ/mol) and prazosin tosylate (490.7 kJ/mol), and was further correlated to a difference in hydrogen bonding strength of the amorphous and the corresponding recrystallized salts. This study has implications in selection of an optimal amorphous salt form for pharmaceutical development. PMID:24310595

Investigation of the atypical glass transition and recrystallization behavior of amorphous prazosin salts.

PubMed

Kumar, Lokesh; Popat, Dharmesh; Bansal, Arvind K

2011-08-25

This manuscript studied the effect of counterion on the glass transition and recrystallization behavior of amorphous salts of prazosin. Three amorphous salts of prazosin, namely, prazosin hydrochloride, prazosin mesylate and prazosin tosylate were prepared by spray drying, and characterized by optical-polarized microscopy, differential scanning calorimetry and powder X-ray diffraction. Modulated differential scanning calorimetry was used to determine the glass transition and recrystallization temperature of amorphous salts. Glass transition of amorphous salts followed the order: prazosin mesylate > prazosin tosylate ~ prazosin hydrochloride. Amorphous prazosin mesylate and prazosin tosylate showed glass transition, followed by recrystallization. In contrast, amorphous prazosin hydrochloride showed glass transition and recrystallization simultaneously. Density Functional Theory, however, suggested the expected order of glass transition as prazosin hydrochloride > prazosin mesylate > prazosin tosylate. The counterintuitive observation of amorphous prazosin hydrochloride having lower glass transition was explained in terms of its lower activation energy (206.1 kJ/mol) for molecular mobility at Tg, compared to that for amorphous prazosin mesylate (448.5 kJ/mol) and prazosin tosylate (490.7 kJ/mol), and was further correlated to a difference in hydrogen bonding strength of the amorphous and the corresponding recrystallized salts. This study has implications in selection of an optimal amorphous salt form for pharmaceutical development.

Inhibition of Recrystallization of Amorphous Lactose in Nanocomposites Formed by Spray-Drying.

PubMed

Hellrup, Joel; Alderborn, Göran; Mahlin, Denny

2015-11-01

This study aims at investigating the recrystallization of amorphous lactose in nanocomposites. In particular, the focus is on the influence of the nano- to micrometer length scale nanofiller arrangement on the amorphous to crystalline transition. Further, the relative significance of formulation composition and manufacturing process parameters for the properties of the nanocomposite was investigated. Nanocomposites of amorphous lactose and fumed silica were produced by co-spray-drying. Solid-state transformation of the lactose was studied at 43%, 84%, and 94% relative humidity using X-ray powder diffraction and microcalorimetry. Design of experiments was used to analyze spray-drying process parameters and nanocomposite composition as factors influencing the time to 50% recrystallization. The spray-drying process parameters showed no significant influence. However, the recrystallization of the lactose in the nanocomposites was affected by the composition (fraction silica). The recrystallization rate constant decreased as a function of silica content. The lowered recrystallization rate of the lactose in the nanocomposites could be explained by three mechanisms: (1) separation of the amorphous lactose into discrete compartments on a micrometer length scale (compartmentalization), (2) lowered molecular mobility caused by molecular interactions between the lactose molecules and the surface of the silica (rigidification), and/or (3) intraparticle confinement of the amorphous lactose. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Preparation and recrystallization behavior of spray-dried co-amorphous naproxen-indomethacin.

PubMed

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

2016-07-01

To improve the dissolution properties and the physical stability of amorphous active pharmaceutical ingredients, small molecule stabilizing agents may be added to prepare co-amorphous systems. The objective of the study was to investigate if spray-drying allows the preparation of co-amorphous drug-drug systems such as naproxen-indomethacin and to examine the influence of the process conditions on the resulting initial sample crystallinity and the recrystallization behavior of the drug(s). For this purpose, the process parameters inlet temperature and pump feed rate were varied according to a 2(2) factorial design and the obtained samples were analyzed with X-ray powder diffractometry and Fourier-transformed infrared spectroscopy. Evaluation of the data revealed that the preparation of fully amorphous samples could be achieved depending on the process conditions. The resulting recrystallization behavior of the samples, such as the total recrystallization rate, the individual recrystallization rates of naproxen and indomethacin as well as the polymorphic form of indomethacin that was formed were influenced by these process conditions. For initially amorphous samples, it was found that naproxen and indomethacin recrystallized almost simultaneously, which supports the theory of formation of drug-drug heterodimers in the co-amorphous phase. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of rolling conditions on recrystallization microstructure and texture in magnetostrictive Fe-Ga-Al rolled sheets

NASA Astrophysics Data System (ADS)

Li, Jiheng; Liu, Yangyang; Li, Xiaojuan; Mu, Xing; Bao, Xiaoqian; Gao, Xuexu

2018-07-01

The effects of different rolling conditions on the microstructure and texture of primary and secondary recrystallization in magnetostrictive Fe82Ga9Al9+0.1at%NbC alloy sheets were investigated. After the primary recrystallization annealing at 850 °C for 5 min, the as-rolled sheets prepared by warm-cold rolling with an intermediate annealing, can be fully recrystallized, and obtain the homogeneous matrix in which the fine dispersed NbC precipitate particles are distributed. The primary recrystallization textures of sheets with different rolling conditions consist mostly of strong {1 0 0} textures, γ-fiber textures, {4 1 1}〈1 4 8〉 texture and weak Goss texture. In the primary recrystallized sheets prepared by warm-cold rolling with an intermediate annealing, the high energy grain boundaries and ∑9 boundaries have the highest proportion. After high temperature annealing, the secondary recrystallizations of Goss grains in these sheets are more complete, and the size of abnormal grown Goss grain is up to several centimeters, which results in the strongest Goss texture. Correspondingly, the largest magnetostriction of 183 ppm is observed. The sample prepared by warm-cold rolling with an intermediate annealing, has homogeneous primary matrix, special texture components and grain boundary distribution, all of which provide a better surrounding for the abnormal growth of Goss grains. This work indicates that the control of rolling conditions of Fe-Ga-Al alloy sheets is necessary to achieve the strong Goss texture and obtain a possible high magnetostriction if other appropriate conditions (stress, domain structure) are achieved.

Surface damage and structure evolution of recrystallized tungsten exposed to ELM-like transient loads

NASA Astrophysics Data System (ADS)

Yuan, Y.; Du, J.; Wirtz, M.; Luo, G.-N.; Lu, G.-H.; Liu, W.

2016-03-01

Surface damage and structure evolution of the full tungsten ITER divertor under transient heat loads is a key concern for component lifetime and plasma operations. Recrystallization caused by transients and steady-state heat loads can lead to degradation of the material properties and is therefore one of the most serious issues for tungsten armor. In order to investigate the thermal response of the recrystallized tungsten under edge localized mode-like transient thermal loads, fully recrystallized tungsten samples with different average grain sizes are exposed to cyclic thermal shocks in the electron beam facility JUDITH 1. The results indicate that not only does the microstructure change due to recrystallization, but that the surface residual stress induced by mechanical polishing strongly influences the surface cracking behavior. The stress-free surface prepared by electro-polishing is shown to be more resistant to cracking than the mechanically polished one. The resulting surface roughness depends largely on the loading conditions instead of the recrystallized-grain size. As the base temperature increases from room temperature to 400 °C, surface roughening mainly due to the shear bands in each grain becomes more pronounced, and sub-grains (up to 3 μm) are simultaneously formed in the sub-surface. The directions of the shear bands exhibit strong grain-orientation dependence, and they are generally aligned with the traces of {1 1 2} twin habit planes. The results suggest that twinning deformation and dynamic recrystallization represent the predominant mechanism for surface roughening and related microstructure evolution.

Improvement of physicomechanical properties of carbamazepine by recrystallization at different pH values.

PubMed

Javadzadeh, Yousef; Mohammadi, Ameneh; Khoei, Nazaninossadat Seyed; Nokhodchi, Ali

2009-06-01

The morphology of crystals has an appreciable impact role on the physicochemical properties of drugs. Drug properties such as flowability, dissolution, hardness and bioavailability may be affected by crystallinity behaviours of drugs. The objective of this study was to achieve an improved physicomechanical property of carbamazepine powder through recrystallization from aqueous solutions at different pH values. For this purpose, carbamazapine was recrystallized from aqueous solutions at different pH values (1, 7, 11). The morphology of crystals was investigated using scanning electron microscopy; X-ray powder diffraction (XRPD) was used to identify polymorphism; thermodynamic properties were analyzed using differential scanning calorimetery (DSC). Dissolution rate was determined using USP dissolution apparatus. Mechanical behavior of recrystallized carbamazepine powders was investigated by making tablets under different compaction pressure and measuring their hardness. SEM studies showed that the carbamazepine crystallization in different media affected the morphology and size of carbamazepine crystals. The shape of carbamazepine crystals changed from flaky or thin plate-like to needle shape. XRPD and DSC results ruled out any crystallinity changes occurring due to the temperature during recrystallization procedure or pH of crystallization media. The crushing strength of tablets indicated that all of the recrystallized carbamazepine samples had better compactiblity than the original carbamazepine powder. In vitro dissolution studies of carbamazepine samples showed a higher dissolution rate for carbamazepine crystals obtained from media with pH 11 and 1. Carbamazepine particles recrystallized from aqueous solutions of different pH values (all media) appeared to have superior mechanical properties to those of the original carbamazepine sample.

Two-step recrystallization of water in concentrated aqueous solution of poly(ethylene glycol).

PubMed

Gemmei-Ide, Makoto; Motonaga, Tetsuya; Kasai, Ryosuke; Kitano, Hiromi

2013-02-21

Crystallization behavior of water in a concentrated aqueous solution of poly(ethylene glycol) (PEG) with a water content of 37.5 wt % was investigated by temperature variable mid-infrared (mid-IR) spectroscopy in a temperature range of 298-170 K. The mid-IR spectrum of water at 298 K showed that a large water cluster was not formed and that most of the water molecules were associated with the PEG chain. Ice formation, however, occurred as found in previous studies by differential scanning calorimetory. Ice formations were grouped into three types: crystallization at 231 K during cooling, that at 198 K during heating, and that at 210 K during heating. The latter two were just recrystallization. These ice formations were the direct transition from hydration species to ice without condensation regardless of crystallization or recrystallization. This means that the recrystallized water in the present system was not generated from low-density amorphous solid water. At a low cooling rate, nearly complete crystallization at 231 K during cooling and no recrystallization were observed. At a high cooling rate, no crystallization and two-step recrystallization at 198 and 210 K were observed. The former and latter recrystallizations were found to be generated from water associated with the PEG chains with ttg (the sequence -O-CH(2)-CH(2)-O- having a trans (t) conformation about the -C-O- bond and a gauche (g) conformation about the -C-C- bond) and random conformations, respectively. These results indicate that recrystallizable water does not have a single specific water structure.

Deformation Mechanism and Recrystallization Relationships in Galfenol Single Crystals: On the Origin of Goss and Cube Orientations

NASA Astrophysics Data System (ADS)

Na, Suok-Min; Smith, Malcolm; Flatau, Alison B.

2018-06-01

In this work, deformation mechanism related to recrystallization behavior in single-crystal disks of Galfenol (Fe-Ga alloy) was investigated to gain insights into the influence of crystal orientations on structural changes and selective grain growth that take place during secondary recrystallization. We started with the three kinds of single-crystal samples with (011)[100], (001)[100], and (001)[110] orientations, which were rolled and annealed to promote the formation of different grain structures and texture evolutions. The initial Goss-oriented (011)[100] crystal mostly rotated into {111}<112> orientations with twofold symmetry and shear band structures by twinning resulted in the exposure of rolled surface along {001}<110> orientation during rolling. In contrast, the Cube-oriented (001)[100] single crystal had no change in texture during rolling with the thickness reduction up to 50 pct. The {123}<111> slip systems were preferentially activated in these single crystals during deformation as well as {112}<111> slip systems that are known to play a role in primary slip of body-centered cubic (BCC) materials such as α-iron and Fe-Si alloys. After annealing, the deformed Cube-oriented single crystal had a small fraction (<10 pct) of recrystallized Goss-oriented grains. The weak Goss component remained in the shear bands of the 50 pct rolled Goss-oriented single crystal, and it appeared to be associated with coalescence of subgrains inside shear band structures during primary recrystallization. Rolling of the (001)[110] single crystal led to the formation of a tilted (001)[100] component close to the <120> orientation, associated with {123}<111> slip systems as well. This was expected to provide potential sites of nucleation for secondary recrystallization; however, no Goss- and Cube-oriented components actually developed in this sample during secondary recrystallization. Those results illustrated how the recrystallization behavior can be influenced by deformed structure and the slip systems.

Evolution of microstructure and grain boundary character distribution of a tin bronze annealed at different temperatures

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

Huang, Weijiu; Chongqing Municipal Key Laboratory of Institutions of Higher Education for Mould Technology, Chongqing University of Technology, Chongqing 400054; Chai, Linjiang, E-mail: chailinjiang@cqut.edu.cn

2016-04-15

Specimens cut from a rolled tin bronze sheet were annealed at 400–800 °C for 1 h and evolution of their microstructures was then characterized in details by electron channeling contrast imaging and electron backscatter diffraction techniques. Particularly, statistics on special boundaries (SBs) with Σ ≤ 29 and network connectivity of random high angle boundaries (HABs) in the annealed specimens were examined to probe optimization potentials of grain boundary character distribution (GBCD) for this material. Results show that the deformed microstructure in the as-received material begins to be recrystallized when the annealing temperature increase to 500 °C and average grain sizesmore » surge with further increasing temperatures. As a result of the recrystallization, a large number of annealing twins (with Σ3 misorientation) are produced, leading to remarkably increased fractions of SBs (f{sub SBs}). Thanks to preexisting dense low angle boundaries, the majority of SBs in the 500 °C specimen with only partial recrystallization are Σ3{sub ic} (incoherent) boundaries, which effectively disrupt connectivity of random HABs network. Although the f{sub SBs} can be further increased (up to 72.5%) in specimens with full recrystallization (at higher temperatures), the Σ3{sub ic} boundaries would be replaced to some extent by Σ3{sub c} (coherent) boundaries which do not contribute directly to optimizing the GBCD. This work should be able to provide clear suggestions on applying the concept of grain boundary engineering to tin bronze alloys. - Highlights: • The rolled tin bronze begins to be recrystallized as temperature increases to 500 °C. • A lot of SBs are produced after recrystallization and the highest f{sub SBs} is 72.5%. • Partially recrystallized specimen has the optimum GBCD due to more Σ3{sub ic} boundaries. • The Σ3{sub ic} boundaries are replaced by Σ3{sub c} boundaries after full recrystallization.« less

Glass fiber processing for the Moon/Mars program: Center director's discretionary fund final report

NASA Technical Reports Server (NTRS)

Tucker, D. S.; Ethridge, E.; Curreri, P.

1992-01-01

Glass fiber has been produced from two lunar soil simulants. These two materials simulate lunar mare soil and lunar highland soil compositions, respectively. Short fibers containing recrystallized areas were produced from the as-received simulants. Doping the highland simulant with 8 weight percent B2-O3 yielded a material which could be spun continuously. The effects of lunar gravity on glass fiber formation were studied utilizing NASA's KC-135 aircraft. Gravity was found to play a major role in final fiber diameter.

Graphitization in Carbon MEMS and Carbon NEMS

NASA Astrophysics Data System (ADS)

Sharma, Swati

Carbon MEMS (CMEMS) and Carbon NEMS (CNEMS) are an emerging class of miniaturized devices. Due to the numerous advantages such as scalable manufacturing processes, inexpensive and readily available precursor polymer materials, tunable surface properties and biocompatibility, carbon has become a preferred material for a wide variety of future sensing applications. Single suspended carbon nanowires (CNWs) integrated on CMEMS structures fabricated by electrospinning of SU8 photoresist on photolithographially patterned SU8 followed by pyrolysis are utilized for understanding the graphitization process in micro and nano carbon materials. These monolithic CNW-CMEMS structures enable the fabrication of very high aspect ratio CNWs of predefined length. The CNWs thus fabricated display core---shell structures having a graphitic shell with a glassy carbon core. The electrical conductivity of these CNWs is increased by about 100% compared to glassy carbon as a result of enhanced graphitization. We explore various tunable fabrication and pyrolysis parameters to improve graphitization in the resulting CNWs. We also suggest gas-sensing application of the thus fabricated single suspended CNW-CMEMS devices by using the CNW as a nano-hotplate for local chemical vapor deposition. In this thesis we also report on results from an optimization study of SU8 photoresist derived carbon electrodes. These electrodes were applied to the simultaneous detection of traces of Cd(II) and Pb(II) through anodic stripping voltammetry and detection limits as low as 0.7 and 0.8 microgL-1 were achieved. To further improve upon the electrochemical behavior of the carbon electrodes we elucidate a modified pyrolysis technique featuring an ultra-fast temperature ramp for obtaining bubbled porous carbon from lithographically patterned SU8. We conclude this dissertation by suggesting the possible future works on enhancing graphitization as well as on electrochemical applications

Retention and effective diffusion of model metabolites on porous graphitic carbon.

PubMed

Lunn, Daniel B; Yun, Young J; Jorgenson, James W

2017-12-29

The study of metabolites in biological samples is of high interest for a wide range of biological and pharmaceutical applications. Reversed phase liquid chromatography is a common technique used for the separation of metabolites, but it provides little retention for polar metabolites. An alternative to C18 bonded phases, porous graphitic carbon has the ability to provide significant retention for both non-polar and polar analytes. The goal of this work is to study the retention and effective diffusion properties of porous graphitic carbon, to see if it is suitable for the wide injection bands and long run times associated with long, packed capillary-scale separations. The retention of a set of standard metabolites was studied for both stationary phases over a wide range of mobile phase conditions. This data showed that porous graphitic carbon benefits from significantly increased retention (often >100 fold) under initial gradient conditions for these metabolites, suggesting much improved ability to focus a wide injection band at the column inlet. The effective diffusion properties of these columns were studied using peak-parking experiments with the standard metabolites under a wide range of retention conditions. Under the high retention conditions, which can be associated with retention after injection loading for gradient separations, D eff /D m ∼0.1 for both the C18-bonded and porous graphitic carbon columns. As C18 bonded particles are widely, and successfully utilized for long gradient separations without issue of increasing peak width from longitudinal diffusion, this suggests that porous graphitic carbon should be amenable for long runtime gradient separations as well. Copyright © 2017 Elsevier B.V. All rights reserved.

Compatibility of the Radio Frequency Mass Gauge with Graphite-Epoxy Composite Tanks

NASA Technical Reports Server (NTRS)

Zimmerli, G. A.; Mueller, C. H.

2015-01-01

The radio frequency mass gauge (RFMG) is a low-gravity propellant quantity gauge being developed at NASA for possible use in long-duration space missions utilizing cryogenic propellants. As part of the RFMG technology development process, we evaluated the compatibility of the RFMG with a graphite-epoxy composite material used to construct propellant tanks. The key material property that can affect compatibility with the RFMG is the electrical conductivity. Using samples of 8552/IM7 graphite-epoxy composite, we characterized the resistivity and reflectivity over a range of frequencies. An RF impedance analyzer was used to characterize the out-of-plane electrical properties (along the sample thickness) in the frequency range 10 to 1800 MHZ. The resistivity value at 500 MHz was 4.8 ohm-cm. Microwave waveguide measurements of samples in the range 1.7 - 2.6 GHz, performed by inserting the samples into a WR-430 waveguide, showed reflectivity values above 98%. Together, these results suggested that a tank constructed from graphite/epoxy composite would produce good quality electromagnetic tank modes, which is needed for the RFMG. This was verified by room-temperature measurements of the electromagnetic modes of a 2.4 m diameter tank constructed by Boeing from similar graphite-epoxy composite material. The quality factor Q of the tank electromagnetic modes, measured via RF reflection measurements from an antenna mounted in the tank, was typically in the range 400 less than Q less than 3000. The good quality modes observed in the tank indicate that the RFMG is compatible with graphite-epoxy tanks, and thus the RFMG could be used as a low-gravity propellant quantity gauge in such tanks filled with cryogenic propellants.

Automated eddy current analysis of materials

NASA Technical Reports Server (NTRS)

Workman, Gary L.

1991-01-01

The use of eddy current techniques for characterizing flaws in graphite-based filament-wound cylindrical structures is described. A major emphasis was also placed upon incorporating artificial intelligence techniques into the signal analysis portion of the inspection process. Developing an eddy current scanning system using a commercial robot for inspecting graphite structures (and others) was a goal in the overall concept and is essential for the final implementation for the expert systems interpretation. Manual scans, as performed in the preliminary work here, do not provide sufficiently reproducible eddy current signatures to be easily built into a real time expert system. The expert systems approach to eddy current signal analysis requires that a suitable knowledge base exist in which correct decisions as to the nature of a flaw can be performed. A robotic workcell using eddy current transducers for the inspection of carbon filament materials with improved sensitivity was developed. Improved coupling efficiencies achieved with the E-probes and horseshoe probes are exceptional for graphite fibers. The eddy current supervisory system and expert system was partially developed on a MacIvory system. Continued utilization of finite element models for predetermining eddy current signals was shown to be useful in this work, both for understanding how electromagnetic fields interact with graphite fibers, and also for use in determining how to develop the knowledge base. Sufficient data was taken to indicate that the E-probe and the horseshoe probe can be useful eddy current transducers for inspecting graphite fiber components. The lacking component at this time is a large enough probe to have sensitivity in both the far and near field of a thick graphite epoxy component.

Magnified fluorescence detection of silver(I) ion in aqueous solutions by using nano-graphite-DNA hybrid and DNase I.

PubMed

Wei, Yin; Li, Bianmiao; Wang, Xu; Duan, Yixiang

2014-08-15

This paper describes a novel approach utilizing nano-graphite-DNA hybrid and DNase I for the amplified detection of silver(I) ion in aqueous solutions for the first time. Nano-graphite can effectively quench the fluorescence of dye-labeled cytosine-rich single-stranded DNA due to its strong π-π stacking interactions; however, in the presence of Ag(+), C-Ag(+)-C coordination induces the probe to fold into a hairpin structure, which does not adsorb on the surface of nano-graphite and thus retains the dye fluorescence. Meanwhile, the hairpin structure can be cleaved by DNase I, and in such case Ag(+) is delivered from the complex. The released Ag(+) then binds other dye-labeled single-stranded DNA on the nano-graphite surface, and touches off another target recycling, resulting in the successive release of dye-labeled single-stranded DNA from the nano-graphite, which leads to significant amplification of the signal. The present magnification sensing system exhibits high sensitivity toward Ag(+) with a limit of detection of 0.3nM (S/N=3), which is much lower than the standard for Ag(+) in drinking water recommended by the Environmental Protection Agency (EPA). The selectivity of the sensor for Ag(+) against other biologically and environmentally related metal ions is outstanding due to the high specificity of C-Ag(+)-C formation. Moreover, the sensing system is used for the determination of Ag(+) in river water samples with satisfying results. The proposed assay is simple, cost-effective, and might open the door for the development of new assays for other metal ions or biomolecules. Copyright © 2014 Elsevier B.V. All rights reserved.

ELECTROCHEMICAL DECHLORINATION OF TRICHLOROETHYLENE USING GRANULAR-GRAPHITE ELECTRODES: IDENTIFICATION AND QUANTIFICATION OF DECHLORINATION PRODUCTS

EPA Science Inventory

Electrochemical degradation (ECD) utilizes high redox potential at the anode and low redox potential at the cathode to oxidize and/or reduce organic and inorganic contaminants. ECD of Trichloroethylene (TCE), although theoretically possible, has not been experimentally proven. Th...

Effect of Aluminum on the Microstructure and Properties of Two Refractory High-Entropy Alloys (Postprint)

DTIC Science & Technology

2014-04-01

The chemical compositions of the recrystallized ic release; distribution unlimited. Fig. 5. (a) Equiaxed grain structure of the annealed...deformation bands crossing a grain boundary; (c) fine recrystallized grains formed at grain boundaries; (d) a higher magnification image shows the...presence of nano-precipitates at the boundaries of the recrystallized grains. 220 O.N. Senkov et al. / Acta Materialia 68 (2014) 214–228and non

High temperature blackbody BB2000/40 for calibration of radiation thermometers and thermocouple

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

Ogarev, S. A.; Khlevnoy, B. B.; Samoylov, M. L.

2013-09-11

The cavity-type high temperature blackbody (HTBB) models of BB3200/3500 series are the most spread among metrological institutes worldwide as sources for radiometry and radiation thermometry, due to their ultra high working temperatures, high emissivity and stability. The materials of radiating cavities are graphite, pyrolytic graphite (PG) and their combination. The paper describes BB2000/40 blackbody with graphite-tube cavity that was developed for calibration of radiation thermometers at SCEI (Singapore). The peculiarity of BB2000/40 is a possibility to use it, besides calibration of pyrometers, as an instrument for thermocouples calibration. Operating within the temperature range from 900 °C to 2000 °C, themore » blackbody has a wide cavity opening of 40 mm. Emissivity of the cavity, with PG heater rings replaced partly by graphite elements, was estimated as 0.998 ± 0.0015 in the spectral range from 350 nm to 2000 nm. The uniformity along the cavity axis, accounting for 10 °C, was measured using a B-type thermocouple at 1500 °C. The BB2000/40, if necessary, can be easily modified, by replacing the graphite radiator with a set of PG rings, to be able to reach temperatures as high as 3200 °C. The HTBB utilizes an optical feedback system which allows temperature stabilization within 0.1 °C. This rear-view feedback allows the whole HTBB aperture to be used for measurements.« less

Research and Process-Optimization on Mixed Crystal Caused Uneven-Performance of High-strength Structural Car Steel QStE500TM

NASA Astrophysics Data System (ADS)

Jian-wen, Li; Hong-yan, Liu

Handan Iron and Steel production of high-strength structural car steel QStE500TM thin gauge products using Nb + Ti composite strengthening, with a small amount of Cr element to improve its hardenability, the process parameter control is inappropriate with Nb + Ti complex steel, it is easy to produce in the mixed crystal phenomenon, resulting in decreasing the toughness and uneven performance. In this paper, Gleeble 3500 thermal simulation testing machine for high-strength structural steel car QStE500TM product deformation austenite recrystallization behavior research, determined completely recrystallized, partial recrystallization and non-recrystallization region, provide theoretical basis and necessary data for reasonable controlled rolling process for production.

Ice-Active Substances from the Infective Juveniles of the Freeze Tolerant Entomopathogenic Nematode, Steinernema feltiae.

PubMed

Ali, Farman; Wharton, David A

2016-01-01

Steinernema feltiae is a moderately freezing tolerant nematode, that can withstand intracellular ice formation. We investigated recrystallization inhibition, thermal hysteresis and ice nucleation activities in the infective juveniles of S. feltiae. Both the splat cooling assay and optical recrystallometry indicate the presence of ice active substances that inhibit recrystallization in the nematode extract. The substance is relatively heat stable and largely retains the recrystallization inhibition activity after heating. No thermal hysteresis activity was detected but the extract had a typical hexagonal crystal shape when grown from a single seed crystal and weak ice nucleation activity. An ice active substance is present in a low concentration, which may be involved in the freezing survival of this species by inhibiting ice recrystallization.

Highly catalytic and stabilized titanium nitride nanowire array-decorated graphite felt electrodes for all vanadium redox flow batteries

NASA Astrophysics Data System (ADS)

Wei, L.; Zhao, T. S.; Zeng, L.; Zeng, Y. K.; Jiang, H. R.

2017-02-01

In this work, we prepare a highly catalytic and stabilized titanium nitride (TiN) nanowire array-decorated graphite felt electrode for all vanadium redox flow batteries (VRFBs). Free-standing TiN nanowires are synthesized by a two-step process, in which TiO2 nanowires are first grown onto the surface of graphite felt via a seed-assisted hydrothermal method and then converted to TiN through nitridation reaction. When applied to VRFBs, the prepared electrode enables the electrolyte utilization and energy efficiency to be 73.9% and 77.4% at a high current density of 300 mA cm-2, which are correspondingly 43.3% and 15.4% higher than that of battery assembled with a pristine electrode. More impressively, the present battery exhibits good stability and high capacity retention during the cycle test. The superior performance is ascribed to the significant improvement in the electrochemical kinetics and enlarged active sites toward V3+/V2+ redox reaction.

Hierarchically Porous Graphitic Carbon with Simultaneously High Surface Area and Colossal Pore Volume Engineered via Ice Templating

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

Estevez, Luis; Prabhakaran, Venkateshkumar; Garcia, Adam L.

Developing hierarchical porous carbon (HPC) materials with competing textural characteristics such as surface area and pore volume in one material is difficult to accomplish—particulalry for an atomically ordered (graphitic) carbon. Herein we describe a synthesis strategy to engineer tunable hierarchically porous carbon (HPC) materials across micro- meso- and macroporous length scales, allowing the fabrication of a graphitic HPC with both very high surface area (> 2500 m2/g) and pore volume (>10 cm3/g), the combination of which has not been seen previously. The mesopore volume alone for these materials is up to 7.91 cm3/g, the highest ever reported. The unique materialmore » was explored for use as a supercapaictor electrode and for oil adsorption; two applications that require textural properties that are typicaly exclusive to one another. This design scheme for HPCs can be utilized in broad applications, including electrochemical systems such as batteries and supercapacitors, sorbents, and catalyst supports.« less

Atomic intercalation to measure adhesion of graphene on graphite

PubMed Central

Wang, Jun; Sorescu, Dan C.; Jeon, Seokmin; Belianinov, Alexei; Kalinin, Sergei V.; Baddorf, Arthur P.; Maksymovych, Petro

2016-01-01

The interest in mechanical properties of two-dimensional materials has emerged in light of new device concepts taking advantage of flexing, adhesion and friction. Here we demonstrate an effective method to measure adhesion of graphene atop highly ordered pyrolytic graphite, utilizing atomic-scale ‘blisters' created in the top layer by neon atom intercalates. Detailed analysis of scanning tunnelling microscopy images is used to reconstruct atomic positions and the strain map within the deformed graphene layer, and demonstrate the tip-induced subsurface translation of neon atoms. We invoke an analytical model, originally devised for graphene macroscopic deformations, to determine the graphite adhesion energy of 0.221±0.011 J m−2. This value is in excellent agreement with reported macroscopic values and our atomistic simulations. This implies mechanical properties of graphene scale down to a few-nanometre length. The simplicity of our method provides a unique opportunity to investigate the local variability of nanomechanical properties in layered materials. PMID:27796294

Barite recrystallization in the presence of 226Ra and 133Ba

NASA Astrophysics Data System (ADS)

Heberling, Frank; Metz, Volker; Böttle, Melanie; Curti, Enzo; Geckeis, Horst

2018-07-01

Despite the long history of studies on (Ba,Ra)SO4, various recent investigations aimed at improving our understanding of its formation processes and thermodynamics. Accumulation of natural Ra isotopes (mainly 226Ra and 228Ra) in (Ba,Ra)SO4 plays an important role in many geotechnical applications and water desalination facilities. In the near field of a nuclear waste repository, barite formation may be expected e.g. as a consequence of contact of spent nuclear fuel or vitrified high level waste with sulfate containing ground water, and may control the potential release of Ra from waste forms upon leakage. Here, we present results of long term batch-type barite recrystallization experiments conducted in the simultaneous presence of 226Ra and 133Ba as a function of initial Ra2+ concentration and pH with the same type and charge of barite powder as used in previous studies (Curti et al., 2010; Klinkenberg et al., 2014; Brandt et al., 2015). Due to the simultaneous measurement of 133Ba and 226Ra our data allow for a direct relation of 226Ra uptake with barite recrystallization, which leads to more accurate partition coefficients compared to previous studies. During a reaction period of five years, barite is continuously recrystallizing. Within the investigated radium concentration range (Ba(1-X)RaXSO4 with X < 0.0006), we measure a partition coefficient of D = 2.1 ± 0.5. The partition coefficient is constant within uncertainty during almost five years (1793 days) of experimental duration. This value is in line with a description of (Ba,Ra)SO4 as an ideal solid solution based on the solubility products (KSP) of the endmembers barite (log10(KSP(barite)) = -9.97) and radium sulfate (log10(KSP(RaSO4)) = -10.26; dimensionless Guggenheim parameter, a0 = 0.0 ± 0.3). Apparent discrepancies to previous theoretical results (a0 = 1.0 ± 0.4) may be resolved when the uncertainties related to the solubility of RaSO4 are considered. Compared to results of previous publications, recrystallization is extremely slow in the experiments presented here. While previous authors suggested complete equilibration of bulk microcrystalline barite within less than three years, a recrystallization of less than 7% of the barite mass is observed within five years. We describe the progress of recrystallization with a new modified homogeneous recrystallization model. Observed recrystallization rates are in the range 0.11-1.5 nmol/(m2 s) and increase with decreasing pH. According to this modified homogeneous recrystallization model, complete bulk barite equilibration is expected in about 1400-16,900 years. The strongly decreased recrystallization kinetics in our experiments is likely related to a strongly prolonged pre-equilibration time (0.8 years), which according to XRD investigations, leads to a higher crystallinity (higher crystal domain size and lower Debye-Waller parameters) of the barite powder.

Deformation Enhanced Recrystallization of Titanite: Insight from the Western Gneiss Region Ultrahigh-Pressure Terrane

NASA Astrophysics Data System (ADS)

Gordon, S. M.; Reddy, S. M.; Blatchford, H.; Whitney, D. L.; Kirkland, C. L.; Teyssier, C.; Evans, N. J.; McDonald, B.

2017-12-01

Titanite readily recrystallizes due to metamorphism, deformation, and/or fluids making it an ideal chronometer for tracking the exhumation of high-grade rocks. The Western Gneiss Region (WGR), Norway, is a giant UHP terrane exhumed as a fairly coherent slab. Parts of the WGR underwent little deformation during exhumation; however, meters-scale shear zones, located across the WGR, deformed over a range of pressures, from (U)HP to amphibolite facies. Titanite from quartzofeldpathic gneiss within, directly adjacent to, and 300 m away from a mylonitic shear zone within the southern WGR have been analyzed to track exhumation and investigate effects of deformation on recrystallization and trace-element mobility. EBSD was used to characterize the microstructural evolution of the gneisses, and trace-element concentrations and timing of recrystallization were estimated by split-stream LA-ICPMS. Titanite grain size decreases from outside (>200) to inside (<75 µm) the shear zone. Gneiss in and directly adjacent to the shear zone contain partially to completely recrystallized grains, with 207-corrected 206Pb/238U ages of <405 Ma. Gneiss within the shear zone shows a greater percentage of recrystallized grains. EBSD data indicate that some titanite comprises multiple subgrains within an optically coherent single grain. Subgrains in titanite cores show evidence of inherited radiogenic Pb, whereas subgrains in rims and tails of deformed sigma grains were recrystallized. In a gneiss directly adjacent to the shear zone, optically coherent grains are zoned, with increasing Sr and decreasing Zr from core to rim; titanite subgrains within the shear-zone gneiss are too small to analyze. In comparison, titanite from the gneiss outside the shear zone does not show any internal microstructures or evidence for Scandian recrystallization and has low U and high 204Pb. These results show that most trace elements are unaffected by deformation of titanite; however, Pb is mobile. Deformation thus plays an important role in resetting U-Pb systematics and allows the timing of shear zone development to be linked to the early stages of eclogite exhumation at ca. 405 Ma. Atom-probe analyses of adjacent subgrains, one that has recrystallized and one with an inherited age, will provide insight into trace-element mobility on the nm-scale.

[Comporison Sduty of Microstructure by Metallographicalk on the Polarized Light and Texture by XRD of CC 5083 and CC 5182 Aluminium Alloy after Cold Rolling and Recrystallization].

PubMed

Chen, Ming-biao; Li, Yong-wei; Tan, Yuan-biao; Ma, Min; Wang, Xue-min; Liu, Wen-chang

2015-03-01

At present the study of relation between microstructure, texture and performance of CC 5083 aluminium alloy after cold tolling and recrystallization processes is still finitude. So that the use of the CC 5083 aluminium alloy be influenced. Be cased into electrical furnace, hot up with unlimited speed followed the furnace hot up to different temperature and annealed 2h respectively, and be cased into salt-beth furnace, hot up quickly to different temperature and annealed 30 min respectively for CC 5083 and CC 5182 aluminum alloy after cold roling with 91.5% reduction. The microstructure be watched use metallographic microscope, the texture be inspected by XRD. The start temperature of recrystallization and grain grow up temperature within annealing in the electric furnace of CC 5083 aluminum alloy board is 343 degrees C, and the shap of grain after grow up with long strip (the innovation point ); The start temperature of recrystallization within annealling in the salt bath furnace of CC 5083 is 343 degrees C. The start temperature and end temperature of recrystallization within annealling of CC 5083 and CC 5182 aluminum alloy is 371 degrees C. The grain grow up outstanding of cold rooled CC 5152 aluminum alloy after annealed with 454 degrees C in the electric furnace and salt bath furnace. The start temperature of grain grow up of CC 5083 alluminurn alloy annealed in the electric furnace and salt bath furnace respectively is higher than the start temperature of grain grow up of CC 5182 alluminum alloy annealed in the electric furnace and salt bath furnace respectively. The strat temperature of recrystallization grain grow up is higher than which annealled with other three manner annealing process. The recrystallization temperature of CC 5182 annealed in the salt bath furnace is higher than which annealed in the electric furnace. The recrystallization temperature of the surface layer of CC 5083 and CC 5182 aluminum alloy is higher than the inner layer (the innovation point). There is a difference each other of the structure and the texture of the four manner annealing aluminum alloy (the innovation point). There is a little difference at the recrystallization processes course reflectived by the observe results of structure transform and by the examination results of texture transmission.

Deformation Enhanced Recrystallization of Titanite: Insight from the Western Gneiss Region Ultrahigh-Pressure Terrane

NASA Astrophysics Data System (ADS)

Gordon, S. M.; Reddy, S. M.; Blatchford, H.; Whitney, D. L.; Kirkland, C. L.; Teyssier, C.; Evans, N. J.; McDonald, B.

2016-12-01

Titanite readily recrystallizes due to metamorphism, deformation, and/or fluids making it an ideal chronometer for tracking the exhumation of high-grade rocks. The Western Gneiss Region (WGR), Norway, is a giant UHP terrane exhumed as a fairly coherent slab. Parts of the WGR underwent little deformation during exhumation; however, meters-scale shear zones, located across the WGR, deformed over a range of pressures, from (U)HP to amphibolite facies. Titanite from quartzofeldpathic gneiss within, directly adjacent to, and 300 m away from a mylonitic shear zone within the southern WGR have been analyzed to track exhumation and investigate effects of deformation on recrystallization and trace-element mobility. EBSD was used to characterize the microstructural evolution of the gneisses, and trace-element concentrations and timing of recrystallization were estimated by split-stream LA-ICPMS. Titanite grain size decreases from outside (>200) to inside (<75 µm) the shear zone. Gneiss in and directly adjacent to the shear zone contain partially to completely recrystallized grains, with 207-corrected 206Pb/238U ages of <405 Ma. Gneiss within the shear zone shows a greater percentage of recrystallized grains. EBSD data indicate that some titanite comprises multiple subgrains within an optically coherent single grain. Subgrains in titanite cores show evidence of inherited radiogenic Pb, whereas subgrains in rims and tails of deformed sigma grains were recrystallized. In a gneiss directly adjacent to the shear zone, optically coherent grains are zoned, with increasing Sr and decreasing Zr from core to rim; titanite subgrains within the shear-zone gneiss are too small to analyze. In comparison, titanite from the gneiss outside the shear zone does not show any internal microstructures or evidence for Scandian recrystallization and has low U and high 204Pb. These results show that most trace elements are unaffected by deformation of titanite; however, Pb is mobile. Deformation thus plays an important role in resetting U-Pb systematics and allows the timing of shear zone development to be linked to the early stages of eclogite exhumation at ca. 405 Ma. Atom-probe analyses of adjacent subgrains, one that has recrystallized and one with an inherited age, will provide insight into trace-element mobility on the nm-scale.

Influence of warm rolling temperature on ferrite recrystallization in low C and IF steels

NASA Astrophysics Data System (ADS)

Barnett, Matthew Robert

Experiments involving single pass laboratory rolling and isothermal salt bath annealing were carried out; three steels were studied: a titanium stabilized interstitial free grade and two low carbon grades, one of which contained a particularly low level of manganese (˜0.009wt.%). The two low carbon grades were produced such that any complication from AlN precipitation was avoided. X-ray, neutron diffraction, optical metallography and mechanical testing measurements were carried out on the samples before and after annealing. The main aim of this work was to further the understanding of the metallurgy of recrystallization after ferrite rolling at temperatures between room temperature and 700sp°C. Deformation textures, recrystallization kinetics, final grain sizes and recrystallization textures were quantified for all the samples and experimental conditions. A major conclusion based on these data is that the influence of rolling temperature is far greater in the low carbon samples than in the IF grade. Indeed, the IF results alter only marginally with increasing temperature. In the low carbon grades, however, the rolling texture sharpens, recrystallization slows, the final grain size coarsens, and the recrystallization texture changes when the rolling temperature is increased. This distinct difference between the two steel types is explained in terms of their contrasting deformation behaviors. Solute carbon and nitrogen in the low carbon grades interact with dislocations causing high stored energy levels after low temperature rolling (due to dynamic strain aging) and high strain rate sensitivities during high temperature rolling (due to the solute drag of dislocations in the transition region between DSA and DRC). Nucleation during subsequent recrystallization is strongly influenced by both the stored energy and the strain rate sensitivity. The latter affects the occurrence of the flow localisations that enhance nucleation.

Effects of V addition on recrystallization resistance of 7150 aluminum alloy after simulative hot deformation

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

Lai, Jing; Shi, Cangji; Chen, X.-Grant, E-mail: xgrant_chen@uqac.ca

2014-10-15

The effects of different V contents (0.01 to 0.19 wt.%) on the recrystallization resistance of 7150 aluminum alloys during post-deformation heat treatment were investigated. The microstructural evolutions at as-cast, as-homogenized conditions and after post-deformation annealing were studied using optical, scanning electron and transmission electron microscopes and using the electron backscattered diffraction technique. The precipitation of Al{sub 21}V{sub 2} dispersoids was observed in alloys containing 0.11 to 0.19 wt.% V after homogenization. The dispersoids were mainly distributed in the dendrite cells, and the precipitate-free zones occurred in the interdendritic regions and near grain boundaries. V addition could significantly enhance the recrystallizationmore » resistance during post-deformation annealing, particularly in the presence of a great number of Al{sub 21}V{sub 2} dispersoids. Recrystallized grain growth was effectively restricted because of the dispersoid pinning effect. The alloy containing 0.15 wt.% V exhibited the highest recrystallization resistance amongst all V-containing alloys studied. - Highlights: • Investigated the effect of V level on microstructure and flow stress of 7150 alloys • Characterized microstructures using optical microscopy, SEM, TEM and EBSD • Described the precipitation behavior of V-dispersoids in the dendritic structure • Studied the V effect on recrystallization resistance during post heat treatment • V addition greatly enhanced the recrystallization resistance during annealing.« less

Recrystallization and grain growth phenomena in a particle-reinforced aluminum composite

NASA Astrophysics Data System (ADS)

van Aken, D. C.; Krajewski, P. E.; Vyletel, G. M.; Allison, J. E.; Jones, J. W.

1995-06-01

Recrystallization and grain growth in a 2219/TiC/15p composite were investigated as functions of the amount of deformation and deformation temperature. Both cold and hot deformed samples were annealed at the normal solution treatment temperature of 535 °C. It was shown that large recrystallized grain diameters, relative to the interparticle spacing, could be produced in a narrow range of deformation for samples cold-worked and those hot-worked below 450 °C. For cold-worked samples, between 4 to 6 pct deformation, the recrystallized grain diameters varied from 530 to 66 μm as the amount of deformation increased. Subsequent grain growth was not observed in these recrystallized materials and noncompact grain shapes were observed. For deformations greater than 15 pct, recrystallized grain diameters less than the interparticle spacing were observed and subsequent grain growth produced a pinned grain diameter of 27 μm. The pinned grain diameter agreed well with an empirical model based on three dimensional (3-D) Monte Carlo simulations of grain growth and particle pinning in a two-phase material. Tensile properties were determined as a function of grain size, and it was shown that grain size had a weak influence on yield strength. A maximum in the yield strength was observed at a grain size larger than the normal grain growth and particle-pinned diameter.

Dynamic Recrystallization of the Constituent γ Phase and Mechanical Properties of Ti-43Al-9V-0.2Y Alloy Sheet.

PubMed

Zhang, Yu; Wang, Xiaopeng; Kong, Fantao; Chen, Yuyong

2017-09-15

A crack-free Ti-43Al-9V-0.2Y alloy sheet was successfully fabricated via hot-pack rolling at 1200 °C. After hot-rolling, the β/γ lamellar microstructure of the as-forged TiAl alloy was completely converted into a homogeneous duplex microstructure with an average γ grain size of 10.5 μm. The dynamic recrystallization (DRX) of the γ phase was systematically investigated. A recrystallization fraction of 62.5% was obtained for the γ phase in the TiAl alloy sheet, when a threshold value of 0.8° was applied to the distribution of grain orientation spread (GOS) values. The high strain rate and high stress associated with hot-rolling are conducive for discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), respectively. A certain high-angle boundary (HAGB: θ = 89° ± 3°<100>), which is associated with DDRX, occurs in both the recrystallized and deformed γ grains. The twin boundaries play an important role in the DDRX of the γ phase. Additionally, the sub-structures and sub-boundaries originating from low-angle boundaries in the deformed grains also indicate that CDRX occurs. The mechanical properties of the alloy sheet were determined at both room and elevated temperatures. At 750 °C, the alloy sheet exhibited excellent elongation (53%), corresponding to a failure strength of 467 MPa.

[Investigation of the recrystallization of trehalose as a good glass-former excipient].

PubMed

Katona, Gábor; Orsolya, Jójártné Laczkovich; Szabóné, Révész Piroska

2014-01-01

An amorphous form of trehalose is easy to prepare by using a solvent method. The recrystallization kinetics can be followed well, which is important because of the occurrence of polymorphic forms of trehalose. This is especially significant in the case of dry powder inhalers. Spray-drying was used as a preparation method this being one of the most efficient technologies with which to obtain an amorphous form. This method can result in the required particle size and a monodisperse distribution with excellent flowability and with moreover considerable amorphization. In our work, trehalose was applied as a technological auxiliary agent, and literature data relating to the spray-drying technology of trehalose were collected. Studies were made of the influence of the spraying process on the amorphization of trehalose and on the recrystallization of amorphous trehalose during storage. Amorphous samples were investigated under 3 different conditions during 3 months. The recrystallization process was followed by differential scanning calorimetry and X-ray powder diffraction. The results demonstrated the perfect amorphization of trehalose during the spray-drying process. The glass transition temperature was well measurable in the samples and proved to be the same as the literature data. Recrystallization under normal conditions was very slow but at high relative humidity the process was accelerated greatly. Amorphous trehalose gave rise to dihydrate forms (gamma- and h-trehaloses) during recrystallization, and beta-trehalose was also identified as an anhydrous form.

Air Proportional Counter

DOEpatents

Simpson, Jr, J A

1950-12-05

A multiple wire counter utilizing air at atmospheric pressure as the ionizing medium and having a window of a nylon sheet of less than 0.5 mil thickness coated with graphite. The window is permeable to alpha particles so that the counter is well adapted to surveying sources of alpha radiation.

Recrystallization in Si upon ion irradiation at room temperature in Co/Si(111) thin film systems

NASA Astrophysics Data System (ADS)

Banu, Nasrin; Satpati, B.; Dev, B. N.

2018-04-01

After several decades of research it was concluded that for a constant flux recrystallization in Si upon ion irradiation is possible only at high temperature. At low temperature or at room temperature only amorphization can take place. However we have observed recrystallization in Si upon ion irradiation at room temperature in a Co/Si thin film system. The Co/Si sample was prepared by deposition of 25 nm Co on clean Si(111) substrate. An oxide layer (˜ 2nm) of cobalt at the top of the film due to air exposure. The ion irradiation was done at room temperature under high vacuum with 1MeV Si+ ion with low beam current < 400 nA. Earlier we have shown similar ion induced recrystallization in Si(100) substrate which had a sandwich Si/Ni/Si structure. This system had an epitaxial buffer Si layer on Si substrate. This study also shows that the phenomenon is independent of substrate orientation and buffer layer. We have used transmission electron microscopy (TEM) to study the recrystallization behavior.

Purification and crystal growth of NPB via imidazolium based ionic liquids

NASA Astrophysics Data System (ADS)

Oh, Yong-Taeg; Shin, Dong-Chan

2018-04-01

Here we report the production of high purity and crystallinity organic electronic material of NPB (N,N‧-Di-[(1-naphthyl)-N,N‧-diphenyl]-1,1‧-biphenyl-4,4‧-diamine (C44H32N2) through solution recrystallization within imidazolium based ionic liquids. When low purity NPB was recrystallized at 170 °C within C8MIM[TFSI], its purity was drastically improved from 82% to 99.92%. These recrystallized NPB crystals showed 0.040° FWHM (Full Width Half Maximum) of X-ray (1 1 1) diffraction peak. Such small FWHM angle indicates single-crystal like crystallinity. Initial NPB powder was dissolved at 100 °C and recrystallized at temperature above 110 °C. At higher temperature of 170 °C, a small number of bigger crystals were formed compared to those at 110 °C. This can be well explained by the classical nucleation and growth theory. Therefore, solution recrystallization process using ionic liquid might be promising for mass production of organic electronic materials by replacing the widely-used sublimation purification method.

Microstructural Evolution During Cold Rolling and Subsequent Annealing in Low-Carbon Steel with Different Initial Microstructures

NASA Astrophysics Data System (ADS)

Ogawa, Toshio; Dannoshita, Hiroyuki; Maruoka, Kuniaki; Ushioda, Kohsaku

2017-08-01

Microstructural evolution during cold rolling and subsequent annealing of low-carbon steel with different initial microstructures was investigated from the perspective of the competitive phenomenon between recrystallization of ferrite and reverse phase transformation from ferrite to austenite. Three kinds of hot-rolled sheet specimens were prepared. Specimen P consisted of ferrite and pearlite, specimen B consisted of bainite, and specimen M consisted of martensite. The progress of recovery and recrystallization of ferrite during annealing was more rapid in specimen M than that in specimens P and B. In particular, the recrystallized ferrite grains in specimen M were fine and equiaxed. The progress of ferrite-to-austenite phase transformation during intercritical annealing was more rapid in specimen M than in specimens P and B. In all specimens, the austenite nucleation sites were mainly at high-angle grain boundaries, such as those between recrystallized ferrite grains. The austenite distribution was the most uniform in specimen M. Thus, we concluded that fine equiaxed recrystallized ferrite grains were formed in specimen M, leading to a uniform distribution of austenite.

High-Temperature Flow Stress and Recrystallization Characteristics of Al-Bearing Microalloyed TWIP Steels

NASA Astrophysics Data System (ADS)

Somani, Mahesh Chandra; Porter, David A.; Hamada, Atef S.; Karjalainen, L. Pentti

2015-11-01

In this study, the effects of microalloying (Nb,V) and aluminum on the constitutive flow behavior and static recrystallization (SRX) characteristics of microalloyed TWIP steels (Fe-20Mn-0.6C-Al-(Nb,V)) have been investigated under hot deformation conditions. Compression tests in a Gleeble simulator, including the double-hit technique, enabled the acquisition of flow stress and recrystallization data. These were analyzed to determine the powers of strain and strain rate as well as the activation energies of deformation and recrystallization ( Q def and Q rex). Aluminum increased the flow stress and activation energy of deformation and delayed the onset of dynamic recrystallization of microalloyed TWIP steels. While microalloying with V up to 0.3 pct seems to have little or no effect on the SRX kinetics, microalloying with 0.026 pct Nb significantly slowed down the SRX rate, similarly as in the case of low C-Mn steels. Addition of high aluminum (4.9 pct) marginally retarded the SRX kinetics in comparison with the steels with low aluminum (1.5 pct), with or without microalloying with V.

Physical aging in graphite/epoxy composites

NASA Technical Reports Server (NTRS)

Kong, E. S. W.

1983-01-01

Sub-Tg annealing has been found to affect the properties of graphite/epoxy composites. The network epoxy studied was based on the chemistry of tetraglycidyl 4,4'-diamino-diphenyl methane (TGDDM) crosslinked by 4,4'-diamino-diphenyl sulfone (DDS). Differential scanning calorimetry, thermal mechanical analysis, and solid-state cross-polarized magic-angle-spinning nuclear magnetic resonance spectroscopy have been utilized in order to characterize this process of recovery towards thermodynamic equilibrium. The volume and enthalpy recovery as well as the 'thermoreversibility' aspects of the physical aging are discussed. This nonequilibrium and time-dependent behavior of network epoxies are considered in view of the increasingly wide applications of TGDDM-DDS epoxies as matrix materials of structural composites in the aerospace industry.

Exploring electrolyte preference of vanadium nitride supercapacitor electrodes

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

Wang, Bo; Chen, Zhaohui; Lu, Gang

Highlights: • Hierarchical VN nanostructures were prepared on graphite foam. • Electrolyte preference of VN supercapacitor electrodes was explored. • VN showed better capacitive property in organic and alkaline electrolytes than LiCl. - Abstract: Vanadium nitride hierarchical nanostructures were prepared through an ammonia annealing procedure utilizing vanadium pentoxide nanostructures grown on graphite foam. The electrochemical properties of hierarchical vanadium nitride was tested in aqueous and organic electrolytes. As a result, the vanadium nitride showed better capacitive energy storage property in organic and alkaline electrolytes. This work provides insight into the charge storage process of vanadium nitride and our findings canmore » shed light on other transition metal nitride-based electrochemical energy storage systems.« less

Self-sensing paper-based actuators employing ferromagnetic nanoparticles and graphite

NASA Astrophysics Data System (ADS)

Phan, Hoang-Phuong; Dinh, Toan; Nguyen, Tuan-Khoa; Vatani, Ashkan; Md Foisal, Abu Riduan; Qamar, Afzaal; Kermany, Atieh Ranjbar; Dao, Dzung Viet; Nguyen, Nam-Trung

2017-04-01

Paper-based microfluidics and sensors have attracted great attention. Although a large number of paper-based devices have been developed, surprisingly there are only a few studies investigating paper actuators. To fulfill the requirements for the integration of both sensors and actuators into paper, this work presents an unprecedented platform which utilizes ferromagnetic particles for actuation and graphite for motion monitoring. The use of the integrated mechanical sensing element eliminates the reliance on image processing for motion detection and also allows real-time measurements of the dynamic response in paper-based actuators. The proposed platform can also be quickly fabricated using a simple process, indicating its potential for controllable paper-based lab on chip.

Annealing Effects on Microstructure and Mechanical Properties of Ultrafine-Grained Al Composites Reinforced with Nano-Al2O3 by Rotary Swaging

NASA Astrophysics Data System (ADS)

Chen, Cunguang; Wang, Wenwen; Guo, Zhimeng; Sun, Chunbao; Volinsky, Alex A.; Paley, Vladislav

2018-03-01

Microstructure evolution and variations in mechanical properties of Al-Al2O3 nanocomposite produced by powder metallurgy were investigated and compared with commercially pure aluminum (Al-1050) after furnace annealing. Fine gas-atomized Al powder compacts were first sintered in flowing nitrogen, subsequently consolidated into wires by rotary swaging and eventually annealed at 300 and 500 °C for 24 h each. Scanning and transmission electron microscopy with energy-dispersive spectroscopy was utilized to document the microstructure evolution. Rotary swaging was proven to lead to a marked decrease in grain size. After heavy swaging to true deformation degree of φ = 6 and annealing at 500 °C, obvious recrystallization was observed at Al-1050's existing grain boundaries and the crystals began to grow perpendicular to the flow direction. In the Al-Al2O3 nanocomposite, fabricated from d 50 = 6 μm Al powder, recrystallization partially occurred, while grains were still extremely fine. Due to the dual role of fine-grained Al2O3 dispersion strengthening, the nanocomposite showed improved mechanical performance in terms of tensile strength, approximately twice higher than Al-1050 after annealing at 500 °C.

Ice-Active Substances from the Infective Juveniles of the Freeze Tolerant Entomopathogenic Nematode, Steinernema feltiae

PubMed Central

Ali, Farman; Wharton, David A.

2016-01-01

Steinernema feltiae is a moderately freezing tolerant nematode, that can withstand intracellular ice formation. We investigated recrystallization inhibition, thermal hysteresis and ice nucleation activities in the infective juveniles of S. feltiae. Both the splat cooling assay and optical recrystallometry indicate the presence of ice active substances that inhibit recrystallization in the nematode extract. The substance is relatively heat stable and largely retains the recrystallization inhibition activity after heating. No thermal hysteresis activity was detected but the extract had a typical hexagonal crystal shape when grown from a single seed crystal and weak ice nucleation activity. An ice active substance is present in a low concentration, which may be involved in the freezing survival of this species by inhibiting ice recrystallization. PMID:27227961

Pairing Heterocyclic Cations with closo-Icosahedral Borane and Carborane Anions. II. Benchtop Alternative Synthetic Methodologies for Binary Triazolium and Tetrazolium Salts with Significant Water Solubility

DTIC Science & Technology

2010-04-01

produced from eutectic melts. Nat. Mater. 2008, 7, 626-630. 9. Any attempt at recrystallizing the 1:1 mixture of cations in (12) is likely to afford... recrystallizations . So, rather than recrystallizing each individual adduct, we concentrated on performing a careful spectroscopic examination of the...suggested. [1] While it is well-known that an admixture of two neutral compounds often affords eutectic behavior, we wondered whether or not the same

Ostwald ripening of clays and metamorphic minerals

USGS Publications Warehouse

Eberl, D.D.; Srodon, J.; Kralik, M.; Taylor, B.E.; Peterman, Z.E.

1990-01-01

Analyses of particle size distributions indicate that clay minerals and other diagenetic and metamorphic minerals commonly undergo recrystallization by Ostwald ripening. The shapes of their particle size distributions can yield the rate law for this process. One consequence of Ostwald ripening is that a record of the recrystallization process is preserved in the various particle sizes. Therefore, one can determine the detailed geologic history of clays and other recrystallized minerals by separating, from a single sample, the various particle sizes for independent chemical, structural, and isotopic analyses.

Orientation filtering for crystalline films

DOEpatents

Smith, Henry I.; Atwater, Harry A.; Thompson, Carl V.; Geis, Michael W.

1986-12-30

A substrate is coated with a film to be recrystallized. A pattern of crystallization barriers is created in the film, for example, by etching voids in the film. An encapsulation layer is generally applied to protect the film, fill the voids and otherwise enhance a recrystallization process. Recrystallization is carried out such that certain orientations pass preferentially through the barrier, generally as a result of growth-velocity anisotropy. The result is a film of a specific predetermined crystallographic orientation, a range of orientations or a set of discrete orientations.

A photoactive bimetallic framework for direct aminoformylation of nitroarenes

EPA Science Inventory

A bimetallic catalyst, AgPd@g-C3N4, was synthesized by immobilizing silver and palladium nanoparticles over the surface of graphitic carbon nitride (g-C3N4) and its utility was demonstrated for the concerted aminoformylation of aromatic nitro compounds under visible light conditi...

Geochemistry of speleothems affected by aragonite to calcite recrystallization - Potential inheritance from the precursor mineral

NASA Astrophysics Data System (ADS)

Domínguez-Villar, David; Krklec, Kristina; Pelicon, Primož; Fairchild, Ian J.; Cheng, Hai; Edwards, Lawrence R.

2017-03-01

Formerly aragonite speleothems recrystallized to calcite result from solutions subsaturated in aragonite and supersaturated in calcite that infiltrate into the speleothem through the interconnected porosity. In most cases, the crystal replacement takes place through a thin solution film. This diagenetic process can occur under open or semi-closed geochemical conditions. Thus, secondary calcite crystals record the composition of the fluid at the time of diagenesis affected by calcite partition coefficients and fractionation factors (open system) or partly inherit the composition of the primary aragonite (semi-closed system). So, whether or not recrystallized aragonite speleothems can record reliable geochemical signals from the time of speleothem primary deposition still is an open debate. We studied a stalagmite from Eagle Cave (Spain) predominantly composed of secondary calcite that replaced aragonite, although a core of primary aragonite extending 45 mm along the growth direction was preserved at the base of the sample. We obtained Mg and Sr compositional maps, paired U-Th dating and δ18O and δ13C profiles across the diagenetic front. Additionally, two parallel isotope records were obtained along the speleothem growth direction in the aragonite and calcite sectors. Our results support that recrystallization of this speleothem took place in open system conditions for δ18O, δ13C, Mg and Sr, but in semi-closed system conditions for U and Th. The recrystallization of this sample took place during one or several events, likely after the Younger Dryas as a result of climate change influencing drip water composition. Based on compositional zoned patterns, we suggest that the advance of diagenetic fronts in this speleothem had an average rate of 50 ± 45 μm/yr. Such recrystallization rate can transform any aragonite speleothem into calcite within a few centuries. We suggest that the volume of water interacting with the speleothem at the time of recrystallization is of critical importance for inheritance of different elements. The volume of solution is controlled by (1) the discharge of water passing through the sample and (2) the lapse time between aragonite dissolution and calcite precipitation. Hydrology and hydrochemistry of the interacting solution, together with the mineralogy and texture of the speleothem are the essential controls for the diagenesis of the speleothem. Recrystallization of aragonite speleothems does not follow stratigraphical levels of the sample but occurs along sites with preferential flow paths in any sector of the speleothem. In these cases the relationship between age and distance from base is not preserved. However, alternation of periods of recrystallization with periods of aragonite precipitation causing speleothem accretion can result in recrystallized speleothems with coherent distance from the base-age relationship. Thus, early diagenesis of speleothems affected by seasonal or inter-annual oscillation of drip waters supersaturated and subsaturated in aragonite may provide best-scenario conditions for dating and preservation of paleoenvironmental records along recrystallized speleothems. However, even in this scenario, the variable discharge and the diagenetic rate control the geochemical inheritance from the primary aragonite crystals.

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

Hu, Shenyang; Lavender, Curt A.; Joshi, Vineet V.

Recrystallization plays an important role in swelling kinetics of irradiated metallic nuclear fuels. This talk will present a three-dimensional microstructure-dependent swelling model by integrating the evolution of intra-and inter- granular gas bubbles, dislocation loop density, and recrystallization.

Recrystallization characteristics and interfacial oxides on the compression bonding interface

NASA Astrophysics Data System (ADS)

Xie, Bijun; Sun, Mingyue; Xu, Bin; Li, Dianzhong

2018-05-01

Up to now, the mechanism of interface bonding is still not fully understood. This work presents interfacial characteristics of 316LN stainless steel bonding joint after cold compression bonding with subsequent annealing. EBSD analysis shows that fine recrystallization grains preferentially appear near the bonding interface and grow towards both sides of the interface. Transmission electron microscopy reveals that initial cold compression bonding disintegrates the native oxide scales and brings pristine metal from both sides of the interface come into intimate contact, while the broken oxide particles are remained at the original interface. The results indicate that partial bonding can be achieved by cold compression bonding with post-annealing treatment and recrystallization firstly occurs along the bonding interface. However, the interfacial oxides impede the recrystallization grains step over the interface and hinder the complete healing of the bonding interface.

Recrystallization as a controlling process in the wear of some f.c.c. metals

NASA Technical Reports Server (NTRS)

Bill, R. C.; Wisander, D.

1977-01-01

Detailed examination of copper specimens after sliding against 440 C steel in liquid methane at speeds up to 25 m/s and loads of up to 2 kg showed the metal comprising the wear surface to possess a fine cell recrystallized structure. Wear proceeded by the plastic shearing of metal in this near surface region without the occurrence of visible metal transfer. A dynamic balance between the intense shear process at the surface and the nucleation of recrystallized grains was proposed to account for the behavior of the metal at the wear surface. Sliding wear experiments were also conducted on Ag, Cu-10% Al, Cu-10% Sn, Ni and Al. It was found that low wear and the absence of heavy metal transfer were associated with those metals observed to undergo recrystallization nucleation without prior recovery.

Recrystallization characteristics of oxide dispersion strengthened nickel-base alloys

NASA Technical Reports Server (NTRS)

Hotzler, R. K.; Glasgow, T. K.

1980-01-01

Electron microscopy was employed to study the process of recrystallization in two oxide dispersion strengthened (ODS) mechanically alloyed nickel-base alloys, MA 754 and MA 6000E. MA 754 contained both fine, uniformly dispersed particles and coarser oxides aligned along the working direction. Hot rolled MA 754 had a grain size of 0.5 microns and high dislocation densities. After partial primary recrystallization, the fine grains transformed to large elongated grains via secondary (or abnormal) grain growth. Extruded and rolled MA 6000E contained equiaxed grains of 0.2 micron diameter. Primary recrystallization occurring during working eliminated virtually all dislocations. Conversion from fine to coarse grains was triggered by gamma prime dissolution; this was also a process of secondary or abnormal grain growth. Comparisons were made to conventional and oxide dispersion strengthened nickel-base alloys.

Dynamic Recrystallization of the Constituent γ Phase and Mechanical Properties of Ti-43Al-9V-0.2Y Alloy Sheet

PubMed Central

Zhang, Yu; Wang, Xiaopeng; Kong, Fantao

2017-01-01

A crack-free Ti-43Al-9V-0.2Y alloy sheet was successfully fabricated via hot-pack rolling at 1200 °C. After hot-rolling, the β/γ lamellar microstructure of the as-forged TiAl alloy was completely converted into a homogeneous duplex microstructure with an average γ grain size of 10.5 μm. The dynamic recrystallization (DRX) of the γ phase was systematically investigated. A recrystallization fraction of 62.5% was obtained for the γ phase in the TiAl alloy sheet, when a threshold value of 0.8° was applied to the distribution of grain orientation spread (GOS) values. The high strain rate and high stress associated with hot-rolling are conducive for discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX), respectively. A certain high-angle boundary (HAGB: θ = 89° ± 3°<100>), which is associated with DDRX, occurs in both the recrystallized and deformed γ grains. The twin boundaries play an important role in the DDRX of the γ phase. Additionally, the sub-structures and sub-boundaries originating from low-angle boundaries in the deformed grains also indicate that CDRX occurs. The mechanical properties of the alloy sheet were determined at both room and elevated temperatures. At 750 °C, the alloy sheet exhibited excellent elongation (53%), corresponding to a failure strength of 467 MPa. PMID:28914797

Cold cap subsidence for in situ vitrification and electrodes therefor

DOEpatents

Buelt, James L.; Carter, John G.; Eschbach, Eugene A.; FitzPatrick, Vincent F.; Koehmstedt, Paul L.; Morgan, William C.; Oma, Kenton H.; Timmerman, Craig L.

1992-01-01

An electrode for use in in situ vitrification of soil comprises a molybdenum rod received within a conductive sleeve or collar formed of graphite. Electrodes of this type are placed on either side of a region containing buried waste material and an electric current is passed therebetween for vitrifying the soil between the electrodes. The graphite collar enhances the thermal conductivity of the electrode, bringing heat to the surface, and preventing the formation of a cold cap of material above the ground surface. The annulus between the molybdenum rod electrode and the graphite collar is filled with a conductive ceramic powder of a type that sinters upon the molybdenum rod, protecting the same from oxidation as the graphite material is consumed, or a metal powder which liquifies at operating temperatures. The molybdenum rod in the former case may be coated with an oxidation protectant, e.g. of molybdenum disilicide. As insulative blanket is suitably placed on the surface of the soil during processing to promote subsidence by allowing off-gassing and reducing surface heat loss. In other embodiments, connection to vitrification electrodes is provided below ground level to avoid loss of connection due to electrodes deterioration, or a sacrificial electrode may be employed when operation is started. Outboard electrodes can be utilized to square up the vitrified area. Further, the center of the molybdenum rod can be made hollow and filled with a powdered metal, such as copper, which liquifies at operating temperatures. In one embodiment, the molybdenum rod and the graphite collar are physically joined at the bottom.

Amplified fluorescent aptasensor through catalytic recycling for highly sensitive detection of ochratoxin A.

PubMed

Wei, Yin; Zhang, Ji; Wang, Xu; Duan, Yixiang

2015-03-15

This paper describes a novel approach utilizing nano-graphite-aptamer hybrid and DNase I for the amplified detection of ochratoxin A (OTA) for the first time. Nano-graphite can effectively quench the fluorescence of carboxyfluorescein (FAM) labeled OTA specific aptamer due to their strong π-π; stacking interactions; while upon OTA addition, it will bind with aptamer to fold into an OTA-aptamerG-quadruplex structure, which does not adsorb on the surface of nano-graphite and thus retains the dye fluorescence. Meanwhile, the G-quadruplex structure can be cleaved by DNase I, and in such case OTA is delivered from the complex. The released OTA then binds other FAM-labeled aptamers on the nano-graphite surface, and touches off another target recycling, resulting in the successive release of dye-labeled aptamers from the nano-graphite, which leads to significant amplification of the signal. Under the optimized conditions, the present amplified sensing system exhibits high sensitivity toward OTA with a limit of detection of 20nM (practical measurement), which is about 100-fold higher than that of traditional unamplified homogeneous assay. Our developed method also showed high selectivity against other interference molecules and can be applied for the detection of OTA in real red wine samples. The proposed assay is simple, cost-effective, and might open a door for the development of new assays for other biomolecules. This aptasensor is of great practical importance in food safety and could be widely extended to the detection of other toxins by replacing the sequence of the recognition aptamer. Copyright © 2014 Elsevier B.V. All rights reserved.

Advanced rotary engine components utilizing fiber reinforced Mg castings

NASA Technical Reports Server (NTRS)

Goddard, D.; Whitman, W.; Pumphrey, R.; Lee, C.-M.

1986-01-01

Under a two-phase program sponsored by NASA, the technology for producing advanced rotary engine components utilizing graphite fiber-reinforced magnesium alloy casting is being developed. In Phase I, the successful casting of a simulated intermediate housing was demonstrated. In Phase II, the goal is to produce an operating rotor housing. The effort involves generation of a material property data base, optimization of parameters, and development of wear- and corrosion-resistant cast surfaces and surface coatings. Results to date are described.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples

NASA Astrophysics Data System (ADS)

Suslova, A.; El-Atwani, O.; Sagapuram, D.; Harilal, S. S.; Hassanein, A.

2014-11-01

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten.

Effect of alloying elements and coiling temperature on the recrystallization behavior and the bainitic transformation in TRIP steels

NASA Astrophysics Data System (ADS)

Han, Seongho; Seong, Hwangoo; Ahn, Yeonsang; Garcia, C. I.; DeArdo, A. J.; Kim, Inbae

2009-08-01

The effects of alloying elements and coiling temperature on recrystallization behavior and bainitic transformation were investigated based on 0.07C-Mn-Cr-Nb steel with a low carbon equivalent. Based on the ferrite recrystallization behavior, the proper intercritical annealing temperature of all studied steels was suggested to produce TRIP steel with good strength and elongation balance. All steels coiled at 550 °C showed much faster ferrite recrystallization behavior than steels coiled at 700 °C. In addition to the coiling temperature, the effect of increasing carbon content on the ferrite recrystallization was minor at a coiling temperature of 550 °C, but much more prominent at a coiling temperature of 700 °C. The highest Mo added steel showed the best strength and elongation balance, and the highest carbon and Mo added steel showed the highest tensile strength at a coiling temperature of 550 °C. The steel containing a higher amount of elemental Al (0.7 wt.% Al) exhibited much better elongation than the lower Al added steel (0.04 wt.% Al) in TS 780 MPa grade, about 24 % and 19 %, respectively.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples

PubMed Central

Suslova, A.; El-Atwani, O.; Sagapuram, D.; Harilal, S. S.; Hassanein, A.

2014-01-01

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten. PMID:25366885

Recrystallization of water in non-water-soluble (meth)acrylate polymers is not rare and is not devitrification.

PubMed

Gemmei-Ide, Makoto; Ohya, Atsushi; Kitano, Hiromi

2012-02-16

Change in the state of water sorbed into four kinds of non-water-soluble poly(meth)acrylates with low water content by temperature (T) perturbation was examined on the basis of T variable mid-infrared (MIR) spectroscopy. Many studies using differential scanning calorimetry suggested that there was no change in the state. T dependence of their MIR spectra, however, clearly demonstrated various changes in the state. Furthermore, recrystallization, which was crystallization during heating, was observed in all four polymers. The recrystallization observed in this study was not devitrification, which is the change in the state from glassy water to crystalline water, but vapor deposition during heating (vapor re-deposition). There were only two reports about recrystallization of water in a non-water-soluble polymer before this report; therefore, it might be considered to be a rare phenomenon. However, as demonstrated in this study, it is not a rare phenomenon. Recrystallization (vapor re-deposition) of water in the polymer matrices is related to a balance between flexibility and strength of the electrostatic interaction sites of polymer matrices but might not be related to the biocompatibility of polymers.

Recrystallization and grain growth induced by ELMs-like transient heat loads in deformed tungsten samples.

PubMed

Suslova, A; El-Atwani, O; Sagapuram, D; Harilal, S S; Hassanein, A

2014-11-04

Tungsten has been chosen as the main candidate for plasma facing components (PFCs) due to its superior properties under extreme operating conditions in future nuclear fusion reactors such as ITER. One of the serious issues for PFCs is the high heat load during transient events such as ELMs and disruption in the reactor. Recrystallization and grain size growth in PFC materials caused by transients are undesirable changes in the material, since the isotropic microstructure developed after recrystallization exhibits a higher ductile-to-brittle transition temperature which increases with the grain size, a lower thermal shock fatigue resistance, a lower mechanical strength, and an increased surface roughening. The current work was focused on careful determination of the threshold parameters for surface recrystallization, grain growth rate, and thermal shock fatigue resistance under ELM-like transient heat events. Transient heat loads were simulated using long pulse laser beams for two different grades of ultrafine-grained tungsten. It was observed that cold rolled tungsten demonstrated better power handling capabilities and higher thermal stress fatigue resistance compared to severely deformed tungsten. Higher recrystallization threshold, slower grain growth, and lower degree of surface roughening were observed in the cold rolled tungsten.

Enhancing substrate utilization and power production of a microbial fuel cell with nitrogen-doped carbon aerogel as cathode catalyst.

PubMed

Tardy, Gábor Márk; Lóránt, Bálint; Lóka, Máté; Nagy, Balázs; László, Krisztina

2017-07-01

Catalytic efficiency of a nitrogen-doped, mesoporous carbon aerogel cathode catalyst was investigated in a two-chambered microbial fuel cell (MFC) applying graphite felt as base material for cathode and anode, utilizing peptone as carbon source. This mesoporous carbon aerogel containing catalyst layer on the cathode increased the maximum power density normalized to the anode volume to 2.7 times higher compared to the maximum power density obtained applying graphite felt cathode without the catalyst layer. At high (2 and 3) cathode/anode volume ratios, maximum power density exceeded 40 W m -3 . At the same time, current density and specific substrate utilization rate increased by 58% resulting in 31.9 A m -3 and 18.8 g COD m -3  h -1 , respectively (normalized to anode volume). Besides the increase of the power and the rate of biodegradation, the investigated catalyst decreased the internal resistance from the range of 450-600 to 350-370 Ω. Although Pt/C catalyst proved to be more efficient, a considerable decrease in the material costs might be achieved by substituting it with nitrogen-doped carbon aerogel in MFCs. Such cathode still displays enhanced catalytic effect.

Friction stir welding process and material microstructure evolution modeling in 2000 and 5000 series of aluminum alloy

NASA Astrophysics Data System (ADS)

Yalavarthy, Harshavardhan

Interactions between the rotating and advancing pin-shaped tool (terminated at one end with a circular-cylindrical shoulder) with the clamped welding-plates and the associated material and heat transport during a Friction Stir Welding (FSW) process are studied computationally using a fully-coupled thermo-mechanical finite-element analysis. To surmount potential numerical problems associated with extensive mesh distortions/entanglement, an Arbitrary Lagrangian Eulerian (ALE) formulation was used which enabled adaptive re-meshing (to ensure the continuing presence of a high-quality mesh) while allowing full tracking of the material free surfaces. To demonstrate the utility of the present computational approach, the analysis is applied to the cases of same-alloy FSW of two Aluminum-alloy grades: (a) AA5083 (a solid-solution strengthened and strain-hardened/stabilized Al-Mg-Mn alloy); and (b) AA2139 (a precipitation hardened quaternary Al-Cu-Mg-Ag alloy). Both of these alloys are currently being used in military-vehicle hull structural and armor systems. In the case of non-age-hardenable AA5083, the dominant microstructure evolution processes taking place during FSW are extensive plastic deformation and dynamic recrystallization of highly-deformed material subjected to elevated temperatures approaching the melting temperature. To account for the competition between plastic-deformation controlled strengthening and dynamic-recrystallization induced softening phenomena during the FSW process, the original Johnson-Cook strain- and strain-rate hardening and temperature-softening material strength model is modified in the present work using the available recrystallization-kinetics experimental data. In the case of AA2139, in addition to plastic deformation and dynamic recrystallization, precipitates coarsening, over-aging, dissolution and re-precipitation had to be also considered. Limited data available in the open literature pertaining to the kinetics of the aforementioned microstructure-evolution processes are used to predict variation in the material hardness and the residual stresses throughout the various FSW zones of the two alloys. The results showed that with proper modeling of the material behavior under high-temperature/severe-plastic-deformation conditions, significantly improved agreement can be attained between the computed and measured post-FSW residual-stress and material-strength distribution results. Keywords: Friction Stir Welding; AA5083; AA2139; Johnson-Cook Strength Model; Finite Element Analysis; Hardness Prediction.

Orientation filtering for crystalline films

DOEpatents

Smith, H.I.; Atwater, H.A.; Thompson, C.V.; Geis, M.W.

1986-12-30

A substrate is coated with a film to be recrystallized. A pattern of crystallization barriers is created in the film, for example, by etching voids in the film. An encapsulation layer is generally applied to protect the film, fill the voids and otherwise enhance a recrystallization process. Recrystallization is carried out such that certain orientations pass preferentially through the barrier, generally as a result of growth-velocity anisotropy. The result is a film of a specific predetermined crystallographic orientation, a range of orientations or a set of discrete orientations. 7 figs.

Strong Surface Diffusion Mediated Glancing-Angle Deposition: Growth, Recrystallization and Reorientation of Tin Nanorods

NASA Astrophysics Data System (ADS)

Wang, Huan-Hua; Shi, Yi-Jian; William, Chu; Yigal, Blum

2008-01-01

Different from usual glancing-angle deposition where low surface diffusion is necessary to form nanorods, strong surface diffusion mediated glancing-angle deposition is exemplified by growing tin nanorod films on both silicon and glass substrates simultaneously via thermal evaporation. During growth, the nanorods were simultaneously baked by the high-temperature evaporator, and therefore re-crystallized into single crystals in consequence of strong surface diffusion. The monocrystalline tin nanorods have a preferred orientation perpendicular to the substrate surface, which is quite different from the usual uniformly oblique nanorods without recrystallization.

Role of the Double-Layer Cation on the Potential-Dependent Stretching Frequencies and Binding Geometries of Carbon Monoxide at Platinum-Nonaqueous Interfaces

DTIC Science & Technology

1992-02-01

were recrystallized twice from water, or water, and then ethanol , and methanol/water, respectively, and dried at 100"C under vacuum for 24 hours. The...hexafluorophosphate, and recrystallized twice from absolute ethanol . The alkali perchlorates (LiCIO4, NaCl0 4, KCIO 4, from G.F. Smith) were recrystallized twice from...which a Ag/AgCl (3M KCI) reference electrode was used. All measurements were made at room 5 temperature , 23 ± VC. RESULTS In our earlier preliminary

Optically induced melting of colloidal crystals and their recrystallization.

PubMed

Harada, Masashi; Ishii, Masahiko; Nakamura, Hiroshi

2007-04-15

Colloidal crystals melt by applying focused light of optical tweezers and recrystallize after removing it. The disturbed zone by the light grows radially from the focus point and the ordering starts from the interface with the crystal. Although the larger disturbed zone is observed for the higher power optical tweezers, a master curve is extracted by normalization of the disturbed zone. The temporal changes of the normalized disturbed zone are well described with exponential functions, indicating that the melting and recrystallization process is governed by a simple relaxation mechanism.

Annealing effects in plated-wire memory elements. II - Recrystallization in Permalloy films.

NASA Technical Reports Server (NTRS)

Marquardt, S. J.; Kench, J. R.

1971-01-01

Results of grain-size measurements in Permalloy platings suggest that recrystallization is possible at temperatures as low as 200 C, but that it is an extremely heterogeneous process. No worthwhile correlation was found to exist between observed grain size and magnetic dispersion in samples aged in the temperature range from 180 to 230 C. It is suggested that the magnetic aging which occurs under these conditions may be due to some other diffusion-controlled process than recrystallization; a process such as chemical homogenization is tentatively preferred.

Unified Static and Dynamic Recrystallization Model for the Minerals of Earth's Mantle Using Internal State Variable Model

NASA Astrophysics Data System (ADS)

Cho, H. E.; Horstemeyer, M. F.; Baumgardner, J. R.

2017-12-01

In this study, we present an internal state variable (ISV) constitutive model developed to model static and dynamic recrystallization and grain size progression in a unified manner. This method accurately captures temperature, pressure and strain rate effect on the recrystallization and grain size. Because this ISV approach treats dislocation density, volume fraction of recrystallization and grain size as internal variables, this model can simultaneously track their history during the deformation with unprecedented realism. Based on this deformation history, this method can capture realistic mechanical properties such as stress-strain behavior in the relationship of microstructure-mechanical property. Also, both the transient grain size during the deformation and the steady-state grain size of dynamic recrystallization can be predicted from the history variable of recrystallization volume fraction. Furthermore, because this model has a capability to simultaneously handle plasticity and creep behaviors (unified creep-plasticity), the mechanisms (static recovery (or diffusion creep), dynamic recovery (or dislocation creep) and hardening) related to dislocation dynamics can also be captured. To model these comprehensive mechanical behaviors, the mathematical formulation of this model includes elasticity to evaluate yield stress, work hardening in treating plasticity, creep, as well as the unified recrystallization and grain size progression. Because pressure sensitivity is especially important for the mantle minerals, we developed a yield function combining Drucker-Prager shear failure and von Mises yield surfaces to model the pressure dependent yield stress, while using pressure dependent work hardening and creep terms. Using these formulations, we calibrated against experimental data of the minerals acquired from the literature. Additionally, we also calibrated experimental data for metals to show the general applicability of our model. Understanding of realistic mantle dynamics can only be acquired once the various deformation regimes and mechanisms are comprehensively modeled. The results of this study demonstrate that this ISV model is a good modeling candidate to help reveal the realistic dynamics of the Earth's mantle.

Multidisciplinary Simulation of Graphite-Composite and Cermet Fuel Elements for NTP Point of Departure Designs

NASA Technical Reports Server (NTRS)

Stewart, Mark E.; Schnitzler, Bruce G.

2015-01-01

This paper compares the expected performance of two Nuclear Thermal Propulsion fuel types. High fidelity, fluid/thermal/structural + neutronic simulations help predict the performance of graphite-composite and cermet fuel types from point of departure engine designs from the Nuclear Thermal Propulsion project. Materials and nuclear reactivity issues are reviewed for each fuel type. Thermal/structural simulations predict thermal stresses in the fuel and thermal expansion mis-match stresses in the coatings. Fluid/thermal/structural/neutronic simulations provide predictions for full fuel elements. Although NTP engines will utilize many existing chemical engine components and technologies, nuclear fuel elements are a less developed engine component and introduce design uncertainty. Consequently, these fuel element simulations provide important insights into NTP engine performance.

Highly Thermal Conductive Nanocomposites

NASA Technical Reports Server (NTRS)

Sun, Ya-Ping (Inventor); Connell, John W. (Inventor); Veca, Lucia Monica (Inventor)

2015-01-01

Disclosed are methods for forming carbon-based fillers as may be utilized in forming highly thermal conductive nanocomposite materials. Formation methods include treatment of an expanded graphite with an alcohol/water mixture followed by further exfoliation of the graphite to form extremely thin carbon nanosheets that are on the order of between about 2 and about 10 nanometers in thickness. Disclosed carbon nanosheets can be functionalized and/or can be incorporated in nanocomposites with extremely high thermal conductivities. Disclosed methods and materials can prove highly valuable in many technological applications including, for instance, in formation of heat management materials for protective clothing and as may be useful in space exploration or in others that require efficient yet light-weight and flexible thermal management solutions.

Highly Thermal Conductive Nanocomposites

NASA Technical Reports Server (NTRS)

Sun, Ya-Ping (Inventor); Connell, John W. (Inventor); Veca, Lucia Monica (Inventor)

2017-01-01

Disclosed are methods for forming carbon-based fillers as may be utilized in forming highly thermal conductive nanocomposite materials. Formation methods include treatment of an expanded graphite with an alcohol/water mixture followed by further exfoliation of the graphite to form extremely thin carbon nanosheets that are on the order of between about 2 and about 10 nanometers in thickness. Disclosed carbon nanosheets can be functionalized and/or can be incorporated in nanocomposites with extremely high thermal conductivities. Disclosed methods and materials can prove highly valuable in many technological applications including, for instance, in formation of heat management materials for protective clothing and as may be useful in space exploration or in others that require efficient yet light-weight and flexible thermal management solutions.

Utilization of Induction Bonding for Automated Fabrication of TIGR

NASA Technical Reports Server (NTRS)

Hinkley, Jeffrey A.; Johnston, Norman J.; Hulcher, A. Bruce; Marchello, Joseph M.; Messier, Bernadette C.

1999-01-01

A laboratory study of magnetic induction heat bonding of titanium foil and graphite fiber reinforced polymer prepreg tape, TiGr, demonstrated that the process is a viable candidate for low cost fabrication of aircraft structure made of this new material form. Data were obtained on weld bonding of PIXA and PETI-5 prepreg to titanium. Both the foil and honeycomb forms of titanium were investigated. The process relies on magnetic susceptor heating of titanium, not on high frequency heating of graphite fiber. The experiments showed that with a toroid magnet configuration, good weld bonds might be obtained with heating times of a few seconds. These results suggest the potential is good for the induction heating process to achieve acceptable commercial production rates.

Silicate Inclusions in IAB Irons: Correlations Between Metal Composition and Inclusion Properties, and Inferences for Their Origin

NASA Astrophysics Data System (ADS)

Benedix, G. K.; McCoy, T. J.; Keil, K.

1995-09-01

IAB irons are the largest group of iron meteorites, exhibit a large range of siderophile element concentrations in their metal, and commonly contain silicate inclusions with roughly chondritic composition. They are closely related to IIICD irons [1,2] and their inclusions resemble winonaites [3]. It has been suggested that IAB's and IIICD's formed in individual impact melt pools [4,2] on a common parent body. However, it has also been suggested that fractional crystallization [5,6] of a S-saturated core could produce the observed siderophile element trends. Metal composition is correlated with silicate inclusion mineralogy in IIICD's [1], indicating reactions between solid silicates and the metallic magma in a core. These trends observed in IIICD's differ from those in IAB's, suggesting different parent bodies. A bi-modal grouping, based primarily on mineralogy and mineral abundances, was suggested for IAB inclusions [7]. However, recent recoveries of several new silicate-bearing IAB's, along with the emergence of new ideas on their origins, prompted a comprehensive study to document more fully the range of inclusions within IAB irons, to examine possible correlations between the compositions of the metallic host and the silicate inclusions, and to elucidate the origin of IAB irons. We are studying troilite-graphite-silicate inclusions in 24 IAB irons with Ni concentrations ranging from 6.6-25.0%. These include Odessa and Copiapo types [7], newly recovered meteorites (e.g., Lueders [8]) and meteorites with extreme Ni contents (e.g., Jenny's Creek, 6.8%; San Cristobal, 25.0% [9]). The inclusions exhibit a range of textures from recrystallized to partial melts (e.g., Caddo County [10]). Rigorous classification [7] is hampered by heterogeneities between group meteorites, between different samples of distinct meteorites, and within individual inclusions. While intergroup heterogeneities make comparisons between the suite of IAB's somewhat difficult, some general trends do exist. Inclusion mineralogy progresses from graphite-troilite nodules in low Ni IAB's, to silicate-dominated inclusions in high Ni IAB's. With increasing Ni abundance in the metal, systematic variations are found in several properties. Two groups are delineated on a Ni vs Fa content plot and both are positively correlated with Ni content. Graphite abundance noticeably decreases with increasing Ni content [7]. Graphite location also varies with Ni: graphite is primarily found interstitial to the silicates in low Ni IAB's, but is located at metal-silicate boundaries in those with higher Ni abundances. With increasing Ni, daubreelite disappears. Inclusion shape also varies [7]: more angular inclusions are associated with low Ni, while more rounded inclusions exist at high Ni contents. These systematic changes suggest interaction between the silicate inclusions and an evolving metallic magma. Troilite and graphite abundances may be related to early nucleation on silicates, hence their depletion in high Ni (later crystallizing) irons. The presence of abundant graphite creates reducing conditions which would result in the formation of daubreelite. Conditions become more oxidizing with loss of graphite, evidenced by lack of daubreelite and more FeO-rich silicates in high Ni irons. Although an overall trend exists, the story is complicated by heterogeneities. Significant variations are found between paired samples (e.g., Toluca and Tacubaya), as well as within individual inclusions (daubreelite and chromite in same inclusion). Local oxidation conditions may be controlled by graphite abundance. Heterogeneities within specific meteorites need documentation. Most of the inclusions exhibit similar textural (metamorphic) features, but a few show evidence of partial melting and melt migration, further complicating the parent body history. While a variety of processes (oxidation-reduction, metamorphism, partial melting) affected the inclusions during formation, systematic changes observed here indicate that the silicates were interacting with a single evolving metallic magma. We suggest that the requirement for a common system is more compatible with core formation [5,6] than with impact-melt pools [2,4]. References: [1] McCoy T. J. et al. (1993) Meteoritics, 28, 552-560. [2] Choi B.-G. et al. (1995) GCA, 59, 593-612. [3] Benedix G. K. et al. (1995) LPS XXVI, 99-100. [4] Wasson J. T. et al. (1980) Z. Naturforsch., 35a, 781-795. [5] Kracher A. (1982) GRL, 9, 412-415. [6] Kracher A. (1985) Proc. LPSC 15th, in JGR, 90, C689-C698. [7] Bunch T. E. et al. (1970) Contrib. Mineral. Petrol., 25, 297-340. [8] McCoy et al. (1995) Meteoritics, in preparation. [9] Scott E. R. D. and Bild R. W. (1974) GCA, 38, 1379-1391. [10] Takeda H. et al. (1993) Meteoritics, 28, 447.

Effects of Static Recrystallization and Precipitation on Mechanical Properties of 00Cr12 Ferritic Stainless Steel

NASA Astrophysics Data System (ADS)

Shao, Yi; Liu, Chenxi; Yue, Tengxiao; Liu, Yongchang; Yan, Zesheng; Li, Huijun

2018-05-01

The 00Cr12 ferritic stainless steel samples were isothermally held at different temperatures in the range of 700 °C to 1000 °C to investigate the effect of static recrystallization and precipitation on mechanical properties, such as microhardness, tensile strength, and yield strength. The results show that the formation of the fine recrystallized grain, as well as precipitation, coarsening, and dissolution of the second-phase particles, influences the mechanical properties remarkably. The fine recrystallized grain can provide a positive grain boundary-strengthening effect in the sample under a relatively high holding temperature. Coarsening and dissolution of M23C6 result in partial depletion of precipitate hardening. In contrast, the size and number density of MX particles are almost constant, regardless of the holding temperature; therefore, it can provide a better precipitation-hardening effect.

Deformation-Induced Dynamic Precipitation and Resulting Microstructure in a Mg-Zn-Ca Alloy

NASA Astrophysics Data System (ADS)

Du, Yuzhou; Zheng, Mingyi; Jiang, Bailing; Zhou, Kesong

2018-05-01

The microstructure of an Mg-Zn-Ca extrusion was investigated by transmission electron microscopy, and the interaction between dynamic precipitation and dynamic recrystallization was analyzed. The results showed that dynamic precipitation significantly affected the microstructure of the as-extruded Mg-Zn-Ca alloy. The pinning effects of precipitates on dislocations effectively prohibited dynamic recrystallization processes, while the grain boundary precipitate Ca2Mg6Zn3, inhibited the growth of dynamically recrystallized grains. Consequently, a bimodal microstructure with fine dynamically recrystallized (DRXed) grains and elongated deformed regions was obtained for the Mg-Zn-Ca extrusion. High-resolution transmission electron microscopy indicated that the intragranular precipitate MgZn2 had a crystal orientation relationship with α-Mg in the form of (0002)Mg//(10-13)MgZn2 and [1-100]Mg//[1-210]MgZn2, which was beneficial for strength improvement.

A comparative study on the direct deposition of μc-Si:H and plasma-induced recrystallization of a-Si:H: Insight into Si crystallization in a high-density plasma

NASA Astrophysics Data System (ADS)

Zhou, H. P.; Xu, M.; Xu, S.; Feng, Y. Y.; Xu, L. X.; Wei, D. Y.; Xiao, S. Q.

2018-03-01

Deep insight into the crystallization mechanism of amorphous silicon is of theoretical and technological significance for the preparation of high-quality microcrystalline/polycrystalline silicon. In this work, we intensively compare the present two plasma-involved routes, i.e., the direct deposition and recrystallization of precursor amorphous silicon (a-Si) films, to fabricate microcrystalline silicon. Both the directly deposited and recrystallized samples show multi-layered structures as revealed by electronic microscopy. High-density hydrogen plasma involved recrystallization process, which is mediated by the hydrogen diffusion into the deep region of the precursor a-Si film, displays significantly different nucleation configuration, interface properties, and crystallite shape. The underlying mechanisms are analyzed in combination with the interplay of high-density plasma and growing or treated surface.

FEM study of recrystallized tungsten under ELM-like heat loads

NASA Astrophysics Data System (ADS)

Du, J.; Yuan, Y.; Wirtz, M.; Linke, J.; Liu, W.; Greuner, H.

2015-08-01

FEM thermal analysis has been performed on rolled tungsten plate loaded with heat load of 23 MW/m2 for 1.5 s. Gradient temperature field is generated due to the Gaussian shape beam profile. Recrystallization and grain growth of various scales were found at different areas of the sample depending on the localized thermal field. FEM thermal-mechanical analyses have been performed on the recrystallized tungsten exposed to ELMs-like heat loads. The analyzed load conditions were 0.38 and 1.14 GW/m2 with different base temperatures. Material deterioration due to recrystallization was implemented by adopting decreased yield stress, tangent modulus, strength coefficient and ductility coefficients. Life time predicted by adopting strain life criterion indicates grain growth from 5 μm to 100 μm causes the life decrease of 80%. This result is gained by pure mathematical calculation based on the empiric assumptions of material properties.

Recrystallization of freezable bound water in aqueous solutions of medium concentration

NASA Astrophysics Data System (ADS)

Lishan, Zhao; Liqing, Pan; Ailing, Ji; Zexian, Cao; Qiang, Wang

2016-07-01

For aqueous solutions with freezable bound water, vitrification and recrystallization are mingled, which brings difficulty to application and misleads the interpretation of relevant experiments. Here, we report a quantification scheme for the freezable bound water based on the water-content dependence of glass transition temperature, by which also the concentration range for the solutions that may undergo recrystallization finds a clear definition. Furthermore, we find that depending on the amount of the freezable bound water, different temperature protocols should be devised to achieve a complete recrystallization. Our results may be helpful for understanding the dynamics of supercooled aqueous solutions and for improving their manipulation in various industries. Project supported by the Knowledge Innovation Project of Chinese Academy of Sciences on Water Science Research (Grant No. KJZD-EW-M03) and the National Natural Science Foundation of China (Grant Nos. 11474325 and 11290161).

Surface premelting/recrystallization governing the collapse of open-cell nanoporous Cu via thermal annealing.

PubMed

Wang, L; Zhang, X M; Deng, L; Tang, J F; Xiao, S F; Deng, H Q; Hu, W Y

2018-06-04

We systematically investigate the collapse of a set of open-cell nanoporous Cu (np-Cu) materials with the same porosity and shape but different specific surface areas, during thermal annealing, by performing large-scale molecular dynamics simulations. Two mechanisms govern the collapse of np-Cu. One is direct surface premelting, facilitating the collapse of np-Cu, when the specific surface area is less than a critical value (∼2.38 nm-1). The other is recrystallization followed by surface premelting, accelerating the sloughing of ligaments and the annihilation of voids, when the critical specific surface area is exceeded. Surface premelting results from surface reconstruction by prompting localized "disordering" and "chaos" on the surface, and the melting temperature reduces linearly with the increase of the specific surface area. Recrystallization is followed by surface premelting as the melting temperature is below the supercooling point, where a liquid is unstable and instantaneously recrystallizes.

Thermoplastic polyimide NEW-TPI (trademark)

NASA Technical Reports Server (NTRS)

Hou, Tan-Hung; Reddy, Rakasi M.

1990-01-01

Thermal and rheological properties of a commercial thermoplastic polyimide, NEW-TPI (trademark), were characterized. The as-received material possesses initially a transient crystallite form with a bimodal distribution in peak melting temperatures. After the melting of the initial crystallite structure, the sample can be recrystallized by various thermal treatments. A bimodal or single modal melting peak distribution is formed for annealing temperatures below or above 360 C, respectively. The recrystallized crystallinities are all transient in nature. The polymers are unable to be recrystallized after being subjected to elevated temperature annealing above 450 C. The recrystallization mechanism was postulated, and a simple kinetics model was found to describe the behavior rather satisfactory under the conditions of prolonged thermal annealing. Rheological measurements made in the linear viscoelastic range support the evidence observed in the thermal analysis. Furthermore, the measurements sustain the manufacturer's recommended processing window of 400 to 420 C for this material.

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

The SAP technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of the alloy Ni-17Cr-5Al-0.2 Y. SAP-NiCrAl was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. A variety of annealing treatments were applied after working to determine the recrystallization response. NiCrAlY, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl of this study exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl as has been reported for other oxide dispersion strengthened alloys. In contrast, unoxidized NiCrAlY exhibited only primary recrystallization.

Recrystallization-induced self-assembly for the growth of Cu₂O superstructures.

PubMed

Shang, Yang; Shao, Yi-Ming; Zhang, Dong-Feng; Guo, Lin

2014-10-20

The assembly of inorganic nanoparticles (NPs) into 3D superstructures with defined morphologies is of particular interest. A novel strategy that is based on recrystallization-induced self-assembly (RISA) for the construction of 3D Cu2O superstructures and employs Cu2O mesoporous spheres with diameters of approximately 300 nm as the building blocks has now been developed. Balancing the hydrolysis and recrystallization rates of the CuCl precursors through precisely adjusting the experimental parameters was key to success. Furthermore, the geometry of the superstructures can be tuned to obtain either cubes or tetrahedra and was shown to be dependent on the growth behavior of bulk CuCl. The overall strategy extends the applicability of recrystallization-based processes for the guided construction of assemblies and offers unique insights for assembling larger particles into complicated 3D superstructures. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Copper Refinement from Anode to Cathode and then to Wire Rod: Effects of Impurities on Recrystallization Kinetics and Wire Ductility.

PubMed

Helbert, Anne-Laure; Moya, Alice; Jil, Tomas; Andrieux, Michel; Ignat, Michel; Brisset, François; Baudin, Thierry

2015-10-01

In this paper, the traceability of copper from the anode to the cathode and then the wire rod has been studied in terms of impurity content, microstructure, texture, recrystallization kinetics, and ductility. These characterizations were obtained based on secondary ion mass spectrometry, differential scanning calorimetry (DSC), X-ray diffraction, HV hardness, and electron backscattered diffraction. It is shown that the recrystallization was delayed by the total amount of impurities. From tensile tests performed on cold drawn and subsequently annealed wires for a given time, a simplified model has been developed to link tensile elongation to the chemical composition. This model allowed quantification of the contribution of some additional elements, present in small quantity, on the recrystallization kinetics. The proposed model adjusted for the cold-drawn wires was also validated on both the cathode and wire rod used for the study of traceability.

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction.

PubMed

Christien, F; Telling, M T F; Knight, K S; Le Gall, R

2015-05-01

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature ramping as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.

Synthesis of 3D iron and carbon-based composite as a bifunctional sorbent and catalyst for remediation of organic pollutants

NASA Astrophysics Data System (ADS)

Li, Ling; Shen, Yi; Wang, Zhaomei

2017-07-01

We prepared a 3D monolith by integrating graphite nanosheet encapsulated iron nanoparticles (Fe@GNS) into graphite felt (GF) supports. The structural properties of the resulting Fe@GNS/GF monolith are characterized by x-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, x-ray photoelectron spectroscopy and N2 adsorption-desorption isotherms. The Fe@GNS/GF monoliths are utilized as a bifunctional sorbent and catalyst for water remediation. Using Congo red and methyl violet 2B as model pollutants, the sorption and catalytic performance of the Fe@GNS/GF composite are examined. The Fe@GNS/GF monolith possesses maximum sorption capacities of 177 and 142 mg g-1 for the sorption of CR and MV-2B, respectively. It also exhibits rate constants of 0.0563 and 0.0464 min-1 for the catalytic degradation of CR and MV-2B, respectively. As a proof of concept, the Fe@GNS/GF is successfully utilized to decontaminate simulated organic waste water via a combination of sorption and catalytic degradation processes.

Interfacial effects in ZnO nanotubes/needle-structured graphitic diamond nanohybrid for detecting dissolved acetone at room temperature

NASA Astrophysics Data System (ADS)

Kathiravan, Deepa; Huang, Bohr-Ran; Saravanan, Adhimoorthy; Yeh, Chien-Jui; Leou, Keh-Chyang; Lin, I.-Nan

2017-12-01

A high-performance ZnO nanotubes (ZNTs)/needle-structured graphitic diamond (NGD) nanohybrid material was prepared and observed the electrochemical sensing properties of liquid acetone in water. Initially, we synthesized NGD film using bias-enhanced growth (BEG) process. Afterwards, a well-etched ZNTs were spatially grown on the NGD film using simple hydrothermal method, and utilized as sensing material for assemble an electrochemical sensor (via EGFET configuration) operating at room temperature. The systematic investigations depict the ultra-high sensing properties attained from ZNTs grown on NGD film. The NGD film mostly have needle or wire shaped diamond grains, which contributes extremely high electrical conductivity. Furthermore, needle shaped diamond grains cover with multi-layer graphitic material generates conduction channels for ZNTs and leads to enhance the oxygen residuals and species. The material stability and conductivity of NGD as well the defects exist with oxygen vacancies in ZNTs offers superior sensing properties. Thus, the interesting combination of these wide band gap semiconductor materials exhibit high sensor response (89 mV/mL), high stability and long-term reliability (tested after 60 days).

Porous graphitic carbon microtubes derived from willow catkins as a substrate of MnO2 for supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiaohua; Zhang, Kang; Li, Hengxiang; Cao, Qing; Jin, Li'e.; Li, Ping

2017-03-01

Biomass is receiving considerable attention because of its significant advantages as a sustainable and renewable material. Willow catkins, which have a single-walled microtubular structure are used as both a template and a precursor for synthesizing porous graphitic carbon microtubes (PGCMT) induced by the simultaneous activation-graphitization of K4Fe(CN)6. In addition to providing low-resistant pathways and short ion diffusion channels, as-obtained PGCMT with tubular structure also serves as an ideal platform for anchoring MnO2. The PGCMT/MnO2 composite electrode obtained by MnO2 electrodeposition expressed excellent electrochemical performance, including a significantly enhanced specific capacitance (550.8 F g-1 for the mass of MnO2 at a current density of 2 A g-1), a high capacitance retention of 61.8% even at a high current density of 50 A g-1, and an excellent cycling stability of 89.6% capability retention after 5000 cycles. These findings offer a simple and environmentally friendly strategy for preparing advanced energy materials by utilizing the unique structure of biomass waste from nature.

Drawing Sensors with Ball-Milled Blends of Metal-Organic Frameworks and Graphite

PubMed Central

Ko, Michael; Aykanat, Aylin; Smith, Merry K.

2017-01-01

The synthetically tunable properties and intrinsic porosity of conductive metal-organic frameworks (MOFs) make them promising materials for transducing selective interactions with gaseous analytes in an electrically addressable platform. Consequently, conductive MOFs are valuable functional materials with high potential utility in chemical detection. The implementation of these materials, however, is limited by the available methods for device incorporation due to their poor solubility and moderate electrical conductivity. This manuscript describes a straightforward method for the integration of moderately conductive MOFs into chemiresistive sensors by mechanical abrasion. To improve electrical contacts, blends of MOFs with graphite were generated using a solvent-free ball-milling procedure. While most bulk powders of pure conductive MOFs were difficult to integrate into devices directly via mechanical abrasion, the compressed solid-state MOF/graphite blends were easily abraded onto the surface of paper substrates equipped with gold electrodes to generate functional sensors. This method was used to prepare an array of chemiresistors, from four conductive MOFs, capable of detecting and differentiating NH3, H2S and NO at parts-per-million concentrations. PMID:28946624

ICP-MS analysis of fission product diffusion in graphite for High-Temperature Gas-Cooled Reactors

NASA Astrophysics Data System (ADS)

Carter, Lukas M.

Release of radioactive fission products from nuclear fuel during normal reactor operation or in accident scenarios is a fundamental safety concern. Of paramount importance are the understanding and elucidation of mechanisms of chemical interaction, nuclear interaction, and transport phenomena involving fission products. Worldwide efforts to reduce fossil fuel dependence coupled with an increasing overall energy demand have generated renewed enthusiasm toward nuclear power technologies, and as such, these mechanisms continue to be the subjects of vigorous research. High-Temperature Gas-Cooled Reactors (HTGRs or VHTRs) remain one of the most promising candidates for the next generation of nuclear power reactors. An extant knowledge gap specific to HTGR technology derives from an incomplete understanding of fission product transport in major core materials under HTGR operational conditions. Our specific interest in the current work is diffusion in reactor graphite. Development of methods for analysis of diffusion of multiple fission products is key to providing accurate models for fission product release from HTGR core components and the reactor as a whole. In the present work, a specialized diffusion cell has been developed and constructed to facilitate real-time diffusion measurements via ICP-MS. The cell utilizes a helium gas-jet system which transports diffusing fission products to the mass spectrometer using carbon nanoparticles. The setup was designed to replicate conditions present in a functioning HTGR, and can be configured for real-time release or permeation measurements of single or multiple fission products from graphite or other core materials. In the present work, we have analyzed release rates of cesium in graphite grades IG-110, NBG-18, and a commercial grade of graphite, as well as release of iodine in IG-110. Additionally we have investigated infusion of graphite samples with Cs, I, Sr, Ag, and other surrogate fission products for use in release or profile measurements of diffusion coefficients.

Dynamic recrystallization behavior of an as-cast TiAl alloy during hot compression

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

Li, Jianbo, E-mail: lijianbo1205@163.com; Liu, Yong, E-mail: yonliu@csu.edu.cn; Wang, Yan, E-mail: wangyan@csu.edu.cn

2014-11-15

High temperature compressive deformation behaviors of as-cast Ti–43Al–4Nb–1.4W–0.6B alloy were investigated at temperatures ranging from 1050 °C to 1200 °C, and strain rates from 0.001 s{sup −1} to 1 s{sup −1}. Electron back scattered diffraction technique, scanning electron microscopy and transmission electron microscopy were employed to investigate the microstructural evolutions and nucleation mechanisms of the dynamic recrystallization. The results indicated that the true stress–true strain curves show a dynamic flow softening behavior. The dependence of the peak stress on the deformation temperature and the strain rate can well be expressed by a hyperbolic-sine type equation. The activation energy decreases withmore » increasing the strain. The size of the dynamically recrystallized β grains decreases with increasing the value of the Zener–Hollomon parameter (Z). When the flow stress reaches a steady state, the size of β grains almost remains constant with increasing the deformation strain. The continuous dynamic recrystallization plays a dominant role in the deformation. In order to characterize the evolution of dynamic recrystallization volume fraction, the dynamic recrystallization kinetics was studied by Avrami-type equation. Besides, the role of β phase and the softening mechanism during the hot deformation was also discussed in details. - Highlights: • The size of DRXed β grains decreases with increasing the value of the Z. • The CDRX plays a dominant role in the deformation. • The broken TiB{sub 2} particles can promote the nucleation of DRX.« less

Microstructure and yield strength effects on hydrogen and tritium induced cracking in HERF (high-energy-rate-forged) stainless steel

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

Morgan, M J; Tosten, M H

1989-01-01

Rising-load J-integral measurements and falling-load threshold stress intensity measurements were used to characterize hydrogen and tritium induced cracking in high-energy-rate-forged (HERF) 21-6-9 stainless steel. Samples having yield strengths in the range 517--930 MPa were thermally charged with either hydrogen or tritium and tested at room temperature in either air or high-pressure hydrogen gas. In general, the hydrogen isotopes reduced the fracture toughness by affecting the fracture process. Static recrystallization in the HERF microstructures affected the material's fracture toughness and its relative susceptibility to hydrogen and tritium induced fracture. In hydrogen-exposed samples, the reduction in fracture toughness was primarily dependent onmore » the susceptibility of the microstructure to intergranular fracture and only secondarily affected by strength in the range of 660 to 930 MPa. Transmission-electron microscopy observations revealed that the microstructures least susceptible to hydrogen-induced intergranular cracking contained patches of fully recrystallized grains. These grains are surrounded by highly deformed regions containing a high number density of dislocations. The microstructure can best be characterized as duplex'', with soft recrystallized grains embedded in a hard, deformed matrix. The microstructures most susceptible to hydrogen-induced intergranular fracture showed no well-developed recrystallized grains. The patches of recrystallized grains seemed to act as crack barriers to hydrogen-induced intergranular fracture. In tritium-exposed-and-aged samples, the amount of static recrystallization also affected the fracture toughness properties but to a lesser degree. 7 refs., 25 figs.« less

Evolution of grain boundary character distributions in alloy 825 tubes during high temperature annealing: Is grain boundary engineering achieved through recrystallization or grain growth?

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

Bai, Qin; Zhao, Qing

Grain boundary engineering (GBE) of nickel-based alloy 825 tubes was carried out with different cold drawing deformations by using a draw-bench on a factory production line and subsequent annealing at various temperatures. The microstructure evolution of alloy 825 during thermal-mechanical processing (TMP) was characterized by means of the electron backscatter diffraction (EBSD) technique to study the TMP effects on the grain boundary network and the evolution of grain boundary character distributions during high temperature annealing. The results showed that the proportion of ∑ 3{sup n} coincidence site lattice (CSL) boundaries of alloy 825 tubes could be increased to > 75%more » by the TMP of 5% cold drawing and subsequent annealing at 1050 °C for 10 min. The microstructures of the partially recrystallized samples and the fully recrystallized samples suggested that the proportion of low ∑ CSL grain boundaries depended on the annealing time. The frequency of low ∑ CSL grain boundaries increases rapidly with increasing annealing time associating with the formation of large-size highly-twinned grains-cluster microstructure during recrystallization. However, upon further increasing annealing time, the frequency of low ∑ CSL grain boundaries decreased markedly during grain growth. So it is concluded that grain boundary engineering is achieved through recrystallization rather than grain growth. - Highlights: •The grain boundary engineering (GBE) is applicable to 825 tubes. •GBE is achieved through recrystallization rather than grain growth. •The low ∑ CSL grain boundaries in 825 tubes can be increased to > 75%.« less

Carbon transfer from magnesia-graphite ladle refractories to ultra-low carbon steel

NASA Astrophysics Data System (ADS)

Russo, Andrew Arthur

Ultra-low carbon steels are utilized in processes which require maximum ductility. Increases in interstitial carbon lower the ductility of steel; therefore, it is important to examine possible sources of carbon. The refractory ladle lining is one such source. Ladle refractories often contain graphite for its desirable thermal shock and slag corrosion resistance. This graphite is a possible source of carbon increase in ultra-low carbon steels. The goal of this research is to understand and evaluate the mechanisms by which carbon transfers to ultra-low carbon steel from magnesia-graphite ladle refractory. Laboratory dip tests were performed in a vacuum induction furnace under an argon atmosphere to investigate these mechanisms. Commercial ladle refractories with carbon contents between 4-12 wt% were used to investigate the effect of refractory carbon content. Slag-free dip tests and slag-containing dip tests with varying MgO concentrations were performed to investigate the influence of slag. Carbon transfer to the steel was controlled by steel penetrating into the refractory and dissolving carbon in dip tests where no slag was present. The rate limiting step for this mechanism is convective mass transport of carbon into the bulk steel. No detectable carbon transfer occurred in dip tests with 4 and 6 wt%C refractories without slag because no significant steel penetration occurred. Carbon transfer was controlled by the corrosion of refractory by slag in dip tests where slag was present.

Development of a Continuum Damage Mechanics Material Model of a Graphite-Kevlar(Registered Trademark) Hybrid Fabric for Simulating the Impact Response of Energy Absorbing Kevlar(Registered Trademark) Hybrid Fabric for Simulating the Impact Response of Energy Absorbing

NASA Technical Reports Server (NTRS)

Jackson, Karen E.; Fasanella, Edwin L.; Littell, Justin D.

2017-01-01

This paper describes the development of input properties for a continuum damage mechanics based material model, Mat 58, within LS-DYNA(Registered Trademark) to simulate the response of a graphite-Kevlar(Registered Trademark) hybrid plain weave fabric. A limited set of material characterization tests were performed on the hybrid graphite-Kevlar(Registered Trademark) fabric. Simple finite element models were executed in LS-DYNA(Registered Trademark) to simulate the material characterization tests and to verify the Mat 58 material model. Once verified, the Mat 58 model was used in finite element models of two composite energy absorbers: a conical-shaped design, designated the "conusoid," fabricated of four layers of hybrid graphite-Kevlar(Registered Trademark) fabric; and, a sinusoidal-shaped foam sandwich design, designated the "sinusoid," fabricated of the same hybrid fabric face sheets with a foam core. Dynamic crush tests were performed on components of the two energy absorbers, which were designed to limit average vertical accelerations to 25- to 40-g, to minimize peak crush loads, and to generate relatively long crush stroke values under dynamic loading conditions. Finite element models of the two energy absorbers utilized the Mat 58 model that had been verified through material characterization testing. Excellent predictions of the dynamic crushing response were obtained.

Deformation-related recrystallization processes

NASA Astrophysics Data System (ADS)

Drury, Martyn R.; Urai, Janos L.

1990-02-01

Recrystallization is a common microstructural transformation that occurs during deformation, metamorphism and diagenesis of rocks. Studies on minerals and rock analogues have demonstrated that a wide range of recrystallization mechanisms can occur. The range of mechanisms is related to the various ways in which two basic processes, grain boundary migration and new grain boundary formation combine to transform the microstructure. Two recent papers (Drury et al., 1985; Urai et al., 1986) have proposed different schemes for the description of recrystallization mechanisms. The purpose of this paper is to provide a unified framework for the description of mechanisms. Recrystallization mechanisms are divided into three main types; rotation mechanisms which principally involve the formation of new grain boundaries; migration mechanisms which principally involve grain boundary migration; and general mechanisms which involve both basic processes. A further distinction is made on the basis of the continuity of the microstructural transformation with respect to time. Each of the three main types of mechanism can be divided into a number of sub-types depending on whether the processes of grain boundary migration, new grain boundary formation and new grain formation occur in a discontinuous or continuous manner with respect to time. As the terms continuous and discontinuous have been used in the metallurgical literature to signify the spatial continuity of the microstructural transformation, the terms discontinuai and continual are used to refer to the temporal continuity of the transformation. It is recommended that the following aspects should be specified, if possible, in a general description of recrystallization mechanisms: (1) How do the basic processes combine to transform the microstructure. (2) If new grain development occurs, what is the development mechanism, and does new grain formation occur in a continual or discontinuai manner. (3) If grain boundary migration is involved in the transformation, what is the migration mechanism (i.e. fast solute escape migration, slow solute loaded migration, fluid assisted migration, etc.), and is migration a continual or discontinuai process. The application of the unified scheme is illustrated by reviewing studies that have provided detailed information on the recrystallization mechanisms involved. The complicating effects of solid solution impurities, dispersed second phase particles and grain boundary fluid films are also considered and it is demonstrated that variations in content of these types of impurity can significantly effect the types of recrystallization that occur in a given material.

Stress in recrystallized quartz by electron backscatter diffraction mapping

NASA Astrophysics Data System (ADS)

Llana-Fúnez, S.

2017-07-01

The long-term state of stress at middle and lower crustal depths can be estimated through the study of the microstructure of exhumed rocks from active and/or ancient shear zones. Constitutive equations for deformation mechanisms in experimentally deformed rocks relate differential stress to the size of recrystallized grains. Cross et al. (2017) take advantage of electron backscatter diffraction mapping to systematically separate new recrystallized grains from host grains on the basis of the measurable lattice distorsion within the grains. They produce the first calibrated piezometer for quartz with this technique, reproducing within error a previous calibration based on optical microscopy.

Application of two-level factorial design to investigate the effect of process parameters on the sonocrystallization of sulfathiazole

NASA Astrophysics Data System (ADS)

Kuo, Peng-Hsuan; Zhang, Bo-Cong; Su, Chie-Shaan; Liu, Jun-Jen; Sheu, Ming-Thau

2017-08-01

In this study, cooling sonocrystallization was used to recrystallize an active pharmaceutical ingredient, sulfathiazole, using methanol as the solvent. The effects of three operating parameters-sonication intensity, sonication duration, and solution concentration-on the recrystallization were investigated by using a 2k factorial design. The solid-state properties of sulfathiazole, including the mean particle size, crystal habit, and polymorphic form, were analyzed. Analysis of variance showed that the effect of the sonication intensity, cross-interaction effect of sonication intensity/sonication duration, and cross-interaction effect of sonication intensity/solution concentration on the recrystallization were significant. The results obtained using the 2k factorial design indicated that a combination of high sonication intensity and long sonication duration is not favorable for sonocrystallization, especially at a high solution concentration. A comparison of the solid-state properties of the original and the recrystallized sulfathiazole revealed that the crystal habit of the recrystallized sulfathiazole was more regular and that its mean particle size could be reduced to approximately 10 μm. Furthermore, the analytical results obtained using the PXRD, DSC, and FTIR spectroscopy indicated that the polymorphic purity of sulfathiazole improved from the original Form III/IV mixture to Form III after sonocrystallization.

Microstructure study of a severely plastically deformed Mg-Zn-Y alloy by application of low angle annular dark field diffraction contrast imaging.

PubMed

Basha, Dudekula Althaf; Rosalie, Julian M; Somekawa, Hidetoshi; Miyawaki, Takashi; Singh, Alok; Tsuchiya, Koichi

2016-01-01

Microstructural investigation of extremely strained samples, such as severely plastically deformed (SPD) materials, by using conventional transmission electron microscopy techniques is very challenging due to strong image contrast resulting from the high defect density. In this study, low angle annular dark field (LAADF) imaging mode of scanning transmission electron microscope (STEM) has been applied to study the microstructure of a Mg-3Zn-0.5Y (at%) alloy processed by high pressure torsion (HPT). LAADF imaging advantages for observation of twinning, grain fragmentation, nucleation of recrystallized grains and precipitation on second phase particles in the alloy processed by HPT are highlighted. By using STEM-LAADF imaging with a range of incident angles, various microstructural features have been imaged, such as nanoscale subgrain structure and recrystallization nucleation even from the thicker region of the highly strained matrix. It is shown that nucleation of recrystallized grains starts at a strain level of revolution [Formula: see text] (earlier than detected by conventional bright field imaging). Occurrence of recrystallization of grains by nucleating heterogeneously on quasicrystalline particles is also confirmed. Minimizing all strain effects by LAADF imaging facilitated grain size measurement of [Formula: see text] nm in fully recrystallized HPT specimen after [Formula: see text].

Study on the dynamic recrystallization model and mechanism of nuclear grade 316LN austenitic stainless steel

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

Wang, Shenglong; Zhang, Mingxian; Wu, Huanchun

In this study, the dynamic recrystallization behaviors of a nuclear grade 316LN austenitic stainless steel were researched through hot compression experiment performed on a Gleeble-1500 simulator at temperatures of 900–1250 °C and strain rates of 0.01–1 s{sup −1}. By multiple linear regressions of the flow stress-strain data, the dynamic recrystallization mathematical models of this steel as functions of strain rate, strain and temperature were developed. Then these models were verified in a real experiment. Furthermore, the dynamic recrystallization mechanism of the steel was determined. The results indicated that the subgrains in this steel are formed through dislocations polygonization and thenmore » grow up through subgrain boundaries migration towards high density dislocation areas and subgrain coalescence mechanism. Dynamic recrystallization nucleation performs in grain boundary bulging mechanism and subgrain growth mechanism. The nuclei grow up through high angle grain boundaries migration. - Highlights: •Establish the DRX mathematical models of nuclear grade 316LN stainless steel •Determine the DRX mechanism of this steel •Subgrains are formed through dislocations polygonization. •Subgrains grow up through subgrain boundaries migration and coalescence mechanism. •DRX nucleation performs in grain boundary bulging mechanism and subgrain growth mechanism.« less

Modeling the microstructural changes during hot tandem rolling of AA5 XXX aluminum alloys: Part II. Textural evolution

NASA Astrophysics Data System (ADS)

Wells, M. A.; Samarasekera, I. V.; Brimacombe, J. K.; Hawbolt, E. B.; Lloyd, D. J.

1998-06-01

In Part II of this article, the experimental work undertaken to measure the effect of deformation parameters (temperature, strain, and strain rate) on the texture formation during hot deformation and the evolution during subsequent recrystallization is described. In addition, the isothermal kinetics of development of individual texture components were also determined. A neutron diffractometer was used to measure the texture in the as-hot-deformed aluminum samples, and the samples were then heat treated in a 400 °C salt bath for various lengths of time, with the texture being remeasured at various stages in the recrystallization process. Using data from the experimental program, the texture evolution during recrystallization was modeled by applying a modified form of the Avrami equation. Results indicated that, of the deformation parameters studied, textural development was most sensitive to the deformation temperature for both alloys. In addition, modeling results revealed that the Cu component ({112} <111>) was the first to recrystallize, typically followed by the S ({123} <634>) and Bs ({110} <112>) components. This is in agreement with earlier work which indicated that the Bs component was the hardest to recrystallize, possibly because it is able to deform on very few slip systems and, hence, the dislocation interaction may be low.

Measurement of process-dependent material properties of pharmaceutical solids by nanoindentation.

PubMed

Liao, Xiangmin; Wiedmann, Timothy Scott

2005-01-01

The purpose of this work was to evaluate nanoindentation as a means to characterize the material properties of pharmaceutical solids. X-ray diffraction of potassium chloride and acetaminophen showed that samples prepared by cooling a melt to a crystalline sample as opposed to slow recrystallization had the same crystal structure. With analysis of the force-displacement curves, the KCl quenched samples had a hardness that was 10 times higher than the recrystallized KCl, while acetaminophen quenched samples were 25% harder than the recrystallized samples. The elastic moduli of the quenched samples were also much greater than that observed for the recrystallized samples. Although the elasticity was independent of load, the hardness increased with load for acetaminophen. With each sample, the flow at constant load increased with applied load. Etching patterns obtained by atomic force microscopy showed that the KCl quenched sample had a higher dislocation density than the recrystallized sample, although there was no evident difference in the acetaminophen samples. Overall, the differences in the observed sample properties may be related to the dislocation density. Thus, nanoindentation has been shown to be a sensitive method for determining a processed-induced change in the hardness, creep, and elasticity of KCl and acetaminophen. (c) 2004 Wiley-Liss, Inc.

Prediction of recrystallization behavior of troglitazone/polyvinylpyrrolidone solid dispersion by solid-state NMR.

PubMed

Ito, Atsutoshi; Watanabe, Tomoyuki; Yada, Shuichi; Hamaura, Takeshi; Nakagami, Hiroaki; Higashi, Kenjirou; Moribe, Kunikazu; Yamamoto, Keiji

2010-01-04

The purpose of this study was to elaborate the relationship between the (13)C CP/MAS NMR spectra and the recrystallization behavior during the storage of troglitazone solid dispersions. The solid dispersions were prepared by either the solvent method or by co-grinding. The recrystallization behavior under storage conditions at 40 degrees C/94% RH was evaluated by the Kolmogorov-Johnson-Mehl-Avrami (KJMA) equation. Solid dispersions prepared by the solvent method or by prolonged grinding brought about inhibition of the nucleation and the nuclei growth at the same time. No differences in the PXRD profiles were found in the samples prepared by the co-grinding and solvent methods, however, (13)C CP/MAS NMR showed significant differences in the spectra. The correlation coefficients using partial least square regression analysis between the PXRD profiles and the apparent nuclei-growth constant or induction period to nucleation were 0.1305 or 0.6350, respectively. In contrast, those between the (13)C CP/MAS NMR spectra and the constant or the period were 0.9916 or 0.9838, respectively. The (13)C CP/MAS NMR spectra had good correlation with the recrystallization kinetic parameters evaluated by the KJMA equation. Consequently, solid-state NMR was judged to be a useful tool for the prediction of the recrystallization behavior of solid dispersions.

Recrystallization Behavior in Mixed Solder Joints of BGA Components during Thermal Shock

NASA Astrophysics Data System (ADS)

Tan, Shihai; Han, Jing; Guo, Fu

2018-03-01

Sn-37Pb and Sn-3.0Ag-0.5Cu solder pastes printed onto a board were attached to ball grid array (BGA) samples using Sn-3.0Ag-0.5Cu solder balls. Before thermal shock, the initial grain orientations on the cross-section were obtained by scanning electron microscopy equipped with an electron backscattered diffraction system. Three mixed solder joints (two from the corner and another from the middle of the BGA component) and three lead-free solder joints (at the same positions) were selected to investigate the recrystallization behavior under thermal shock (TS) cycling conditions. All of the mixed and lead-free solder joints were initially single crystal. The results showed that recrystallization occurred in both the mixed and lead-free solder joints after 200 TS. For the mixed solder joints, more recrystallization was observed and the location of samples had a significant influence on their recrystallization behavior, while location was not as important for the lead-free samples after 200 TS in this study. Both the mixed and lead-free solder joints at the corner of BGA components showed the poorest reliability. According to misorientation distribution maps and subgrain rotation behaviors, the reliability of mixed solder joints was much poorer than that of lead-free solder joints.

Dynamic recrystallization mechanisms and their transition in the Daling Thrust (DT) zone, Darjeeling-Sikkim Himalaya

NASA Astrophysics Data System (ADS)

Ghosh, Subhajit; Bose, Santanu; Mandal, Nibir; Dasgupta, Sujoy

2016-04-01

The Daling Thrust (DT) delineates a zone of intense shear localization in the Lesser Himalayan Sequence (LHS) of the Darjeeling-Sikkim Himalaya. From microstructural studies of deformed quartzite samples, we show a transition in the dynamic recrystallization mechanism with increasing distance from the DT, dominated by grain boundary bulging (BLG) recrystallization closest to the DT, and progressively replaced by sub-grain rotation (SGR) recrystallization away from the thrust. The transition is marked by a characteristic variation in the fractal dimension (D) of grain boundaries, estimated from the area-perimeter method. For the BLG regime, D ≈ 1.046, which decreases significantly to a value as low as 1.025 for the SGR regime. Using the available thermal data for BLG and SGR recrystallization, we infer increasing deformation temperatures away from the DT in the hanging wall. Based on the quartz piezometer our estimates reveal strong variations in the flow stress (59.00 MPa to 16.00 MPa) over a distance of 1.2 km from the DT. Deformation mechanism maps constructed for different temperatures indicate that the strain rates (10- 12 S- 1 to 10- 14 S- 1) comply with the geologically possible range. Finally, we present a mechanical model to provide a possible explanation for the cause of stress intensification along the DT.

Effect of cold deformation on the recrystallization behavior of FePd alloy at the ordering temperature using electron backscatter diffraction

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

Lin, Hung-Pin; Chen, Yen-Chun; Chen, Delphic

2014-08-15

In this study, the evolution of the recrystallization texture and microstructure was investigated after annealing of 50% and 90% cold-rolled FePd alloy at 530 °C. The FePd alloy was produced by vacuum arc melting in an atmosphere of 97% Ar and 3% H{sub 2}. The specimens were cold rolled to achieve 50% and 90% reduction in thickness. Electron backscatter diffraction measurements were performed on the rolling direction–normal direction section. With increased deformation from 50% to 90%, recrystallized texture transition occurs. For the 50% cold-rolled alloy, the preferred orientation is (0 1 0) [11 0 1], which is close to themore » cubic orientation after 400 h of annealing. For the 90% cold-rolled alloy, the orientation changes to (0 5 4) [22–4 5] after 16 h of annealing. - Highlights: • Texture and microstructure in cold-rolled FePd alloy was investigated during annealing using EBSD. • The recrystallized texture of 50% cold-rolled FePd is (0 1 0) [11 0 1] at 530 °C for 400 hours. • The recrystallized texture of 90% cold-rolled FePd is changed to (0 5 4) [22–4 5] at 530 °C after 16 hours.« less

Dynamic recrystallization and texture evolution of Mg–Y–Zn alloy during hot extrusion process

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

Tong, L.B.; Li, X.; Guangzhou Research Institute of Non-ferrous Metals, Guangzhou 510651

2014-06-01

The microstructure and texture evolution of Mg{sub 98.5}Y{sub 1}Zn{sub 0.5} and Mg{sub 92.5}Y{sub 5}Zn{sub 2.5} (atomic percent) alloys during hot extrusion were systematically investigated. The coarse LPSO phases with higher volume fraction (∼ 57%) suppressed the twinning generation in the initial stage of extrusion, and accelerated the dynamic recrystallization through the particle deformation zones. Therefore, the volume fraction of DRXed grains in as-extruded Mg{sub 92.5}Y{sub 5}Zn{sub 2.5} alloy was much higher than that of Mg{sub 98.5}Y{sub 1}Zn{sub 0.5} alloy. The intensive recrystallization process resulted in the conventional basal texture weakening, although the texture evolution was mainly dominated by flow behavior.more » The dynamic recrystallization behavior in Mg{sub 92.5}Y{sub 5}Zn{sub 2.5} alloy restricted the formation of deformation texture, and thus the more random texture was observed during the whole extrusion process. - Highlights: • The densely coarse LPSO phases suppressed the twinning deformation. • Coarse LPSO phases induced the particle stimulated nucleation effect. • Dynamic recrystallization resulted in the basal texture weakening effect.« less

Pioneering In Situ Recrystallization during Bead Milling: A Top-down Approach to Prepare Zeolite A Nanocrystals.

PubMed

Anand, Chokkalingam; Yamaguchi, Yudai; Liu, Zhendong; Ibe, Sayoko; Elangovan, Shanmugam P; Ishii, Toshihiro; Ishikawa, Tsuyoshi; Endo, Akira; Okubo, Tatsuya; Wakihara, Toru

2016-07-05

Top-down approach has been viewed as an efficient and straightforward method to prepare nanosized zeolites. Yet, the mechanical breaking of zeolite causes amorphization, which usually requires a post-milling recrystallization to obtain fully crystalline nanoparticles. Herein we present a facile methodology to prepare zeolite nanocrystals, where milling and recrystallization can be performed in situ. A milling apparatus specially designed to work under conditions of high alkalinity and temperature enables the in situ recrystallization during milling. Taking zeolite A as an example, we demonstrate its size reduction from ~3 μm to 66 nm in 30 min, which is quite faster than previous methods reported. Three functions, viz., miniaturization, amorphization and recrystallization were found to take effect concurrently during this one-pot process. The dynamic balance between these three functions was achieved by adjusting the milling period and temperature, which lead to the tuning of zeolite A particle size. Particle size and crystallinity of the zeolite A nanocrystals were confirmed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and water adsorption-desorption. This work presents a pioneering advancement in this field of nanosized zeolites, and will facilitate the mass production as well as boost the wide applications of nanosized zeolites.

Pioneering In Situ Recrystallization during Bead Milling: A Top-down Approach to Prepare Zeolite A Nanocrystals

PubMed Central

Anand, Chokkalingam; Yamaguchi, Yudai; Liu, Zhendong; Ibe, Sayoko; Elangovan, Shanmugam P.; Ishii, Toshihiro; Ishikawa, Tsuyoshi; Endo, Akira; Okubo, Tatsuya; Wakihara, Toru

2016-01-01

Top-down approach has been viewed as an efficient and straightforward method to prepare nanosized zeolites. Yet, the mechanical breaking of zeolite causes amorphization, which usually requires a post-milling recrystallization to obtain fully crystalline nanoparticles. Herein we present a facile methodology to prepare zeolite nanocrystals, where milling and recrystallization can be performed in situ. A milling apparatus specially designed to work under conditions of high alkalinity and temperature enables the in situ recrystallization during milling. Taking zeolite A as an example, we demonstrate its size reduction from ~3 μm to 66 nm in 30 min, which is quite faster than previous methods reported. Three functions, viz., miniaturization, amorphization and recrystallization were found to take effect concurrently during this one-pot process. The dynamic balance between these three functions was achieved by adjusting the milling period and temperature, which lead to the tuning of zeolite A particle size. Particle size and crystallinity of the zeolite A nanocrystals were confirmed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and water adsorption-desorption. This work presents a pioneering advancement in this field of nanosized zeolites, and will facilitate the mass production as well as boost the wide applications of nanosized zeolites. PMID:27378145

Compatibility of the Radio Frequency Mass Gauge with Composite Tanks

NASA Technical Reports Server (NTRS)

Zimmerli, Greg; Mueller, Carl

2015-01-01

The radio frequency mass gauge (RFMG) is a low-gravity propellant quantity gauge being developed at NASA for possible use in long-duration space missions utilizing cryogenic propellants. As part of the RFMG technology development process, we evaluated the compatibility of the RFMG with a graphite-epoxy composite material used to construct propellant tanks. The key material property that can affect compatibility with the RFMG is the electrical conductivity. Using samples of 8552IM7 graphite-epoxy composite, we characterized the resistivity and reflectivity over a range of frequencies. An RF impedance analyzer was used to characterize the out-of-plane electrical properties (along the sample thickness) in the frequency range 10 to 1800 MHZ. The resistivity value at 500 MHz was 4.8 ohm-cm. Microwave waveguide measurements of samples in the range 1.7 2.6 GHz, performed by inserting the samples into a WR-430 waveguide, showed reflectivity values above 98. Together, these results suggested that a tank constructed from graphite-epoxy composite would produce good quality electromagnetic tank modes, which is needed for the RFMG. This was verified by room-temperature measurements of the electromagnetic modes of a 2.4 m diameter tank constructed by Boeing from similar graphite-epoxy composite material. The quality factor Q of the tank electromagnetic modes, measured via RF reflection measurements from an antenna mounted in the tank, was typically in the range 400 Q 3000. The good quality modes observed in the tank indicate that the RFMG is compatible with graphite-epoxy tanks, and thus the RFMG could be used as a low-gravity propellant quantity gauge in such tanks filled with cryogenic propellants.

13C 12C exchange between calcite and graphite: A possible thermometer in Grenville marbles

USGS Publications Warehouse

Valley, J.W.; O'Neil, J.R.

1981-01-01

The fractionation of 13C between calcite and graphite, ??(Cc-Gr). is consistently small (2.6-4.8 permil) in 34 assemblages from upper amphibolite- and granulite-facies marbles of the Grenville Province. In 25 samples from the Adirondack Mountains, New York, it decreases regularly with increasing metamorphic temperature. The fractionations are independent of absolute ??13C values of calcite (-2.9 to +5.0). For T = 600-800??C, the Adirondack data are described by ??(Cc-Gr) = -0.00748T (??C) + 8.68. This good correlation between ?? and T suggests that carbon isotope equilibrium was attained in these high-grade marbles and that the theoretical calculations of this fractionation by Bottinga are approximately 2 permil too large in this temperature range. Because of the relatively high temperature sensitivity suggested by these results and by Bottinga's calculations, and the pressure independence of isotope fractionation, ??(Cc-Gr) may provide a very good thermometer for high-grade marbles. Comparison of this field calibration for ??(Cc-Gr) vs temperature with results from other terranes supports the utility of ??(Cc-Gr) for geothermometry and suggests that graphite is much more sluggish to exchange than calcite, that exchange between calcite and graphite occurs at temperatures as low as 300??C, and that equilibrium may normally be attained only when peak metamorphic temperatures are greater than 500-600??C. Because 13C exchange is an unavoidable metamorphic process at temperatures above 300??C, high values of ??13C(Gr) in moderate- to high-grade carbonate-bearing rocks do not provide a sufficient criterion to infer an abiogenic origin for the graphite. ?? 1981.

Carbohydrate-Based Ice Recrystallization Inhibitors Increase Infectivity and Thermostability of Viral Vectors

NASA Astrophysics Data System (ADS)

Ghobadloo, Shahrokh M.; Balcerzak, Anna K.; Gargaun, Ana; Muharemagic, Darija; Mironov, Gleb G.; Capicciotti, Chantelle J.; Briard, Jennie G.; Ben, Robert N.; Berezovski, Maxim V.

2014-07-01

The inability of vaccines to retain sufficient thermostability has been an obstacle to global vaccination programs. To address this major limitation, we utilized carbohydrate-based ice recrystallization inhibitors (IRIs) to eliminate the cold chain and stabilize the potency of Vaccinia virus (VV), Vesicular Stomatitis virus (VSV) and Herpes virus-1 (HSV-1). The impact of these IRIs was tested on the potency of the viral vectors using a plaque forming unit assay following room temperature storage, cryopreservation with successive freeze-thaw cycles and lyophilization. Viral potency after storage with all three conditions demonstrated that N-octyl-gluconamide (NOGlc) recovered the infectivity of shelf stored VV, 5.6 Log10 PFU mL-1 during 40 days, and HSV-1, 2.7 Log10 PFU mL-1 during 9 days. Carbon-linked antifreeze glycoprotein analogue ornithine-glycine-glycine-galactose (OGG-Gal) increases the recovery of VV and VSV more than 1 Log10 PFU mL-1 after 10 freeze-thaw cycles. In VSV, cryostorage with OGG-Gal maintains high infectivity and reduces temperature-induced aggregation of viral particles by 2 times that of the control. In total, OGG-Gal and NOGlc preserve virus potency during cryostorage. Remarkably, NOGlc has potential to eliminate the cold chain and permit room temperature storage of viral vectors.

Structure/property (constitutive and dynamic strength/damage) characterization of additively manufactured 316L SS

NASA Astrophysics Data System (ADS)

Gray, G. T., III; Livescu, V.; Rigg, P. A.; Trujillo, C. P.; Cady, C. M.; Chen, S. R.; Carpenter, J. S.; Lienert, T. J.; Fensin, S.

2015-09-01

For additive manufacturing (AM), the certification and qualification paradigm needs to evolve as there exists no "ASTM-type" additive manufacturing certified process or AM-material produced specifications. Accordingly, utilization of AM materials to meet engineering applications requires quantification of the constitutive properties of these evolving materials in comparison to conventionally-manufactured metals and alloys. Cylinders of 316L SS were produced using a LENS MR-7 laser additive manufacturing system from Optomec (Albuquerque, NM) equipped with a 1kW Yb-fiber laser. The microstructure of the AM-316L SS is detailed in both the as-built condition and following heat-treatments designed to obtain full recrystallization. The constitutive behavior as a function of strain rate and temperature is presented and compared to that of nominal annealed wrought 316L SS plate. The dynamic damage evolution and failure response of all three materials was probed using flyer-plate impact driven spallation experiments at a peak stress of 4.5 GPa to examine incipient spallation response. The spall strength of AM-produced 316L SS was found to be very similar for the peak shock stress studied to that of annealed wrought or AM-316L SS following recrystallization. The damage evolution as a function of microstructure was characterized using optical metallography.

Carbohydrate-Based Ice Recrystallization Inhibitors Increase Infectivity and Thermostability of Viral Vectors

PubMed Central

Ghobadloo, Shahrokh M.; Balcerzak, Anna K.; Gargaun, Ana; Muharemagic, Darija; Mironov, Gleb G.; Capicciotti, Chantelle J.; Briard, Jennie G.; Ben, Robert N.; Berezovski, Maxim V.

2014-01-01

The inability of vaccines to retain sufficient thermostability has been an obstacle to global vaccination programs. To address this major limitation, we utilized carbohydrate-based ice recrystallization inhibitors (IRIs) to eliminate the cold chain and stabilize the potency of Vaccinia virus (VV), Vesicular Stomatitis virus (VSV) and Herpes virus-1 (HSV-1). The impact of these IRIs was tested on the potency of the viral vectors using a plaque forming unit assay following room temperature storage, cryopreservation with successive freeze-thaw cycles and lyophilization. Viral potency after storage with all three conditions demonstrated that N-octyl-gluconamide (NOGlc) recovered the infectivity of shelf stored VV, 5.6 Log10 PFU mL−1 during 40 days, and HSV-1, 2.7 Log10 PFU mL−1 during 9 days. Carbon-linked antifreeze glycoprotein analogue ornithine-glycine-glycine-galactose (OGG-Gal) increases the recovery of VV and VSV more than 1 Log10 PFU mL−1 after 10 freeze-thaw cycles. In VSV, cryostorage with OGG-Gal maintains high infectivity and reduces temperature-induced aggregation of viral particles by 2 times that of the control. In total, OGG-Gal and NOGlc preserve virus potency during cryostorage. Remarkably, NOGlc has potential to eliminate the cold chain and permit room temperature storage of viral vectors. PMID:25078058

Biosignatures in the Recrystallized Shock Melt Pocket of ALH-77005 Shergottite — Clues to Martian Life

NASA Astrophysics Data System (ADS)

Gyollai, I.; Polgári, M.; Bérczi, Sz.; Gucsik, A.; Pál-Molnár, E.

2017-11-01

In the spinifex textured, recrystallized shock melt portion in ALH 77005 shergottite mineralized microbially produced texture (MMPT) - in form of pearl necklace-like, vermiform inner signatures - was measured, which we propose to have Martian origin.

Microstructural and rheological evolution of calcite mylonites during shear zone thinning: Constraints from the Mount Irene shear zone, Fiordland, New Zealand

NASA Astrophysics Data System (ADS)

Negrini, Marianne; Smith, Steven A. F.; Scott, James M.; Tarling, Matthew S.

2018-01-01

Layers of calc-mylonite in the Mount Irene shear zone, Fiordland, New Zealand, show substantial variations in thickness due to deflection of the shear zone boundaries around wall rock asperities. In relatively thick parts (c. 2.6 m) of the shear zone, calcite porphyroclasts are internally strained, contain abundant subgrain boundaries and have a strong shape preferred orientation (SPO) and crystallographic preferred orientation (CPO), suggesting that deformation occurred mainly by dislocation creep involving subgrain-rotation recrystallization. In relatively thin parts (c. 1.5 m) of the shear zone, aggregates of fine-grained recrystallized calcite surrounding flattened porphyroclasts have a weak SPO and CPO, and contain polygonal calcite grains with low degrees of internal misorientation. The recrystallized aggregates also contain microstructures (e.g. grain quadruple junctions, randomized misorientation axes) similar to those reported for neighbor-switching processes during grain-boundary sliding. Comparison of subgrain sizes in the porphyroclasts to published grain-size differential-stress relationships indicates that stresses and strain rates were substantially higher in relatively thin parts of the shear zone. The primary microstructural response to higher stresses and strain rates was an increase in the amount of recrystallization to produce aggregates that deformed by grain-boundary sliding. However, even after the development of interconnected networks of recrystallized grains, dislocation creep by subgrain-rotation recrystallization continued to occur within porphyroclasts. This behavior suggests that the bulk rheology of shear zones undergoing thinning and thickening can be controlled by concomitant grain-size insensitive and grain-size sensitive mechanisms. Overall, our observations show that shear zone thickness variations at constant P-T can result in highly variable stresses and strain rates, which in turn modifies microstructure, deformation mechanism and shear zone rheology.

Effects of two-step homogenization on precipitation behavior of Al{sub 3}Zr dispersoids and recrystallization resistance in 7150 aluminum alloy

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

Guo, Zhanying; Key Laboratory for Anisotropy and Texture of Materials, Northeastern University, Shenyang 110819, China,; Zhao, Gang

2015-04-15

The effect of two-step homogenization treatments on the precipitation behavior of Al{sub 3}Zr dispersoids was investigated by transmission electron microscopy (TEM) in 7150 alloys. Two-step treatments with the first step in the temperature range of 300–400 °C followed by the second step at 470 °C were applied during homogenization. Compared with the conventional one-step homogenization, both a finer particle size and a higher number density of Al{sub 3}Zr dispersoids were obtained with two-step homogenization treatments. The most effective dispersoid distribution was attained using the first step held at 300 °C. In addition, the two-step homogenization minimized the precipitate free zonesmore » and greatly increased the number density of dispersoids near dendrite grain boundaries. The effect of two-step homogenization on recrystallization resistance of 7150 alloys with different Zr contents was quantitatively analyzed using the electron backscattered diffraction (EBSD) technique. It was found that the improved dispersoid distribution through the two-step treatment can effectively inhibit the recrystallization process during the post-deformation annealing for 7150 alloys containing 0.04–0.09 wt.% Zr, resulting in a remarkable reduction of the volume fraction and grain size of recrystallization grains. - Highlights: • Effect of two-step homogenization on Al{sub 3}Zr dispersoids was investigated by TEM. • Finer and higher number of dispersoids obtained with two-step homogenization • Minimized the precipitate free zones and improved the dispersoid distribution • Recrystallization resistance with varying Zr content was quantified by EBSD. • Effectively inhibit the recrystallization through two-step treatments in 7150 alloy.« less

Dissolution enhancement of gliclazide using pH change approach in presence of twelve stabilizers with various physico-chemical properties.

PubMed

Talari, Roya; Varshosaz, Jaleh; Mostafavi, Seyed Abolfazl; Nokhodchi, Ali

2009-01-01

The micronization using milling process to enhance dissolution rate is extremely inefficient due to a high energy input, and disruptions in the crystal lattice which can cause physical or chemical instability. Therefore, the aim of the present study is to use in situ micronization process through pH change method to produce micron-size gliclazide particles for fast dissolution hence better bioavailability. Gliclazide was recrystallized in presence of 12 different stabilizers and the effects of each stabilizer on micromeritic behaviors, morphology of microcrystals, dissolution rate and solid state of recrystallized drug particles were investigated. The results showed that recrystallized samples showed faster dissolution rate than untreated gliclazide particles and the fastest dissolution rate was observed for the samples recrystallized in presence of PEG 1500. Some of the recrystallized drug samples in presence of stabilizers dissolved 100% within the first 5 min showing at least 10 times greater dissolution rate than the dissolution rate of untreated gliclazide powders. Micromeritic studies showed that in situ micronization technique via pH change method is able to produce smaller particle size with a high surface area. The results also showed that the type of stabilizer had significant impact on morphology of recrystallized drug particles. The untreated gliclazide is rod or rectangular shape, whereas the crystals produced in presence of stabilizers, depending on the type of stabilizer, were very fine particles with irregular, cubic, rectangular, granular and spherical/modular shape. The results showed that crystallization of gliclazide in presence of stabilizers reduced the crystallinity of the samples as confirmed by XRPD and DSC results. In situ micronization of gliclazide through pH change method can successfully be used to produce micron-sized drug particles to enhance dissolution rate.

Predicting the Kinetics of Ice Recrystallization in Aqueous Sugar Solutions

PubMed Central

2018-01-01

The quality of stored frozen products such as foods and biomaterials generally degrades in time due to the growth of large ice crystals by recrystallization. While there is ample experimental evidence that recrystallization within such products (or model systems thereof) is often dominated by diffusion-limited Ostwald ripening, the application of Ostwald-ripening theories to predict measured recrystallization rates has only met with limited success. For a model system of polycrystalline ice within an aqueous solution of sugars, we here show recrystallization rates can be predicted on the basis of Ostwald ripening theory, provided (1) the theory accounts for the fact the solution can be nonideal, nondilute and of different density than the crystals, (2) the effect of ice-phase volume fraction on the diffusional flux of water between crystals is accurately described, and (3) all relevant material properties (involving binary Fick diffusion coefficients, the thermodynamic factor of the solution, and the surface energy of ice) are carefully estimated. To enable calculation of material properties, we derive an alternative formulation of Ostwald ripening in terms of the Maxwell–Stefan instead of the Fick approach to diffusion. First, this leads to a cancellation of the thermodynamic factor (a measure for the nonideality of a solution), which is a notoriously difficult property to obtain. Second, we show that Maxwell–Stefan diffusion coefficients can to a reasonable approximation be related to self-diffusion coefficients, which are relatively easy to measure or predict in comparison to Fick diffusion coefficients. Our approach is validated for a binary system of water and sucrose, for which we show predicted recrystallization rates of ice compare well to experimental results, with relative deviations of at most a factor of 2. PMID:29651228

Predicting the Kinetics of Ice Recrystallization in Aqueous Sugar Solutions.

PubMed

van Westen, Thijs; Groot, Robert D

2018-04-04

The quality of stored frozen products such as foods and biomaterials generally degrades in time due to the growth of large ice crystals by recrystallization. While there is ample experimental evidence that recrystallization within such products (or model systems thereof) is often dominated by diffusion-limited Ostwald ripening, the application of Ostwald-ripening theories to predict measured recrystallization rates has only met with limited success. For a model system of polycrystalline ice within an aqueous solution of sugars, we here show recrystallization rates can be predicted on the basis of Ostwald ripening theory, provided (1) the theory accounts for the fact the solution can be nonideal, nondilute and of different density than the crystals, (2) the effect of ice-phase volume fraction on the diffusional flux of water between crystals is accurately described, and (3) all relevant material properties (involving binary Fick diffusion coefficients, the thermodynamic factor of the solution, and the surface energy of ice) are carefully estimated. To enable calculation of material properties, we derive an alternative formulation of Ostwald ripening in terms of the Maxwell-Stefan instead of the Fick approach to diffusion. First, this leads to a cancellation of the thermodynamic factor (a measure for the nonideality of a solution), which is a notoriously difficult property to obtain. Second, we show that Maxwell-Stefan diffusion coefficients can to a reasonable approximation be related to self-diffusion coefficients, which are relatively easy to measure or predict in comparison to Fick diffusion coefficients. Our approach is validated for a binary system of water and sucrose, for which we show predicted recrystallization rates of ice compare well to experimental results, with relative deviations of at most a factor of 2.

Utilization of the Philippine Research Reactor as a training facility for nuclear power plant operators

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

Palabrica, R.J.

1981-01-01

The Philippines has a 1-MW swimming-pool reactor facility operated by the Philippine Atomic Energy Commission (PAEC). The reactor is light-water moderated and cooled, graphite reflected, and fueled with 90% enriched uranium. Since it became critical in 1963 it has been utilized for research, radioisotope production, and training. It was used initially in the training of PAEC personnel and other research institutions and universities. During the last few years, however, it has played a key role in training personnel for the Philippine Nuclear Power Project (PNPP).

Reinforced Carbon Carbon (RCC) oxidation resistant material samples - Baseline coated, and baseline coated with tetraethyl orthosilicate (TEOS) impregnation

NASA Technical Reports Server (NTRS)

Gantz, E. E.

1977-01-01

Reinforced carbon-carbon material specimens were machined from 19 and 33 ply flat panels which were fabricated and processed in accordance with the specifications and procedures accepted for the fabrication and processing of the leading edge structural subsystem (LESS) elements for the space shuttle orbiter. The specimens were then baseline coated and tetraethyl orthosilicate impregnated, as applicable, in accordance with the procedures and requirements of the appropriate LESS production specifications. Three heater bars were ATJ graphite silicon carbide coated with the Vought 'pack cementation' coating process, and three were stackpole grade 2020 graphite silicon carbide coated with the chemical vapor deposition process utilized by Vought in coating the LESS shell development program entry heater elements. Nondestructive test results are reported.

Three-dimensional direct laser written graphitic electrical contacts to randomly distributed components

NASA Astrophysics Data System (ADS)

Dorin, Bryce; Parkinson, Patrick; Scully, Patricia

2018-04-01

The development of cost-effective electrical packaging for randomly distributed micro/nano-scale devices is a widely recognized challenge for fabrication technologies. Three-dimensional direct laser writing (DLW) has been proposed as a solution to this challenge, and has enabled the creation of rapid and low resistance graphitic wires within commercial polyimide substrates. In this work, we utilize the DLW technique to electrically contact three fully encapsulated and randomly positioned light-emitting diodes (LEDs) in a one-step process. The resolution of the contacts is in the order of 20 μ m, with an average circuit resistance of 29 ± 18 kΩ per LED contacted. The speed and simplicity of this technique is promising to meet the needs of future microelectronics and device packaging.

The electrophoretic deposition of ZnO on highly oriented pyrolytic graphite

NASA Astrophysics Data System (ADS)

Ghalamboran, Milad; Jahangiri, Mojtaba; Yousefiazari, Ehsan

2017-12-01

Intensive research has been conducted on ZnO thin and thick films in recent years. Such layers, used in different electronic devices, are deposited utilizing various methods, but electrophoretic deposition (EPD) has been chosen because of the advantages like low energy consumption, economical superiority, ecofriendliness, controllability, and high deposition rate. Here, we report electrophoretically depositing ZnO layers onto highly oriented pyrolytic graphite. Well-dispersed and stable ZnO suspensions are used for the deposition of continuous and even layers of ZnO on the substrate. ZnO powder is dispersed in acetone. The electric field applied is in the 250 V/cm to 2000 V/cm range. The morphology of the deposits are studied by SEM at the different stages of the deposition process.

Metadynamic and static recrystallization softening behavior of a bainite steel

NASA Astrophysics Data System (ADS)

Li, Lixin; Zheng, Liangyu; Ye, Ben; Tong, Zeqiong

2018-01-01

The metadynamic recrystallization (MDRX) and static recrystallization (SRX) softening behavior of a bainite steel was investigated by two-pass isothermal compression experiments at temperatures of 1173, 1273, 1373, and 1473 K and strain rates of 0.01, 0.1, 1, and 10 s-1 with inter-pass times of 1, 5, 10, and 30 s on a Gleeble-1500 thermo-mechanical simulator. Kinetic equations were developed to evaluate the softening fractions caused by MDRX and SRX. A comparison between the experimental and predicted softening fractions showed that the proposed kinetic equations can provide a precise estimation of the MDRX and SRX behavior of the studied steel. The results based on the kinetic equations indicated that the MDRX and SRX softening fraction increases with the increase in strain rate, deformation temperature, inter-pass time, and pre-strain; the activation energy of MDRX is much smaller than that of SRX; and the no-recrystallization temperature of the investigated steel is 1179.4 K.

Fabric and texture at Siple Dome, Antarctica

USGS Publications Warehouse

Diprinzio, C.L.; Wilen, Lawrence A.; Alley, R.B.; Fitzpatrick, J.J.; Spencer, M.K.; Gow, A.J.

2005-01-01

Preferred c-axis orientations are present in the firn at Siple Dome, West Antarctica, and recrystallization begins as shallow as 200 m depth in ice below -20??C, based on digital analysis of c-axis fabrics, grain-sizes and other characteristics of 52 vertical thin sections prepared in the field from the kilometer-long Siple Dome ice core. The shallowest section analyzed, from 22 m, shows clustering of c axes toward the vertical. By 200 m depth, girdle fabric and other features of recrystallized ice are evident in layers (or regions), separated by layers (regions) of typically finer-grained ice lacking evidence of recrystallization. Ice from about 700-780 m depth, which was deposited during the last ice age, is especially fine-grained, with strongly vertical c axes, but deeper ice shows much larger crystals and strong evidence of recrystallization. Azimuthal asymmetry of some c-axis fabrics, trends in grain-size, and other indicators reveal additional information on processes and history of ice flow at Siple Dome.

Effect of Thermomechanical Processing on Texture and Superelasticity in Fe-Ni-Co-Al-Ti-B Alloy

NASA Astrophysics Data System (ADS)

Lee, Doyup; Omori, Toshihiro; Han, Kwangsik; Hayakawa, Yasuyuki; Kainuma, Ryosuke

2018-03-01

The texture and superelasticity were investigated in austenitic Fe-Ni-Co-Al-Ti-B alloy with various reduction ratios of cold rolling and heating ratios in annealing. The rolled sheets show the {110} <112> deformation texture at a reduction ratio higher than 80%, while the texture hardly changes in the primary recrystallization at 1000 °C. The β (B2) precipitates inhibit the grain growth at this temperature, but they dissolve during heating, and secondary recrystallization occurs due to decreased pinning force at temperatures higher than 1100 °C, resulting in texture change to {210} <001> . The recrystallization texture is more strongly developed when the reduction ratio and heating rate are high and slow, respectively. The 90% cold-rolled and slowly heated sheet shows the recrystallization texture and high fraction of low-angle boundaries. As a result, ductility and superelasticity can be drastically improved in the 90% cold-rolled sheet, although superelasticity was previously obtained only in thin sheets with 98.5% reduction.

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

The sintered aluminum powder (SAP) technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of a nickel alloy containing, by weight, 17% Cr, 5% Al, and 0.2% Y. The SAP-NiCrAl alloy (without the ytterbium removed by oxdation) was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. Annealing treatments were applied after working to determine the recrystallization response. The NiCrAlY alloy, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl alloy exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl alloy as has been reported for other oxide dispersion strengthened alloys. In contrast, the unoxidized NiCrAlY alloy exhibited only primary recrystallization.

Modeling Deformation Flow Curves and Dynamic Recrystallization of BA-160 Steel During Hot Compression

NASA Astrophysics Data System (ADS)

Shahriari, Babak; Vafaei, Reza; Mohammad Sharifi, Ehsan; Farmanesh, Khosro

2018-03-01

The hot deformation behavior of a high strength low carbon steel was investigated using hot compression test at the temperature range of 850-1100 °C and under strain rates varying from 0.001 to 1 s-1. It was found that the flow curves of the steel were typical of dynamic recrystallization at the temperature of 950 °C and above; at tested strain rates lower than 1 s-1. A very good correlation between the flow stress and Zener-Hollomon parameter was obtained using a hyperbolic sine function. The activation energy of deformation was found to be around 390 kJ mol-1. The kinetics of dynamic recrystallization of the steel was studied by comparing it with a hypothetical dynamic recovery curve, and the dynamically fraction recrystallized was modeled by the Kolmogorov-Johnson-Mehl-Avrami relation. The Avrami exponent was approximately constant around 1.8, which suggested that the type of nucleation was one of site saturation on grain boundaries and edges.

Effects of Laves phase particles on recovery and recrystallization behaviors of Nb-containing FeCrAl alloys

DOE PAGES

Sun, Zhiqian; Edmondson, Philip D.; Yamamoto, Yukinori

2017-11-15

The microstructures and mechanical properties of deformed and annealed Nb-containing FeCrAl alloys were investigated. Fine dispersion of Fe 2Nb-type Laves phase particles was observed in the bcc-Fe matrix after applying a thermomechanical treatment, especially along grain/subgrain boundaries, which effectively stabilized the recovered and recrystallized microstructures compared with the Nb-free FeCrAl alloy. The stability of recovered areas increased with Nb content up to 1 wt%. The recrystallized grain structure in Nb-containing FeCrAl alloys consisted of elongated grains along the rolling direction with a weak texture when annealed below 1100 °C. An abnormal relationship between recrystallized grain size and annealing temperature wasmore » found. Microstructural inhomogeneity in the deformed and annealed states was explained based on the Taylor factor. Annealed Nb-containing FeCrAl alloys showed a good combination of strength and ductility, which is desirable for their application as fuel cladding in light-water reactors.« less

A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction

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

Christien, F., E-mail: frederic.christien@univ-nantes.fr; Le Gall, R.; Telling, M. T. F.

2015-05-15

A method is proposed for the monitoring of metal recrystallization using neutron diffraction that is based on the measurement of stored energy. Experiments were performed using deformed metal specimens heated in-situ while mounted at the sample position of the High Resolution Powder Diffractometer, HRPD (ISIS Facility), UK. Monitoring the breadth of the resulting Bragg lines during heating not only allows the time-dependence (or temperature-dependence) of the stored energy to be determined but also the recrystallized fraction. The analysis method presented here was developed using pure nickel (Ni270) specimens with different deformation levels from 0.29 to 0.94. In situ temperature rampingmore » as well as isothermal annealing was undertaken. The method developed in this work allows accurate and quantitative monitoring of the recrystallization process. The results from neutron diffraction are satisfactorily compared to data obtained from calorimetry and hardness measurements.« less

Shock-induced fine-grained recrystallization of olivine - Evidence against subsolidus reduction of Fe/2+/

NASA Technical Reports Server (NTRS)

Ahrens, T. J.; Tsay, F.-D.; Live, D. H.

1976-01-01

Electron spin resonance (ESR) studies have been carried out on three single grains of terrestrial olivine (Fo90) shock loaded along the 010 line to peak pressures of 280, 330, and 440 kbar. The results indicate that neither metallic Fe similar to that observed in returned lunar soils nor paramagnetic Fe(3+) caused by oxidation of Fe(2+) has been produced in these shock experiments. Trace amounts of Mn (2+) have been detected in both shocked and unshocked olivine. The ESR signals of Mn(2+) show spectral features which are found to correlate with the degree of shock-induced recrystallization observed petrographically. The increasing mass fraction of recrystallized olivine correlates with increasing shock pressures. This phenomenon is modelled assuming it results from the progressive effect of the shock-induced transformation of the olivine to a yet unknown high-pressure phase and its subsequent reversion to the low-pressure olivine phase. The mass fraction of recrystallized material is predicted to be nearly linear with shock pressure.

The Effect of Dynamic Recrystallization on Monotonic and Cyclic Behaviour of Al-Cu-Mg Alloy.

PubMed

Tomczyk, Adam; Seweryn, Andrzej; Grądzka-Dahlke, Małgorzata

2018-05-23

The paper presents an investigation that was conducted to determine the possibility of the occurrence of the process of dynamic recrystallization in 2024 alloy during monotonic tensile and creep tests at the elevated temperatures of 100 °C, 200 °C, and 300 °C. As-extruded material was subjected to creep process with constant force at elevated temperatures, until two varying degrees of deformation were reached. After cooling at ambient temperature, the pre-deformed material was subjected to monotonic and fatigue tests as well as metallographic analysis. The process of dynamic recrystallization was determined in monotonic tests to occur at low strain rate (0.0015/s) only at the temperature of 300 °C. However, in the creep tests, this process occurred with varying efficiency, both during creep at 200 °C and 300 °C. Dynamic recrystallization was indicated to have a significant influence on the monotonic and cyclic properties of the material.

Influence of initial heating during final high temperature annealing on the offset of primary and secondary recrystallization in Cu-bearing grain oriented electrical steels

NASA Astrophysics Data System (ADS)

Rodriguez-Calvillo, P.; Leunis, E.; Van De Putte, T.; Jacobs, S.; Zacek, O.; Saikaly, W.

2018-04-01

The industrial production route of Grain Oriented Electrical Steels (GOES) is complex and fine-tuned for each grade. Its metallurgical process requires in all cases the abnormal grain growth (AGG) of the Goss orientation during the final high temperature annealing (HTA). The exact mechanism of AGG is not yet fully understood, but is controlled by the different inhibition systems, namely MnS, AlN and CuxS, their size and distribution, and the initial primary recrystallized grain size. Therefore, among other parameters, the initial heating stage during the HTA is crucial for the proper development of primary and secondary recrystallized microstructures. Cold rolled 0.3 mm Cu-bearing Grain Oriented Electrical Steel has been submitted to interrupted annealing experiments in a lab tubular furnace. Two different annealing cycles were applied:• Constant heating at 30°C/h up to 1000°C. Two step cycle with initial heating at 100°C/h up to 600°C, followed by 18 h soaking at 600°C and then heating at 30°C/h up to 1050°C. The materials are analyzed in terms of their magnetic properties, grain size, texture and precipitates. The characteristic magnetic properties are analyzed for the different extraction temperatures and Cycles. As the annealing was progressing, the coercivity values (Hc 1.7T [A/m]) decreased, showing two abrupt drops, which can be associated to the on-set of primary and secondary recrystallization. The primary recrystallized grain sizes and recrystallized fractions are fitted to a model using a non-isothermal approach. This analysis shows that, although the resulting grain sizes were similar, the kinetics for the two step annealing were faster due to the lower recovery. The on-set of secondary recrystallization was also shifted to higher temperatures in the case of the continuous heating cycle, which might end in different final grain sizes and final magnetic properties. In both samples, nearly all the observed precipitates are Al-Si-Mn nitrides, ranging from pure AlN to Si4Mn-nitride.

Intragranular Recrystallization and Lattice Reorientation of Calcite Grains in Experimentally Deformed Crinoids and Trilobites

NASA Astrophysics Data System (ADS)

Kim, N.; Takahashi, M.; Shigematsu, N.; Ree, J. H.; Jung, H.

2017-12-01

Intragranular recrystallization, including subgrain-rotation-recrystallization (SGR) and nucleation (and growth) of new grains along boundaries of deformation twins and bands, is an important process leading to grain-size reduction and causing rheological change depending on deformation condition. Despite of its importance, the detailed processes of intragranular recrystallization are still somewhat unclear. We deformed a limestone using triaxial testing machine at AIST of Japan at temperature of 500 700 °, strain rate of 10-4 10-5 s-1, confining pressure of 200 MPa and strain of up to 30%, to explore intragranular recrystallization processes of calcite. The limestone contains two abundant fossils, crinoid and trilobite. The crinoids are mono- or poly-crystalline. We focus on the monocrystalline crinoids with a coarser grain size ( 700 μm). The trilobites are polycrystalline and much finer-grained ( 7 μm) with initially a strong c-axis preferred orientation. At a lower temperature condition, subgrains develop both in twin and host domains of crinoids and evolve into new grains by SGR. At a higher temperature, recrystallized grains have irregular grain boundaries and bimodal grain-size distribution, implying grain-boundary migration (GBM) recrystallization. At a lower temperature, new grains nucleating and growing along twin boundaries inherit lattice orientation of twin domain, and with the nucleation site and usually a smaller grain size, they can be distinguished from new grains by SGR. At a higher temperature, however, the distinction is difficult at present due to extensive GBM. For the trilobites, there is only local GBM with no significant change in grain size, and flattening of grains reflects the bulk strain at a lower temperature. At a higher temperature, individual grains of the trilobites are equi-axed with weakened LPO, although the strain of trilobites is higher than bulk strain. These microfabrics suggest that the dominant deformation mechanism of the trilobites is diffusion creep. Although the initial LPO of the trilobites is weakened, the LPO is still preserved up to strain of 30%. This implies that even if the grain size of trilobites and matrix is similar in naturally deformed limestones, the lattice orientation map may be useful in recognizing trilobite fossils.

Recrystallization and Grain Growth Kinetics in Binary Alpha Titanium-Aluminum Alloys

NASA Astrophysics Data System (ADS)

Trump, Anna Marie

Titanium alloys are used in a variety of important naval and aerospace applications and often undergo thermomechanical processing which leads to recrystallization and grain growth. Both of these processes have a significant impact on the mechanical properties of the material. Therefore, understanding the kinetics of these processes is crucial to being able to predict the final properties. Three alloys are studied with varying concentrations of aluminum which allows for the direct quantification of the effect of aluminum content on the kinetics of recrystallization and grain growth. Aluminum is the most common alpha stabilizing alloying element used in titanium alloys, however the effect of aluminum on these processes has not been previously studied. This work is also part of a larger Integrated Computational Materials Engineering (ICME) effort whose goal is to combine both computational and experimental efforts to develop computationally efficient models that predict materials microstructure and properties based on processing history. The static recrystallization kinetics are measured using an electron backscatter diffraction (EBSD) technique and a significant retardation in the kinetics is observed with increasing aluminum concentration. An analytical model is then used to capture these results and is able to successfully predict the effect of solute concentration on the time to 50% recrystallization. The model reveals that this solute effect is due to a combination of a decrease in grain boundary mobility and a decrease in driving force with increasing aluminum concentration. The effect of microstructural inhomogeneities is also experimentally quantified and the results are validated with a phase field model for recrystallization. These microstructural inhomogeneities explain the experimentally measured Avrami exponent, which is lower than the theoretical value calculated by the JMAK model. Similar to the effect seen in recrystallization, the addition of aluminum also significantly slows downs the grain growth kinetics. This is generally attributed to the solute drag effect due to segregation of solute atoms at the grain boundaries, however aluminum segregation is not observed in these alloys. The mechanism for this result is explained and is used to validate the prediction of an existing model for solute drag.

Various Recrystallizations of CL-20 (HNIW hexanitrohexaazaisowurtzitane).

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

Phillips, Jason Joe

Impact sensitivity testing was performed using a modified Bureau of Mines (MBOM) impactor manufactured by Safety Management Services, Inc., shown in Figure 1. Type-12 tooling was utilized on this machine with a 2.5kg impactor and matching intermediate mass. This particular machine is capable of a maximum drop height of 115cm with 0.1cm increments, though 1cm increments are typically used. Sample material was placed (35 ± 2mg) onto 1 inch squares of Norton brand 180A Garnet sandpaper. Positive results were detected visually or audibly by the operator as smoke, flash, report, charring/tearing of the sandpaper, etc.

Microstructure in Worn Surface of Hadfield Steel Crossing

NASA Astrophysics Data System (ADS)

Zhang, F. C.; Lv, B.; Wang, T. S.; Zheng, C. L.; Li, M.; Zhang, M.

In this paper a failed Hadfield (high manganese austenite) steel crossing used in railway system was studied. The microstructure in the worn surfaces of the crossing was investigated using optical microscopy, scanning electron microscopy, transmission electron microscopy and Mössbauer spectroscopy. The results indicated that a nanocrystallization layer formed on the surface of the crossing served. The formation mechanism of the nanocrystalline is the discontinuous dynamic recrystallization. The energy for the recrystallization nucleus formation originates from the interactions between the twins, the dislocations, as well as twin and dislocation. High-density vacancies promoted the recrystallization process including the dislocation climb and the atom diffusion.

Plasticity-mediated collapse and recrystallization in hollow copper nanowires: a molecular dynamics simulation.

PubMed

Dutta, Amlan; Raychaudhuri, Arup Kumar; Saha-Dasgupta, Tanusri

2016-01-01

We study the thermal stability of hollow copper nanowires using molecular dynamics simulation. We find that the plasticity-mediated structural evolution leads to transformation of the initial hollow structure to a solid wire. The process involves three distinct stages, namely, collapse, recrystallization and slow recovery. We calculate the time scales associated with different stages of the evolution process. Our findings suggest a plasticity-mediated mechanism of collapse and recrystallization. This contradicts the prevailing notion of diffusion driven transport of vacancies from the interior to outer surface being responsible for collapse, which would involve much longer time scales as compared to the plasticity-based mechanism.

Influence of crystal habit on trimethoprim suspension formulation.

PubMed

Tiwary, A K; Panpalia, G M

1999-02-01

The role of crystal habit in influencing the physical stability and pharmacokinetics of trimethoprim suspensions was examined. Different habits for trimethoprim (TMP) were obtained by recrystallizing the commercial sample (PD) utilizing solvent-change precipitation method. Four distinct habits (microscopic observation) belonging to the same polymorphic state (DSC studies) were selected for studies. Preformulation and formulation studies were carried out on suspension dosage forms containing these crystals. The freshly prepared suspensions were also evaluated for their pharmacokinetic behaviour on healthy human volunteers using a cross over study. Variation of crystallization conditions produces different habits of TMP. Among the different crystal habits exhibiting same polymorphic state, the most anisometric crystal showed best physical stability in terms of sedimentation volume and redispersibility. However, habit did not significantly affect the extent of TMP excreted in urine. Modification of surface morphology without significantly altering the polymorphic state can be utilized for improving physical stability of TMP suspensions. However, the pharmacokinetic profile remains unaltered.

Evolution of quartz microstructure and c-axis crystallographic preferred orientation within ductilely deformed granitoids (Arolla unit, Western Alps)

NASA Astrophysics Data System (ADS)

Menegon, Luca; Pennacchioni, Giorgio; Heilbronner, Renee; Pittarello, Lidia

2008-11-01

We have studied quartz microstructures and the c-axis crystallographic preferred orientations (CPOs) in four granitoid samples representative of increasing ductile shear deformation, from a weakly deformed granitoid (stage 1) to a mylonitic granitoid (stage 4). The quartz c-axis CPO measured in the mylonitic granitoid has been compared with the one observed in a fully recrystallized quartz mylonite from the same area. All the samples belong to the Austroalpine Arolla unit (Western Alps) and were deformed at greenschist facies conditions. The quartz c-axis CPO was analyzed using a U-stage and the optical orientation imaging technique. The magmatic plagioclase, forming more than 50% of the volume of the granitoid, is extensively replaced by a mica-rich aggregate even in weakly deformed samples of stage 1. These aggregates flow to form an interconnected weak matrix with increasing deformation, wrapping relatively less strained quartz grains that undergo dominantly coaxial strain. Recrystallization of quartz ranges from less than 1% in the weakly deformed granitoid to up to 85% in the mylonitic granitoid, with average grain strain of 41% and 64%, respectively. With increasing strain and recrystallization, quartz grains in the granitoids show a sequence of transient microstructures and CPOs. Crystal plastic deformation is initially accomplished by dislocation glide with limited recovery, and at 50% grain strain it results in a CPO consistent with dominantly basal < a> slip. At 60% grain strain, recrystallization is preferentially localized along shear bands, which appear to develop along former intragranular cracks, and the recrystallized grains develop a strong c-axis CPO with maxima orthogonal to the shear band boundaries and independent of the host grain orientation. Within the granitoid mylonite, at an average quartz grain strain of 64%, recrystallization is extensive and the c-axis CPO of new grains displays maxima overlapping the host c-axis orientation and, therefore, unrelated to the bulk sense of shear. The host-controlled CPO is inferred to reflect pervasive recrystallization by progressive subgrain rotation. The switch from 'shear band-control' to 'host-control' on c-axis CPO occurred between 40% and 70% of recrystallization. In the quartz mylonite, the quartz c-axis CPO develops an asymmetric single girdle consistent with the bulk sense of shear and the synkinematic greenschist facies conditions. This study indicates that the CPO evolution of quartz may significantly differ in cases of polymineralic vs. monomineralic rocks under the same deformation conditions, if quartz in the polymineralic rock behaves as a 'strong' phase.

Ca. 400 Ma Recrystallization of Norwegian Ultrahigh-pressure Eclogites: an ion Microprobe and Chemical Abrasion Study

NASA Astrophysics Data System (ADS)

Root, D. B.; Mattinson, J. M.; Hacker, B. R.; Wooden, J. L.

2002-12-01

Understanding the formation and exhumation of the ultrahigh-pressure (UHP) rocks of western Norway hinges on precise determination of the time of eclogite recrystallization. Our study consists of SHRIMP analysis, in conjunction with CL imagery, of zircon from four UHP and high-pressure (HP) eclogites; and detailed TIMS analysis of zircon from two samples subjected to combined thermal annealing and multi-step chemical abrasion (CA). SHRIMP analyses of the Otnheim and Langenes eclogites yield Caledonian spot ages of ca. 400 Ma from zircon rims. CL imagery and Th/U ratios from the Langenes eclogite indicate formation of rims by recrystallization of inherited zircon. SHRIMP analysis of the UHP Flatraket eclogite yielded a broad range of apparently concordant Caledonian ages. CA analyses of two fractions yielded moderate Pb loss from the first (lowest T) steps; possible minor Pb loss or minor growth at 400 Ma from the second steps; and a 407-404 Ma cluster of slightly discordant 206Pb/238U ages, most likely free from Pb loss, from the remaining steps. We interpret the latter to reflect recrystallization of inherited zircon, with possible new growth, at ca. 400-395 Ma. Alternatively, the high-temperature CA steps could represent growth at 407-404 Ma, with apparent discordance due to intermediate daughter product effects. HP/UHP zircon recrystallization in the Flatraket eclogite is inferred from three lines of evidence: i) zircon occurs as inclusions in garnet, omphacite, breunnerite, dolomite, and quartz, as well as in symplectites after phengite and omphacite; ii) association of zircon with rutile implies zircon formation during HP breakdown of Zr-ilmenite; and iii) chondrite-normalized ICP-MS analyses of the CA steps reveal small Eu anomalies and shallow HREE profiles, indicating zircon recrystallization in the presence of garnet. CA analysis of the Verpeneset eclogite yielded distinctly discordant step ages from two steps comprising <90% of the sample, with 206Pb/238U ages of 408 and 414 Ma. CL imagery indicates incomplete recrystallization of inherited igneous zircon, in keeping with steep HREE profiles determined from chondrite-normalized ICP-MS analyses. Our zircon age of ca. 400-395 Ma for the Flatraket eclogite is significantly younger than the 425 Ma age often cited for western Norway eclogite recrystallization, implying, in conjunction with 390-385 Ma 40Ar/39Ar white mica cooling ages, faster rates of exhumation (ca. 15 km/m.y.), and weakening the link between UHP metamorphism and ophiolite emplacement at 430-425 Ma.

Factors controlling in vitro recrystallization of the Caulobacter crescentus paracrystalline S-layer.

PubMed Central

Nomellini, J F; Kupcu, S; Sleytr, U B; Smit, J

1997-01-01

The S-layer of Caulobacter is a two-dimensional paracrystalline array on the cell surface composed of a single protein, RsaA. We have established conditions for preparation of stable, soluble protein and then efficient in vitro recrystallization of the purified protein. Efficient recrystallization and long range order could not be obtained with pure protein only, though it was apparent that calcium was required for crystallization. Recrystallization was obtained when lipid vesicles were provided, but only when the vesicles contained the specific species of Caulobacter smooth lipopolysaccharide (SLPS) that previous studies implicated as a requirement for attaching the S-layer to the cell surface. The specific type of phospholipids did not appear critical; phospholipids rather different from those present in Caulobacter membranes or archaebacterial tetraether lipids worked equally well. The source of LPS was critical; rough and smooth variants of Salmonella typhimurium LPS as well as the rough form of Caulobacter LPS were ineffective. The requirement for calcium ions for recrystallization was further evaluated; strontium ions could substitute for calcium, and to a lesser extent, cobalt, barium, manganese and magnesium ions also stimulated crystallization. On the other hand, nickel and cadmium provided only weak crystallization stimulation, and zinc, copper, iron, aluminum ions, and the monovalent potassium, sodium, and lithium ions were ineffective. The recrystallization could also be reproduced with Langmuir-Blodgett lipid monolayers at an air-water interface. As with the vesicle experiments, this was only successful when SLPS was incorporated into the lipid mix. The best method for RsaA preparation, leading to apparently monomeric protein that was stable for many months, was an extraction with a low pH aqueous solution. We also achieved recrystallization, albeit at lower efficiency, using RsaA protein solubilized by 8 M urea, a method which allows retrieval of protein from inclusions, when expressed as heterologous protein in Escherichia coli or when retrieved as shed, precipitated protein from certain mutant caulobacters. In summary, the clarification of recrystallization methods has confirmed the requirement of SLPS as a surface attachment component and suggests that its presence in a membrane-like structure greatly stimulates the extent and quality of S-layer formation. The in vitro approach allowed the demonstration that specific ions are capable of participating in crystallization and now provides an assay for the crystallization potential of modified S-layer proteins, whether they were produced in or can be secreted by caulobacters. PMID:9335282

Relationship of Technological Properties with Dynamic Recrystallization of Quartz on the Example of Objects of the Karelian-Kola Region

NASA Astrophysics Data System (ADS)

Skamnitskaya, Lubov; Rakov, Leonid; Bubnova, Tatyana; Shchiptsov, Vladimir

2017-12-01

Despite the significant reserves of quartz raw materials, there is a deficit of high purity quartz. It is due to the strict technical requirements imposed by standards for this type of raw materials and technological properties of quartz, which are determined by the features of the crystal structure. The crystalline structure is of particular importance for the technological properties of quartz, since such important characteristics as the limit of raw material enrichment, dissolution rate in acid, melting point of quartz, etc., are determined. The formation of the crystal structure of quartz under natural conditions is associated with the successive dynamic recrystallization of the mineral. The degree of dynamic recrystallization of quartz reflects the distribution of dispersed impurities. If it is weakly manifested, the dispersed impurities are not displaced from one zone to another, and all quartz microblocks contain approximately the same concentration. In this case, more or less uniform dissolution of various regions of quartz is observed, and the pattern of distribution of submicroscopic inhomogeneities is monotonic. If intensive dynamic recrystallization of quartz takes place, then it causes a significant redistribution of the scattered impurities. Then the treatment in HF leads to the appearance of a contrast pattern of the distribution of submicroscopic inhomogeneities. The details of the crystal structure of quartz in this work were investigated by the electron paramagnetic resonance (EPR) method using the ER-420 “Bruker” spectrometer. In the selected samples of quartz, the concentrations of isomorphic impurities Al and Ti were measured, and the degree of crystallinity D of the mineral was estimated from the EPR spectra of each of them. Thus, the technological properties of quartz are determined by various geological processes. The results of the studies show that when evaluating the prospects of quartz raw materials, it is necessary to take into account the staged dynamic dynamical recrystallization of quartz in natural conditions. This factor can play both a positive and a negative role at various stages of mineral formation. Its influence is reflected in the state of the crystal structure of quartz, which should be taken into account when developing effective technologies for its enrichment. The intermediate stage of dynamic recrystallization corresponding to the end of the second stage-the beginning of the third stage of quartz recrystallization-is optimal for the formation of high-purity quartz. When choosing a site for the first-stage quartz mining at large deposits in the Karelian-Kola region, one should be guided by the stage of dynamic recrystallization.

Calcium phosphates recovery from digester supernatant by fast precipitation and recrystallization

NASA Astrophysics Data System (ADS)

Vasenko, Liubov; Qu, Haiyan

2018-01-01

Conditional solubility of dicalcium phosphate dihydrate (DCPD) and hydroxyapatite (HAp) in digester supernatant was determined as a function of pH and was compared to its conditional solubility in distilled water. Conditional solubility of both substances in digester supernatant at pH >5-6 was higher than their conditional solubility in pure water due to the presence of impurities, and this influence is more significant for HAp. Amorphous CaP was precipitated through a fast precipitation process from digester supernatant with initial total phosphate concentration 0.008 mol/L and 0.015 mol/L and Ca/P ratios 2 and 5. The amorphous CaP can be subsequently recrystallized into crystalline CaP. Obtained amorphous products have Ca/P ratio > 1, which allow performing the recrystallization process without further Ca dosing into the system. Batch recrystallization of the amorphous products resulted in crystallization of HAp, DCPD or their mixture depending on the conditions of the process. Maximum achieved P-recovery was 69.5%. The increase of phosphate concentration and the addition of seeding decreased the yield of the process but promoted crystallization of DCPD. The increase of Ca/P ratio had a positive effect on the total P-recovery. Compared with the direct batch crystallization of CaP from digester supernatant, the two-step process with fast precipitation and recrystallization significantly improved the color of the obtained products.

Solid-state characterization of nevirapine.

PubMed

Sarkar, Mahua; Perumal, O P; Panchagnula, R

2008-09-01

The purpose of this investigation is to characterize nevirapine from commercial samples and samples crystallized from different solvents under various conditions. The solid-state behavior of nevirapine samples was investigated using a variety of complementary techniques such as microscopy (optical, polarized, hot stage microscopy), differential scanning calorimeter, thermogravimetric analysis, Fourier transform infrared spectroscopy and powder X-ray diffractometry. The commercial samples of nevirapine had the same polymorphic crystalline form with an anhedral crystal habit. Intrinsic dissolution of nevirapine was similar for both the commercial batches. Powder dissolution showed pH dependency, with maximum dissolution in acidic pH and there was no significant effect of particle size. The samples recrystallized from different solvent systems with varying polarity yielded different crystal habits. Stirring and degrees of supersaturation influenced the size and shape of the crystals. The recrystallized samples did not produce any new polymorphic form, but weak solvates with varying crystal habit were produced. Recrystallized samples showed differences in the x-ray diffractograms. However, all the samples had the same internal crystal lattice as revealed from their similar melting points and heat of fusion. The intrinsic dissolution rate of recrystallized samples was lower than the commercial sample. It was found that the compression pressure resulted in desolvation and partial conversion of the crystal form. After compression, the recrystallized samples showed similar x-ray diffractograms to the commercial sample. Amorphous form showed slightly higher aqueous solubility than the commercial crystalline form.

Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

PubMed

Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

2016-07-01

Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Molecular Dynamics at the Interface between Ice and Poly(vinyl alcohol) and Ice Recrystallization Inhibition.

PubMed

Weng, Lindong; Stott, Shannon L; Toner, Mehmet

2018-05-01

Ice formation is a ubiquitous process that poses serious challenges for many areas. Nature has evolved a variety of different mechanisms to regulate ice formation. For example, many cold-adapted species produce antifreeze proteins (AFPs) and/or antifreeze glycoproteins (AFGPs) to inhibit ice recrystallization. Although several synthetic substitutes for AF(G)Ps have been developed, the fundamental principles of designing AF(G)P mimics are still missing. In this study, we explored the molecular dynamics of ice recrystallization inhibition (IRI) by poly(vinyl alcohol) (PVA), a well-recognized ice recrystallization inhibitor, to shed light on the otherwise hidden ice-binding mechanisms of chain polymers. Our molecular dynamics simulations revealed a stereoscopic, geometrical match between the hydroxyl groups of PVA and the water molecules of ice, and provided microscopic evidence of the adsorption of PVA to both the basal and prism faces of ice and the incorporation of short-chain PVA into the ice lattice. The length of PVA, i.e., the number of hydroxyl groups, seems to be a key factor dictating the performance of IRI, as the PVA molecule must be large enough to prevent the joining together of adjacent curvatures in the ice front. The findings in this study will help pave the path for addressing a pressing challenge in designing synthetic ice recrystallization inhibitors rationally, by enriching our mechanistic understanding of IRI process by macromolecules.

Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

USGS Publications Warehouse

Elsheimer, H.N.; Fries, T.L.

1990-01-01

A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

One-step preparation of nanostructured martite catalyst and graphite electrode by glow discharge plasma for heterogeneous electro-Fenton like process.

PubMed

Khataee, Alireza; Sajjadi, Saeed; Hasanzadeh, Aliyeh; Vahid, Behrouz; Joo, Sang Woo

2017-09-01

Natural Martite ore particles and graphite were modified by alternating current (AC) glow discharge plasma to form nanostructured catalyst and cathode electrode for using in the heterogeneous-electro Fenton-like (Het-EF-like) process. The performance of the plasma-treated martite (PTM) and graphite electrode (PTGE) was studied for the treatment of paraquat herbicide in a batch system. 85.78% degradation efficiency for 20 mg L -1 paraquat was achieved in the modified process under desired operational conditions (i.e. current intensity of 300 mA, catalyst amount of 1 g L -1 , pH = 6, and background electrolyte (Na 2 SO 4 ) concentration of 0.05 mol L -1 ) which was higher than the 41.03% for the unmodified one after 150 min of treatment. The ecofriendly modification of the martite particles and the graphite electrode, no chemical needed, low leached iron and milder operational pH were the main privileges of plasma utilization. Moreover, the degradation efficiency through the process was not declined after five repeated cycles at the optimized conditions, which proved the stability of the nanostructured PTM and PTGE in the long-term usage. The archived results exhibit this method is the first example of high efficient, cost-effective, and environment-friendly method for generation of nanostructured samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

A Behavioral Analysis of the Laboratory Learning Process: Redesigning a Teaching Unit on Recrystallization.

ERIC Educational Resources Information Center

Mulder, T.; Verdonk, A. H.

1984-01-01

Reports on a project in which observations of student and teaching assistant behavior were used to redesign a teaching unit on recrystallization. Comments on the instruction manual, starting points for teaching the unit, and list of objectives with related tasks are included. (JN)

Electrode wells for powerline-frequency electrical heating of soils

DOEpatents

Buettner, H.M.; Daily, W.D.; Aines, R.D.; Newmark, R.L.; Ramirez, A.L.; Siegel, W.H.

1999-05-25

An electrode well is described for use in powerline-frequency heating of soils for decontamination of the soil. Heating of soils enables the removal of volatile organic compounds from soil when utilized in combination with vacuum extraction. A preferred embodiment of the electrode well utilizes a mild steel pipe as the current-carrying conductor to at least one stainless steel electrode surrounded by a conductive backfill material, preferably graphite or steel shot. A covering is also provided for electrically insulating the current-carrying pipe. One of the electrode wells is utilized with an extraction well which is under subatmospheric pressure to withdraw the volatile material, such as gasoline and trichloroethylene (TCE) as it is heated. 4 figs.

Electrode wells for powerline-frequency electrical heating of soils

DOEpatents

Buettner, Harley M.; Daily, William D.; Aines, Roger D.; Newmark, Robin L.; Ramirez, Abelardo L.; Siegel, William H.

1999-01-01

An electrode well for use in powerline-frequency heating of soils for decontamination of the soil. Heating of soils enables the removal of volatile organic compounds from soil when utilized in combination with vacuum extraction. A preferred embodiment of the electrode well utilizes a mild steel pipe as the current-carrying conductor to at least one stainless steel electrode surrounded by a conductive backfill material, preferably graphite or steel shot. A covering is also provided for electrically insulating the current-carrying pipe. One of the electrode wells is utilized with an extraction well which is under subatmospheric pressure to withdraw the volatile material, such as gasoline and trichioroethylene (TCE) as it is heated.

Calculated criticality for sup 235 U/graphite systems using the VIM Monte Carlo code

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

Collins, P.J.; Grasseschi, G.L.; Olsen, D.N.

1992-01-01

Calculations for highly enriched uranium and graphite systems gained renewed interest recently for the new production modular high-temperature gas-cooled reactor (MHTGR). Experiments to validate the physics calculations for these systems are being prepared for the Transient Reactor Test Facility (TREAT) reactor at Argonne National Laboratory (ANL-West) and in the Compact Nuclear Power Source facility at Los Alamos National Laboratory. The continuous-energy Monte Carlo code VIM, or equivalently the MCNP code, can utilize fully detailed models of the MHTGR and serve as benchmarks for the approximate multigroup methods necessary in full reactor calculations. Validation of these codes and their associated nuclearmore » data did not exist for highly enriched {sup 235}U/graphite systems. Experimental data, used in development of more approximate methods, dates back to the 1960s. The authors have selected two independent sets of experiments for calculation with the VIM code. The carbon-to-uranium (C/U) ratios encompass the range of 2,000, representative of the new production MHTGR, to the ratio of 10,000 in the fuel of TREAT. Calculations used the ENDF/B-V data.« less

Lithium dendrite and solid electrolyte interphase investigation using OsO4

NASA Astrophysics Data System (ADS)

Zier, Martin; Scheiba, Frieder; Oswald, Steffen; Thomas, Jürgen; Goers, Dietrich; Scherer, Torsten; Klose, Markus; Ehrenberg, Helmut; Eckert, Jürgen

2014-11-01

Osmium tetroxide (OsO4) staining, commonly used to enhance scattering contrast in electron microscopy of biologic tissue and polymer blends, has been adopted for studies of graphite anodes in lithium-ion batteries. OsO4 shows a coordinated reaction with components of the solid electrolyte interphase (SEI) and lithium dendrites, thereby increasing material contrast for scanning electron microscopy investigations. Utilizing the high affinity of lithium metal to react with osmium tetroxide it was possible to localize even small lithium deposits on graphite electrodes. In spite of their reaction with the OsO4 fume, the lithium dendrite morphology remains almost untouched by the staining procedure, offering information on the dendrite growth process. Correlating the quantity of osmium detected with the amount of residual ("dead") lithium of a discharged electrode, it was possible to obtain a practical measure for lithium plating and stripping efficiencies. EDX mappings allowed for a localization of electrochemically stripped lithium dendrites by their residual stained SEI shells. Cross sections, prepared by focused ion beam (FIB) of cycled graphite electrodes treated with OsO4, revealed important information about deposition and distribution of metallic lithium and the electrolyte reduction layer across the electrode.

Skin inspired fractal strain sensors using a copper nanowire and graphite microflake hybrid conductive network.

PubMed

Jason, Naveen N; Wang, Stephen J; Bhanushali, Sushrut; Cheng, Wenlong

2016-09-22

This work demonstrates a facile "paint-on" approach to fabricate highly stretchable and highly sensitive strain sensors by combining one-dimensional copper nanowire networks with two-dimensional graphite microflakes. This paint-on approach allows for the fabrication of electronic skin (e-skin) patches which can directly replicate with high fidelity the human skin surface they are on, regardless of the topological complexity. This leads to high accuracy for detecting biometric signals for applications in personalised wearable sensors. The copper nanowires contribute to high stretchability and the graphite flakes offer high sensitivity, and their hybrid coating offers the advantages of both. To understand the topological effects on the sensing performance, we utilized fractal shaped elastomeric substrates and systematically compared their stretchability and sensitivity. We could achieve a high stretchability of up to 600% and a maximum gauge factor of 3000. Our simple yet efficient paint-on approach enabled facile fine-tuning of sensitivity/stretchability simply by adjusting ratios of 1D vs. 2D materials in the hybrid coating, and the topological structural designs. This capability leads to a wide range of biomedical sensors demonstrated here, including pulse sensors, prosthetic hands, and a wireless ankle motion sensor.

Alkaline electrochemical advanced oxidation process for chromium oxidation at graphitized multi-walled carbon nanotubes.

PubMed

Xue, Yudong; Zheng, Shili; Sun, Zhi; Zhang, Yi; Jin, Wei

2017-09-01

Alkaline electrochemical advanced oxidation processes for chromium oxidation and Cr-contaminated waste disposal were reported in this study. The highly graphitized multi-walled carbon nanotubes g-MWCNTs modified electrode was prepared for the in-situ electrochemical generation of HO 2 - . RRDE test results illustrated that g-MWCNTs exhibited much higher two-electron oxygen reduction activity than other nanocarbon materials with peak current density of 1.24 mA cm -2 , %HO 2 - of 77.0% and onset potential of -0.15 V (vs. Hg/HgO). It was originated from the highly graphitized structure and good electrical conductivity as illustrated from the Raman, XRD and EIS characterizations, respectively. Large amount of reactive oxygen species (HO 2 - and ·OH) were in-situ electro-generated from the two-electron oxygen reduction and chromium-induced alkaline electro-Fenton-like reaction. The oxidation of Cr(III) was efficiently achieved within 90 min and the conversion ratio maintained more than 95% of the original value after stability test, offering an efficient and green approach for the utilization of Cr-containing wastes. Copyright © 2017 Elsevier Ltd. All rights reserved.

Thermally stable laminating resins

NASA Technical Reports Server (NTRS)

Jones, R. J.; Vaughan, R. W.; Burns, E. A.

1972-01-01

Improved thermally stable laminating resins were developed based on the addition-type pyrolytic polymerization. Detailed monomer and polymer synthesis and characterization studies identified formulations which facilitate press molding processing and autoclave fabrication of glass and graphite fiber reinforced composites. A specific resin formulation, termed P10P was utilized to prepare a Courtaulds HMS reinforced simulated airfoil demonstration part by an autoclave molding process.

Carbon chemistry: The high temperature syntheses and applications of nanotubes andsp-hybridized compounds

NASA Astrophysics Data System (ADS)

Mitchell, Daniel Robert

A brief introduction to carbon chemistry is given with an emphasis on the use high-temperature reactions that use carbon vapor, generated from graphite, to synthesize nano-structured materials. Laser and electric are ablation of graphite was utilized to create a variety of high carbon content materials ranging from discrete acetylenic molecules to extremely large multi-wall nanotubes. A new synthesis for large carbon nanotubes, containing 1--5 atom percent nitrogen bound into the graphite lattice, was realized by the reaction of carbon vapor, nickel/yttrium catalyst and cyanogen gas. These carbon "megatubes" were then employed as a substrate to tether a wide variety of molecules both inorganic and organic. The megatubes, in their native and derivatized states, were then assembled into simple circuits to explore their electronic transport properties. Direct fluorination was used to post-treat the surface of the multi-wall carbon nanotubes in order to alter the inherent physical and chemical properties of the tubes, as well as to serve as another route to functionalize their surfaces. Fluorine sites on the walls of the tube were allowed to react with Grignard reagents to produce nantoubes with the chosen alkyl chemically bonded to the surface. Products were characterized with techniques similar to unfluorinated tubules. Using similar carbon vaporization techniques, sp-hybridized carbon chain compounds were synthesized. Using a one-step method dicyanopolyynes were synthesized and characterized with nuclear magnetic resonance and mass spectroscopy, containing up to 8 acetylenic repeat units. A two-step method was also utilized to create polyynes terminated with trifluoromethyl or nitrile radicals generated in a capacitively coupled radio frequency glow plasma discharge. A partial characterization of these products was accomplished with nuclear magnetic resonance, mass, and infrared spectroscopy techniques.

Holographic fabrication of gratings in metal substrates

NASA Technical Reports Server (NTRS)

Fletcher, R. M.; Wagner, D. K.; Ballantyne, J. M.

1982-01-01

A program for investigating the grain enlargement resulting from the laser recrystallization of a thin gallium arsenide film on a patterned substrate, a technique known as graphoepitaxy was evaluated. More specifically, the effects of recrystallizing an uncapped gallium arsenide film using a continuous wave neodymium YAG laser operating at 1.06 microns were studied. In an effort to minimize arsenic loss from the film, the specimens were held in an arsine atmosphere during recrystallization. Two methods for fabricating patterned substrates were developed, one using reactive ion etching of a molybdenum film on both sapphire and silicon substates and another by preferential wet etching of a silicon substrate onto which a film of molybdenum was subsequently deposited.

Copper phthalocyanine films deposited by liquid-liquid interface recrystallization technique (LLIRCT).

PubMed

Patil, K R; Sathaye, S D; Hawaldar, R; Sathe, B R; Mandale, A B; Mitra, A

2007-11-15

The simple recrystallization process is innovatively used to obtain the nanoparticles of copper phthalocyanine by a simple method. Liquid-liquid interface recrystallization technique (LLIRCT) has been employed successfully to produce small sized copper phthalocyanine nanoparticles with diameter between 3-5 nm. The TEM-SAED studies revealed the formation of 3-5 nm sized with beta-phase dominated mixture of alpha and beta copper phthalocyanine nanoparticles. The XRD, SEM, and the UV-vis studies were further carried out to confirm the formation of copper phthalocyanine thin films. The cyclic voltametry (CV) studies conclude that redox reaction is totally reversible one electron transfer process. The process is attributed to Cu(II)/Cu(I) redox reaction.

Plasticity-mediated collapse and recrystallization in hollow copper nanowires: a molecular dynamics simulation

PubMed Central

Raychaudhuri, Arup Kumar; Saha-Dasgupta, Tanusri

2016-01-01

Summary We study the thermal stability of hollow copper nanowires using molecular dynamics simulation. We find that the plasticity-mediated structural evolution leads to transformation of the initial hollow structure to a solid wire. The process involves three distinct stages, namely, collapse, recrystallization and slow recovery. We calculate the time scales associated with different stages of the evolution process. Our findings suggest a plasticity-mediated mechanism of collapse and recrystallization. This contradicts the prevailing notion of diffusion driven transport of vacancies from the interior to outer surface being responsible for collapse, which would involve much longer time scales as compared to the plasticity-based mechanism. PMID:26977380

Resin/graphite fiber composites

NASA Technical Reports Server (NTRS)

Cavano, P. J.

1974-01-01

Processing techniques were developed for the fabrication of both polyphenylquinoxaline and polyimide composites by the in situ polymerization of monomeric reactants directly on the graphite reinforcing fibers, rather than using previously prepared prepolymer varnishes. Void-free polyphenylquinoxaline composites were fabricated and evaluated for room and elevated flexure and shear properties. The technology of the polyimide system was advanced to the point where the material is ready for commercial exploitation. A reproducible processing cycle free of operator judgment factors was developed for fabrication of void-free composites exhibiting excellent mechanical properties and a long time isothermal life in the range of 288 C to 316 C. The effects of monomer reactant stoichiometry and process modification on resin flow were investigated. Demonstration of the utility and quality of this polyimide system was provided through the successful fabrication and evaluation of four complex high tip speed fan blades.

Self-Assembled Polystyrene Beads for Templated Covalent Functionalization of Graphitic Substrates Using Diazonium Chemistry.

PubMed

Van Gorp, Hans; Walke, Peter; Bragança, Ana M; Greenwood, John; Ivasenko, Oleksandr; Hirsch, Brandon E; De Feyter, Steven

2018-04-11

A network of self-assembled polystyrene beads was employed as a lithographic mask during covalent functionalization reactions on graphitic surfaces to create nanocorrals for confined molecular self-assembly studies. The beads were initially assembled into hexagonal arrays at the air-liquid interface and then transferred to the substrate surface. Subsequent electrochemical grafting reactions involving aryl diazonium molecules created covalently bound molecular units that were localized in the void space between the nanospheres. Removal of the bead template exposed hexagonally arranged circular nanocorrals separated by regions of chemisorbed molecules. Small molecule self-assembly was then investigated inside the resultant nanocorrals using scanning tunneling microscopy to highlight localized confinement effects. Overall, this work illustrates the utility of self-assembly principles to transcend length scale gaps in the development of hierarchically patterned molecular materials.

Morphology and Structural Characterization of Carbon Nanowalls Grown via VHF-PECVD

NASA Astrophysics Data System (ADS)

Akmal Hasanudin, M.; Wahab, Y.; Ismail, A. K.; Zahid Jamal, Z. A.

2018-03-01

A 150 MHz very high frequency plasma enhanced chemical vapor deposition (150 MHz VHF-PECVD) system was utilized to fabricate two-dimensional carbon nanostructure from the mixture of methane and hydrogen. Morphology and structural properties of the grown nanostructure were investigated by FESEM imaging and Raman spectroscopy. Carbon nanowalls (CNW) with dense and wavy-like structure were successfully synthesized. The wavy-like morphology of CNW was found to be more distinct during growth at small electrode spacing and denser with increasing deposition time due to better flux of hydrocarbon radicals to the substrate and higher rate of reaction, respectively. Typical characteristics of CNW were observed from strong D band, narrow bandwidth of G band and single broad peak of 2D band of Raman spectra indicating the presence of disordered nanocrystalline graphite structure with high degree of graphitization.

Mesoporous Phosphorus-Doped g-C3N4 Nanostructured Flowers with Superior Photocatalytic Hydrogen Evolution Performance.

PubMed

Zhu, Yun-Pei; Ren, Tie-Zhen; Yuan, Zhong-Yong

2015-08-05

Graphitic carbon nitride (g-C3N4) has been deemed a promising heterogeneous metal-free catalyst for a wide range of applications, such as solar energy utilization toward water splitting, and its photocatalytic performance is reasonably adjustable through tailoring its texture and its electronic and optical properties. Here phosphorus-doped graphitic carbon nitride nanostructured flowers of in-plane mesopores are synthesized by a co-condensation method in the absence of any templates. The interesting structures, together with the phosphorus doping, can promote light trapping, mass transfer, and charge separation, enabling it to perform as a more impressive catalyst than its pristine carbon nitride counterpart for catalytic hydrogen evolution under visible light irradiation. The catalyst has low cost, is environmentally friendly, and represents a potential candidate in photoelectrochemistry.

Analysis of Semiconductor Structures by Nuclear and Electrical Techniques.

DTIC Science & Technology

temperatures well below the Si-Al eutectic (577C), fine grained polycrystalline Si in contact with Al films recrystallizes in the Al matrix. The... recrystallization can be deferred or suppressed by placing a buffer layer of V or Ti between the Al film and poly Si. (2) When annealing Pt films deposited on Si

Manufacturing process to reduce large grain growth in zirconium alloys

DOEpatents

Rosecrans, Peter M.

1987-01-01

A method of treating cold-worked zirconium alloys to reduce large grain gth during thermal treatment at temperatures above the recrystallization temperature of the alloy comprising heating the cold-worked alloy between about 1300.degree.-1350.degree. F. for 1 to 3 hours prior to treatment above its recrystallization temperature.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules

NASA Astrophysics Data System (ADS)

Mitchell, Daniel E.; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I.

2015-10-01

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used ‘splat’ methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics.

Plasma deposited stability enhancement coating for amorphous ketoprofen.

PubMed

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

2011-05-01

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

Constitutive relations for determining the critical conditions for dynamic recrystallization behavior

NASA Astrophysics Data System (ADS)

Choe, J. I.

2016-04-01

A series mathematical model has been developed for the prediction of flow stress and microstructure evolution during the hot deformation of metals such as copper or austenitic steels with low stacking fault energies, involving features of both diffusional flow and dislocation motion. As the strain rate increases, multiple peaks on the stress-strain curve decrease. At a high strain rate, the stress rises to a single peak, while dynamic recrystallization causes an oscillatory behavior. At a low strain rate (when there is sufficient time for the recrystallizing grains to grow before they become saturated with high dislocation density with an increase in strain rate), the difference in stored stress between recrystallizing and old grains diminishes, resulting in reduced driving force for grain growth and rendering smaller grains in the alloy. The final average grain size at the steady stage (large strain) increases with a decrease in the strain rate. During large strain deformation, grain size reduction accompanying dislocation creep might be balanced by the grain growth at the border delimiting the ranges of realization (field boundary) of the dislocation-creep and diffusion-creep mechanisms.

Effect of strain and deformation route on grain boundary characteristics and recrystallization behavior of aluminum

NASA Astrophysics Data System (ADS)

Sakai, Tetsuo; Utsunomiya, Hiroshi; Takahashi, Yasuo

2014-08-01

The effect of strain and deformation route on the recrystallization behavior of aluminum sheets has been investigated using well lubricated cold rolling and continuous equal channel angular extrusion. Three different deformation routes in plane strain corresponding to (1) simple shear, (2) compression, and (3) the combination of simple shear and compression were performed on 1100 aluminum sheet. Fixed amounts of the equivalent strain of 1.28 and 1.06 were accumulated in each route. In case of the combined deformation route, the ratio of shear strain to the total equivalent strain was varied. The recrystallized grain size was finer if the combined deformation route was employed instead of the monotonic route under the same amount of equivalent strain at either strain level. The density of high angle grain boundaries that act as nucleation sites for recrystallization was higher in materials deformed by the combined route. The orientation imaging micrographs revealed that the change in deformation route is effective for introducing a larger number of new high angle grain boundaries with relatively low misorientation angle.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules

PubMed Central

Mitchell, Daniel E.; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I.

2015-01-01

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used ‘splat’ methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics. PMID:26499135

Devitrification and recrystallization of nanoparticle-containing glycerol and PEG-600 solutions.

PubMed

Lv, Fukou; Liu, Baolin; Li, Weijie; Jaganathan, Ganesh K

2014-02-01

Nanoparticles in solution offer unique electrical, mechanical and thermal properties due to their physical presence and interaction with the state of dispersion. This work is aimed to study the effects of hydroxyapatite (HA) nanoparticles on the devitrification and recrystallization events of two important cryoprotective solutions used in cell and tissue preservation namely glycerol (60%w/w) and PEG-600 (50%w/w). HA nanoparticles (20, 40 or 60 nm) were incorporated into solutions at the content of 0.1% or 0.5%(w/w), and were studied by differential scanning calorimeter (DSC) and cryomicroscopy. The presence of nanoparticles does not change the glass transition temperatures and melting temperatures of quenched solutions, but significantly affects the behavior of devitrification and recrystallization upon warming. Cryomicroscopic investigation showed the complex interactions among solution type, nanoparticle size and nanoparticle content, which apparently influence ice crystal growth or recrystallization in the quenched dispersions. These findings have significant implications for biomaterial cryopreservation, cryosurgery, and food manufacturing. The complexity of ice crystal growth kinetics in nanoparticle-containing dispersions remains to be poorly understood at the moment. Copyright © 2013 Elsevier Inc. All rights reserved.

Gold Nanoparticle Aggregation as a Probe of Antifreeze (Glyco) Protein-Inspired Ice Recrystallization Inhibition and Identification of New IRI Active Macromolecules.

PubMed

Mitchell, Daniel E; Congdon, Thomas; Rodger, Alison; Gibson, Matthew I

2015-10-26

Antifreeze (glyco)proteins are found in polar fish species and act to slow the rate of growth of ice crystals; a property known as ice recrystallization inhibition. The ability to slow ice growth is of huge technological importance especially in the cryopreservation of donor cells and tissue, but native antifreeze proteins are often not suitable, nor easily available. Therefore, the search for new materials that mimic this function is important, but currently limited by the low-throughout assays associated with the antifreeze properties. Here 30 nm gold nanoparticles are demonstrated to be useful colorimetric probes for ice recrystallization inhibition, giving a visible optical response and is compatible with 96 well plates for high-throughout studies. This method is faster, requires less infrastructure, and has easier interpretation than the currently used 'splat' methods. Using this method, a series of serum proteins were identified to have weak, but specific ice recrystallization inhibition activity, which was removed upon denaturation. It is hoped that high-throughput tools such as this will accelerate the discovery of new antifreeze mimics.

A Continuum Model for the Effect of Dynamic Recrystallization on the Stress⁻Strain Response.

PubMed

Kooiker, H; Perdahcıoğlu, E S; van den Boogaard, A H

2018-05-22

Austenitic Stainless Steels and High-Strength Low-Alloy (HSLA) steels show significant dynamic recovery and dynamic recrystallization (DRX) during hot forming. In order to design optimal and safe hot-formed products, a good understanding and constitutive description of the material behavior is vital. A new continuum model is presented and validated on a wide range of deformation conditions including high strain rate deformation. The model is presented in rate form to allow for the prediction of material behavior in transient process conditions. The proposed model is capable of accurately describing the stress⁻strain behavior of AISI 316LN in hot forming conditions, also the high strain rate DRX-induced softening observed during hot torsion of HSLA is accurately predicted. It is shown that the increase in recrystallization rate at high strain rates observed in experiments can be captured by including the elastic energy due to the dynamic stress in the driving pressure for recrystallization. Furthermore, the predicted resulting grain sizes follow the power-law dependence with steady state stress that is often reported in literature and the evolution during hot deformation shows the expected trend.

Tensile Properties of Molybdenum and Tungsten from 2500 to 3700 F

NASA Technical Reports Server (NTRS)

Hall, Robert W.; Sikora, Paul F.

1959-01-01

Specimens of commercially pure sintered tungsten, arc-cast unalloyed molybdenum, and two arc-cast molybdenum-base alloys (one with 0.5 percent titanium, the other with 0.46 percent titanium and 0.07 percent zirconium) were fabricated from 1/2-inch-diameter rolled or swaged bars. All specimens were evaluated in short-time tensile tests in the as-received condition, and all except the molybdenum-titanium-zirconium alloy were tested after a 30-minute recrystallization anneal at 3800 F in a vacuum of approximately 0.1 micron. Results showed that the tungsten was considerably stronger than either the arc-cast unalloyed molybdenum or the molybdenum-base alloys over the 2500 to 3700 F temperature range. Recrystallization of swaged tungsten at 3800 F considerably reduced its tensile strength at 2500 F. However, above 3100 F, the as-swaged tungsten specimens recrystallized during testing, and had about the same strength as when recrystallized at 3800 F before evaluation. The ductility of molybdenum-base materials was very high at all test temperatures; the ductility of tungsten decreased sharply above about 3120 F.

Subgrain Rotation Behavior in Sn3.0Ag0.5Cu-Sn37Pb Solder Joints During Thermal Shock

NASA Astrophysics Data System (ADS)

Han, Jing; Tan, Shihai; Guo, Fu

2018-01-01

Ball grid array (BGA) samples were soldered on a printed circuit board with Sn37Pb solder paste to investigate the recrystallization induced by subgrain rotation during thermal shock. The composition of the solder balls was Sn3.0Ag0.5Cu-Sn37Pb, which comprised mixed solder joints. The BGA component was cross-sectioned before thermal shock. The microstructure and grain orientations were obtained by a scanning electron microscope equipped with an electron back-scattered diffraction system. Two mixed solder joints at corners of the BGA component were selected as the subjects. The results showed that recrystallization occurred at the corner of the solder joints after 200 thermal shock cycles. The recrystallized subgrains had various new grain orientations. The newly generated grain orientations were closely related to the initial grain orientations, which indicated that different subgrain rotation behaviors could occur in one mixed solder joint with the same initial grain orientation. When the misorientation angles were very small, the rotation axes were about Sn [100], [010] and [001], as shown by analyzing the misorientation angles and subgrain rotation axes, while the subgrain rotation behavior with large misorientation angles in the solder joints was much more complicated. As Pb was contained in the solder joints and the stress was concentrated on the corner of the mixed solder joints, concaves and cracks were formed. When the adjacent recrystallized subgrains were separated, and the process of the continuous recrystallization was limited.

Content of toxic and essential metals in recrystallized and washed table salt in Shiraz, Iran

PubMed Central

2014-01-01

Background Table salt is the most commonly used food additive. Since most of the salt consumed in Iran comes from mines, contamination with heavy metals is a health concern. The commonest salt purification method in Iran is washing with water. But recently, some industries have turned to recrystallization method. The present study aimed to determine the level of essential and non-essential heavy metals in the table salt refined with recrystallization and washing methods. Methods Thirty eight pre-packed salt samples were directly collected from retail market in Shiraz (22 samples refined with recrystallization method and 16 with washing method). The level of lead, cadmium, copper, zinc, nickel and cobalt was determined using Voltammetric method. Daily intakes of lead and cadmium as well as their weekly intakes were calculated. Results The levels of lead, cadmium, copper, zinc, nickel and cobalt in recrystallized samples were 0. 30 ± 0.26, 0.02 ± 0.02, 0.11 ± 0.06, 0.34 ± 0.22, 0.15 ± 0.19 and 0.008 ± 0.007 μg/g, respectively, and also 0.37 ± 0.27, 0.017 ± 0.021, 0.19 ± 0.18, 0.37 ± 0.20, 0.13 ± 0.23 and 0.037 ± 0.06 μg/g in washed salt samples. The calculated weekly intake of lead and cadmium was 0.216 and 0.014 μg/kg, respectively for the recrystallized and 0.2653 and 0.0119 μg/kg for the washed salts. Conclusion All values for toxic metals were lower than the permitted maximum for human consumption as prescribed by Codex and Institute of Standards and Industrial Research of Iran. Only 0.8652-1.0612% of lead and 0.17-0.2% of cadmium PTWIs are received via salt consumption weekly. PMID:24398299

Hydration index--a better parameter for explaining small molecule hydration in inhibition of ice recrystallization.

PubMed

Tam, Roger Y; Ferreira, Sandra S; Czechura, Pawel; Chaytor, Jennifer L; Ben, Robert N

2008-12-24

Several simple mono- and disaccharides have been assessed for their ability to inhibit ice recrystallization. Two carbohydrates were found to be effective recrystallization inhibitors. D-galactose (1) was the best monosaccharide and D-melibiose (5) was the most active disaccharide. The ability of each carbohydrate to inhibit ice growth was correlated to its respective hydration number reported in the literature. A hydration number reflects the number of tightly bound water molecules to the carbohydrate and is a function of carbohydrate stereochemistry. It was discovered that using the absolute hydration number of a carbohydrate does not allow one to accurately predict its ability to inhibit ice recrystallization. Consequently, we have defined a hydration index in which the hydration number is divided by the molar volume of the carbohydrate. This new parameter not only takes into account the number of water molecules tightly bound to a carbohydrate but also the size or volume of a particular solute and ultimately the concentration of hydrated water molecules. The hydration index of both mono- and disaccharides correlates well with experimentally measured RI activity. C-Linked derivatives of the monosaccharides appear to have RI activity comparable to that of their O-linked saccharides but a more thorough investigation is required. The relationship between carbohydrate concentration and RI activity was shown to be noncolligative and a 0.022 M solution of D-galactose (1) and C-linked galactose derivative (10) inhibited recrystallization as well as a 3% DMSO solution. The carbohydrates examined in this study did not possess any thermal hysteresis activity (selective depression of freezing point relative to melting point) or dynamic ice shaping. As such, we propose that they are inhibiting recrystallization at the interface between bulk water and the quasi liquid layer (a semiordered interface between ice and bulk water) by disrupting the preordering of water.

Crystallographic control and texture inheritance during mylonitization of coarse grained quartz veins

NASA Astrophysics Data System (ADS)

Ceccato, Alberto; Pennacchioni, Giorgio; Menegon, Luca; Bestmann, Michel

2017-10-01

Quartz veins within Rieserferner pluton underwent deformation during post-magmatic cooling at temperature around 450 °C. Different crystallographic orientations of cm-sized quartz vein crystals conditioned the evolution of microstructures and crystallographic preferred orientations (CPO) during vein-parallel simple shear up to high shear strains (γ ≈ 10). For γ < 2, crystals stretched to ribbons of variable aspect ratios. The highest aspect ratios resulted from {m} glide in ribbons with c-axis sub-parallel to the shear zone vorticity Y-axis. Ribbons with c-axis orthogonal to Y (XZ-type ribbons) were stronger and hardened more quickly: they show lower aspect ratios and fine (grain size 10-20 μm) recrystallization along sets of microshear zones (μSZs) exploiting crystallographic planes. Distortion of XZ-type ribbons and recrystallization preferentially exploited the slip systems with misorientation axis close to Y. New grains of μSZs initiated by subgrain rotation recrystallization (SGR) and thereupon achieved high angle misorientations by a concurrent process of heterogeneous rigid grain rotation around Y associated with the confined shear within the μSZ. Dauphiné twinning occurred pervasively, but did not play a dominant role on μSZ nucleation. Recrystallization became widespread at γ > 2 and pervasive at γ ≈ 10. Ultramylonitic quartz veins are fine grained ( 10 μm, similar to new grains of μSZ) and show a CPO banding resulting in a bulk c-axis CPO with a Y-maximum, as part of a single girdle about orthogonal to the foliation, and orientations at the pole figure periphery at moderate to high angle to the foliation. This bulk CPO derives from steady-state SGR associated with preferential activity, in the different CPO bands, of slip systems generating subgrain boundaries with misorientation axes close to Y. The CPO of individual recrystallized bands is largely inherited from the original crystallographic orientation of the ribbons (and therefore vein crystals) from which they derived. High strain and pervasive recrystallization were not enough to reset the initial crystallographic heterogeneity and this CPO memory is explained by the dominance of SGR. This contrast with experimental observation of a rapid erasure of a pristine CPO by cannibalism from grains with the most favourably oriented slip system under dominant grain boundary migration recrystallization.

Correlated NanoSIMS, TEM, and XANES Studies of Presolar Grains

NASA Astrophysics Data System (ADS)

Groopman, Evan Edward

The objective of this thesis is to describe the correlated study of individual presolar grains via Nano-scale Secondary Ion Mass Spectrometry (NanoSIMS), Transmission Electron Microscopy (TEM), and Scanning Transmission X-ray Microscopy (STXM) utilizing X-ray Absorption Near Edge Structure (XANES), with a focus on connecting these correlated laboratory studies to astrophysical phenomena. The correlated isotopic, chemical, and microstructural studies of individual presolar grains provide the most detailed description of their formation environments, and help to inform astrophysical models and observations of stellar objects. As a part of this thesis I have developed and improved upon laboratory techniques for micromanipulating presolar grains and embedding them in resin for ultramicrotomy after NanoSIMS analyses and prior to TEM characterization. The new methods have yielded a 100% success rate and allow for the specific correlation of microstructural and isotopic properties of individual grains. Knowing these properties allows for inferences to be made regarding the condensation sequences and the origins of the stellar material that condensed to form these grains. NanoSIMS studies of ultramicrotomed sections of presolar graphite grains have revealed complex isotopic heterogeneities that appear to be primary products of the grains' formation environments and not secondary processing during the grains' lifetimes. Correlated excesses in 15N and 18O were identified as being carried by TiC subgrains within presolar graphite grains from supernovae (SNe). These spatially-correlated isotopic anomalies pinpoint the origin of the material that formed these grains: the inner He/C zone. Complex microstructures and isotopic heterogeneities also provide evidence for mixing in globular SN ejecta, which is corroborated by models and telescopic observations. In addition to these significant isotopic discoveries, I have also observed the first reported nanocrystalline core surrounded by turbostratic graphite within a low-density SN graphite grain. Nanocrystalline cores consisting of randomly-oriented 2-4 nm sheets of graphene and surrounded by concentric shells of graphite have been observed in high-density presolar graphite grains from Asymptotic Giant Branch stars, whose grains are typically microstructurally distinct from SN graphite grains. These vastly different stellar environments briefly formed similar nanocrystalline structures before diverging in the structure of their mantling graphite to be typical of AGB and SN grains. While relatively few correlated NanoSIMS and TEM studies have been performed previously, which this research thesis aims to expand, my collaborators and I also endeavored to add a third correlated technique, STXM/XANES, which had previously not been applied to presolar grains. XANES allows for the investigation of molecular bonds, which we used to help infer physical and chemical properties of stellar ejecta. I investigated the C K-edge and Ti L-edge of molecular bonds in both presolar graphite grains and their TiC subgrains. The presolar graphite grains, while overwhelmingly composed of aromatic C molecules, host a wide variety of minor organic molecules. Considering the large isotopic anomalies in the grains, these minor components are not likely due to contamination. I also investigated the valence state of Ti in Ti-rich subgrains and plan to work towards illuminating the effect that V in solid solution has upon the TiC bonds.

Lightweight Towed Howitzer Demonstrator. Phase 1 and Partial Phase 2. Volume A. Overview.

DTIC Science & Technology

1987-04-01

Reliability Floyd Manson............................... Test Plans Errol Quick................................. Systems Engrnq Coordi nati on Bob Schmidt ...FMC Structur*1 Verification o Beam stress calculations on the supporting trails which allow 70kpsi in a quasi-isotropic lay up of graphite epoxy...addressed utilizing a damage tolerant design criteria. o Strength calculations are questionable because of the dry room temperature values used. The

Solid Lubricants for Space Structures

DTIC Science & Technology

1993-04-17

will utilize mechanically interlocked hardware (caged bearings or bearings for ultra precision gimbals pointing mechanisms) controlled through precision...structure unless the lubricant were of low vapor pressure and/or suitably sealed to I prevent molecular effusion . While temperatures within spacecraft or...incorporation in the continuous cast system. The die made of graphite, consists of a plurality of openings or holes located in the die and positioned (unlined

Sustainable pathway to furanics from biomass via ...

EPA Pesticide Factsheets

An organic sulfonated graphitic carbon nitride is synthesized and its application has been demonstrated inthe conversion of carbohydrates into furanics and related value-added products. The most importantfeature of the material is the stability and acidity, which could be utilized at elevated temperatures forcleaving carbohydrates and converting them into biologically important scaffolds and platform chemicals. Prepared for submission to the Royal Society of Chemistry (RSC) Journal, Green Chemistry.

An electron microscopy examination of primary recrystallization in TD-nickel.

NASA Technical Reports Server (NTRS)

Petrovic, J. J.; Ebert, L. J.

1972-01-01

Primary recrystallization in TD-nickel 1 in. bar has previously been regarded as the process by which the initial fine grain structure is converted to a coarse grain size (increases in grain size by 500 times) under suitable deformation and annealing conditions. This process is dependent on deformation mode. While it occurs readily after rolling transverse to the bar axis and annealing (800 C), it is completely inhibited by longitudinal rolling and swaging deformations, even for very high (1320 C) annealing temperatures. A transmission electron microscopy examination of deformation and annealing substructures indicates that primary recrystallization in TD-nickel 1 in. bar actually occurs on the sub-light optical level, to produce a grain structure similar in size to the initial fine grained state.

Facially Amphipathic Glycopolymers Inhibit Ice Recrystallization.

PubMed

Graham, Ben; Fayter, Alice E R; Houston, Judith E; Evans, Rachel C; Gibson, Matthew I

2018-05-02

Antifreeze glycoproteins (AFGPs) from polar fish are the most potent ice recrystallization (growth) inhibitors known, and synthetic mimics are required for low-temperature applications such as cell cryopreservation. Here we introduce facially amphipathic glycopolymers that mimic the three-dimensional structure of AFGPs. Glycopolymers featuring segregated hydrophilic and hydrophobic faces were prepared by ring-opening metathesis polymerization, and their rigid conformation was confirmed by small-angle neutron scattering. Ice recrystallization inhibition (IRI) activity was reduced when a hydrophilic oxo-ether was installed on the glycan-opposing face, but significant activity was restored by incorporating a hydrophobic dimethylfulvene residue. This biomimetic strategy demonstrates that segregated domains of distinct hydrophilicity/hydrophobicity are a crucial motif to introduce IRI activity, which increases our understanding of the complex ice crystal inhibition processes.

Graphite fiber textile preform/copper matrix composites

NASA Technical Reports Server (NTRS)

Gilatovs, G. J.; Lee, Bruce; Bass, Lowell

1995-01-01

Graphite fiber reinforced/copper matrix composites have sufficiently high thermal conduction to make them candidate materials for critical heat transmitting and rejection components. The term textile composites arises because the preform is braided from fiber tows, conferring three-dimensional reinforcement and near net shape. The principal issues investigated in the past two years have centered on developing methods to characterize the preform and fabricated composite and on braidability. It is necessary to have an analytic structural description for both processing and final property modeling. The structure of the true 3-D braids used is complex and has required considerable effort to model. A structural mapping has been developed as a foundation for analytic models for thermal conduction and mechanical properties. The conductivity has contributions both from the copper and the reinforcement. The latter is accomplished by graphitization of the fibers, the higher the amount of graphitization the greater the conduction. This is accompanied by an increase in the fiber modulus, which is desirable from a stiffness point of view but decreases the braidability; the highest conductivity fibers are simply too brittle to be braided. Considerable effort has been expended on determining the optimal braidability--conductivity region. While a number of preforms have been fabricated, one other complication intervenes; graphite and copper are immiscible, resulting in a poor mechanical bond and difficulties in infiltration by molten copper. The approach taken is to utilize a proprietary fiber coating process developed by TRA, of Salt Lake City, Utah, which forms an itermediary bond. A number of preforms have been fabricated from a variety of fiber types and two sets of these have been infiltrated with OFHC copper, one with the TRA coating and one without. Mechanical tests have been performed using a small-scale specimen method and show the coated specimens to have superior mechanical properties. Final batches of preforms, including a finned, near net shape tube, are being fabricated and will be infiltrated before summer.

Method for producing dustless graphite spheres from waste graphite fines

DOEpatents

Pappano, Peter J [Oak Ridge, TN; Rogers, Michael R [Clinton, TN

2012-05-08

A method for producing graphite spheres from graphite fines by charging a quantity of spherical media into a rotatable cylindrical overcoater, charging a quantity of graphite fines into the overcoater thereby forming a first mixture of spherical media and graphite fines, rotating the overcoater at a speed such that the first mixture climbs the wall of the overcoater before rolling back down to the bottom thereby forming a second mixture of spherical media, graphite fines, and graphite spheres, removing the second mixture from the overcoater, sieving the second mixture to separate graphite spheres, charging the first mixture back into the overcoater, charging an additional quantity of graphite fines into the overcoater, adjusting processing parameters like overcoater dimensions, graphite fines charge, overcoater rotation speed, overcoater angle of rotation, and overcoater time of rotation, before repeating the steps until graphite fines are converted to graphite spheres.

Electrochemical Control of Peptide Self-Organization on Atomically Flat Solid Surfaces: A Case Study with Graphite.

PubMed

Seki, Takakazu; So, Christopher R; Page, Tamon R; Starkebaum, David; Hayamizu, Yuhei; Sarikaya, Mehmet

2018-02-06

The nanoscale self-organization of biomolecules, such as proteins and peptides, on solid surfaces under controlled conditions is an important issue in establishing functional bio/solid soft interfaces for bioassays, biosensors, and biofuel cells. Electrostatic interaction between proteins and surfaces is one of the most essential parameters in the adsorption and self-assembly of proteins on solid surfaces. Although the adsorption of proteins has been studied with respect to the electrochemical surface potential, the self-assembly of proteins or peptides forming well-organized nanostructures templated by lattice structure of the solid surfaces has not been studied in the relation to the surface potential. In this work, we utilize graphite-binding peptides (GrBPs) selected by the phage display method to investigate the relationship between the electrochemical potential of the highly ordered pyrolytic graphite (HOPG) and peptide self-organization forming long-range-ordered structures. Under modulated electrical bias, graphite-binding peptides form various ordered structures, such as well-ordered nanowires, dendritic structures, wavy wires, amorphous (disordered) structures, and islands. A systematic investigation of the correlation between peptide sequence and self-organizational characteristics reveals that the presence of the bias-sensitive amino acid modules in the peptide sequence has a significant effect on not only surface coverage but also on the morphological features of self-assembled structures. Our results show a new method to control peptide self-assembly by means of applied electrochemical bias as well as peptide design-rules for the construction of functional soft bio/solid interfaces that could be integrated in a wide range of practical implementations.

Surface modification of amine-functionalised graphite for preparation of cobalt hexacyanoferrate (CoHCF)-modified electrode: an amperometric sensor for determination of butylated hydroxyanisole (BHA).

PubMed

Prabakar, S J Richard; Narayanan, S Sriman

2006-12-01

A cobalt hexacyanoferrate (CoHCF)-modified graphite paraffin wax composite electrode was prepared by a new approach. An amine-functionalised graphite powder was used for the fabrication of the electrode. A functionalised graphite paraffin wax composite electrode was prepared and the surface of the electrode was modified with a thin film of CoHCF. Various parameters that influence the electrochemical behaviour of the modified electrode were studied by varying the background electrolytes, scan rates and pH. The modified electrode showed good electrocatalytic activity towards the oxidation of butylated hydroxyanisole (BHA) under optimal conditions and showed a linear response over the range from 7.9 x 10(-7) to 1.9 x 10(-4) M of BHA with a correlation coefficient of 0.9988. The limit of detection was 1.9 x 10(-7) M. Electrocatalytic oxidation of BHA was effective at the modified electrode at a significantly reduced potential and at a broader pH range. The utility of the modified electrode as an amperometric sensor for the determination of BHA in flow systems was evaluated by carrying out hydrodynamic and chronoamperometric experiments. The modified electrode showed very good stability and a longer shelf life. The modified electrode was applied for the determination of BHA in spiked samples of chewing gum and edible sunflower oil. The advantage of this method is the ease of electrode fabrication, good stability, longer shelf life, low cost and its diverse application for BHA determination.

Multilayer Approach for Advanced Hybrid Lithium Battery.

PubMed

Ming, Jun; Li, Mengliu; Kumar, Pushpendra; Li, Lain-Jong

2016-06-28

Conventional intercalated rechargeable batteries have shown their capacity limit, and the development of an alternative battery system with higher capacity is strongly needed for sustainable electrical vehicles and hand-held devices. Herein, we introduce a feasible and scalable multilayer approach to fabricate a promising hybrid lithium battery with superior capacity and multivoltage plateaus. A sulfur-rich electrode (90 wt % S) is covered by a dual layer of graphite/Li4Ti5O12, where the active materials S and Li4Ti5O12 can both take part in redox reactions and thus deliver a high capacity of 572 mAh gcathode(-1) (vs the total mass of electrode) or 1866 mAh gs(-1) (vs the mass of sulfur) at 0.1C (with the definition of 1C = 1675 mA gs(-1)). The battery shows unique voltage platforms at 2.35 and 2.1 V, contributed from S, and 1.55 V from Li4Ti5O12. A high rate capability of 566 mAh gcathode(-1) at 0.25C and 376 mAh gcathode(-1) at 1C with durable cycle ability over 100 cycles can be achieved. Operando Raman and electron microscope analysis confirm that the graphite/Li4Ti5O12 layer slows the dissolution/migration of polysulfides, thereby giving rise to a higher sulfur utilization and a slower capacity decay. This advanced hybrid battery with a multilayer concept for marrying different voltage plateaus from various electrode materials opens a way of providing tunable capacity and multiple voltage platforms for energy device applications.

Facile synthesis of nanorod-type graphitic carbon nitride/Fe{sub 2}O{sub 3} composite with enhanced photocatalytic performance

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

Wang, Jiangpeng; Li, Changqing; Cong, Jingkun

2016-06-15

Here we report a facile synthesis of nanorod-type graphitic carbon nitride/Fe{sub 2}O{sub 3} composite (Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4}) by using Fe-melamine supramolecular framework as precursor. The chemical and optical properties of the nanocomposites are well-characterized. The Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4} nanocomposite demonstrated excellent photocatalytic activities under visible light due to the efficient utilization of sunlight and the construction of Z-scheme electron transfer pathway. The results indicated that it could be a promising approach for the preparation of efficient g-C{sub 3}N{sub 4} nanocomposites photocatalysts by using metal-melamine supramolecular framework as precursors. - Graphical abstract: Nanorod-type graphitic carbon nitride/Fe{sub 2}O{submore » 3} composite (Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4}) was synthesized by using Fe-melamine supramolecular framework as precursor. The Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4} nanocomposite demonstrated excellent photocatalytic activities under visible light. Display Omitted - Highlights: • Nanorod-type graphitic carbon nitride/Fe{sub 2}O{sub 3} composite (Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4}) was synthesized. • Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4} showed strong optical absorption in the visible-light region. • The Fe{sub 2}O{sub 3}-g-C{sub 3}N{sub 4} nanocomposite demonstrated excellent photocatalytic activities.« less

Recrystallization of Manganite (γ-MnOOH) and Implications for Trace Element Cycling.

PubMed

Hens, Tobias; Brugger, Joël; Cumberland, Susan A; Etschmann, Barbara; Frierdich, Andrew J

2018-02-06

The recrystallization of Mn(III,IV) oxides is catalyzed by aqueous Mn(II) (Mn(II) aq ) during (bio)geochemical Mn redox cycling. It is poorly understood how trace metals associated with Mn oxides (e.g., Ni) are cycled during such recrystallization. Here, we use X-ray absorption spectroscopy (XAS) to examine the speciation of Ni associated with Manganite (γ-Mn(III)OOH) suspensions in the presence or absence of Mn(II) aq under variable pH conditions (pH 5.5 and 7.5). In a second set of experiments, we used a 62 Ni isotope tracer to quantify the amount of dissolved Ni that exchanges with Ni incorporated in the Manganite crystal structure during reactions in 1 mM Mn(II) aq and in Mn(II)-free solutions. XAS spectra show that Ni is initially sorbed on the Manganite mineral surface and is progressively incorporated into the mineral structure over time (13% after 51 days) even in the absence of dissolved Mn(II). The amount of Ni incorporation significantly increases to about 40% over a period of 51 days when Mn(II) aq is present in solution. Similarly, Mn(II) aq promotes Ni exchange between Ni-substituted Manganite and dissolved Ni(II), with around 30% of Ni exchanged at pH 7.5 over the duration of the experiment. No new mineral phases are detected following recrystallization as determined by X-ray diffraction and XAS. Our results reveal that Mn(II)-catalyzed mineral recrystallization partitions Ni between Mn oxides and aqueous fluids and can therefore affect Ni speciation and mobility in the environment.

Polymer matrix and graphite fiber interface study

NASA Technical Reports Server (NTRS)

Adams, D. F.; Zimmerman, R. S.; Odom, E. M.

1985-01-01

Hercules AS4 graphite fiber, unsized, or with EPON 828, PVA, or polysulfone sizing, was combined with three different polymer matrices. These included Hercules 3501-6 epoxy, Hercules 4001 bismaleimide, and Hexcel F155 rubber toughened epoxy. Unidirectional composites in all twelve combinations were fabricated and tested in transverse tension and axial compression. Quasi-isotropic laminates were tested in axial tension and compression, flexure, interlaminar shear, and tensile impact. All tests were conducted at both room temperature, dry and elevated temperature, and wet conditions. Single fiber pullout testing was also performed. Extensive scanning electron microphotographs of fracture surfaces are included, along with photographs of single fiber pullout failures. Analytical/experimental correlations are presented, based on the results of a finite element micromechanics analysis. Correlations between matrix type, fiber sizing, hygrothermal environment, and loading mode are presented. Results indicate that the various composite properties were only moderately influenced by the fiber sizings utilized.

Computational Reduction of Specimen Noise to Enable Improved Thermography Characterization of Flaws in Graphite Polymer Composites

NASA Technical Reports Server (NTRS)

Winfree, William P.; Howell, Patricia A.; Zalameda, Joseph N.

2014-01-01

Flaw detection and characterization with thermographic techniques in graphite polymer composites are often limited by localized variations in the thermographic response. Variations in properties such as acceptable porosity, fiber volume content and surface polymer thickness result in variations in the thermal response that in general cause significant variations in the initial thermal response. These result in a "noise" floor that increases the difficulty of detecting and characterizing deeper flaws. A method is presented for computationally removing a significant amount of the "noise" from near surface porosity by diffusing the early time response, then subtracting it from subsequent responses. Simulations of the thermal response of a composite are utilized in defining the limitations of the technique. This method for reducing the data is shown to give considerable improvement characterizing both the size and depth of damage. Examples are shown for data acquired on specimens with fabricated delaminations and impact damage.

Study to investigate design, fabrication and test of low cost concepts for large hybrid composite helicopter fuselage, phase 2

NASA Technical Reports Server (NTRS)

Adams, K. M.; Lucas, J. J.

1977-01-01

The development of a frame/stringer/skin fabrication technique for composite airframe construction was studied as a low cost approach to the manufacturer of larger helicopter airframe components. A center cabin aluminum airframe section of the Sikorsky CH-53D, was selected for evaluation as a composite structure. The design, as developed, is composed of a woven KEVLAR R-49/epoxy skin and graphite/epoxy frames and stringers. The single cure concept is made possible by the utilization of pre-molded foam cores, over which the graphite/epoxy pre-impregnated frame and stringer reinforcements are positioned. Bolted composite channel sections were selected as the optimum joint construction. The applicability of the single cure concept to larger realistic curved airframe sections, and the durability of the composite structure in a realistic spectrum fatigue environment, was described.

Student research with 400keV beams: {sup 13}N radioisotope production target development

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

Fru, L. Che; Clymer, J.; Compton, N.

2013-04-19

The AN400 Van de Graaff accelerator at the Minnesota State University, Mankato, Applied Nuclear Science Lab has demonstrated utility as an accessible and versatile platform for student research. Despite the limits of low energy, the research team successfully developed projects with applications to the wider radioisotope production community. A target system has been developed for producing and extracting {sup 13}N by the {sup 12}C(d,n){sup 13}N reaction below 400keV. The system is both reusable and robust, with future applications to higher energy machines producing this important radioisotope for physiological imaging studies with Positron Emission Tomography. Up to 36({+-}1)% of the {supmore » 13}N was extracted from the graphite matrix when 35 A current was externally applied to the graphite target while simultaneously flushing the target chamber with CO{sub 2} gas.« less

APPARATUS FOR DETECTING AND LOCATING PRESENCE OF FLUIDS

DOEpatents

Williamson, R.R.

1958-09-16

A system is described fur detecting water leaks in water-cooled neutronic reactors by utilizing an electrical hygrometer having a resistance element variable with the moisture content. The graphite blocks, forming the moderator in many types of reactors, coniain ducts in which helium gas is circulated. When a leak occurs in a coolant tube, the water will seep through the graphite until it oozes into one of the helium ducts, where it will be swept along with the helium into a system of pipes that connect each of the helium ducts. By inserting an electric hygrometer in each of these pipes and connecting it to an alarm system, the moisture content of the helium will cause a change in the electrical resistance of the hygrometer which will initiate a signal alarm indicating the presence and position of the leaky water tube in the reactor.

Promoting mechanism of N-doped single-walled carbon nanotubes for O2 dissociation and SO2 oxidation

NASA Astrophysics Data System (ADS)

Chen, Yanqiu; Yin, Shi; Chen, Yang; Cen, Wanglai; Li, Jianjun; Yin, Huaqiang

2018-03-01

Although heteroatom doping in carbon based catalysts have recently received intensive attentions, the role of the intrinsically porous structure of practical carbon materials and their potential synergy with doping atoms are still unclear. To investigate the complex effects, a range of N-doped single-walled carbon nanotubes (SWCNTs) were used to investigate their potential use for O2 dissociation and the subsequent SO2 oxidation using density functional theory. It is found that graphite N doping can synergize with the outer surface of SWCNTs to facilitate the dissociation of O2. The barrier for the dissociation on dual graphite N-doped SWCNT-(8, 8) is as low as 0.3 eV, and the subsequent SO2 oxidation is thermodynamically favorable and kinetically feasible. These results spotlight on developing promising carboncatalyst via utilization of porous gemometry and heteroatom-doping of carbon materials simultaneously.

Computational reduction of specimen noise to enable improved thermography characterization of flaws in graphite polymer composites

NASA Astrophysics Data System (ADS)

Winfree, William P.; Howell, Patricia A.; Zalameda, Joseph N.

2014-05-01

Flaw detection and characterization with thermographic techniques in graphite polymer composites are often limited by localized variations in the thermographic response. Variations in properties such as acceptable porosity, fiber volume content and surface polymer thickness result in variations in the thermal response that in general cause significant variations in the initial thermal response. These result in a "noise" floor that increases the difficulty of detecting and characterizing deeper flaws. A method is presented for computationally removing a significant amount of the "noise" from near surface porosity by diffusing the early time response, then subtracting it from subsequent responses. Simulations of the thermal response of a composite are utilized in defining the limitations of the technique. This method for reducing the data is shown to give considerable improvement characterizing both the size and depth of damage. Examples are shown for data acquired on specimens with fabricated delaminations and impact damage.

Chemistry of carbon nanomaterials: Uses of lithium nanotube salts in organic syntheses and functionalization of graphite

NASA Astrophysics Data System (ADS)

Chattopadhyay, Jayanta

The effective utilization of carbon nanomaterials, such as single-walled carbon nanotubes (SWNTs) and graphite, has been hindered due to difficulties (poor solubility, poly-dispersity) in processing. Therefore, a high degree of sidewall functionalization, either covalent or non-covalent, is often required to overcome these difficulties as the functionalized nanomaterials exhibit better solubility (either in organic solvents or in water), dispersity, manipulation, and processibility. This thesis presents a series of convenient and efficient organic synthetic routes to functionalize carbon nanomaterials. Carbon nanotube salts, prepared by treating SWNTs with lithium in liquid ammonia, react readily with aryl halides to yield aryl-functionalized SWNTs. These arylated SWNTs are soluble in methanol and water upon treatment with oleum. Similarly, SWNTs can be covalently functionalized by different heteroatoms (nitrogen, oxygen, and sulfur). Using the reductive alkylation approach, a synthetic scheme is designed to prepare long chain carboxylic acid functionalized SWNTs [SWNTs-(RCOOH)] that can react with (1) amine-terminated polyethylene glycol (PEG) chains to yield water-soluble biocompatible PEGylated SWNTs that are likely to be useful in a variety of biomedical applications; (2) polyethyleneimine (PEI) to prepare a SWNTs-PEI based adsorbent material that shows a four-fold improvement in the adsorption capacity of carbon dioxide over commonly used materials, making it useful for regenerable carbon dioxide removal in spaceflight; (3) chemically modified SWNTs-(RCOOH) to permit covalent bonding to the nylon matrix, thus allowing the formation of nylon 6,10 and nylon 6,10/SWNTs-(RCOOH) nanocomposites. Furthermore, we find that the lithium salts of carbon nanotubes serve as a source of electrons to induce polymerization of simple alkenes and alkynes onto the surface of carbon nanotubes. In the presence of sulfide/disulfide bonds, SWNT salts can initiate the single electron transfer (SET) mechanism to functionalize carbon nanotubes with different alkyl/aryl groups. Using the reductive alkylation approach, we can also functionalize graphites by alkyl/carboxylic acid groups, making graphite soluble in organic solvents and water. Tailoring of graphite layers is also accomplished by using different metals in liquid ammonia. Finally, SWNT-epoxides/graphite epoxides are synthesized using m-CPBA. Quantification of the epoxide substituents on the nanotube/graphite surface is evaluated through the catalytic de-epoxidation reaction using MeReO 3/PPh3 as heterogeneous catalyst. In summary, the proposed covalent functionalization methods yield derivatized nanomaterials that can provide a solid platform for a number of exciting applications, ranging from material science to biomedical devices. Furthermore, the results presented in this thesis provide insight into the molecular chemistry at nano-resolution.

Internal Shear Forging Processes for Missile Primary Structures.

DTIC Science & Technology

1981-07-20

received condition. The as-received micro- structure displayed elongated recrystallized grains interspersed with particles of precipitate phases. SEM...re- crystallization regime for this alloy, and rolled specimens were reheated to 3160 C between passes, some recrystallization and grain size changes...experiment revealed that the actual solution treatment temperature was probably higher than 5000C. This resulted in melting of the eutectic and solid

Chemical Characterization of Dimethylsulfoxide (DMSO) Munitions Recrystallization Process Samples.

DTIC Science & Technology

1984-10-01

position unless so designated by other aulthorized documents. Disposition Destroy this report when it is no longer needed. Do riot return it to the... DESTRIBUTION LIST ....... ........... ... ................................. -12 rABLES 1. HPLC Analyses of Munitions from DMS0 Recrystallization Process...characterization and identification of any trace organics present in addition to the nitramines. Portions of the two samples, designated as evaporator

Effect of Post-deformation Annealing Treatment on the Microstructural Evolution of a Cold-Worked Corrosion-Resistant Superalloy (CRSA) Steel

NASA Astrophysics Data System (ADS)

Mirzaei, A.; Zarei-Hanzaki, A.; Mohamadizadeh, A.; Lin, Y. C.

2018-03-01

The post-deformation annealing treatments of a commercial cold-worked corrosion-resistant superalloy steel (Sanicro 28 steel) were carried out at different temperatures in the range of 900-1100 °C for different holding durations of 5, 10, and 15 min. The effects of post-deformation annealing time and temperature on the microstructural evolution and subsequent mechanical properties of the processed Sanicro 28 steel were investigated. The observations indicated that twin-twin hardening in cold deformation condition mainly correlates with abundant nucleation of mechanical twins in multiple directions resulting in considerable strain hardening behavior. Microstructural investigations showed that the static recrystallization takes place after isothermal holding at 900 °C for 5 min. Increasing the annealing temperature from 900 to 1050 °C leads to recrystallization development and grain refinement in the as-recrystallized state. In addition, an increase in annealing duration from 5 to 15 min leads to subgrain coarsening and subsequently larger recrystallized grains size. The occurrence of large proportion of the grain refinement, which is achieved in the first annealing stage at 1050 °C after 5 min, is considered as the main factor for the maximum elongation at this stage.

Microstructural Evolution and Dynamic Softening Mechanisms of Al-Zn-Mg-Cu Alloy during Hot Compressive Deformation

PubMed Central

Shi, Cangji; Lai, Jing; Chen, X.-Grant

2014-01-01

The hot deformation behavior and microstructural evolution of an Al-Zn-Mg-Cu (7150) alloy was studied during hot compression at various temperatures (300 to 450 °C) and strain rates (0.001 to 10 s−1). A decline ratio map of flow stresses was proposed and divided into five deformation domains, in which the flow stress behavior was correlated with different microstructures and dynamic softening mechanisms. The results reveal that the dynamic recovery is the sole softening mechanism at temperatures of 300 to 400 °C with various strain rates and at temperatures of 400 to 450 °C with strain rates between 1 and 10 s−1. The level of dynamic recovery increases with increasing temperature and with decreasing strain rate. At the high deformation temperature of 450 °C with strain rates of 0.001 to 0.1 s−1, a partially recrystallized microstructure was observed, and the dynamic recrystallization (DRX) provided an alternative softening mechanism. Two kinds of DRX might operate at the high temperature, in which discontinuous dynamic recrystallization was involved at higher strain rates and continuous dynamic recrystallization was implied at lower strain rates. PMID:28788454

Ice recrystallization kinetics in the presence of synthetic antifreeze glycoprotein analogues using the framework of LSW theory.

PubMed

Budke, C; Heggemann, C; Koch, M; Sewald, N; Koop, T

2009-03-05

The Ostwald ripening of polycrystalline ice in aqueous sucrose solutions was investigated experimentally. The kinetics of this ice recrystallization process was studied at temperatures between -6 and -10 degrees C and varying ice volume fractions. Using the theory of Lifshitz, Slyozov, and Wagner (LSW), the diffusion-limited rate constant for ice recrystallization was determined. Also, the effects of synthetic analogues of natural antifreeze glycoproteins (AFGP) were studied. These analogues synAFGPmi (i = 3-5) contained monosaccharide side groups instead of disaccharide side groups that occur in natural AFGP. In order to account for the inhibition effect of the synAFGPmi, we have modified classical LSW theory, allowing for the derivation of inhibition rate constants. It was found that the investigated synAFGPmi inhibit ice recrystallization at concentrations down to approximately 3 microg mL(-1) or, equivalently, approximately 1 micromol L(-1) for the largest synAFGPmi investigated: synAFGPm5. Hence, our new method is capable of quantitatively assessing the efficiency of very similar AFGP with a sensitivity that is at least 2 orders of magnitude larger than that typical for quantitative thermal hysteresis measurements.

Influence of phosphate glass recrystallization on the stability of a waste matrix to leaching

NASA Astrophysics Data System (ADS)

Yudintsev, S. V.; Pervukhina, A. M.; Mokhov, A. V.; Malkovsky, V. I.; Stefanovsky, S. V.

2017-04-01

In Russia, highly radioactive liquid wastes from recycling of spent fuel of nuclear reactors are solidified into Na-Al-P glass for underground storage. The properties of the matrix including the radionuclide fixation will change with time due to crystallization. This is supported by the results of study of the interaction between glassy matrices, products of their crystallization, and water. The concentration of Cs in a solution at the contact of a recrystallized sample increased by three orders of magnitude in comparison with an experiment with glass. This difference is nearly one order of magnitude for Sr, Ce, and Nd (simulators of actinides) and U due to their incorporation into phases with low solubility in water. Based on data on the compositional change of solutions after passing through filters of various diameters, it is concluded that Cs occurs in the dissolved state in runs with a glass and recrystallized matrix. At the same time, Sr, lanthanides, and U occur in the dissolved state and in the composition of colloids in runs with glass, and mostly in colloid particles after contact with the recrystallized sample. These results should be regarded for substantiation of safety for geological waste storage.

S-Isovaline Contained in Meteorites, Induces Enantiomeric Excess in D,L-glutamic Acid During Recrystallization

NASA Astrophysics Data System (ADS)

Kojo, Shosuke

2015-06-01

S-Isovaline (S-Iva: 6.7 mmol) and D,L-glutamic acid (Glu: 2 mmol) were dissolved in 10 ml of hot water, and the resulting solution was divided in 5 vessels. After recrystallization, the crystals were collected from each vessel, and the enantiomeric excess (ee) of Glu was determined with chemical derivatization using 1-fluoro-2,4-dinitrophenyl- 5-L-leucinamide followed by high-performance liquid chromatography. Ten crystallizations provided all D-rich Glu with ee values of 2.69 % ± 0.81 % (mean ± standard deviation), and those using R-Iva provided all L-rich Glu with ee values of 6.24 % ± 2.20 %. Five recrystallizations of D,L-Glu alone provided ee values of 0.474 % ± 0.33 %. The differences among these three ee values were statistically significant, showing that S-Iva, which was present in meteorites caused a significant induction of ee in this physiological amino acid. This is the first outcome that S-Iva induced ee changes in a physiological amino acid. S-Iva did not induce any ee changes in D,L-asparagine, leucine, valine, methionine, phenylalanine, tryptophan, glutamine, tyrosine, aspartic acid, or histidine under similar recrystallizations.

Quarzt Fabric Insights Across a Low P-High T Shear Zone

NASA Astrophysics Data System (ADS)

Gomez Barreiro, J.; Martinez-Catalan, J. R.; Benitez Perez, J.; Wenk, H.; Vogel, S. C.; Alcock, J. E.

2013-12-01

The evolution of mylonitic fabric in quartzites across a Low-P / High-T gradient within the Lugo Dome Extensional system (NW Spain) is analyzed. Quantitative texture measurements with TOF neutron diffraction, Shape preferred orientation (SPO) and Crystal Size Distribution (CSD) analyses were correlated with tectonothermal data to constraint the prevalence of ductile deformative fabrics exposed to cycles of dynamic and static recrystallization. Results suggest two stages in the evolution of mylonites in close correlation to thermal gradient, 1) a pervasive ductile deformation affecting most of the shear zone volume, with the development of symmetric cross girdle c-axes fabric suggesting slip on {c,r,m} and dynamically recrystallized microstructures which resulted into the refinement of the grain-size. 2) An heterogeneous deformation stage where strain partition led to the formation of relatively active and passive domains. During this late stage, at deeper levels, High T detachments show [c]{m} slip system and dynamic recrystallization activation, with monoclinic texture patterns, meanwhile, passive domains followed an static recrystallization with abnormal grain growth and minor variation of early orthogonal texture patterns Neutron diffraction data (cross) and Rietveld model obtained with MAUD (solid line) of a mylonitic quartzite. Some important planes are indicated for the major phases.

Hot Deformation Behavior and Dynamic Recrystallization of Medium Carbon LZ50 Steel

NASA Astrophysics Data System (ADS)

Du, Shiwen; Chen, Shuangmei; Song, Jianjun; Li, Yongtang

2017-03-01

Hot deformation and dynamic recrystallization behaviors of a medium carbon steel LZ50 were systematically investigated in the temperature range from 1143 K to 1443 K (870 °C to 1170 °C) at strain rates from 0.05 to 3s-1 using a Gleeble-3500 thermo-simulation machine. The flow stress constitutive equation for hot deformation of this steel was developed with the two-stage Laasraoui equation. The activation energy of the tested steel was 304.27 KJ/mol, which was in reasonable agreement with those reported previously. The flow stress of this steel in hot deformation was mainly controlled by dislocation climb during their intragranular motion. The effect of Zener-Hollomon parameter on the characteristic points of the flow curves was studied, and the dependence of critical strain on peak strain obeyed a linear equation. Dynamic recrystallization was the most important softening mechanism for the tested steel during hot deformation. Kinetic equation of this steel was also established based on the flow stress. The austenite grain size of complete dynamic recrystallization was a power law function of Zener-Hollomon parameter with an exponent of -0.2956. Moreover, the microstructures induced under different deformation conditions were analyzed.

Effects of Al3(Sc,Zr) and Shear Band Formation on the Tensile Properties and Fracture Behavior of Al-Mg-Sc-Zr Alloy

NASA Astrophysics Data System (ADS)

Huang, Hongfeng; Jiang, Feng; Zhou, Jiang; Wei, Lili; Qu, Jiping; Liu, Lele

2015-11-01

The mechanical properties and microstructures of Al-6Mg-0.25Sc-0.1Zr alloy (wt.%) during annealing were investigated by means of uniaxial tensile testing, optical microscope, scanning electron microscope, transmission electron microscope, and high-resolution transmission electron microscope. The results show that a large number of micro and grain-scale shear bands form in this alloy after cold rolling. As the tensile-loading force rises, strain softening would generate in shear bands, resulting in the occurrence of shear banding fracture in cold-rolled Al-Mg-Sc-Zr alloys. Recrystallization takes place preferentially in shear bands during annealing. Due to the formation of coarse-grain bands constructed by new subgrains, recrystallization softening tends to occur in these regions. During low-temperature annealing, recrystallization is inhibited by nano-scale Al3(Sc,Zr) precipitates which exert significant coherency strengthening and modulus hardening. However, the strengthening effect of Al3(Sc,Zr) decreases with the increasing of particle diameter at elevated annealing temperature. The mechanical properties of the recrystallized Al-Mg-Sc-Zr alloy decrease to a minimum level, and the fracture plane exhibits pure ductile fracture characteristics.

A Continuum Model for the Effect of Dynamic Recrystallization on the Stress–Strain Response

PubMed Central

Perdahcıoğlu, E. S.; van den Boogaard, A. H.

2018-01-01

Austenitic Stainless Steels and High-Strength Low-Alloy (HSLA) steels show significant dynamic recovery and dynamic recrystallization (DRX) during hot forming. In order to design optimal and safe hot-formed products, a good understanding and constitutive description of the material behavior is vital. A new continuum model is presented and validated on a wide range of deformation conditions including high strain rate deformation. The model is presented in rate form to allow for the prediction of material behavior in transient process conditions. The proposed model is capable of accurately describing the stress–strain behavior of AISI 316LN in hot forming conditions, also the high strain rate DRX-induced softening observed during hot torsion of HSLA is accurately predicted. It is shown that the increase in recrystallization rate at high strain rates observed in experiments can be captured by including the elastic energy due to the dynamic stress in the driving pressure for recrystallization. Furthermore, the predicted resulting grain sizes follow the power-law dependence with steady state stress that is often reported in literature and the evolution during hot deformation shows the expected trend. PMID:29789492

Effect of storage conditions on the recrystallization of drugs in solid dispersions with crospovidone.

PubMed

Shibata, Yusuke; Fujii, Makiko; Suzuki, Ayako; Koizumi, Naoya; Kanada, Ken; Yamada, Masaki; Watanabe, Yoshiteru

2014-06-01

The physical stability of amorphous solid dispersions (SDs) is influenced by their storage conditions. The goal of this work was to investigate the factors affecting the recrystallization of drugs in SDs after storage under conditions of high temperature and high humidity. SDs of three drugs (dipyridamole, nifedipine and indomethacin) with different functional groups (amino, carbonyl and hydroxyl) and onset times for crystallization of the amorphous state were prepared using crospovidone (CrosPVP). All of the drugs in the SDs remained in an amorphous state at 25 °C/50% relative humidity (RH) in closed glass bottles for at least six months. Under conditions of high temperature (40 °C/75%RH/closed and 60 °C/open), differences in interactions between the hydrogen bond donors of the drugs and the amide carbonyl group of CrosPVP are essential factors for recrystallization of the drugs in the SDs. On the other hand, under condition of high humidity (40 °C/75%RH/open), in addition to the difference in the interaction between the drug and CrosPVP, the rate of increase in moisture content affects their recrystallization in SDs.

Reduced graphene oxide-induced recrystallization of NiS nanorods to nanosheets and the improved Na-storage properties.

PubMed

Pan, Qin; Xie, Jian; Zhu, Tiejun; Cao, Gaoshao; Zhao, Xinbing; Zhang, Shichao

2014-04-07

Preparation of two-dimensional (2D) graphene-like materials is currently an emerging field in materials science since the discovery of single-atom-thick graphene prepared by mechanical cleavage. In this work, we proposed a new method to prepare 2D NiS, where reduced graphene oxide (rGO) was found to induce the recrystallization of NiS from nanorods to nanosheets in a hydrothermal process. The process and mechanism of recrystallization have been clarified by various characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) mapping, and X-ray photoelectron spectroscopy (XPS). The characterization of ex situ NiS/rGO products by SEM and EDS mapping indicates that the recrystallization of NiS from nanorods to nanosheets is realized actually through an exfoliation process, while the characterization of in situ NiS/rGO products by SEM, TEM, and EDS mapping reveals the exfoliation process. The XPS result demonstrates that hydrothermally assisted chemical bonding occurs between NiS and rGO, which induces the exfoliation of NiS nanorods into nanosheets. The obtained NiS/rGO composite shows promising Na-storage properties.

Voronoi-Tessellated Graphite Produced by Low-Temperature Catalytic Graphitization from Renewable Resources.

PubMed

Zhao, Leyi; Zhao, Xiuyun; Burke, Luke T; Bennett, J Craig; Dunlap, Richard A; Obrovac, Mark N

2017-09-11

A highly crystalline graphite powder was prepared from the low temperature (800-1000 °C) graphitization of renewable hard carbon precursors using a magnesium catalyst. The resulting graphite particles are composed of Voronoi-tessellated regions comprising irregular sheets; each Voronoi-tessellated region having a small "seed" particle located near their centroid on the surface. This suggests nucleated outward growth of graphitic carbon, which has not been previously observed. Each seed particle consists of a spheroidal graphite shell on the inside of which hexagonal graphite platelets are perpendicularly affixed. This results in a unique high surface area graphite with a high degree of graphitization that is made with renewable feedstocks at temperatures far below that conventionally used for artificial graphites. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Vertically aligned GaAs nanowires on graphite and few-layer graphene: generic model and epitaxial growth.

PubMed

Munshi, A Mazid; Dheeraj, Dasa L; Fauske, Vidar T; Kim, Dong-Chul; van Helvoort, Antonius T J; Fimland, Bjørn-Ove; Weman, Helge

2012-09-12

By utilizing the reduced contact area of nanowires, we show that epitaxial growth of a broad range of semiconductors on graphene can in principle be achieved. A generic atomic model is presented which describes the epitaxial growth configurations applicable to all conventional semiconductor materials. The model is experimentally verified by demonstrating the growth of vertically aligned GaAs nanowires on graphite and few-layer graphene by the self-catalyzed vapor-liquid-solid technique using molecular beam epitaxy. A two-temperature growth strategy was used to increase the nanowire density. Due to the self-catalyzed growth technique used, the nanowires were found to have a regular hexagonal cross-sectional shape, and are uniform in length and diameter. Electron microscopy studies reveal an epitaxial relationship of the grown nanowires with the underlying graphitic substrates. Two relative orientations of the nanowire side-facets were observed, which is well explained by the proposed atomic model. A prototype of a single GaAs nanowire photodetector demonstrates a high-quality material. With GaAs being a model system, as well as a very useful material for various optoelectronic applications, we anticipate this particular GaAs nanowire/graphene hybrid to be promising for flexible and low-cost solar cells.

Optical Band Gap Alteration of Graphene Oxide via Ozone Treatment.

PubMed

Hasan, Md Tanvir; Senger, Brian J; Ryan, Conor; Culp, Marais; Gonzalez-Rodriguez, Roberto; Coffer, Jeffery L; Naumov, Anton V

2017-07-25

Graphene oxide (GO) is a graphene derivative that emits fluorescence, which makes GO an attractive material for optoelectronics and biotechnology. In this work, we utilize ozone treatment to controllably tune the band gap of GO, which can significantly enhance its applications. Ozone treatment in aqueous GO suspensions yields the addition/rearrangement of oxygen-containing functional groups suggested by the increase in vibrational transitions of C-O and C=O moieties. Concomitantly it leads to an initial increase in GO fluorescence intensity and significant (100 nm) blue shifts in emission maxima. Based on the model of GO fluorescence originating from sp 2 graphitic islands confined by oxygenated addends, we propose that ozone-induced functionalization decreases the size of graphitic islands affecting the GO band gap and emission energies. TEM analyses of GO flakes confirm the size decrease of ordered sp 2 domains with ozone treatment, whereas semi-empirical PM3 calculations on model addend-confined graphitic clusters predict the inverse dependence of the band gap energies on sp 2 cluster size. This model explains ozone-induced increase in emission energies yielding fluorescence blue shifts and helps develop an understanding of the origins of GO fluorescence emission. Furthermore, ozone treatment provides a versatile approach to controllably alter GO band gap for optoelectronics and bio-sensing applications.

Influence of Metal-Coated Graphite Powders on Microstructure and Properties of the Bronze-Matrix/Graphite Composites

NASA Astrophysics Data System (ADS)

Zhao, Jian-hua; Li, Pu; Tang, Qi; Zhang, Yan-qing; He, Jian-sheng; He, Ke

2017-02-01

In this study, the bronze-matrix/x-graphite (x = 0, 1, 3 and 5%) composites were fabricated by powder metallurgy route by using Cu-coated graphite, Ni-coated graphite and pure graphite, respectively. The microstructure, mechanical properties and corrosive behaviors of bronze/Cu-coated-graphite (BCG), bronze/Ni-coated-graphite (BNG) and bronze/pure-graphite (BPG) were characterized and investigated. Results show that the Cu-coated and Ni-coated graphite could definitely increase the bonding quality between the bronze matrix and graphite. In general, with the increase in graphite content in bronze-matrix/graphite composites, the friction coefficients, ultimate density and wear rates of BPG, BCG and BNG composites all went down. However, the Vickers microhardness of the BNG composite would increase as the graphite content increased, which was contrary to the BPG and BCG composites. When the graphite content was 3%, the friction coefficient of BNG composite was more stable than that of BCG and BPG composites, indicating that BNG composite had a better tribological performance than the others. Under all the values of applied loads (10, 20, 40 and 60N), the BCG and BNG composites exhibited a lower wear rate than BPG composite. What is more, the existence of nickel in graphite powders could effectively improve the corrosion resistance of the BNG composite.

Garnet peridotites from Williams kimberlites, north-central Montana, U.S.A

USGS Publications Warehouse

Hearn, B.C.; McGee, E.S.

1983-01-01

Two Williams kimberlites, 250x350m and 37x390m, in the eastern part of a swarm of 30 middle Eocene alnoitic diatremes in north-central Montana, USA, contain xenoliths of garnet-bearing lherzolites, harzburgites and dunites, in addition to spinel peridotites and upper and lower crustal amphibolites and granulites. Colluvial purple, red, and pink garnets are dominantly Mg- and Cr-rich, indicating their derivation From peridotites or megacrysts, and have CaO and Cr2O3 contents that fall in the lherzolite trend. Temperatures were calculated by the Lindsley-Dixon 20 kb method for lherzolites and by the O'Neill-Wood method for harzburgites and dunites, and pressures were calculated by the MacGregor method, or were assumed to be 50 kb for dunites. Most peridotites equilibrated at 1220-1350?C and 50-60 kb, well above a 44mW/m2 shield geotherm and on or at higher P than the graphite-diamond boundary. Four lherzolites are low T-P (830-990?C, 23-42 kb) and are close to the shield geotherm. All four low T-P lherzolites have coarse textures whereas the high T-P cluster has both coarse and porphyroclastic textures, indicating a range of conditions of deformation and recrystallization in a restricted high T-P range. The tiny size (0.01-0.2 mm) of granulated and euhedral olivines in several xenoliths shows that deformation was occurring just prior to incorporation in kimberlite and that ascent was rapid enough (40-70 km/hr) to retard Further coarsening of fine-grained olivine. For other high T-P peridotites, cessation of deformation and beginning of recrystallization before or during inclusion in kimberlite is suggested by larger (up to 3mm) euhedral olivines in a matrix of fine granulated olivine or by optical continuity of large and nearby small olivines. Two low T-P lherzolites contain distinctive, phlogopite-rimmed, 5-8mm clots of moderate-Cr garnet + Cr-spinel + Cr-diopside + enstatite that are inferred to have formed by reaction of an initial high-Cr garnet brought into the garnet + spinel stability Field. This suggests a reduction in pressure and temperature prior to inclusion in the kimberlite, followed by metasomatic introduction of phlogopite. These textural and compositional variations of peridotites seem most compatible with kimberlite generation and ascent during dynamic diapiric perturbation of the upper mantle.

Development of high-temperature Kolsky compression bar techniques for recrystallization investigation

NASA Astrophysics Data System (ADS)

Song, B.; Antoun, B. R.; Boston, M.

2012-05-01

We modified the design originally developed by Kuokkala's group to develop an automated high-temperature Kolsky compression bar for characterizing high-rate properties of 304L stainless steel at elevated temperatures. Additional features have been implemented to this high-temperature Kolsky compression bar for recrystallization investigation. The new features ensure a single loading on the specimen and precise time and temperature control for quenching to the specimen after dynamic loading. Dynamic compressive stress-strain curves of 304L stainless steel were obtained at 21, 204, 427, 649, and 871 °C (or 70, 400, 800, 1200, and 1600 °F) at the same constant strain rate of 332 s-1. The specimen subjected to specific time and temperature control for quenching after a single dynamic loading was preserved for investigating microstructure recrystallization.

A re-evaluation of the mechanism of SIBM

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

Bate, P.; Hutchinson, B.

The process for creating a new recrystallized grain by the bulging out of an existing grain boundary within the deformed structure was recognized by Beck and Sperry and described as strain induced boundary migration, often now as SIBM. For many years SIBM seemed to be accorded less significance than the subgrain growth models for nucleation of recrystallization. However, the importance of SIBM is increasingly recognized, for example in the case of cube texture development in aluminum alloys. There is increasing evidence that high angle boundaries in deformed metals are not only residues of the prior grain structure but may alsomore » be generated by the deformation itself. These also participate in the nucleation of recrystallization on annealing and must do so by some form of SIBM mechanism.« less

Etude de la texture des rubans EPR de silicium polycristallin photovoltaïque

NASA Astrophysics Data System (ADS)

Chibani, A.; Gauthier, R.; Pinard, P.; Andonov, P.

1991-09-01

EPR polysilicon ribbons are obtained from a 5N-6N purity grade silicon powder melting followed by a recrystallization step. Being assigned to the photocell manufacture, we study the texture by X-ray diffraction method to reveal the majority of the crystal orientations and prove the eventual existence of specific orientations adapted to the best photovoltaic conversion efficiencies such as (100), (110) or (111). Moreover, we tested the possibility to induce the (111) orientation with a monocrystalline seed having this orientation. It appears that the crystal growth is essentially anisotropic and that only the orientation of the grains with their (331) planes parallel to the ribbon surface may be considered as dominant after the recrystallization step; finally, the (111) starting seed has an effect only at the recrystallization onset.

Producing graphite with desired properties

NASA Technical Reports Server (NTRS)

Dickinson, J. M.; Imprescia, R. J.; Reiswig, R. D.; Smith, M. C.

1971-01-01

Isotropic or anisotropic graphite is synthesized with precise control of particle size, distribution, and shape. The isotropic graphites are nearly perfectly isotropic, with thermal expansion coefficients two or three times those of ordinary graphites. The anisotropic graphites approach the anisotropy of pyrolytic graphite.

Brazing graphite to graphite

DOEpatents

Peterson, George R.

1976-01-01

Graphite is joined to graphite by employing both fine molybdenum powder as the brazing material and an annealing step that together produce a virtually metal-free joint exhibiting properties similar to those found in the parent graphite. Molybdenum powder is placed between the faying surfaces of two graphite parts and melted to form molybdenum carbide. The joint area is thereafter subjected to an annealing operation which diffuses the carbide away from the joint and into the graphite parts. Graphite dissolved by the dispersed molybdenum carbide precipitates into the joint area, replacing the molybdenum carbide to provide a joint of virtually graphite.

Method of Joining Graphite Fibers to a Substrate

NASA Technical Reports Server (NTRS)

Beringer, Durwood M. (Inventor); Caron, Mark E. (Inventor); Taddey, Edmund P. (Inventor); Gleason, Brian P. (Inventor)

2014-01-01

A method of assembling a metallic-graphite structure includes forming a wetted graphite subassembly by arranging one or more layers of graphite fiber material including a plurality of graphite fibers and applying a layer of metallization material to ends of the plurality of graphite fibers. At least one metallic substrate is secured to the wetted graphite subassembly via the layer of metallization material.

Laser paint stripping

NASA Astrophysics Data System (ADS)

Head, J. D.; Niedzielski, J. Peter

1991-06-01

A study to assess the utility of high powered CO2 pulsed laser depainting methods was conducted on aluminum and graphite epoxy composites. The various tests were designed to detect potential forms of damage or loss of properties of various aircraft structural materials during removal of paint with pulsed laser energy. Tests for changes in physical properties, paint adhesion and corrosion protection of repainted materials showed no detectable adverse changes in any of the samples studied.

Laser ablative synthesis of carbon nanotubes

DOEpatents

Smith, Michael W.; Jordan, Kevin; Park, Cheol

2010-03-02

An improved method for the production of single walled carbon nanotubes that utilizes an RF-induction heated side-pumped synthesis chamber for the production of such. Such a method, while capable of producing large volumes of carbon nanotubes, concurrently permits the use of a simplified apparatus that allows for greatly reduced heat up and cool down times and flexible flowpaths that can be readily modified for production efficiency optimization. The method of the present invention utilizes a free electron laser operating at high average and peak fluence to illuminate a rotating and translating graphite/catalyst target to obtain high yields of SWNTs without the use of a vacuum chamber.

Thermally exfoliated graphite oxide

NASA Technical Reports Server (NTRS)

Prud'Homme, Robert K. (Inventor); Aksay, Ilhan A. (Inventor); Abdala, Ahmed (Inventor)

2011-01-01

A modified graphite oxide material contains a thermally exfoliated graphite oxide with a surface area of from about 300 sq m/g to 2600 sq m/g, wherein the thermally exfoliated graphite oxide displays no signature of the original graphite and/or graphite oxide, as determined by X-ray diffraction.

Pulsed Electrodeposition of Amorphous and Composite Alloys.

DTIC Science & Technology

1983-09-01

lamellar- eutectic composites. A new phenomenon was dis- covered that deposits consisting of alternate layers of the same phase and essentially the...phenomenon will be discussed in connection with the Cu-Zn alloys. The recrystallization kinetics of the Ni-Mo alloys were investigated in order to find...transmission-electron-microscopic examination. The percent of the area which had recrystallized was determined on photographs using a planimeter. From a

Materials processing apparatus development for fluoride glass

NASA Technical Reports Server (NTRS)

Smith, Guy A.; Kosten, Sue; Workman, Gary L.

1994-01-01

Fluoride glasses have great potential for optical fiber communications due to the high transmittance when no microcrystallites occur during drawing operations. This work has developed apparatus to test the occurrence of microcrystallites during recrystallization in reduced gravity on the KC-135. The apparatus allows fluoride glass fiber, such as ZBLAN, to be melted and recrystallized during both the low and high g portions the parabolic flight.

Dynamic recrystallization and grain boundary migration in B2 FeAl

NASA Technical Reports Server (NTRS)

Baker, I.; Gaydosh, D. J.

1987-01-01

Transmission electron microscopy and optical microscopy were used to examine polycrystalline specimens of the B2-structured alloy FeAl strained under tension to fracture at elevated temperature. Strain-induced grain boundary migration was observed above 900 K and dynamic recrystallization was found at 1000 K and 1100 K. Little evidence of dynamic recovery was evident but some networks were formed at 1100 K.

U-Th dating of calcite corals from the Gulf of Aqaba

NASA Astrophysics Data System (ADS)

Yehudai, Maayan; Lazar, Boaz; Bar, Neta; Kiro, Yael; Agnon, Amotz; Shaked, Yonathan; Stein, Mordechai

2017-02-01

Most of the fossil corals in the elevated reef terraces along the Gulf of Aqaba (GOA) were extensively altered to calcite. This observation indicates extensive interaction with freshwater, possibly when the terraces passed through a coastal aquifer that existed along the shores of the GOA, implying a wetter climate during the time of recrystallization from aragonite to calcite. Thus, dating of the recrystallization events should yield the timing of past wetter conditions in the current hyper-arid area of the GOA. In the present study, 18 aragonite and calcite corals were collected from several elevated coral reef terraces off the coast, south of the city of Aqaba. While aragonite corals were dated with the conventional closed system age equation (assuming zero initial Th), the dating of the calcite corals required the development of adequate equations to allow the calculation of both the initial formation age of the aragonite corals and the time of recrystallization to calcite. The two age calculations were based on the assumptions that each reef terrace went through a single and rapid recrystallization event and that the pristine aragonite corals were characterized by a rather uniform initial U concentration, typical for pristine modern corals. Two recrystallization events were identified at 104 ± 6 ka and 124 ± 8 ka. The ages coincide with the timing of sapropel events S4 and S5, respectively, when the African monsoon induced enhanced wetness in the desert area. Considering the age uncertainties, the times of formation of the two major reef terraces are estimated to be ∼124 ka (reef terrace R2) and ∼130 ka (reef terrace R3), matching the peaks in the global sea level during the last interglacial MIS 5e stage. Apparently, sea level of the GOA did not fluctuate a lot during the period between ∼130 ka and ∼104 ka and remained close to the Marine Isotopic stage (MIS) 5e highstand. The availability of freshwater (during the sapropel periods) and limited sea level fluctuations facilitated the recrystallization of the GOA reef corals to calcite.

Constraining the Texture and Composition of Pore-Filling Cements at Gale Crater, Mars

NASA Technical Reports Server (NTRS)

Siebach, K. L.; Grotzinger, J. P.; McLennan, S. M.; Hurowitz, J. A.; Ming, D. W.; Vaniman, D. T.; Rampe, E. B.; Blaney, D. L.; Kah, L. C.

2015-01-01

The Mars Science Laboratory (MSL) rover Curiosity has encountered a wide variety of sedimentary rocks deposited in fluvio-lacuestrine sequences at the base of Gale Crater. The presence of sedimentary rocks requires that initial sediments underwent diagenesis and were lithified. Lithification involves sediment compaction, cementation, and re-crystallization (or authigenic) processes. Analysis of the texture and composition of the cement can reveal the environmental conditions when the cements were deposited, enabling better understanding of early environments present within Gale Crater. The first step in lithification is sediment compaction. The Gale crater sediments do not show evidence for extensive compaction prior to cementation; the Sheepbed mudstone in Yellowknife Bay (YKB) has preserved void spaces ("hollow nodules"), indicating that sediments were cemented around the hollow prior to compaction, and conglomerates show imbrication, indicating minimal grain reorganization prior to lithification. Furthermore, assuming the maximum burial depth of these sediments is equivalent to the depth of Gale Crater, the sediments were never under more than 1 kb of pressure, and assuming a 15 C/km thermal gradient in the late Noachian, the maximum temperature of diagenesis would have been approximately 75 C. This is comparable to shallow burial diagenetic conditions on Earth. The cementation and recrystallization components of lithification are closely intertwined. Cementation describes the precipitation of minerals between grains from pore fluids, and recrystallization (or authigenesis) is when the original sedimentary mineral grains are altered into secondary minerals. The presence of authigenic smectites and magnetite in the YKB formation suggests that some recrystallization has taken place. The relatively high percentage of XRD-amorphous material (25-40%) detected by CheMin suggests that this recrystallization may be limited in scope, and therefore may not contribute significantly to the cementing material. However, relatively persistent amorphous components could exist in the Martian environment (e.g. amorphous MgSO4), so recrystallization, including loss of crystallinity, cannot yet be excluded as a method of cementation. In order to describe the rock cementation, both the rock textures and their composition must be considered. Here, we attempt to summarize the current understanding of the textural and compositional aspects of the cement across the rocks analyzed by Curiosity to this point.

Hydride reorientation and its impact on ambient temperature mechanical properties of high burn-up irradiated and unirradiated recrystallized Zircaloy-2 nuclear fuel cladding with an inner liner

NASA Astrophysics Data System (ADS)

Auzoux, Q.; Bouffioux, P.; Machiels, A.; Yagnik, S.; Bourdiliau, B.; Mallet, C.; Mozzani, N.; Colas, K.

2017-10-01

Precipitation of radial hydrides in zirconium-based alloy cladding concomitant with the cooling of spent nuclear fuel during dry storage can potentially compromise cladding integrity during its subsequent handling and transportation. This paper investigates hydride reorientation and its impact on ductility in unirradiated and irradiated recrystallized Zircaloy-2 cladding with an inner liner (cladding for boiling water reactors) subjected to hydride reorientation treatments. Cooling from 400 °C, hydride reorientation occurs in recrystallized Zircaloy-2 with liner at a lower effective stress in irradiated samples (below 40 MPa) than in unirradiated specimens (between 40 and 80 MPa). Despite significant hydride reorientation, unirradiated recrystallized Zircaloy-2 with liner cladding containing ∼200 wppm hydrogen shows a high diametral strain at fracture (>15%) during burst tests at ambient temperature. This ductile behavior is due to (1) the lower yield stress of the recrystallized cladding materials in comparison to hydride fracture strength (corrected by the compression stress arising from the precipitation) and (2) the hydride or hydrogen-depleted zone as a result of segregation of hydrogen into the liner layer. In irradiated Zircaloy-2 with liner cladding containing ∼340 wppm hydrogen, the conservation of some ductility during ring tensile tests at ambient temperature after reorientation treatment at 400 °C with cooling rates of ∼60 °C/h is also attributed to the existence of a hydride-depleted zone. Treatments at lower cooling rates (∼6 °C/h and 0.6 °C/h) promote greater levels of hydrogen segregation into the liner and allow for increased irradiation defect annealing, both of which result in a significant increase in ductility. Based on this investigation, given the very low cooling rates typical of dry storage systems, it can be concluded that the thermal transients associated with dry storage should not degrade, and more likely should actually improve, ductility of recrystallized Zircaloy-2 cladding with inner liner with such hydrogen content.

Perspectives on geochemical proxies: The impact of model and parameter selection on the quantification of carbonate recrystallization rates

NASA Astrophysics Data System (ADS)

Huber, Christian; Druhan, Jennifer L.; Fantle, Matthew S.

2017-11-01

Diagenetic reactions in marine sediments, such as the recrystallization of carbonates, can impact the accuracy of paleo-environmental and paleo-climatic reconstructions by geochemical proxies. The extent to which the recrystallization of carbonates affects the chemistry of sedimentary archives depends on the reaction rate, extent of isotopic disequilibrium, and duration of reaction. The reaction rate, which is obviously critical, can be constrained by the elemental and isotopic compositions of pore fluids. Such constraints are affected by assumptions regarding the temperature in the sedimentary column relative to the temperature of formation, the burial rate, pore fluid advection, the composition of the sediments (carbonate-rich versus siliciclastic), and the porosity of the sediment column. In this study, we use a steady-state analytical solution to the diagenetic equations to constrain depth-dependent reaction rates (and extents of recrystallization) based on the Ca isotopic compositions of pore fluids in sedimentary columns at multiple ocean drilling sites (Sites 807, 984, 1170, and 1171), which encompass a diverse range of sedimentary compositions and conditions. We find that carbonates in siliciclastic sediments are generally less altered by diagenesis than their carbonate-rich counterparts. The discrepancy in recrystallization rates between siliciclastic and carbonate-rich sedimentary sections is, however, significantly smaller than previously estimated, suggesting that siliciclastic archives are not immune to diagenetic effects. While we find that diagenesis can decouple contemporaneous proxies of sea surface temperature (Mg/Ca and δ18O), our calculations also reveal that δ18O-based temperature estimates are more robust in siliciclastic sections relative to carbonate-rich sections. Sensitivity tests of the calculated extent of recrystallization suggest that uncertainties in porosity and burial rate are generally the greatest sources of error to proxy reconstruction from diagenetically altered sediments. The conclusions drawn using the analytical solution are benchmarked against a depth-dependent, forward numerical model using the CrunchFlow software (Steefel et al., 2015); ultimately, this comparison demonstrates that the assumptions necessary in deriving the analytical solutions have a relatively minor impact on the resulting conclusions.

The action of macrosounds on graphite ore and derived products

NASA Technical Reports Server (NTRS)

Bradeteanu, C.; Dragan, O.

1974-01-01

A suspension of graphite ore, floated graphite, and the gangue left over from flotation were subjected to the action of macrosounds under determinant conditions. The following was found: (1) The graphite ore undergoes an efficient settling action. (2) The floated graphite is strongly crushed down to the dimensions of colloidal graphite. (3) The gangue left over from flotation can be further processed to recuperate graphite from its nuclei.

Graphene prepared by thermal reduction–exfoliation of graphite oxide: Effect of raw graphite particle size on the properties of graphite oxide and graphene

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

Dao, Trung Dung; Jeong, Han Mo, E-mail: hmjeong@mail.ulsan.ac.kr

Highlights: • Effect of raw graphite particle size on properties of GO and graphene is reported. • Size of raw graphite affects oxidation degree and chemical structure of GO. • Highly oxidized GO results in small-sized but well-exfoliated graphene. • GO properties affect reduction degree, structure, and conductivity of graphene. - Abstract: We report the effect of raw graphite size on the properties of graphite oxide and graphene prepared by thermal reduction–exfoliation of graphite oxide. Transmission electron microscope analysis shows that the lateral size of graphene becomes smaller when smaller size graphite is used. X-ray diffraction analysis confirms that graphitemore » with smaller size is more effectively oxidized, resulting in a more effective subsequent exfoliation of the obtained graphite oxide toward graphene. X-ray photoelectron spectroscopy demonstrates that reduction of the graphite oxide derived from smaller size graphite into graphene is more efficient. However, Raman analysis suggests that the average size of the in-plane sp{sup 2}-carbon domains on graphene is smaller when smaller size graphite is used. The enhanced reduction degree and the reduced size of sp{sup 2}-carbon domains contribute contradictively to the electrical conductivity of graphene when the particle size of raw graphite reduces.« less

Enhanced performance of graphite anode materials by AlF3 coating for lithium-ion batteries

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

Ding, Fei; Xu, Wu; Choi, Daiwon

2012-04-27

In order to form the stable surface film and to further enhance the long-term cycling stability of the graphite anodes of lithium-ion batteries, the surface of graphite powders has been modified by AlF3 coating through chemical precipitation method. The AlF3-coated graphite shows no evident changes in the bulk structure and a thin AlF3-coating layer of about 2 nm thick is found to uniformly cover the graphite particles with 2 wt% AlF3 content. However, it delivers a higher initial discharge capacity and largely improved rate performances compared to the pristine graphite. Remarkably, AlF3 coated graphite demonstrated a much better cycle life.more » After 300 cycles, AlF3 coated graphite and uncoated graphite show capacity retention of 92% and 81%, respectively. XPS measurement shows that a more conductive solid electrode interface (SEI) layer was formed on AlF3 coated graphite as compared to uncoated graphite. SEM monograph also reveals that the AlF3-coated graphite particles have a much more stable surface morphology after long-term cycling. Therefore, the improved electrochemical performance of AlF3 coated graphite can be attributed to a more stable and conductive SEI formed on coated graphite anode during cycling process.« less

Graphite

USGS Publications Warehouse

Robinson, Gilpin R.; Hammarstrom, Jane M.; Olson, Donald W.; Schulz, Klaus J.; DeYoung,, John H.; Seal, Robert R.; Bradley, Dwight C.

2017-12-19

Graphite is a form of pure carbon that normally occurs as black crystal flakes and masses. It has important properties, such as chemical inertness, thermal stability, high electrical conductivity, and lubricity (slipperiness) that make it suitable for many industrial applications, including electronics, lubricants, metallurgy, and steelmaking. For some of these uses, no suitable substitutes are available. Steelmaking and refractory applications in metallurgy use the largest amount of produced graphite; however, emerging technology uses in large-scale fuel cell, battery, and lightweight high-strength composite applications could substantially increase world demand for graphite.Graphite ores are classified as “amorphous” (microcrystalline), and “crystalline” (“flake” or “lump or chip”) based on the ore’s crystallinity, grain-size, and morphology. All graphite deposits mined today formed from metamorphism of carbonaceous sedimentary rocks, and the ore type is determined by the geologic setting. Thermally metamorphosed coal is the usual source of amorphous graphite. Disseminated crystalline flake graphite is mined from carbonaceous metamorphic rocks, and lump or chip graphite is mined from veins in high-grade metamorphic regions. Because graphite is chemically inert and nontoxic, the main environmental concerns associated with graphite mining are inhalation of fine-grained dusts, including silicate and sulfide mineral particles, and hydrocarbon vapors produced during the mining and processing of ore. Synthetic graphite is manufactured from hydrocarbon sources using high-temperature heat treatment, and it is more expensive to produce than natural graphite.Production of natural graphite is dominated by China, India, and Brazil, which export graphite worldwide. China provides approximately 67 percent of worldwide output of natural graphite, and, as the dominant exporter, has the ability to set world prices. China has significant graphite reserves, and China’s graphite production is expected to increase, although rising labor costs and some mine production problems are developing. China is expected to continue to be the dominant exporter for the near future. Mexico and Canada export graphite mainly to the United States, which has not had domestic production of natural graphite since the 1950s. Most graphite deposits in the United States are too small, low-grade, or remote to be of commercial value in the near future, and the likelihood of discovering larger, higher-grade, or favorably located domestic deposits is unlikely. The United States is a major producer of synthetic graphite.

Strategic graphite, a survey

USGS Publications Warehouse

Cameron, Eugene N.; Weis, Paul L.

1960-01-01

Strategic graphite consists of certain grades of lump and flake graphite for which the United States is largely or entirely dependent on sources abroad. Lump graphite of high purity, necessary in the manufacture of carbon brushes, is imported from Ceylon, where it occurs in vein deposits. Flake graphite, obtained from deposits consisting of graphite disseminated in schists and other metamorphic rocks, is an essential ingredient of crucibles used in the nonferrous metal industries and in the manufacture of lubricants and packings. High-quality flake graphite for these uses has been obtained mostly from Madagascar since World War I. Some flake graphite of strategic grade has been produced, however, from deposits in Texas, Alabama, and Pennsylvania. The development of the carbon-bonded crucible, which does not require coarse flake, should lessen the competitive advantage of the Madagascar producers of crucible flake. Graphite of various grades has been produced intermittently in the United States since 1644. The principal domestic deposits of flake graphite are in Texas, Alabama, Pennsylvania, and New York. Reserves of flake graphite in these four States are very large, but production has been sporadic and on the whole unprofitable since World War I, owing principally to competition from producers in Madagascar. Deposits in Madagascar are large and relatively high in content of flake graphite. Production costs are low and the flake produced is of high quality. Coarseness of flake and uniformity of the graphite products marketed are cited as major advantages of Madagascar flake. In addition, the usability of Madagascar flake for various purposes has been thoroughly demonstrated, whereas the usability of domestic flake for strategic purposes is still in question. Domestic graphite deposits are of five kinds: deposits consisting of graphite disseminated in metamorphosed siliceous sediments, deposits consisting of graphite disseminated in marble, deposits formed by thermal or dynamothermal metamorphism of coal beds or other highly carbonaceous sediments, vein deposits, and contact metasomatic deposits in marble. Only the first kind comprises deposits sufficiently large and rich in flake graphite to be significant potential sources of strategic grades of graphite. Vein deposits in several localities are known, but none is known to contain substantial reserves of graphite of strategic quality.Large resources of flake graphite exist in central Texas, in northeastern Alabama, in eastern Pennsylvania, and in the eastern Adirondack Mountains of New York. Tonnages available, compared with the tonnages of flake graphite consumed annually in the United States, are very large. There have been indications that flake graphite from Texas, Alabama, and Pennsylvania can be used in clay-graphite crucibles as a substitute for Madagascar flake, and one producer has made progress in establishing markets for his flake products as ingredients of lubricants. The tonnages of various commercial grades of graphite recoverable from various domestic deposits, however, have not been established; hence, the adequacy of domestic resources of graphite in a time of emergency is not known.The only vein deposits from which significant quantities of lump graphite have been produced are those of the Crystal Graphite mine, Beaverhead County, Mont. The deposits are fracture fillings in Precambrian gneiss and pegmatite. Known reserves in the deposits are small. In Texas, numerous flake-graphite deposits occur in the Precambrian Packsaddle schist in Llano and Burnet Counties. Graphite disseminated in certain parts of this formation ranges from extremely fine to medium grained. The principal producer has been the mine of the Southwestern Graphite Co., west of the town of Burnet. Substantial reserves of medium-grained graphite are present in the deposit mined by the company. In northeastern Alabama, flake-graphite deposits occur in the Ashland mica schist in two belts that trend northeastward across Clay, Goosa, and Chilton Counties. The northeastern belt has been the most productive. About 40 mines have been operated at one time or another, but only a few have been active during or since World War I. The deposits consist of flake graphite disseminated in certain zones or "leads" consisting of quartz-mica-feldspar schists and mica quartzite. Most of past production has come from the weathered upper parts of the deposits, but unweathered rock has been mined at several localities. Reserves of weathered rock containing 3 to 5 percent graphite are very large, and reserves of unweathered rock are even greater. Flake graphite deposits in Chester County, Pa., have been worked intermittently since about 1890. The deposits consist of medium- to coarse-grained graphite disseminated in certain belts of the Pickering gneiss. The most promising deposit is one worked in the Benjamin Franklin and the Eynon Just mines. Reserves of weathered rock containing 1.5 percent graphite are of moderate size; reserves of unweathered rock are large. In the eastern Adirondack Mountains in New York there are two principal kinds of flake-graphite deposits: contact-metasomatic deposits and those consisting of flake graphite disseminated in quartz schist. The contact-metasomatic deposits are small, irregular, and very erratic in graphite content. The deposits in quartz schist are very large, persistent, and uniform in grade. There are large reserves of schist containing 3 to 5 percent graphite, but the graphite is relatively fine grained.

Thermal stability of Cu-Cr-Zr alloy processed by equal-channel angular pressing

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

Abib, Khadidja

Thermal stability of a Cu-Cr-Zr alloy processed by equal-channel angular pressing up to16 passes was investigated using isochronal annealing ranging from 250 to 850 °C for 1 h. The microstructure, crystallographic texture and micro hardness of samples were characterized through electron back scatter diffraction and Vickers micro hardness measurements. The recrystallized grain size was stable between 250 °C and 500 °C then increased quickly. The achieved mean grain size, after 1, 4 and 16 ECAP passes, was around 5.5 μm. A discontinuous mode of recrystallization was found to occur and a Particle Simulated Nucleation mechanism was evidenced. The evolution ofmore » the high angle grain boundary fraction increased notably after annealing above 550 °C. The crystallographic texture after isochronal annealing was similar to that of ECAP simple shear, no change of the texture during annealing was observed but only slight intensity variations. Micro hardness of all Cu–Cr–Zr samples showed a hardening with two peaks at 400 and 500 °C associated with precipitation of Cu cluster and Cu{sub 5}Zr phase respectively, followed by a subsequent softening upon increasing the annealing temperature due to recrystallization. - Highlight: •The Cu-1Cr-0.1Zr alloy shows a very good thermal stability up to 550 °C after ECAP. •A discontinuous recrystallization was found to occur and PSN mechanism was evidenced. •The annealing texture was found weak and some new components appear. •Hardening is attributed to the Cr clustering followed by the Cu{sub 51}Zr{sub 14} precipitation. •Softening is a result of recrystallization and grain growth progressing.« less

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Through-process characterization of local anisotropy of Non-oriented electrical steel using magnetic Barkhausen noise

NASA Astrophysics Data System (ADS)

He, Youliang; Mehdi, Mehdi; Hilinski, Erik J.; Edrisy, Afsaneh

2018-05-01

Magnetic Barkhausen noise (MBN) signals were measured on a non-oriented electrical steel through all the thermomechanical processing stages, i.e. hot rolling, hot band annealing, cold rolling and final annealing. The temperature of the final annealing was varied from 600 °C to 750 °C so that the steel consisted of partially or completely recrystallized microstructures and different levels of residual stresses. The angular MBNrms (root mean square) values were compared to the texture factors in the same directions, the latter being calculated from the crystallographic texture measured by electron backscatter diffraction (EBSD). It was found that, in the cold-rolled, hot-rolled and completely recrystallized steels, the angular MBNrms followed a cosine function with respect to the angle of magnetization, while in partially recrystallized state such a relation does not exist. After cold rolling, the maximum MBNrms was observed in the rolling direction (RD) and the minimum MBNrms was in the transverse direction (TD), which was inconsistent with the magnetocrystalline anisotropy as indicated by the texture factor. After hot rolling, the maximum and minimum MBNrms values were observed in the TD and RD, respectively, exactly opposite to the cold-rolled state. If the steel was completely recrystallized, the maximum MBNrms was normally observed at a direction that was 15-30° from the minimum texture factor. If the steel was partially recrystallized, both the magnetocrystalline anisotropy of the material and the residual stress contributed to the angular MBNrms, which resulted in the deviation of the relationship from a cosine function. The relative strength of the two factors determined which factor would dominate the overall magnetic anisotropy.

Analysis of soft magnetic materials by electron backscatter diffraction as a powerful tool

NASA Astrophysics Data System (ADS)

Schuller, David; Hohs, Dominic; Loeffler, Ralf; Bernthaler, Timo; Goll, Dagmar; Schneider, Gerhard

2018-04-01

The current work demonstrates that electron backscatter diffraction (EBSD) is a powerful and versatile characterization technique for investigating soft magnetic materials. The properties of soft magnets, e.g., magnetic losses strongly depend on the materials chemical composition and microstructure, including grain size and shape, texture, degree of plastic deformation and elastic strain. In electrical sheet stacks for e-motor applications, the quality of the machined edges/surfaces of each individual sheet is of special interest. Using EBSD, the influence of the punching process on the microstructure at the cutting edge is quantitatively assessed by evaluating the crystallographic misorientation distribution of the deformed grains. Using an industrial punching process, the maximum affected deformation depth is determined to be 200 - 300 μm. In the case of laser cutting, the affected deformation depth is determined to be approximately zero. Reliability and detection limits of the developed EBSD approach are evaluated on non-affected sample regions and model samples containing different indentation test bodies. A second application case is the investigation of the recrystallization process during the annealing step of soft magnetic composites (SMC) toroids produced by powder metallurgy as a function of compaction pressure, annealing parameters and powder particle size. With increasing pressure and temperature, the recrystallized area fraction (e.g., grains with crystallographic misorientations < 3°) increases from 71 % (200 MPa, 800°C) to 90% (800 MPa, 800°C). Recrystallization of the compacted powder material starts at the particle boundaries or areas with existing plastic deformation. The progress of recrystallization is visualized as a function of time and of different particle to grain size distributions. Here, large particles with coarse internal grain structures show a favorable recrystallization behavior which results in large bulk permeability of up to 600 - 700 and lower amount of residual misorientations (>3°).

Uptake of Ra during the recrystallization of barite: a microscopic and time of flight-secondary ion mass spectrometry study.

PubMed

Klinkenberg, Martina; Brandt, Felix; Breuer, Uwe; Bosbach, Dirk

2014-06-17

A combined macroscopic and microanalytical approach was applied on two distinct barite samples from Ra uptake batch experiments using time of flight-secondary ion mass spectrometry (ToF-SIMS) and detailed scanning electron microscopy (SEM) investigations. The experiments were set up at near to equilibrium conditions to distinguish between two possible scenarios for the uptake of Ra by already existent barite: (1) formation of a Ba1-xRaxSO4 solid solution surface layer on the barite or (2) a complete recrystallization, leading to homogeneous Ba1-xRaxSO4 crystals. It could be clearly shown that Ra uptake in all barite particles analyzed within this study is not limited to the surface but extends to the entire solid. For most grains a homogeneous distribution of Ra could be determined, indicating a complete recrystallization of barite into a Ba1-xRaxSO4 solid solution. The maxima of the Ra/Ba intensity ratio distribution histograms calculated from ToF-SIMS are identical with the expected Ra/Ba ratios calculated from mass balance assuming a complete recrystallization. In addition, the role of Ra during the recrystallization of barite was examined via detailed SEM investigations. Depending on the type of barite used, an additional coarsening effect or a strong formation of oriented aggregates was observed compared to blank samples without Ra. In conclusion, the addition of Ra to a barite at close to equilibrium conditions has a major impact on the system leading to a fast re-equilibration of the solid to a Ba1-xRaxSO4 solid solution and visible effects on the particle size distribution, even at room temperature.

Graphite grain-size spectrum and molecules from core-collapse supernovae

NASA Astrophysics Data System (ADS)

Clayton, Donald D.; Meyer, Bradley S.

2018-01-01

Our goal is to compute the abundances of carbon atomic complexes that emerge from the C + O cores of core-collapse supernovae. We utilize our chemical reaction network in which every atomic step of growth employs a quantum-mechanically guided reaction rate. This tool follows step-by-step the growth of linear carbon chain molecules from C atoms in the oxygen-rich C + O cores. We postulate that once linear chain molecules reach a sufficiently large size, they isomerize to ringed molecules, which serve as seeds for graphite grain growth. We demonstrate our technique for merging the molecular reaction network with a parallel program that can follow 1017 steps of C addition onto the rare seed species. Due to radioactivity within the C + O core, abundant ambient oxygen is unable to convert C to CO, except to a limited degree that actually facilitates carbon molecular ejecta. But oxygen severely minimizes the linear-carbon-chain abundances. Despite the tiny abundances of these linear-carbon-chain molecules, they can give rise to a small abundance of ringed-carbon molecules that serve as the nucleations on which graphite grain growth builds. We expand the C + O-core gas adiabatically from 6000 K for 109 s when reactions have essentially stopped. These adiabatic tracks emulate the actual expansions of the supernova cores. Using a standard model of 1056 atoms of C + O core ejecta having O/C = 3, we calculate standard ejection yields of graphite grains of all sizes produced, of the CO molecular abundance, of the abundances of linear-carbon molecules, and of Buckminsterfullerene. None of these except CO was expected from the C + O cores just a few years past.

CMB-13 research on carbon and graphite

NASA Technical Reports Server (NTRS)

Smith, M. C.

1972-01-01

Preliminary results of the research on carbon and graphite accomplished during this report period are presented. Included are: particle characteristics of Santa Maria fillers, compositions and density data for hot-molded Santa Maria graphites, properties of hot-molded Santa Maria graphites, and properties of hot-molded anisotropic graphites. Ablation-resistant graphites are also discussed.

METHOD OF FABRICATING A GRAPHITE MODERATED REACTOR

DOEpatents

Kratz, H.R.

1963-05-01

S>A nuclear reactor formed of spaced bodies of uranium and graphite blocks is improved by diffusing helium through the graphite blocks in order to replace the air in the pores of the graphite with helium. The helium-impregnated graphite conducts heat better, and absorbs neutrons less, than the original air- impregnated graphite. (AEC)

Development of Ti microalloyed high strength steel plate by controlling thermo-mechanical control process schedule

NASA Astrophysics Data System (ADS)

Xia, Jinian; Huo, Xiangdong; Li, Liejun; Peng, Zhengwu; Chen, Songjun

2017-12-01

In this study, the TMCP parameters including non-recrystallization temperature (Tnr) and optimal isothermal temperature were determined by thermal simulation experiments, and a new Ti microalloyed high strength steel plate was developed by controlling thermo-mechanical control process (TMCP) schedule. The effects of TMCP process on microstructural features, precipitation behavior and mechanical properties of Ti microalloyed high strength steel plate were investigated. The results revealed that the double-stage rolling process consist of rolling in the γ recrystallization region and the γ non-recrystallization region was benefical to promoting the mechanical properties of Ti microalloyed steel by achieving grain refinement. It was also found that large amounts of fine TiC (<10 nm) particles were precipitated during the isothermal treatment at 600 °C, which generated a 215 MPa precipitation strengthening effect.

The Microstructure and Gamma Prime Distributions in Inertia Friction Welded Joint of P/M Superalloy FGH96

NASA Astrophysics Data System (ADS)

Zhang, Chi; Shen, Wenfei; Zhang, Liwen; Xia, Yingnan; Li, Ruiqin

2017-04-01

A gamma prime ( γ') precipitation ( 35% in volume)-hardened powder metallurgy (P/M) superalloy FGH96 was welded using inertia friction welding (IFW). The microstructure and γ' distributions in the joints in two conditions, hot isostatic pressed state and solution-treated and aged state, were characterized. The recrystallization of grains, the dissolution and re-precipitation of γ' in the joints were discussed in terms of the temperature evolutions which were calculated by finite element model analysis. Regardless of the initial states, fully recrystallized fine grain structure formed at welded zone. Meanwhile, very fine γ' precipitations were re-precipitated at the welded zone. These recrystallized grain structure and fine re-precipitated γ' resulted in increasing hardness of IFW joint while making the hardness dependent on the microstructure and γ' precipitation.

Decoration of Chondroitin Polysaccharide with Threonine: Synthesis, Conformational Study, and Ice-Recrystallization Inhibition Activity.

PubMed

Laezza, Antonio; Casillo, Angela; Cosconati, Sandro; Biggs, Caroline I; Fabozzi, Antonio; Paduano, Luigi; Iadonisi, Alfonso; Novellino, Ettore; Gibson, Matthew I; Randazzo, Antonio; Corsaro, Maria M; Bedini, Emiliano

2017-08-14

Several threonine (Thr)- and alanine (Ala)-rich antifreeze glycoproteins (AFGPs) and polysaccharides act in nature as ice recrystallization inhibitors. Among them, the Thr-decorated capsular polysaccharide (CPS) from the cold-adapted Colwellia psychrerythraea 34H bacterium was recently investigated for its cryoprotectant activity. A semisynthetic mimic thereof was here prepared from microbial sourced chondroitin through a four-step strategy, involving a partial protection of the chondroitin polysaccharide as a key step for gaining an unprecedented quantitative amidation of its glucuronic acid units. In-depth NMR and computational analysis suggested a fairly linear conformation for the semisynthetic polysaccharide, for which the antifreeze activity by a quantitative ice recrystallization inhibition assay was measured. We compared the structure-activity relationships for the Thr-derivatized chondroitin and the natural Thr-decorated CPS from C. psychrerythraea.

Role of Y-Al Oxides During Extended Recovery Process of a Ferritic ODS Alloy

NASA Astrophysics Data System (ADS)

Capdevila, C.; Pimentel, G.; Aranda, M. M.; Rementeria, R.; Dawson, K.; Urones-Garrote, E.; Tatlock, G. J.; Miller, M. K.

2015-08-01

The microstructural stability of Y-Al oxides during the recrystallization of Fe-Cr-Al oxide dispersion strengthened alloy is studied in this work. The goal is to determine the specific distribution pattern of oxides depending where they are located: in the matrix or at the grain boundaries. It was concluded that those located at the grain boundaries yielded a faster coarsening than the ones in the matrix, although no significant differences in composition and/or crystal structure were observed. However, the recrystallization heat treatment leads to the dissolution of the Y2O3 and its combination with Al to form the YAlO3 perovskite oxide particles process, mainly located at the grain boundaries. Finally, atom probe tomography analysis revealed a significant Ti build-up at the grain boundaries that might affect subsequent migration during recrystallization.

AGC-2 Irradiation Report

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

Rohrbaugh, David Thomas; Windes, William; Swank, W. David

The Next Generation Nuclear Plant (NGNP) will be a helium-cooled, very high temperature reactor (VHTR) with a large graphite core. In past applications, graphite has been used effectively as a structural and moderator material in both research and commercial high temperature gas cooled reactor (HTGR) designs.[ , ] Nuclear graphite H 451, used previously in the United States for nuclear reactor graphite components, is no longer available. New nuclear graphites have been developed and are considered suitable candidates for the new NGNP reactor design. To support the design and licensing of NGNP core components within a commercial reactor, a completemore » properties database must be developed for these current grades of graphite. Quantitative data on in service material performance are required for the physical, mechanical, and thermal properties of each graphite grade with a specific emphasis on data related to the life limiting effects of irradiation creep on key physical properties of the NGNP candidate graphites. Based on experience with previous graphite core components, the phenomenon of irradiation induced creep within the graphite has been shown to be critical to the total useful lifetime of graphite components. Irradiation induced creep occurs under the simultaneous application of high temperatures, neutron irradiation, and applied stresses within the graphite components. Significant internal stresses within the graphite components can result from a second phenomenon—irradiation induced dimensional change. In this case, the graphite physically changes i.e., first shrinking and then expanding with increasing neutron dose. This disparity in material volume change can induce significant internal stresses within graphite components. Irradiation induced creep relaxes these large internal stresses, thus reducing the risk of crack formation and component failure. Obviously, higher irradiation creep levels tend to relieve more internal stress, thus allowing the components longer useful lifetimes within the core. Determining the irradiation creep rates of nuclear grade graphites is critical for determining the useful lifetime of graphite components and is a major component of the Advanced Graphite Creep (AGC) experiment.« less

Stable dispersions of polymer-coated graphitic nanoplatelets

NASA Technical Reports Server (NTRS)

Nguyen, Sonbinh T. (Inventor); Stankovich, Sasha (Inventor); Ruoff, Rodney S. (Inventor)

2011-01-01

A method of making a dispersion of reduced graphite oxide nanoplatelets involves providing a dispersion of graphite oxide nanoplatelets and reducing the graphite oxide nanoplatelets in the dispersion in the presence of a reducing agent and a polymer. The reduced graphite oxide nanoplatelets are reduced to an extent to provide a higher C/O ratio than graphite oxide. A stable dispersion having polymer-treated reduced graphite oxide nanoplatelets dispersed in a dispersing medium, such as water or organic liquid is provided. The polymer-treated, reduced graphite oxide nanoplatelets can be distributed in a polymer matrix to provide a composite material.