Numerical and Experimental Study of Ti6Al4V Components Manufactured Using Powder Bed Fusion Additive Manufacturing

NASA Astrophysics Data System (ADS)

Zielinski, Jonas; Mindt, Hans-Wilfried; Düchting, Jan; Schleifenbaum, Johannes Henrich; Megahed, Mustafa

2017-12-01

Powder bed fusion additive manufacturing of titanium alloys is an interesting manufacturing route for many applications requiring high material strength combined with geometric complexity. Managing powder bed fusion challenges, including porosity, surface finish, distortions and residual stresses of as-built material, is the key to bringing the advantages of this process to production main stream. This paper discusses the application of experimental and numerical analysis towards optimizing the manufacturing process of a demonstration component. Powder characterization including assessment of the reusability, assessment of material consolidation and process window optimization is pursued prior to applying the identified optima to study the distortion and residual stresses of the demonstrator. Comparisons of numerical predictions with measurements show good correlations along the complete numerical chain.

(ZrO 2) 0.85( REO 1.5) 0.15 ( RE=Sc, Y) solid solutions prepared via three Pechini-type gel routes: 1—gel formation and calcination behaviors

NASA Astrophysics Data System (ADS)

Zhang, Yawen; Li, Ang; Yan, Zhengguang; Xu, Gang; Liao, Chunsheng; Yan, Chunhua

2003-02-01

(ZrO2)0.85(REO1.5)0.15 (RE=Sc, Y) nanoparticles with pure cubic fluorite structure have been synthesized by three Pechini-type gel routes, viz. poly(vinyl alcohol) containing-process (route I), poly(ethylene glycol) and formic acid-containing process (route II), and in situ polymerizable complex method (route III). The coordination modes between metal ions and polymers in the gels are shown to be highly correlative with the synthesis route used. The gels prepared by route III have the strongest coordination throughout their network and therefore the best chemical homogeneity. The altered variety of polymer and cross-linking within the gels adopted by these three routes has made the as-synthesized samples show appreciable differences in thermal behavior, powder reactivity and nanoparticle properties.

A polymer solution technique for the synthesis of nano-sized Li 2TiO 3 ceramic breeder powders

NASA Astrophysics Data System (ADS)

Jung, Choong-Hwan; Lee, Sang Jin; Kriven, Waltraud M.; Park, Ji-Yeon; Ryu, Woo-Seog

2008-02-01

Nano-sized Li 2TiO 3 powder was fabricated by an organic-inorganic solution route. A steric entrapment route employing ethylene glycol was used for the preparation of the nano-sized Li 2TiO 3 particles. Titanium isopropoxide and lithium nitrate were dissolved in liquid-type ethylene glycol without any precipitation. With the optimum amount of the polymer, the metal cations (Li and Ti) were dispersed in the solution and a homogeneous polymeric network was formed. The organic-inorganic precursor gels were turned to crystalline powders through an oxidation reaction during a calcination process. The dried precursor gel showed the carbon-free Li 2TiO 3 crystalline form which was observed above 400 °C. The primary particle size of the carbon-free Li 2TiO 3 was about 70 nm, and the structure of the crystallized powder was porous and agglomerated. The powder compact was densified to 92% of TD at a relatively low sintering temperature of 1100 °C for 2 h.

Effects of microstructures on the performance of rare-earth-free MnBi magnetic materials and magnets

NASA Astrophysics Data System (ADS)

Nguyen, Vuong Van; Nguyen, Truong Xuan

2018-03-01

Since the solidification of MnBi alloys is peritectic, their microstructures always consist of the starting phases of Mn and Bi and the productive phase MnBi. The high performance of MnBi bulk magnets requires appropriate routes of preparing MnBi powders of high spontaneous magnetization Ms and large coercivity iHc as well a route of producing bulk magnets thereof. In these routes, the microstructures of arc-melted alloys, annealed alloys and magnets strongly related to the quality of powders and the performance of magnets. The paper proves that: i) The microstructure of fine Mn-inclusions embedded in the matrix of Bi is preferred for arc-melted alloys to realize the rapid evolution of the ferromagnetic phase inside them during their sequent annealing process; ii) The time-controlled annealing process plays a key role in controlling the microstructure with the main ferromagnetic phase matrix, in which the rest of Mn and the Bi accumulations are embedded; iii) The cold (in-liquid-nitrogen) ball milling annealed alloys is required for preparing a high quality powders with the preferred sub-micrometer microstructure without a Bi-decomposition; iv) The short-time warm compaction is crucial to fabricate dense, highly textured bulk magnets with the micrometer microstructure. The realization and control of these preferred microstructures figured in these routes enhance the chance of preparing MnBi bulk magnets with the energy product (BH)max larger than 8 MGOe.

Effect of Processing Route on Strain Controlled Low Cycle Fatigue Behavior of Polycrystalline NiAl

NASA Technical Reports Server (NTRS)

Rao, K. Bhanu Sankara; Lerch, B. A.; Noebe, R. D.

1995-01-01

The present investigation examines the effects of manufacturing process on the total axial strain controlled low cycle fatigue behavior of polycrystalline NiAl at 1000 K, a temperature above the monotonic Brittle-to-Ductile Transition Temperature (BDTT). The nickel aluminide samples were produced by three different processing routes: hot isostatic pressing of pre- alloyed powders, extrusion of prealloyed powders, and extrusion of vacuum induction melted ingots. The LCF behavior of the cast plus extruded material was also determined at room temperature (below the BD77) for comparison to the high temperature data. The cyclic stress response, cyclic stress-strain behavior, and strain-life relationships were influenced by the alloy preparation technique and the testing temperature. Detailed characterization of the LCF tested samples was conducted by optical and electron microscopy to determine the variations in fracture and deformation modes and to determine any microstructural changes that occurred during LCF testing. The dependence of LCF properties on processing route was rationalized on the basis of starting microstructure, brittle-to-ductile transition temperature, deformation induced changes in the basic microstructure, deformation substructure, and synergistic interaction between the damage modes.

Characterization of SrCo1.5Ti1.5Fe9O19 hexagonal ferrite synthesized by sol-gel combustion and solid state route

NASA Astrophysics Data System (ADS)

Vinaykumar, R.; Mazumder, R.; Bera, J.

2017-05-01

Co-Ti co-substituted SrM hexagonal ferrite (SrCo1.5Ti1.5Fe9O19) was synthesized by sol-gel combustion and solid state route. The effects of sources of TiO2 raw materials; titanium tetra-isopropoxide (TTIP) and titanyl nitrate (TN) on the phase formation behavior and properties of the ferrite were studied. The thermal decomposition behavior of the gel was studied using TG-DSC. The phase formation behavior of the ferrite was studied by using X-ray powder diffraction and FTIR analysis. Phase formation was comparatively easier in the TN-based sol-gel process. The morphology of powder and sintered ferrite was investigated using scanning electron microscope. Magnetic properties like magnetization, coercivity, permeability, tan δμ and dielectric properties were investigated. The ferrite synthesized by sol-gel based chemical route showed higher saturation magnetization, permeability and permittivity compared to the ferrite synthesized by solid state route.

Raman and dielectric studies of GdMnO3 bulk ceramics synthesized from nano powders

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Roul, B. K.

2017-05-01

Nanocrystalline GdMnO3 (GMO) powders has been synthesized by a simple chemical route i. e. pyrophoric reaction technique and then sintered in the form of bulk pellet at 850°C for 24 hours by adopting slow step sintering schedule. It is observed that by reducing the particles size, chemical route enhances the mixing process as well as decreasing the sintering temperature to get single phase material system in compared to the polycrystalline sample prepared directly from the micron sized commercial powder. Raman spectroscopic studies confirm that the sample is in single phase without any detectable impurity. Frequency dependent dielectric properties i.e., dielectric constant (K) and dielectric loss (tanδ) of GMO ceramics sintered at 850°C for 24 hours were studied at room temperature. The sample showed high K value (˜2736) in the frequency of 100 Hz at room temperature.

Development of Duplex Stainless Steels by Field-Assisted Hot Pressing: Influence of the Particle Size and Morphology of the Powders on the Final Mechanical Properties

NASA Astrophysics Data System (ADS)

García-Junceda, A.; Rincón, M.; Torralba, J. M.

2018-01-01

The feasibility of processing duplex stainless steels with promising properties using a powder metallurgical route, including the consolidation by field-assisted hot pressing, is assessed in this investigation. The influence of the particle size and morphology of the raw austenitic and ferritic powders on the final microstructure and properties is also evaluated for an austenitic content of 60 wt pct. In addition, the properties of a new microconstituent generated between the initial constituents are analyzed. The maximum sintered density (98.9 pct) and the best mechanical behavior, in terms of elastic modulus, nanohardness, yield strength, ultimate tensile strength, and ductility, are reached by the duplex stainless steel processed with austenitic and ferritic gas atomized stainless steel powders.

Development of Impregnated Agglomerate Pelletization (IAP) process for fabrication of (Th,U)O 2 mixed oxide pellets

NASA Astrophysics Data System (ADS)

Khot, P. M.; Nehete, Y. G.; Fulzele, A. K.; Baghra, Chetan; Mishra, A. K.; Afzal, Mohd.; Panakkal, J. P.; Kamath, H. S.

2012-01-01

Impregnated Agglomerate Pelletization (IAP) technique has been developed at Advanced Fuel Fabrication Facility (AFFF), BARC, Tarapur, for manufacturing (Th, 233U)O 2 mixed oxide fuel pellets, which are remotely fabricated in hot cell or shielded glove box facilities to reduce man-rem problem associated with 232U daughter radionuclides. This technique is being investigated to fabricate the fuel for Indian Advanced Heavy Water Reactor (AHWR). In the IAP process, ThO 2 is converted to free flowing spheroids by powder extrusion route in an unshielded facility which are then coated with uranyl nitrate solution in a shielded facility. The dried coated agglomerate is finally compacted and then sintered in oxidizing/reducing atmosphere to obtain high density (Th,U)O 2 pellets. In this study, fabrication of (Th,U)O 2 mixed oxide pellets containing 3-5 wt.% UO 2 was carried out by IAP process. The pellets obtained were characterized using optical microscopy, XRD and alpha autoradiography. The results obtained were compared with the results for the pellets fabricated by other routes such as Coated Agglomerate Pelletization (CAP) and Powder Oxide Pelletization (POP) route.

Review of the Methods for Production of Spherical Ti and Ti Alloy Powder

NASA Astrophysics Data System (ADS)

Sun, Pei; Fang, Zhigang Zak; Zhang, Ying; Xia, Yang

2017-10-01

Spherical titanium alloy powder is an important raw material for near-net-shape fabrication via a powder metallurgy (PM) manufacturing route, as well as feedstock for powder injection molding, and additive manufacturing (AM). Nevertheless, the cost of Ti powder including spherical Ti alloy has been a major hurdle that prevented PM Ti from being adopted for a wide range of applications. Especially with the increasing importance of powder-bed based AM technologies, the demand for spherical Ti powder has brought renewed attention on properties and cost, as well as on powder-producing processes. The performance of Ti components manufactured from powder has a strong dependence on the quality of powder, and it is therefore crucial to understand the properties and production methods of powder. This article aims to provide a cursory review of the basic techniques of commercial and emerging methods for making spherical Ti powder. The advantages as well as limitations of different methods are discussed.

The role of yttrium and titanium during the development of ODS ferritic steels obtained through the STARS route: TEM and XAS study

NASA Astrophysics Data System (ADS)

Ordás, Nerea; Gil, Emma; Cintins, Arturs; de Castro, Vanessa; Leguey, Teresa; Iturriza, Iñigo; Purans, Juris; Anspoks, Andris; Kuzmin, Alexei; Kalinko, Alexandr

2018-06-01

Oxide Dispersion Strengthened Ferritic Steels (ODS FS) are candidate materials for structural components in future fusion reactors. Their high strength and creep resistance at elevated temperatures and their good resistance to neutron radiation damage is obtained through extremely fine microstructures containing a high density of nanometric precipitates, generally yttrium and titanium oxides. This work shows transmission electron microscopy (TEM) and extended X-ray absorption fine structure (EXAFS) characterization of Fe-14Cr-2W-0.3Ti-0.24Y ODS FS obtained by the STARS route (Surface Treatment of gas Atomized powder followed by Reactive Synthesis), an alternative method to obtain ODS alloys that avoids the mechanical alloying to introduce Y2O3 powder particles. In this route, FS powders already containing Ti and Y, precursors of the nanometric oxides, are obtained by gas atomization. Then, a metastable Cr- and Fe-rich oxide layer is formed on the surface of the powder particles. During consolidation by HIP at elevated temperatures, and post-HIP heat treatments above the HIP temperature, this oxide layer at Prior Particle Boundaries (PPBs) dissociates, the oxygen diffuses, and Y-Ti-O nano-oxides precipitate in the ferritic matrix. TEM characterization combined with XAFS and XANES analyses have proven to be suitable tools to follow the evolution of the nature of the different oxides present in the material during the whole processing route and select appropriate HIP and post-HIP parameters to promote profuse and fine Y-Ti-O nanometric precipitates.

A new powder production route for transparent spinel windows: powder synthesis and window properties

NASA Astrophysics Data System (ADS)

Cook, Ronald; Kochis, Michael; Reimanis, Ivar; Kleebe, Hans-Joachim

2005-05-01

Spinel powders for the production of transparent polycrystalline ceramic windows have been produced using a number of traditional ceramic and sol-gel methods. We have demonstrated that magnesium aluminate spinel powders produced from the reaction of organo-magnesium compounds with surface modified boehmite precursors can be used to produce high quality transparent spinel parts. The new powder production method allows fine control over the starting particle size, size distribution, purity and stoichiometry. The new process involves formation of a boehmite sol-gel from the hydrolysis of aluminum alkoxides followed by surface modification of the boehmite nanoparticles using carboxylic acids. The resulting surface modified boehmite nanoparticles can then be metal exchanged at room temperature with magnesium acetylacetonate to make a precursor powder that is readily transformed into pure phase spinel.

Innovative technologies for powder metallurgy-based disk superalloys: Progress and proposal

NASA Astrophysics Data System (ADS)

Chong-Lin, Jia; Chang-Chun, Ge; Qing-Zhi, Yan

2016-02-01

Powder metallurgy (PM) superalloys are an important class of high temperature structural materials, key to the rotating components of aero engines. In the purview of the present challenges associated with PM superalloys, two novel approaches namely, powder preparation and the innovative spray-forming technique (for making turbine disk) are proposed and studied. Subsequently, advanced technologies like electrode-induction-melting gas atomization (EIGA), and spark-plasma discharge spheroidization (SPDS) are introduced, for ceramic-free superalloy powders. Presently, new processing routes are sought after for preparing finer and cleaner raw powders for disk superalloys. The progress of research in spray-formed PM superalloys is first summarized in detail. The spray-formed superalloy disks specifically exhibit excellent mechanical properties. This paper reviews the recent progress in innovative technologies for PM superalloys, with an emphasis on new ideas and approaches, central to the innovation driving techniques like powder processing and spray forming. Project supported by the National Natural Science Foundation of China (Grant Nos. 50974016 and 50071014).

The Effect of Particles Shape and Size on Feedstock Flowibility and Chemical content of As-sintered NiTi Alloys

NASA Astrophysics Data System (ADS)

Kadir, R. A. Abdul; Razali, R.; Mohamad Nor, N. H.; Subuki, I.; Ismail, M. H.

2018-05-01

This paper presents a comparative study of two different titanium powders in fabrication of NiTi alloys by metal injection moulding (MIM) route. Two batches of powder mixture consisted of Ni-Ti and Ni-TiH2 with atomic ratio (at%) of 50-50 were prepared. TiH2 powder was used as a substitution for pure Ti powder owing to its relatively cheaper cost and has been claimed favourable in producing less impurity uptake in sintering process. The binder system used for both mixtures comprised of composite binder of palm stearin (PS) and polyethylene (PE) at weigth ratio (wt%) of 60-40. The flow behaviour of the mixtures was analysed using a capillary rheometer at different shear rates and temperatures. The results showed that owing to irregular shape of TiH2 compared to Ti powder, the viscosity of the feedstock was significantly higher, thus required greater temperature in order to improve the mouldability of the feedstock. Nevertheless, both feedstocks exhibited pseudoplastic, a shear thinning behavior with shear rate and temperature, desirable properties for injection moulding process. Samples prepared with Ni-Ti feedstock were sintered in a high vacuum furnace, while Ni-TiH2 feedstock was sintered in a tube furnace under a flowing of Argon gas. The results showed that the impurity contents (Carbon and Oxygen) for both feedstocks were almost comparable, suggesting NiTi alloy samples prepared with TiH2 powder is an attractive route for manufacturing of NiTi alloys.

The sol-gel route: A versatile process for up-scaling the fabrication of gas-tight thin electrolyte layers

NASA Astrophysics Data System (ADS)

Viazzi, Céline; Rouessac, Vincent; Lenormand, Pascal; Julbe, Anne; Ansart, Florence; Guizard, Christian

2011-03-01

Sol-gel routes are often investigated and adapted to prepare, by suitable chemical modifications, submicronic powders and derived materials with controlled morphology, which cannot be obtained by conventional solid state chemistry paths. Wet chemistry methods provide attractive alternative routes because mixing of species occurs at the atomic scale. In this paper, ultrafine powders were prepared by a novel synthesis method based on the sol-gel process and were dispersed into suspensions before processing. This paper presents new developments for the preparation of functional materials like yttria-stabilized-zirconia (YSZ, 8% Y2O3) used as electrolyte for solid oxide fuel cells. YSZ thick films were coated onto porous Ni-YSZ substrates using a suspension with an optimized formulation deposited by either a dip-coating or a spin-coating process. The suspension composition is based on YSZ particles encapsulated by a zirconium alkoxide which was added with an alkoxide derived colloidal sol. The in situ growth of these colloids increases significantly the layer density after an appropriated heat treatment. The derived films were continuous, homogeneous and around 20 μm thick. The possible up-scaling of this process has been also considered and the suitable processing parameters were defined in order to obtain, at an industrial scale, homogeneous, crack-free, thick and adherent films after heat treatment at 1400 °C.

Role of precursor chemistry in the direct fluorination to form titanium based conversion anodes for lithium ion batteries

DOE PAGES

Adcock, Jamie; Dai, Sheng; Veith, Gabriel M.; ...

2015-10-13

In this study, a new synthetic route for the formation of titanium oxydifluoride (TiOF 2) through the process of direct fluorination via a fluidized bed reactor system and the associated electrochemical properties of the powders formed from this approach are reported. The flexibility of this synthetic route was demonstrated using precursor powders of titanium dioxide (TiO 2) nanoparticles, as well as a reduced TiO xN y. An advantage of this synthetic method is the ability to directly control the extent of fluorination as a function of reaction temperature and time. The reversible capacity of TiOF 2 anodes was found tomore » depend greatly upon the precursor employed. The TiOF 2 synthesized from TiO 2 and TiO xN y showed reversible capacities of 300 mAh g -1 and 440 mAh g -1, respectively, over 100 cycles. The higher reversible capacity of the TiOF 2 powders derived from TiO xN y likely relate to the partial reduction of the Ti in the fluorinated electrode material, highlighting a route to optimize the properties of conversion electrode materials.« less

Collaboration for the Advancement of Indirect 3D Printing Technology

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

Cordero, Zachary; Elliott, Amy M.

Amorphous powders often possess high hardness values and other useful mechanical properties. However, densifying these powders into complex shapes while retaining their unique properties is a challenge with standard processing routes. Pressureless sintering, for example, can densify intricate green parts composed of rapidly-solidified powders. But this process typically involves long exposures to elevated temperatures, during which the non-equilibrium microstructure of the powder can evolve towards lower energy configurations with inferior properties. Pressure-assisted compaction techniques, by contrast, can consolidate green parts with simple shapes while preserving the microstructure and properties of the powder feedstock. But parts made with these processes generallymore » require additional post-processing, including machining, which introduces new challenges due to the high hardness of these materials. One processing route that can potentially avoid these issues is Indirect 3D Printing (I-3DP; aka Binder Jetting) followed by melt infiltration. In I-3DP, an organic binder is used to join powder feedstock, layer-by-layer, into a green part. In melt infiltration, this green preform is densified by placing it in contact with a molten alloy that wets the preform and wicks into the pores as a result of capillary forces. When these processes are paired together, they offer two key advantages for the densification of rapidly-solidified powders. The first advantage is that the timescale associated with melt infiltration is on the order of seconds for parts with cm-scale dimensions. So in many instances, infiltration requires only a brief thermal excursion that does not degrade the feedstock’s microstructure. The second advantage is that the combination of binder-jet 3D printing and melt infiltration gives fully-dense net shape objects, minimizing the need for subsequent post-processing. In this work, fully-dense, net shape objects have been fabricated from an amorphous powder using I-3DP and molten bronze infiltration while maintaining the amorphous microstructure. X-ray diffraction, scanning electron microscopy, and differential thermal analysis were used to characterize the structural evolution of the powder feedstock during an infiltration heating cycle. Microindentation and bend tests were performed on the infiltrated material to evaluate its mechanical properties. It was found that infiltration improved both the ductility and strength of the sintered preforms by eliminating the stress concentration at the interparticle necks. The infiltrated material had an 11 GPa Vickers hardness and moderate damage tolerance, making it well-suited for applications requiring hard, net shape parts.« less

High-Temperature Metal Matrix Composites

DTIC Science & Technology

1990-06-01

Graduate Student, PhD Candidate Oct 1986 - August 1989. H. Henein: Principal Investigator of Blending Task. Productivity : Papers - J.O.G. Parent, J. Iyengar...the powder metallurgy route provides a better controlled means of forming the product . An overview of the P/M processing route is shown in Figure 1...This approach has its inherent problems. The requirement of a uniform distrihution of the reinforcement material is not always readily achieved. In P/M

Identification of Optimum Magnetic Behavior of NanoCrystalline CmFeAl Type Heusler Alloy Powders Using Response Surface Methodology

NASA Astrophysics Data System (ADS)

Srivastava, Y.; Srivastava, S.; Boriwal, L.

2016-09-01

Mechanical alloying is a novelistic solid state process that has received considerable attention due to many advantages over other conventional processes. In the present work, Co2FeAl healer alloy powder, prepared successfully from premix basic powders of Cobalt (Co), Iron (Fe) and Aluminum (Al) in stoichiometric of 60Co-26Fe-14Al (weight %) by novelistic mechano-chemical route. Magnetic properties of mechanically alloyed powders were characterized by vibrating sample magnetometer (VSM). 2 factor 5 level design matrix was applied to experiment process. Experimental results were used for response surface methodology. Interaction between the input process parameters and the response has been established with the help of regression analysis. Further analysis of variance technique was applied to check the adequacy of developed model and significance of process parameters. Test case study was performed with those parameters, which was not selected for main experimentation but range was same. Response surface methodology, the process parameters must be optimized to obtain improved magnetic properties. Further optimum process parameters were identified using numerical and graphical optimization techniques.

XPS and SEM analysis of the surface of gas atomized powder precursor of ODS ferritic steels obtained through the STARS route

NASA Astrophysics Data System (ADS)

Gil, E.; Cortés, J.; Iturriza, I.; Ordás, N.

2018-01-01

An innovative powder metallurgy route to produce ODS FS, named STARS, has succeeded in atomizing steel powders containing the oxide formers (Y and Ti) and, hence, avoids the mechanical alloying (MA) step to dissolve Y in the matrix. A metastable oxide layer forms at the surface of atomized powders and dissociates during HIP consolidation at high temperatures, leading to precipitation of more stable Y-Ti-O nanoparticles.

Mullite and Mullite/ZrO2-7wt.%Y2O3 Powders for Thermal Spraying of Environmental Barrier Coatings

NASA Astrophysics Data System (ADS)

Garcia, E.; Mesquita-Guimarães, J.; Miranzo, P.; Osendi, M. I.; Wang, Y.; Lima, R. S.; Moreau, C.

2010-01-01

Mullite and mullite/ZrO2-7wt.%Y2O3 coatings could be thought among the main protective layers for environment barrier coatings (EBCs) to protect Si-based substrates in future gas turbine engines. Considering that feedstock of the compound powder is not commercially available, two powder processing routes Spray Drying (SD) and Flame Spheroidization (FS) were implemented for both types of powders. For each method the particle size, the morphology, and microstructure of the powder particles was determined. In addition, the effect of the heat treatment on the powder crystallinity and microstructure of FS powders was also investigated. To evaluate their suitability as feedstock materials, the powders were plasma sprayed and their in-flight particle characteristics monitored for coatings production. The powder morphology was correlated to the in-flight particle characteristics and splat morphology to gain insight about into the influence of powder characteristics on the coating formation.

Synthesis of monodisperse spherical nanometer ZrO{sub 2} (Y{sub 2}O{sub 3}) powders via the coupling route of w/o emulsion with urea homogenous precipitation

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

Chang, Ying; Dong, Shijie, E-mail: dongsjsj@163.com; Wang, Huihu

2012-03-15

Graphical abstract: In this paper, the weight loss and reaction evolution of ZrO{sub 2} precursor powders are determined by TG-DTA, and 600 Degree-Sign C is the most reasonable calcination temperature of precursor according to the TG-DTA. At the same time, we study the effect of reaction conditions upon the particle sizes, such as concentration of zirconium nitrate solution, reaction temperature and urea content. TEM micrographs of zirconia powders indicated that ZrO{sub 2} nano-powders prepared via the coupling route of w/o emulsion with homogenous precipitation possess spherical shape and excellent dispersing. Highlights: Black-Right-Pointing-Pointer The monodisperse spherical nanometer ZrO{sub 2} (Y{sub 2}O{submore » 3}) powders have been prepared via the coupling route of w/o emulsion with urea homogenous precipitation. Black-Right-Pointing-Pointer The principle of the coupling route of emulsion with homogenous precipitation has been studied. Black-Right-Pointing-Pointer The concentration of zirconium nitrate, reaction temperature of water bath and the quantity of urea effect regularly on the average particle size of products. -- Abstract: Using xylol as the oil phase, span-80 as the surfactant, and an aqueous solution containing zirconium (3 mol% Y{sub 2}O{sub 3}) and urea as the water phase, tetragonal phase ZrO{sub 2} nano-powders have been prepared via the coupling route of w/o emulsion with urea homogenous precipitation. The effects of the zirconium concentration, the reaction temperature and the urea content on the average size of the products have been examined. The as-prepared ZrO{sub 2} powders and the precursor powders were characterized by TGA-DTA, XRD, TEM and BET. Experimental results indicate that ZrO{sub 2} powders prepared via the coupling route of w/o emulsion with urea homogenous precipitation possess some excellent characteristics, such as well-rounded spherical shape and excellent dispersing.« less

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

PubMed

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

2015-01-01

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

Weldability Characteristics of Sintered Hot-Forged AISI 4135 Steel Produced through P/M Route by Using Pulsed Current Gas Tungsten Arc Welding

NASA Astrophysics Data System (ADS)

Joseph, Joby; Muthukumaran, S.; Pandey, K. S.

2016-01-01

Present investigation is an attempt to study the weldability characteristics of sintered hot-forged plates of AISI 4135 steel produced through powder metallurgy (P/M) route using matching filler materials of ER80S B2. Compacts of homogeneously blended elemental powders corresponding to the above steel were prepared on a universal testing machine (UTM) by taking pre-weighed powder blend with a suitable die, punch and bottom insert assembly. Indigenously developed ceramic coating was applied on the entire surface of the compacts in order to protect them from oxidation during sintering. Sintered preforms were hot forged to flat, approximately rectangular plates, welded by pulsed current gas tungsten arc welding (PCGTAW) processes with aforementioned filler materials. Microstructural, tensile and hardness evaluations revealed that PCGTAW process with low heat input could produce weldments of good quality with almost nil defects. It was established that PCGTAW joints possess improved tensile properties compared to the base metal and it was mainly attributed to lower heat input, resulting in finer fusion zone grains and higher fusion zone hardness. Thus, the present investigation opens a new and demanding field in research.

A novel process for production of spherical PBT powders and their processing behavior during laser beam melting

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

Schmidt, Jochen, E-mail: jochen.schmidt@fau.de; Sachs, Marius; Fanselow, Stephanie

2016-03-09

Additive manufacturing processes like laser beam melting of polymers are established for production of prototypes and individualized parts. The transfer to other areas of application and to serial production is currently hindered by the limited availability of polymer powders with good processability. Within this contribution a novel process route for the production of spherical polymer micron-sized particles of good flowability has been established and applied to produce polybutylene terephthalate (PBT) powders. Moreover, the applicability of the PBT powders in selective laser beam melting and the dependencies of process parameters on device properties will be outlined. First, polymer micro particles aremore » produced by a novel wet grinding method. To improve the flowability the produced particles the particle shape is optimized by rounding in a heated downer reactor. A further improvement of flowability of the cohesive spherical PBT particles is realized by dry coating. An improvement of flowability by a factor of about 5 is achieved by subsequent rounding of the comminution product and dry-coating as proven by tensile strength measurements of the powders. The produced PBT powders were characterized with respect to their processability. Therefore thermal, rheological, optical and bulk properties were analyzed. Based on these investigations a range of processing parameters was derived. Parameter studies on thin layers, produced in a selective laser melting system, were conducted. Hence appropriate parameters for processing the PBT powders by laser beam melting, like building chamber temperature, scan speed and laser power have been identified.« less

Spark plasma sintering of pure and doped tungsten as plasma facing material

NASA Astrophysics Data System (ADS)

Autissier, E.; Richou, M.; Minier, L.; Naimi, F.; Pintsuk, G.; Bernard, F.

2014-04-01

In the current water cooled divertor concept, tungsten is an armour material and CuCrZr is a structural material. In this work, a fabrication route via a powder metallurgy process such as spark plasma sintering is proposed to fully control the microstructure of W and W composites. The effect of chemical composition (additives) and the powder grain size was investigated. To reduce the sintering temperature, W powders doped with a nano-oxide dispersion of Y2O3 are used. Consequently, the sintering temperature for W-oxide dispersed strengthened (1800 °C) is lower than for pure W powder. Edge localized mode tests were performed on pure W and compared to other preparation techniques and showed promising results.

Vacuum Pressureless Sintering of Ti-6Al-4V Alloy with Full Densification and Forged-Like Mechanical Properties

NASA Astrophysics Data System (ADS)

Zhang, Ce; Lu, Boxin; Wang, Haiying; Guo, Zhimeng; Paley, Vladislav; Volinsky, Alex A.

2018-01-01

Ti-6Al-4V ingots with a nearly 100% density, fine and homogeneous basket-weave microstructure, and better comprehensive mechanical properties (UTS = 935 MPa, Y.S. = 865 MPa, El. = 15.8%), have been manufactured by vacuum pressureless sintering of blended elemental powders. Coarse TiH2 powder, Al powder (2, 20 μm), V powder, and Al-V master alloy powder were used as raw materials to produce different powder mixtures ( D 50 = 10 μm). Then, the compacts made by cold isostatic pressing were consolidated by different sintering curves. A detailed investigation of different as-sintered samples revealed that a higher density can be obtained by generating transient molten Al in the sintering process. Coarse Al powder and a rapid heating rate under the melting point of Al contribute to molten Al formation. The presence of temporary liquid phase changes the sintering mechanism, accelerating the sintering neck formation, improving sinterability of the powder mixtures. Density of 99.5% was achieved at 1150 °C, which is markedly lower than the sintering temperatures reported for conventional blended elemental powder metallurgy routes. In addition, low interstitial content, especially for oxygen (0.17 wt.%), is obtained by strict process control.

Functionalization of polymer powders for SLS-processes using an atmospheric plasma jet in a fluidized bed reactor

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

Sachs, Marius; Schmitt, Adeliene; Schmidt, Jochen

2015-05-22

Recently additive manufacturing processes such as selective laser sintering (SLS) of polymers have gained more importance for industrial applications [1]. Tailor-made modification of polymers is essential in order to make these processes more efficient and to cover the industrial demands. The so far used polymer materials show weak performance regarding the mechanical stability of processed parts. To overcome this limitation, a new route to functionalize the surface of commercially available polymer particles (PA12; PE-HD; PP) using an atmospheric plasma jet in combination with a fluidized bed reactor has been investigated. Consequently, an improvement of adhesion and wettability [2] of themore » polymer surface without restraining the bulk properties of the powder is achieved. The atmospheric plasma jet process can provide reactive species at moderate temperatures which are suitable for polymer material. The functionalization of the polymer powders improves the quality of the devices build in a SLS-process.« less

Comparison of Reactive and Non-Reactive Spark Plasma Sintering Routes for the Fabrication of Monolithic and Composite Ultra High Temperature Ceramics (UHTC) Materials

PubMed Central

Orrù, Roberto; Cao, Giacomo

2013-01-01

A wider utilization of ultra high temperature ceramics (UHTC) materials strongly depends on the availability of efficient techniques for their fabrication as dense bodies. Based on recent results reported in the literature, it is possible to state that Spark Plasma Sintering (SPS) technology offers a useful contribution in this direction. Along these lines, the use of two different SPS-based processing routes for the preparation of massive UHTCs is examined in this work. One method, the so-called reactive SPS (R-SPS), consists of the synthesis and densification of the material in a single step. Alternatively, the ceramic powders are first synthesized by Self-propagating High-temperature Synthesis (SHS) and then sintered by SPS. The obtained results evidenced that R-SPS method is preferable for the preparation of dense monolithic products, while the sintering of SHS powders requires relatively milder conditions when considering binary composites. The different kinetic mechanisms involved during R-SPS of the monolithic and composite systems, i.e., combustion-like or gradual solid-diffusion, respectively, provides a possible explanation. An important role is also played by the SHS process, particularly for the preparation of composite powders, since stronger interfaces are established between the ceramic constituents formed in situ, thus favoring diffusion processes during the subsequent SPS step. PMID:28809229

Original Synthetic Route To Obtain a SrAl2O4 Phosphor by the Molten Salt Method: Insights into the Reaction Mechanism and Enhancement of the Persistent Luminescence.

PubMed

Rojas-Hernandez, Rocío Estefanía; Rubio-Marcos, Fernando; Gonçalves, Ricardo Henrique; Rodriguez, Miguel Ángel; Véron, Emmanuel; Allix, Mathieu; Bessada, Catherine; Fernandez, José Francisco

2015-10-19

SrAl2O4:Eu(2+), Dy(3+) has been extensively studied for industrial applications in the luminescent materials field, because of its excellent persistent luminescence properties and chemical stability. Traditionally, this strontium aluminate material is synthesized in bulk form and/or fine powder by the classic solid-state method. Here, we report an original synthetic route, a molten salt assisted process, to obtain highly crystalline SrAl2O4 powder with nanometer-scale crystals. The main advantages of salt addition are the increase of the reaction rate and the significant reduction of the synthesis temperature because of much higher mobility of reactants in the liquid medium than in the solid-state method. In particular, the formation mechanism of SrAl2O4, the role of the salt, and the phase's evolution have been explored as a function of temperature and time. Phosphorescent powders based on SrAl2O4:Eu(2+), Dy(3+) with high crystallinity are obtained after 1 h treatment at 900 °C. This work could promote further interest in adopting the molten salt strategy to process high-crystallinity materials with enhanced luminescence to design technologically relevant phosphors.

Inorganic-organic nanocomposites for optical coatings

NASA Astrophysics Data System (ADS)

Schmidt, Helmut K.; Krug, Herbert; Sepeur-Zeitz, Bernhard; Geiter, Elisabeth

1997-10-01

The fabrication of nanoparticles by the sol-gel process and their use in polymeric or sol-gel-derived inorganic-organic composite matrices opens up interesting possibilities for designing new optical materials. Two different routes have been chosen for preparing optical nanocomposites: The first is the so-called 'in situ route,' where the nanoparticles are synthesized in a liquid mixture from Zr-alkoxides in a polymerizable system and diffractive gratings were produced by embossing uncured film. The second is the 'separate' preparation route, where a sterically stabilized dry nanoboehmite powder was completely redispersed in an epoxy group-containing matrix and hard coatings with optical quality on polycarbonate were prepared.

Study on the RF inductively coupled plasma spheroidization of refractory W and W-Ta alloy powders

NASA Astrophysics Data System (ADS)

Chenfan, YU; Xin, ZHOU; Dianzheng, WANG; Neuyen VAN, LINH; Wei, LIU

2018-01-01

Spherical powders with good flowability and high stacking density are mandatory for powder bed additive manufacturing. Nevertheless, the preparation of spherical refractory tungsten and tungsten alloy powders is a formidable task. In this paper, spherical refractory metal powders processed by high-energy stir ball milling and RF inductively coupled plasma were investigated. By utilizing the technical route, pure spherical tungsten powders were prepared successfully, the flowability increased from 10.7 s/50 g to 5.5 s/50 g and apparent density increased from 6.916 g cm-3 to 11.041 g cm-3. Alloying element tantalum can reduce the tendency to micro-crack during tungsten laser melting and rapid solidification process. Spherical W-6Ta (%wt) powders were prepared in this way, homogeneous dispersion of tantalum in a tungsten matrix occurred but a small amount of flake-like shape particles appeared after high-energy stir ball milling. The flake-like shape particles can hardly be spheroidized in subsequent RF inductively coupled plasma process, might result from the unique suspended state of flaky particles under complex electric and magnetic fields as well as plasma-particle heat exchange was different under various turbulence models. As a result, the flake-like shape particles cannot pass through the high-temperature area of thermal plasma torch and cannot be spheroidized properly.

A new synthesis route to high surface area sol gel bioactive glass through alcohol washing

PubMed Central

M. Mukundan, Lakshmi; Nirmal, Remya; Vaikkath, Dhanesh; Nair, Prabha D.

2013-01-01

Bioactive glass is one of the widely used bone repair material due to its unique properties like osteoconductivity, osteoinductivity and biodegradability. In this study bioactive glass is prepared by the sol gel process and stabilized by a novel method that involves a solvent instead of the conventional calcinations process. This study represents the first attempt to use this method for the stabilization of bioactive glass. The bioactive glass stabilized by this ethanol washing process was characterized for its physicochemical and biomimetic property in comparison with similar composition of calcined bioactive glass. The compositional similarity of the two stabilized glass powders was confirmed by spectroscopic and thermogravimetric analysis. Other physicochemical characterizations together with the cell culture studies with L929 fibroblast cells and bone marrow mesenchymal stem cells proved that the stabilization was achieved with the retention of its inherent bioactive potential. However an increase in the surface area of the glass powder was obtained as a result of this ethanol washing process and this add up to the success of the study. Hence the present study exhibits a promising route for high surface area bioactive glass for increasing biomimicity. PMID:23512012

Powder metallurgy inspired low-temperature fabrication of high-performance stereocomplexed polylactide products with good optical transparency

PubMed Central

Bai, Dongyu; Liu, Huili; Bai, Hongwei; Zhang, Qin; Fu, Qiang

2016-01-01

Stereocomplexation between enantiomeric poly(l-lactide) (PLLA) and poly(d-lactide) (PDLA) provides an avenue to greatly enhance performance of eco-friendly polylactide (PLA). Unfortunately, although the manufacturing of semicrystalline polymers generally involves melt processing, it is still hugely challenging to create high-performance stereocomplexed polylactide (sc-PLA) products from melt-processed high-molecular-weight PLLA/PDLA blends due to the weak crystallization memory effect of stereocomplex (sc) crystallites after complete melting as well as the substantial degradation of PLA chains at elevated melt-processing temperatures of ca. 240–260 °C. Inspired by the concept of powder metallurgy, here we report a new facile route to address these obstacles by sintering of sc-PLA powder at temperatures as low as 180–210 °C, which is distinctly different from traditional sintering of polymer powders performed at temperatures far exceeding their melting temperatures. The enantiomeric PLA chain segments from adjacent powder particles can interdiffuse across particle interfaces and co-crystallize into new sc crystallites capable of tightly welding the interfaces during the low-temperature sintering process, and thus highly transparent sc-PLA products with outstanding heat resistance, mechanical strength, and hydrolytic stability have been successfully fabricated for the first time. PMID:26837848

Powder metallurgy inspired low-temperature fabrication of high-performance stereocomplexed polylactide products with good optical transparency

NASA Astrophysics Data System (ADS)

Bai, Dongyu; Liu, Huili; Bai, Hongwei; Zhang, Qin; Fu, Qiang

2016-02-01

Stereocomplexation between enantiomeric poly(L-lactide) (PLLA) and poly(D-lactide) (PDLA) provides an avenue to greatly enhance performance of eco-friendly polylactide (PLA). Unfortunately, although the manufacturing of semicrystalline polymers generally involves melt processing, it is still hugely challenging to create high-performance stereocomplexed polylactide (sc-PLA) products from melt-processed high-molecular-weight PLLA/PDLA blends due to the weak crystallization memory effect of stereocomplex (sc) crystallites after complete melting as well as the substantial degradation of PLA chains at elevated melt-processing temperatures of ca. 240-260 °C. Inspired by the concept of powder metallurgy, here we report a new facile route to address these obstacles by sintering of sc-PLA powder at temperatures as low as 180-210 °C, which is distinctly different from traditional sintering of polymer powders performed at temperatures far exceeding their melting temperatures. The enantiomeric PLA chain segments from adjacent powder particles can interdiffuse across particle interfaces and co-crystallize into new sc crystallites capable of tightly welding the interfaces during the low-temperature sintering process, and thus highly transparent sc-PLA products with outstanding heat resistance, mechanical strength, and hydrolytic stability have been successfully fabricated for the first time.

Powder metallurgy inspired low-temperature fabrication of high-performance stereocomplexed polylactide products with good optical transparency.

PubMed

Bai, Dongyu; Liu, Huili; Bai, Hongwei; Zhang, Qin; Fu, Qiang

2016-02-03

Stereocomplexation between enantiomeric poly(l-lactide) (PLLA) and poly(d-lactide) (PDLA) provides an avenue to greatly enhance performance of eco-friendly polylactide (PLA). Unfortunately, although the manufacturing of semicrystalline polymers generally involves melt processing, it is still hugely challenging to create high-performance stereocomplexed polylactide (sc-PLA) products from melt-processed high-molecular-weight PLLA/PDLA blends due to the weak crystallization memory effect of stereocomplex (sc) crystallites after complete melting as well as the substantial degradation of PLA chains at elevated melt-processing temperatures of ca. 240-260 °C. Inspired by the concept of powder metallurgy, here we report a new facile route to address these obstacles by sintering of sc-PLA powder at temperatures as low as 180-210 °C, which is distinctly different from traditional sintering of polymer powders performed at temperatures far exceeding their melting temperatures. The enantiomeric PLA chain segments from adjacent powder particles can interdiffuse across particle interfaces and co-crystallize into new sc crystallites capable of tightly welding the interfaces during the low-temperature sintering process, and thus highly transparent sc-PLA products with outstanding heat resistance, mechanical strength, and hydrolytic stability have been successfully fabricated for the first time.

Microstructure and mechanical properties of NiCoCrAlYTa alloy processed by press and sintering route

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

Pereira, J.C., E-mail: jpereira@uc.edu.ve; Centro de Investigaciones en Mecánica, Facultad de Ingeniería, Universidad de Carabobo; Zambrano, J.C.

2015-03-15

Nickel-based superalloys such as NiCoCrAlY are widely used in high-temperature applications, such as gas turbine components in the energy and aerospace industries, due to their strength, high elastic modulus, and high-temperature oxidation resistance. However, the processing of these alloys is complex and costly, and the alloys are currently used as a bond coat in thermal barrier coatings. In this work, the effect of cold press and sintering processing parameters on the microstructure and mechanical properties of NiCoCrAlY alloy were studied using the powder metallurgy route as a new way to obtain NiCoCrAlYTa samples from a gas atomized prealloyed powder feedstock.more » High mechanical strength and adequate densification up to 98% were achieved. The most suitable compaction pressure and sintering temperature were determined for NiCoCrAlYTa alloy through microstructure characterization. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and energy dispersive spectroscopy microanalysis (EDS) were performed to confirm the expected γ-Ni matrix and β-NiAl phase distribution. Additionally, the results demonstrated the unexpected presence of carbides and Ni–Y-rich zones in the microstructure due to the powder metallurgy processing parameters used. Thus, microhardness, nanoindentation and uniaxial compression tests were conducted to correlate the microstructure of the alloy samples with their mechanical properties under the different studied conditions. The results show that the compaction pressure did not significantly affect the mechanical properties of the alloy samples. In this work, the compaction pressures of 400, 700 and 1000 MPa were used. The sintering temperature of 1200 °C for NiCoCrAlYTa alloy was preferred; above this temperature, the improvement in mechanical properties is not significant due to grain coarsening, whereas a lower temperature produces a decrease in mechanical properties due to high porosity and poor solid-state diffusion. - Graphical abstract: Display Omitted - Highlights: • We made NiCoCrAlYTa alloy by a conventional powder metallurgy route. • High densification and adequate strength were observed. • The presence of unexpected carbides found along γ/γ and γ/β grain boundaries was detected. • The effect of cold press and sintering processing parameters on the microstructure and mechanical properties were studied.« less

A general route for the rapid synthesis of one-dimensional nanostructured single-crystal Te, Se and Se Te alloys directly from Te or/and Se powders

NASA Astrophysics Data System (ADS)

Zhou, Bo; Zhu, Jun-Jie

2006-03-01

A general and template-free 'disproportionation and reversal' route was developed to synthesize one-dimensional (1D) nanostructures of Te, Se and Se-Te alloys directly from Te or/and Se powders. The products were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and scanning electron microscopy (SEM). Te nanorods and nanowires with a width varying from about 40 nm to about 300 nm, Se nanowires with a width of 60-100 nm and a length of 4-6 µm, and SexTe100-x alloy nanorods with x in a wide range, and with a width of 30-70 nm and an aspect ratio of three to five, were prepared. The mechanism of formation of the nanorods and nanowires and the effects of the experimental conditions, such as solution concentration, cooling rate, solvent nature and heating process, on the morphology and size of the products have been discussed. We believe that this general route and some other proper reversible processes between solid state and solution state can be extended to the transformations from various bulk materials into nanosized materials with various morphologies.

Carbothermal Production of Magnesium: Csiro's Magsonic™ Process

NASA Astrophysics Data System (ADS)

Prentice, Leon H.; Nagle, Michael W.; Barton, Timothy R. D.; Tassios, Steven; Kuan, Benny T.; Witt, Peter J.; Constanti-Carey, Keri K.

Carbothermal production has been recognized as conceptually the simplest and cleanest route to magnesium metal, but has suffered from technical challenges of development and scale-up. Work by CSIRO has now successfully demonstrated the technology using supersonic quenching of magnesium vapor (the MagSonic™ Process). Key barriers to process development have been overcome: the experimental program has achieved sustained operation, no nozzle blockage, minimal reversion, and safe handling of pyrophoric powders. The laboratory equipment has been operated at industrially relevant magnesium vapor concentrations (>25% Mg) for multiple runs with no blockage. Novel computational fluid dynamics (CFD) modeling of the shock quenching and metal vapor condensation has informed nozzle design and is supported by experimental data. Reversion below 10% has been demonstrated, and magnesium successfully purified (>99.9%) from the collected powder. Safe operating procedures have been developed and demonstrated, minimizing the risk of powder explosion. The MagSonic™ Process is now ready to progress to significantly larger scale and continuous operation.

Ultra High Temperature Ceramics' Processing Routes and Microstructures Compared

NASA Technical Reports Server (NTRS)

Gusman, Michael; Stackpoole, Mairead; Johnson, Sylvia; Gasch, Matt; Lau, Kai-Hung; Sanjurjo, Angel

2009-01-01

Ultra High Temperature Ceramics (UHTCs), such as HfB2 and ZrB2 composites containing SiC, are known to have good thermal shock resistance and high thermal conductivity at elevated temperatures. These UHTCs have been proposed for a number of structural applications in hypersonic vehicles, nozzles, and sharp leading edges. NASA Ames is working on controlling UHTC properties (especially, mechanical properties, thermal conductivity, and oxidation resistance) through processing, composition, and microstructure. In addition to using traditional methods of combining additives to boride powders, we are preparing UHTCs using coat ing powders to produce both borides and additives. These coatings and additions to the powders are used to manipulate and control grain-boundary composition and second- and third-phase variations within the UHTCs. Controlling the composition of high temperature oxidation by-products is also an important consideration. The powders are consolidated by hot-pressing or field-assisted sintering (FAS). Comparisons of microstructures and hardness data will be presented.

Comparison of the surface charge behavior of commercial silicon nitride and silicon carbide powders

NASA Technical Reports Server (NTRS)

Whitman, Pamela K.; Feke, Donald L.

1988-01-01

The adsorption and desorption of protons from aqueous solution onto the surfaces of a variety of commercial silicon carbide and silicon nitride powders has been examined using a surface titration methodology. This method provides information on some colloidal characteristics, such as the point of zero charge (pzc) and the variation of proton adsorption with dispersion pH, useful for the prediction of optimal ceramic-processing conditions. Qualitatively, the magnitude of the proton adsorption from solution reveals small differences among all of the materials studied. However, the results show that the pzc for the various silicon nitride powders is affected by the powder synthesis route. Complementary investigations have shown that milling can also act to shift the pzc exhibited by silicon nitride powder. Also, studies of the role of the electrolyte in the development of surface charge have indicated no evidence of specific adsorption of ammonium ion on either silicon nitride or silicon carbide powders.

Injection molding as a one-step process for the direct production of pharmaceutical dosage forms from primary powders.

PubMed

Eggenreich, K; Windhab, S; Schrank, S; Treffer, D; Juster, H; Steinbichler, G; Laske, S; Koscher, G; Roblegg, E; Khinast, J G

2016-05-30

The objective of the present study was to develop a one-step process for the production of tablets directly from primary powder by means of injection molding (IM), to create solid-dispersion based tablets. Fenofibrate was used as the model API, a polyvinyl caprolactame-polyvinyl acetate-polyethylene glycol graft co-polymer served as a matrix system. Formulations were injection-molded into tablets using state-of-the-art IM equipment. The resulting tablets were physico-chemically characterized and the drug release kinetics and mechanism were determined. Comparison tablets were produced, either directly from powder or from pre-processed pellets prepared via hot melt extrusion (HME). The content of the model drug in the formulations was 10% (w/w), 20% (w/w) and 30% (w/w), respectively. After 120min, both powder-based and pellet-based injection-molded tablets exhibited a drug release of 60% independent of the processing route. Content uniformity analysis demonstrated that the model drug was homogeneously distributed. Moreover, analysis of single dose uniformity also revealed geometric drug homogeneity between tablets of one shot. Copyright © 2016 Elsevier B.V. All rights reserved.

66. BUILDING NO. 554, REWORK POWDER GRINDING ROUSE, PULVERIZING, WATER ...

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

66. BUILDING NO. 554, REWORK POWDER GRINDING ROUSE, PULVERIZING, WATER DRY HOUSE, LOOKING NORTH (DEMOLITION IN PROGRESS). - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Analysis of the Influence of Starting Materials and Processing Conditions on the Properties of W/Cu Alloys.

PubMed

Montealegre-Meléndez, Isabel; Arévalo, Cristina; Perez-Soriano, Eva M; Neubauer, Erich; Rubio-Escudero, Cristina; Kitzmantel, Michael

2017-02-08

In this work, a study of the influence of the starting materials and the processing time used to develop W/Cu alloys is carried out. Regarding powder metallurgy as a promising fabrication route, the difficulties in producing W/Cu alloys motivated us to investigate the influential factors on the final properties of the most industrially demanding alloys: 85-W/15-Cu, 80-W/20-Cu, and 75-W/25-Cu alloys. Two different tungsten powders with large variation among their particle size-fine (W f ) and coarse (W c ) powders-were used for the preparation of W/Cu alloys. Three weight ratios of fine and coarse (W f :W c ) tungsten particles were analyzed. These powders were labelled as "tungsten bimodal powders". The powder blends were consolidated by rapid sinter pressing (RSP) at 900 °C and 150 MPa, and were thus sintered and compacted simultaneously. The elemental powders and W/Cu alloys were studied by optical microscopy (OM) and scanning electron microscopy (SEM). Thermal conductivity, hardness, and densification were measured. Results showed that the synthesis of W/Cu using bimodal tungsten powders significantly affects the final alloy properties. The higher the tungsten content, the more noticeable the effect of the bimodal powder. The best bimodal W powder was the blend with 10 wt % of fine tungsten particles (10-W f :90-W c ). These specimens present good values of densification and hardness, and higher values of thermal conductivity than other bimodal mixtures.

Development of a Cr-Based Hard Composite Processed by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

García-Junceda, A.; Sáez, I.; Deng, X. X.; Torralba, J. M.

2018-04-01

This investigation analyzes the feasibility of processing a composite material comprising WC particles randomly dispersed in a matrix in which Cr is the main metallic binder. Thus, a new composite material is processed using a commercial, economic, and easily available Cr-based alloy, assuming that there is a certain Cr solubility in the WC particles acting as reinforcement. The processing route followed includes mechanical milling of the powders and consolidation by spark plasma sintering.

Low-temperature solution route to macroscopic amounts of hydrogen terminated silicon nanoparticles.

PubMed

Neiner, Doinita; Chiu, Hsiang Wei; Kauzlarich, Susan M

2006-08-30

A new solution route for preparing gram-scale, hydrogen terminated silicon nanoparticles is presented. Dimethoxyethane and diocytl ether have been used to prepare silicon nanoparticles via a solution reaction between sodium silicide and ammonium bromide. The reaction products are isolated as a clear yellow-orange solution and a dark black powder. Both the solution and the powder have been characterized.

Growing three-dimensional biomorphic graphene powders using naturally abundant diatomite templates towards high solution processability.

PubMed

Chen, Ke; Li, Cong; Shi, Liurong; Gao, Teng; Song, Xiuju; Bachmatiuk, Alicja; Zou, Zhiyu; Deng, Bing; Ji, Qingqing; Ma, Donglin; Peng, Hailin; Du, Zuliang; Rümmeli, Mark Hermann; Zhang, Yanfeng; Liu, Zhongfan

2016-11-07

Mass production of high-quality graphene with low cost is the footstone for its widespread practical applications. We present herein a self-limited growth approach for producing graphene powders by a small-methane-flow chemical vapour deposition process on naturally abundant and industrially widely used diatomite (biosilica) substrates. Distinct from the chemically exfoliated graphene, thus-produced biomorphic graphene is highly crystallized with atomic layer-thickness controllability, structural designability and less noncarbon impurities. In particular, the individual graphene microarchitectures preserve a three-dimensional naturally curved surface morphology of original diatom frustules, effectively overcoming the interlayer stacking and hence giving excellent dispersion performance in fabricating solution-processible electrodes. The graphene films derived from as-made graphene powders, compatible with either rod-coating, or inkjet and roll-to-roll printing techniques, exhibit much higher electrical conductivity (∼110,700 S m -1 at 80% transmittance) than previously reported solution-based counterparts. This work thus puts forward a practical route for low-cost mass production of various powdery two-dimensional materials.

Growing three-dimensional biomorphic graphene powders using naturally abundant diatomite templates towards high solution processability

NASA Astrophysics Data System (ADS)

Chen, Ke; Li, Cong; Shi, Liurong; Gao, Teng; Song, Xiuju; Bachmatiuk, Alicja; Zou, Zhiyu; Deng, Bing; Ji, Qingqing; Ma, Donglin; Peng, Hailin; Du, Zuliang; Rümmeli, Mark Hermann; Zhang, Yanfeng; Liu, Zhongfan

2016-11-01

Mass production of high-quality graphene with low cost is the footstone for its widespread practical applications. We present herein a self-limited growth approach for producing graphene powders by a small-methane-flow chemical vapour deposition process on naturally abundant and industrially widely used diatomite (biosilica) substrates. Distinct from the chemically exfoliated graphene, thus-produced biomorphic graphene is highly crystallized with atomic layer-thickness controllability, structural designability and less noncarbon impurities. In particular, the individual graphene microarchitectures preserve a three-dimensional naturally curved surface morphology of original diatom frustules, effectively overcoming the interlayer stacking and hence giving excellent dispersion performance in fabricating solution-processible electrodes. The graphene films derived from as-made graphene powders, compatible with either rod-coating, or inkjet and roll-to-roll printing techniques, exhibit much higher electrical conductivity (~110,700 S m-1 at 80% transmittance) than previously reported solution-based counterparts. This work thus puts forward a practical route for low-cost mass production of various powdery two-dimensional materials.

Depositing laser-generated nanoparticles on powders for additive manufacturing of oxide dispersed strengthened alloy parts via laser metal deposition

NASA Astrophysics Data System (ADS)

Streubel, René; Wilms, Markus B.; Doñate-Buendía, Carlos; Weisheit, Andreas; Barcikowski, Stephan; Henrich Schleifenbaum, Johannes; Gökce, Bilal

2018-04-01

We present a novel route for the adsorption of pulsed laser-dispersed nanoparticles onto metal powders in aqueous solution without using any binders or surfactants. By electrostatic interaction, we deposit Y2O3 nanoparticles onto iron-chromium based powders and obtain a high dispersion of nano-sized particles on the metallic powders. Within the additively manufactured component, we show that the particle spacing of the oxide inclusion can be adjusted by the initial mass fraction of the adsorbed Y2O3 particles on the micropowder. Thus, our procedure constitutes a robust route for additive manufacturing of oxide dispersion-strengthened alloys via oxide nanoparticles supported on steel micropowders.

Structural materials by powder HIP for fusion reactors

NASA Astrophysics Data System (ADS)

Dellis, C.; Le Marois, G.; van Osch, E. V.

1998-10-01

Tokamak blankets have complex shapes and geometries with double curvature and embedded cooling channels. Usual manufacturing techniques such as forging, bending and welding generate very complex fabrication routes. Hot Isostatic Pressing (HIP) is a versatile and flexible fabrication technique that has a broad range of commercial applications. Powder HIP appears to be one of the most suitable techniques for the manufacturing of such complex shape components as fusion reactor modules. During the HIP cycle, consolidation of the powder is made and porosity in the material disappears. This involves a variation of 30% in volume of the component. These deformations are not isotropic due to temperature gradients in the part and the stiffness of the canister. This paper discusses the following points: (i) Availability of manufacturing process by powder HIP of 316LN stainless steel (ITER modules) and F82H martensitic steel (ITER Test Module and DEMO blanket) with properties equivalent to the forged one.(ii) Availability of powerful modelling techniques to simulate the densification of powder during the HIP cycle, and to control the deformation of components during consolidation by improving the canister design.(iii) Material data base needed for simulation of the HIP process, and the optimisation of canister geometry.(iv) Irradiation behaviour on powder HIP materials from preliminary results.

Structure and luminescence of nanocrystalline gallium nitride synthesized by a novel polymer pyrolysis route

NASA Astrophysics Data System (ADS)

Garcia, Rafael; Hirata, Gustavo A.; Thomas, Alan C.; Ponce, Fernando A.

2006-10-01

Thermal decomposition in a horizontal quartz tube reactor of a polymer [-(CH 6N 4O) 3Ga(NO 3) 3-] in a nitrogen atmosphere, yield directly nano-structured gallium nitride (GaN) powder. The polymer was obtained by the reaction between high purity gallium nitrate (Ga(NO 3) 3) dissolved in toluene and carbohydrazide as an azotic ligand. The powder synthesized by this method showed a yellow color and elemental analysis suggested that the color is due to some carbon and oxygen impurities in the as-synthesized powder. Electron microscopy showed that the as-synthesized powders consist of a mixture of various porous particles containing nanowires and nano-sized platelets. The size of the crystallites can be controlled by annealing processes under ammonia. Photoluminescence analysis at 10 K on as-synthesized powders showed a broad red luminescence around 668 nm under UV laser excitation (He-Cd laser, 325 nm). However after annealing process the red luminescence disappears and the typical band edge emission of GaN around 357 nm (3.47 eV) and the UV band were the dominant emissions in the PL spectra.

Compressive Deformation Behavior of Open-Cell Cu-Zn-Al Alloy Foam Made Through P/M Route Using Mechanically Alloyed Powder

NASA Astrophysics Data System (ADS)

Barnwal, Ajay Kumar; Mondal, D. P.; Kumar, Rajeev; Prasanth, N.; Dasgupta, R.

2018-03-01

Cu-Zn-Al foams of varying porosity fractions using mechanical alloyed powder have been made through powder metallurgy route. Here, NH4 (HCO3) was used as a space holder. Mechanically alloyed Cu-Zn-Al is made using a planetary ball mill taking the ratio of Cu/Zn/Al = 70:25:5 (by weight ratio). The ball/powder ratios were varied in the four ranges 10:1, 15:1, 20:1, and 25:1. Green compacts of milled powder and space holder samples were sintered at three stages at three different temperatures 350, 550, and 850 °C for 1 h at each stage. The crystalline size and particle size as a function of ball/powder ratios were examined. The compressive deformation responses of foams are varied with relative density and the ball/powder ratio. The plateau stress and energy absorption of these foams increase with an increase in relative density but decreases with increase in ball/powder ratio, even though crystalline size decreases. This has further been explained on the basis of particle morphology as a function of ball/powder ratio.

Soft chemistry routes for synthesis of rare earth oxide nanoparticles with well defined morphological and structural characteristics

NASA Astrophysics Data System (ADS)

Mancic, L.; Marinkovic, B. A.; Marinkovic, K.; Dramicanin, M.; Milosevic, O.

2011-11-01

Phosphors of (Y0.75Gd0.25)2O3:Eu3+ (5 at.%) have been prepared through soft chemistry routes. Conversion of the starting nitrates mixture into oxide is performed through two approaches: (a) hydrothermal treatment (HT) at 200 °C/3 h of an ammonium hydrogen carbonate precipitated mixture and (b) by thermally decomposition of pure nitrate precursor solution at 900 °C in dispersed phase (aerosol) within a tubular flow reactor by spray pyrolysis process (SP). The powders are additionally thermally treated at different temperatures: 600, 1000, and 1100 °C for either 3 or 12 h. HT—derived particles present exclusively one-dimensional morphology (nanorods) up to the temperatures of 600 °C, while the leaf-like particles start to grow afterward. SP—derived particles maintain their spherical shape up to the temperatures of 1100 °C. These submicron sized spheres were actually composed of randomly aggregated nanoparticles. All powders exhibits cubic Ia- 3 structure (Y0.75Gd0.25)2O3:Eu and have improved optical characteristics due to their nanocrystalline nature. The detailed study of the influence of structural and morphological powder characteristics on their emission properties is performed based on the results of X-ray powder diffractometry, scanning electron microscopy, X-ray energy dispersive spectroscopy, transmission electron microscopy, and photoluminescence measurements.

Rapid and direct synthesis of complex perovskite oxides through a highly energetic planetary milling

PubMed Central

Lee, Gyoung-Ja; Park, Eun-Kwang; Yang, Sun-A; Park, Jin-Ju; Bu, Sang-Don; Lee, Min-Ku

2017-01-01

The search for a new and facile synthetic route that is simple, economical and environmentally safe is one of the most challenging issues related to the synthesis of functional complex oxides. Herein, we report the expeditious synthesis of single-phase perovskite oxides by a high-rate mechanochemical reaction, which is generally difficult through conventional milling methods. With the help of a highly energetic planetary ball mill, lead-free piezoelectric perovskite oxides of (Bi, Na)TiO3, (K, Na)NbO3 and their modified complex compositions were directly synthesized with low contamination. The reaction time necessary to fully convert the micron-sized reactant powder mixture into a single-phase perovskite structure was markedly short at only 30–40 min regardless of the chemical composition. The cumulative kinetic energy required to overtake the activation period necessary for predominant formation of perovskite products was ca. 387 kJ/g for (Bi, Na)TiO3 and ca. 580 kJ/g for (K, Na)NbO3. The mechanochemically derived powders, when sintered, showed piezoelectric performance capabilities comparable to those of powders obtained by conventional solid-state reaction processes. The observed mechanochemical synthetic route may lead to the realization of a rapid, one-step preparation method by which to create other promising functional oxides without time-consuming homogenization and high-temperature calcination powder procedures. PMID:28387324

Particle morphology influence on mechanical and biocompatibility properties of injection molded Ti alloy powder.

PubMed

Gülsoy, H Özkan; Gülsoy, Nagihan; Calışıcı, Rahmi

2014-01-01

Titanium and Titanium alloys exhibits properties that are excellent for various bio-applications. Metal injection molding is a processing route that offers reduction in costs, with the added advantage of near net-shape components. Different physical properties of Titanium alloy powders, shaped and processed via injection molding can achieve high complexity of part geometry with mechanical and bioactivity properties, similar or superior to wrought material. This study describes that the effect of particle morphology on the microstructural, mechanical and biocompatibility properties of injection molded Ti-6Al-4V (Ti64) alloy powder for biomaterials applications. Ti64 powders irregular and spherical in shape were injection molded with wax based binder. Binder debinding was performed in solvent and thermal method. After debinding the samples were sintered under high vacuum. Metallographic studies were determined to densification and the corresponding microstructural changes. Sintered samples were immersed in a simulated body fluid (SBF) with elemental concentrations that were comparable to those of human blood plasma for a total period of 15 days. Both materials were implanted in fibroblast culture for biocompatibility evaluations were carried out. The results show that spherical and irregular powder could be sintered to a maximum theoretical density. Maximum tensile strength was obtained for spherical shape powder sintered. The tensile strength of the irregular shape powder sintered at the same temperature was lower due to higher porosity. Finally, mechanical tests show that the irregular shape powder has lower mechanical properties than spherical shape powder. The sintered irregular Ti64 powder exhibited better biocompatibility than sintered spherical Ti64 powder. Results of study showed that sintered spherical and irregular Ti64 powders exhibited high mechanical properties and good biocompatibility properties.

Experimental use of Line-X coated steel pipe piles, Clay Hill Bridge (#2157) replacement project over the Mousam River, Route 9/Western Avenue, Kennebunk, Maine.

DOT National Transportation Integrated Search

2013-02-01

Steel pipe piles used by MaineDOT for bridge construction are typically coated with a fusion-bonded epoxy (FBE). FBE is a powder-based coating with properties similar to traditional : epoxies. Its name is derived from the process by which it adheres ...

Nucleation of biomimetic apatite in synthetic body fluids: dense and porous scaffold development.

PubMed

Landi, Elena; Tampieri, Anna; Celotti, Giancarlo; Langenati, Ratih; Sandri, Monica; Sprio, Simone

2005-06-01

The effectiveness of synthetic body fluids (SBF) as biomimetic sources to synthesize carbonated hydroxyapatite (CHA) powder similar to the biological inorganic phase, in terms of composition and microstructure, was investigated. CHA apatite powders were prepared following two widely experimented routes: (1) calcium nitrate tetrahydrate and diammonium hydrogen phosphate and (2) calcium hydroxide and ortophosphoric acid, but using SBF as synthesis medium instead of pure water. The characteristics of the as-prepared powders were compared, also with the features of apatite powders synthesized via pure water-based classical methods. The powder thermal resistance and behaviour during densification were studied together with the mechanical properties of the dense samples. The sponge impregnation process was used to prepare porous samples having morphological and mechanical characteristics suitable for bone substitution. Using this novel synthesis was it possible to prepare nanosized (approximately equal to 20 nm), pure, carbonate apatite powder containing Mg, Na, K ions, with morphological and compositional features mimicking natural apatite and with improved thermal properties. After sintering at 1250 degrees C the carbonate-free apatite porous samples showed a surprising, high compressive strength together with a biomimetic morphology.

Analysis of the Influence of Starting Materials and Processing Conditions on the Properties of W/Cu Alloys

PubMed Central

Montealegre-Meléndez, Isabel; Arévalo, Cristina; Perez-Soriano, Eva M.; Neubauer, Erich; Rubio-Escudero, Cristina; Kitzmantel, Michael

2017-01-01

In this work, a study of the influence of the starting materials and the processing time used to develop W/Cu alloys is carried out. Regarding powder metallurgy as a promising fabrication route, the difficulties in producing W/Cu alloys motivated us to investigate the influential factors on the final properties of the most industrially demanding alloys: 85-W/15-Cu, 80-W/20-Cu, and 75-W/25-Cu alloys. Two different tungsten powders with large variation among their particle size—fine (Wf) and coarse (Wc) powders—were used for the preparation of W/Cu alloys. Three weight ratios of fine and coarse (Wf:Wc) tungsten particles were analyzed. These powders were labelled as “tungsten bimodal powders”. The powder blends were consolidated by rapid sinter pressing (RSP) at 900 °C and 150 MPa, and were thus sintered and compacted simultaneously. The elemental powders and W/Cu alloys were studied by optical microscopy (OM) and scanning electron microscopy (SEM). Thermal conductivity, hardness, and densification were measured. Results showed that the synthesis of W/Cu using bimodal tungsten powders significantly affects the final alloy properties. The higher the tungsten content, the more noticeable the effect of the bimodal powder. The best bimodal W powder was the blend with 10 wt % of fine tungsten particles (10-Wf:90-Wc). These specimens present good values of densification and hardness, and higher values of thermal conductivity than other bimodal mixtures. PMID:28772502

Development of dispersion-strengthened XD (trademark) Cu alloys for high heat-flux applications

NASA Technical Reports Server (NTRS)

Kumar, K. Sharvan

1993-01-01

In a previous effort sponsored by NASA LeRC, the XD(trademark) process was used to produce ZrB2 particulate reinforcements in Cu and the resulting extruded material was microstructurally characterized and evaluated in tension over a range of temperatures. A problem that was encountered in that study was microstructural inhomogeneity resulting from the frequent presence of 'ZrB2 agglomerates' that were several microns in size. The presence of these agglomerates was attributed to improper mixing of powders in the green compact used in the XD process for elemental boron powder segregation. In this program, several milling parameters were examined in an effort to optimize this processing step; two levels of ZrB2 reinforcements were considered (7 vol. percent and 15 vol. percent). Microstructures of the reacted powder mass were examined to verify the absence of these agglomerates. Larger bathes of powder were then mixed, reacted, machined to size, canned, and extruded. The microstructure and tensile properties of these extrusions were examined, and the measured properties were correlated with the observed microstructure. Large unreacted or partially reacted Zr particles were present. These particles affected the mechanical properties deleteriously, and their presence is attributed to insufficient heat of reaction during XD synthesis. Alternate processing routes are recommended.

A review on recent technologies for the manufacture of pulmonary drugs.

PubMed

Hadiwinoto, Gabriela Daisy; Lip Kwok, Philip Chi; Lakerveld, Richard

2018-01-01

This review discusses recent developments in the manufacture of inhalable dry powder formulations. Pulmonary drugs have distinct advantages compared with other drug administration routes. However, requirements of drugs properties complicate the manufacture. Control over crystallization to make particles with the desired properties in a single step is often infeasible, which calls for micronization techniques. Although spray drying produces particles in the desired size range, a stable solid state may not be attainable. Supercritical fluids may be used as a solvent or antisolvent, which significantly reduces solvent waste. Future directions include application areas such as biopharmaceuticals for dry powder inhalers and new processing strategies to improve the control over particle formation such as continuous manufacturing with in-line process analytical technologies.

Stability and rheology of dispersions of silicon nitride and silicon carbide

NASA Technical Reports Server (NTRS)

Feke, Donald L.

1987-01-01

The relationship between the surface and colloid chemistry of commercial ultra-fine silicon carbide and silicon nitride powders was examined by a variety of standard characterization techniques and by methodologies especially developed for ceramic dispersions. These include electrokinetic measurement, surface titration, and surface spectroscopies. The effects of powder pretreatment and modification strategies, which can be utilized to augment control of processing characteristics, were monitored with these technologies. Both silicon carbide and nitride were found to exhibit silica-like surface chemistries, but silicon nitride powders possess an additional amine surface functionality. Colloidal characteristics of the various nitride powders in aqueous suspension is believed to be highly dependent on the relative amounts of the two types of surface groups, which in turn is determined by the powder synthesis route. The differences in the apparent colloidal characteristics for silicon nitride powders cannot be attributed to the specific absorption of ammonium ions. Development of a model for the prediction of double-layer characteristics of materials with a hybrid site interface facilitated understanding and prediction of the behavior of both surface charge and surface potential for these materials. The utility of the model in application to silicon nitride powders was demonstrated.

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

Ahmed, Sazzad Hossain; Mian, Ahsan, E-mail: ahsan.mian@wright.edu; Srinivasan, Raghavan

In DMLS process objects are fabricated layer by layer from powdered material by melting induced by a controlled laser beam. Metallic powder melts and solidifies to form a single layer. Solidification map during layer formation is an important route to characterize micro-structure and grain morphology of sintered layer. Generally, solidification leads to columnar, equiaxed or mixture of these two types grain morphology depending on solidification rate and thermal gradient. Eutectic or dendritic structure can be formed in fully equiaxed zone. This dendritic growth has a large effect on material properties. Smaller dendrites generally increase ductility of the layer. Thus, materialsmore » can be designed by creating desired grain morphology in certain regions using DMLS process. To accomplish this, hardness, temperature distribution, thermal gradient and solidification cooling rate in processed layers will be studied under change of process variables by using finite element analysis, with specific application to Ti-6Al-4V.« less

New Bond Coat Materials for Thermal Barrier Coating Systems Processed Via Different Routes

NASA Astrophysics Data System (ADS)

Soare, A.; Csaki, I.; Sohaciu, M.; Oprea, C.; Soare, S.; Costina, I.; Petrescu, M. I.

2017-06-01

This paper aims at describing the development of new Ru-based Bond Coats (BC) as part of Thermal Barrier Coatings. The challenge of this research was to obtain an adherent and uniform layer of alumina protective layer after high temperature exposure. We have prepared a RuAl 50/50 at% alloy in an induction furnace which was subsequently subjected to oxidation in an electric furnace, in air, at 1100C, for 10h and 100h. Mechanical alloying of Ru and Al powders was another processing route used in an attempt to obtain a stoichiometric RuAl. The alloy was sintered by Spark Plasma Sintering (SPS) and then oxidized at 1100C for 1 and10h. The alloys obtained as such were analysed before and after oxidation using advanced microscopy techniques (SEM and TEM). The encouraging results in case of RuAl alloys prepared by induction melting reveal that we obtained an adherent and uniform layer of alumina, free of delta-Ru. The results for the samples processed by powder metallurgy were positive but need to be further investigated. We should note here the novelty of this method for this particular type of application - as a BC part of a TBC system.

Demonstration of Shear Localization in Ultrafine Grained Tungsten Alloys via Powder Metallurgy Processing Route

DTIC Science & Technology

2012-09-01

of a di-tungsten boride (W2B) phase was not detected in the nW-B sample, but the low concentration of boron may have made this phase undetectable by...Split Hopkinson Bar UFG ultrafine grained W2B di-tungsten boride XRD x-ray diffraction NO. OF NO. OF COPIES ORGANIZATION COPIES

63. BUILDING NO. 1301, ORDNANCE FACILITY (MORTAR POWDER BUILDING), INTERIOR, ...

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

63. BUILDING NO. 1301, ORDNANCE FACILITY (MORTAR POWDER BUILDING), INTERIOR, LOOKING SOUTHEAST DOWN SCREENED WALKWAY ON NORTHWEST SIDE. - Picatinny Arsenal, State Route 15 near I-80, Dover, Morris County, NJ

Optimization of the Hot Forging Processing Parameters for Powder Metallurgy Fe-Cu-C Connecting Rods Based on Finite Element Simulation

NASA Astrophysics Data System (ADS)

Li, Fengxian; Yi, Jianhong; Eckert, Jürgen

2017-12-01

Powder forged connecting rods have the problem of non-uniform density distributions because of their complex geometric shape. The densification behaviors of powder metallurgy (PM) connecting rod preforms during hot forging processes play a significant role in optimizing the connecting rod quality. The deformation behaviors of a connecting rod preform, a Fe-3Cu-0.5C (wt pct) alloy compacted and sintered by the powder metallurgy route (PM Fe-Cu-C), were investigated using the finite element method, while damage and friction behaviors of the material were considered in the complicated forging process. The calculated results agree well with the experimental results. The relationship between the processing parameters of hot forging and the relative density of the connecting rod was revealed. The results showed that the relative density of the hot forged connecting rod at the central shank changed significantly compared with the relative density at the big end and at the small end. Moreover, the relative density of the connecting rod was sensitive to the processing parameters such as the forging velocity and the initial density of the preform. The optimum forging processing parameters were determined and presented by using an orthogonal design method. This work suggests that the processing parameters can be optimized to prepare a connecting rod with uniform density distribution and can help to better meet the requirements of the connecting rod industry.

Growing three-dimensional biomorphic graphene powders using naturally abundant diatomite templates towards high solution processability

PubMed Central

Chen, Ke; Li, Cong; Shi, Liurong; Gao, Teng; Song, Xiuju; Bachmatiuk, Alicja; Zou, Zhiyu; Deng, Bing; Ji, Qingqing; Ma, Donglin; Peng, Hailin; Du, Zuliang; Rümmeli, Mark Hermann; Zhang, Yanfeng; Liu, Zhongfan

2016-01-01

Mass production of high-quality graphene with low cost is the footstone for its widespread practical applications. We present herein a self-limited growth approach for producing graphene powders by a small-methane-flow chemical vapour deposition process on naturally abundant and industrially widely used diatomite (biosilica) substrates. Distinct from the chemically exfoliated graphene, thus-produced biomorphic graphene is highly crystallized with atomic layer-thickness controllability, structural designability and less noncarbon impurities. In particular, the individual graphene microarchitectures preserve a three-dimensional naturally curved surface morphology of original diatom frustules, effectively overcoming the interlayer stacking and hence giving excellent dispersion performance in fabricating solution-processible electrodes. The graphene films derived from as-made graphene powders, compatible with either rod-coating, or inkjet and roll-to-roll printing techniques, exhibit much higher electrical conductivity (∼110,700 S m−1 at 80% transmittance) than previously reported solution-based counterparts. This work thus puts forward a practical route for low-cost mass production of various powdery two-dimensional materials. PMID:27819652

Development of Oxide Dispersion Strengthened (ODS) Ferritic Steel Through Powder Forging

NASA Astrophysics Data System (ADS)

Kumar, Deepak; Prakash, Ujjwal; Dabhade, Vikram V.; Laha, K.; Sakthivel, T.

2017-04-01

Oxide dispersion strengthened (ODS) ferritic steels are candidates for cladding tubes in fast breeder nuclear reactors. In this study, an 18%Cr ODS ferritic steel was prepared through powder forging route. Elemental powders with a nominal composition of Fe-18Cr-2 W-0.2Ti (composition in wt.%) with 0 and 0.35% yttria were prepared by mechanical alloying in a Simoloyer attritor under argon atmosphere. The alloyed powders were heated in a mild steel can to 1473 K under flowing hydrogen atmosphere. The can was then hot forged. Steps of sealing, degassing and evacuation are eliminated by using powder forging. Heating ODS powder in hydrogen atmosphere ensures good bonding between alloy powders. A dense ODS alloy with an attractive combination of strength and ductility was obtained after re-forging. On testing at 973 K, a loss in ductility was observed in yttria-containing alloy. The strength and ductility increased with increase in strain rate at 973 K. Reasons for this are discussed. The ODS alloy exhibited a recrystallized microstructure which is difficult to achieve by extrusion. No prior particle boundaries were observed after forging. The forged compacts exhibited isotropic mechanical properties. It is suggested that powder forging may offer several advantages over the traditional extrusion/HIP routes for fabrication of ODS alloys.

Effect of process parameters on hardness, temperature profile and solidification of different layers processed by direct metal laser sintering (DMLS)

NASA Astrophysics Data System (ADS)

Ahmed, Sazzad Hossain; Mian, Ahsan; Srinivasan, Raghavan

2016-07-01

In DMLS process objects are fabricated layer by layer from powdered material by melting induced by a controlled laser beam. Metallic powder melts and solidifies to form a single layer. Solidification map during layer formation is an important route to characterize micro-structure and grain morphology of sintered layer. Generally, solidification leads to columnar, equiaxed or mixture of these two types grain morphology depending on solidification rate and thermal gradient. Eutectic or dendritic structure can be formed in fully equiaxed zone. This dendritic growth has a large effect on material properties. Smaller dendrites generally increase ductility of the layer. Thus, materials can be designed by creating desired grain morphology in certain regions using DMLS process. To accomplish this, hardness, temperature distribution, thermal gradient and solidification cooling rate in processed layers will be studied under change of process variables by using finite element analysis, with specific application to Ti-6Al-4V.

Nonequiatomic NiTi Alloy Produced by Self Propagating High Temperature Synthesis

NASA Astrophysics Data System (ADS)

Bassani, P.; Bassani, E.; Tuissi, A.; Giuliani, P.; Zanotti, C.

2014-07-01

Shape memory alloy NiTi in porous form is of high interest as implantable material, as low apparent elastic modulus, comparable to that of bone, can be achieved. This condition, combined with proper pore size, allows good osteointegration. Porous NiTi can be produced by self propagating high temperature synthesis (SHS), starting from mixed powders of pure Ni and Ti. Process parameters, among which powder compaction degree and preheating temperature, strongly influence the reaction temperature and the resulting product: at low reaction temperatures, high quantity of secondary phases are formed, which are generally considered detrimental for biocompatibility. On the contrary, at higher reaction temperatures, the powders melt and crystallize in ingots. The porous structure is lost and huge pores are formed. Mechanical activation of powders through ball milling and addition of TiH x are investigated as means to reduce reaction temperature and overheating, in order to preserve high porosity and limit secondary phases content. Both processes affect SHS reaction, and require adjustment of parameters such as heating rate. Changes in porous shape and size were observed especially for TiH x additions: the latter could be a promising route to obtain shaped porous products of improved quality.

Neutron diffraction studies for realtime leaching of catalytic Ni

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

Iles, Gail N., E-mail: gail.iles@helmholtz-berlin.de; Reinhart, Guillaume, E-mail: guillaume.reinhart@im2np.fr; Institut Laue-Langevin, 6 rue Jules Horowitz, BP 156, 38042 Grenoble

2014-07-21

The leaching of Al from intermetallic samples of Nickel Aluminium alloys to form Raney-type nickel catalysts is widely used in the hydrogenation industry, however, little is known of the leaching process itself. In this study, the leaching of Al was measured in realtime, in situ, using the high-flux powder neutron diffractometer, D20, at the Institut Laue-Langevin. Despite the liberation of hydrogen and effervescent nature of the reaction the transformation of the dry powder phases into Raney-type Ni was determined. Samples produced by gas-atomisation were found to leach faster than those produced using the cast and crushed technique. Regardless of processingmore » route of the precursor powder, the formation of spongy-Ni occurs almost immediately, while Ni{sub 2}Al{sub 3} and NiAl{sub 3} continue to transform over longer periods of time. Small-angle scattering and broadening of the diffraction peaks is an evidence for the formation of the smaller Ni particles. Understanding the kinetics of the leaching process will allow industry to refine production of catalysts for optimum manufacturing time while knowledge of leaching dynamics of powders produced by different manufacturing techniques will allow further tailoring of catalytic materials.« less

Mechanical behaviour of pressed and sintered CP Ti and Ti-6Al-7Nb alloy obtained from master alloy addition powder.

PubMed

Bolzoni, L; Weissgaerber, T; Kieback, B; Ruiz-Navas, E M; Gordo, E

2013-04-01

The Ti-6Al-7Nb alloy was obtained using the blending elemental approach with a master alloy and elemental titanium powders. Both the elemental titanium and the Ti-6Al-7Nb powders were characterised using X-ray diffraction, differential thermal analysis and dilatometry. The powders were processed using the conventional powder metallurgy route that includes uniaxial pressing and sintering. The trend of the relative density with the sintering temperature and the microstructural evolution of the materials sintered at different temperatures were analysed using scanning electron microscopy and X-ray diffraction. A minimum sintering temperature of 1200°C has to be used to ensure the homogenisation of the alloying elements and to obtain a pore structure composed of spherical pores. The sintered samples achieve relative density values that are typical for powder metallurgy titanium and no intermetallic phases were detected. Mechanical properties comparable to those specified for wrought Ti-6Al-7Nb medical devices are normally obtained. Therefore, the produced materials are promising candidates for load bearing applications as implant materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

Novel pre-alloyed powder processing of modified alnico 8: Correlation of microstructure and magnetic properties

DOE PAGES

Anderson, I. E.; Kassen, A. G.; White, E. M. H.; ...

2015-04-13

Progress is reviewed on development of an improved near-final bulk magnet fabrication process for alnico 8, as a non-rare earth permanent magnet with promise for sufficient energy density and coercivity for electric drive motors. This study showed that alnico bulk magnets in near-final shape can be made by simple compression molding from spherical high purity gas atomized pre-alloyed powder. Dwell time at peak sintering temperature (1250°C) greatly affected grain size of the resulting magnet alloys. This microstructure transformation was demonstrated to be useful for gaining partially aligned magnetic properties and boosting energy product. Furthermore, while a route to increased coercivitymore » was not identified by these experiments, manufacturability of bulk alnico magnet alloys in near-final shapes was demonstrated, permitting further processing and alloy modification experiments that can target higher coercivity and better control of grain anisotropy during grain growth.« less

Preparation and in vivo absorption evaluation of spray dried powders containing salmon calcitonin loaded chitosan nanoparticles for pulmonary delivery

PubMed Central

Sinsuebpol, Chutima; Chatchawalsaisin, Jittima; Kulvanich, Poj

2013-01-01

Purpose The aim of the present study was to prepare inhalable co-spray dried powders of salmon calcitonin loaded chitosan nanoparticles (sCT-CS-NPs) with mannitol and investigate pulmonary absorption in rats. Methods The sCT-CS-NPs were prepared by the ionic gelation method using sodium tripolyphosphate (TPP) as a cross-linking polyion. Inhalable dry powders were obtained by co-spray drying aqueous dispersion of sCT-CS-NPs and mannitol. sCT-CS-NPs co-spray dried powders were characterized with respect to morphology, particle size, powder density, aerodynamic diameter, protein integrity, in vitro release of sCT, and aerosolization. The plasmatic sCT levels following intratracheal administration of sCT-CS-NPs spray dried powders to the rats was also determined. Results sCT-CS-NPs were able to be incorporated into mannitol forming inhalable microparticles by the spray drying process. The sCT-CS-NPs/mannitol ratios and spray drying process affected the properties of the microparticles obtained. The conformation of the secondary structures of sCTs was affected by both mannitol content and spray dry inlet temperature. The sCT-CS-NPs were recovered after reconstitution of spray dried powders in an aqueous medium. The sCT release profile from spray dried powders was similar to that from sCT-CS-NPs. In vitro inhalation parameters measured by the Andersen cascade impactor indicated sCT-CS-NPs spray dried powders having promising aerodynamic properties for deposition in the deep lung. Determination of the plasmatic sCT levels following intratracheal administration to rats revealed that the inhalable sCT-CS NPs spray dried powders provided higher protein absorption compared to native sCT powders. Conclusion The sCT-CS-NPs with mannitol based spray dried powders were prepared to have appropriate aerodynamic properties for pulmonary delivery. The developed system was able to deliver sCT via a pulmonary route into the systemic circulation. PMID:24039397

Preparation and in vivo absorption evaluation of spray dried powders containing salmon calcitonin loaded chitosan nanoparticles for pulmonary delivery.

PubMed

Sinsuebpol, Chutima; Chatchawalsaisin, Jittima; Kulvanich, Poj

2013-01-01

The aim of the present study was to prepare inhalable co-spray dried powders of salmon calcitonin loaded chitosan nanoparticles (sCT-CS-NPs) with mannitol and investigate pulmonary absorption in rats. The sCT-CS-NPs were prepared by the ionic gelation method using sodium tripolyphosphate (TPP) as a cross-linking polyion. Inhalable dry powders were obtained by co-spray drying aqueous dispersion of sCT-CS-NPs and mannitol. sCT-CS-NPs co-spray dried powders were characterized with respect to morphology, particle size, powder density, aerodynamic diameter, protein integrity, in vitro release of sCT, and aerosolization. The plasmatic sCT levels following intratracheal administration of sCT-CS-NPs spray dried powders to the rats was also determined. sCT-CS-NPs were able to be incorporated into mannitol forming inhalable microparticles by the spray drying process. The sCT-CS-NPs/mannitol ratios and spray drying process affected the properties of the microparticles obtained. The conformation of the secondary structures of sCTs was affected by both mannitol content and spray dry inlet temperature. The sCT-CS-NPs were recovered after reconstitution of spray dried powders in an aqueous medium. The sCT release profile from spray dried powders was similar to that from sCT-CS-NPs. In vitro inhalation parameters measured by the Andersen cascade impactor indicated sCT-CS-NPs spray dried powders having promising aerodynamic properties for deposition in the deep lung. Determination of the plasmatic sCT levels following intratracheal administration to rats revealed that the inhalable sCT-CS NPs spray dried powders provided higher protein absorption compared to native sCT powders. The sCT-CS-NPs with mannitol based spray dried powders were prepared to have appropriate aerodynamic properties for pulmonary delivery. The developed system was able to deliver sCT via a pulmonary route into the systemic circulation.

Processing of sintered alpha SiC

NASA Technical Reports Server (NTRS)

Storm, R. S.

1984-01-01

Processing methods of sintered alpha SiC for engine applications are developed in a cost effective manner, using a submicron sized powder blended with sintering aids (boron and carbon). The processes for forming a green powder compact, such as dry pressing, cold isostatic pressing and green machining, slip casting, aqueous extrusion, plastic extrusion, and injection molding, are described. Dry pressing is the simplest route to component fabrication, and is carried out at approximately 10,000 psi pressure, while in the cold isostatic method the pressure could go as high as 20,000 psi. Surfactants are added to control settling rates and casting characteristics in the slip casting. The aqueous extrusion process is accomplished by a hydraulic ram forcing the aqueous mixture through a die. The plastic forming processes of extrusion and injection molding offer the potential of greater diversity in shape capacity. The physical properties of sintered alpha SiC (hardness, Young's modulus, shear modulus, and thermal diffusivity) are extensively tested. Corrosion resistance test results of silicon carbide are included.

Processing, phase equilibria and environmental degradation of molybdenum (silicom,aluminum)(2) intermetallic compound

NASA Astrophysics Data System (ADS)

Eason, Paul Duane

The Mo(Si,Al)2 C40 compound was chosen for investigation as a possible high temperature structural material. To produce the C40 phase, several processing routes were explored with emphasis on obtaining microstructure/property relationships (i.e. control of grain size and minimization of secondary phases). To facilitate processing of single phase material, the phase equilibria of the Mo-Si-Al ternary system were reevaluated with respect to the phases adjacent to the C40 compound. An anomalous environmental degradation appeared to be the primary obstacle to further study of the compound and was investigated accordingly. Several processing routes were assessed for the production of dense, nearly single-phase Mo(Si,Al)2. Hot powder compaction was chosen as the method of sample production as is the case with many refractory silicide based materials. Therefore, variations in the processing techniques came from the choice of precursor materials and methods of powder production. Mechanical alloying, arc-melting and comminution, and blending of both elemental and compound powders were all employed to produce charges for hot uniaxial pressing. The final compacts were compared on the basis of density, grain size and presence of secondary phases. Establishment of a Mo-Si-Al ternary isothermal phase diagram at 1400°C was performed. Multiphase alloy compositions were selected to identify the phase boundaries of the C40, C54, T1 and Mo3Al8 phase fields, as well as to verify the existence of the C54 phase at 1400°C. The alloys were equilibrated by heat treatment and analyzed for phase identification and quantitative compositional information. The environmental degradation phenomenon was approached as a classical "pest" with an emphasis of study on grain boundary chemistry and atmospheric dependence of attack. Both Auger spectroscopy and electron microscopy revealed carbon-impurity-induced grain boundary segregation responsible for the embrittlement and material loss. Means of preventing the attack by alloying techniques used in traditional alloys were explored.

Biocompatibility of Advanced Manufactured Titanium Implants-A Review.

PubMed

Sidambe, Alfred T

2014-12-19

Titanium (Ti) and its alloys may be processed via advanced powder manufacturing routes such as additive layer manufacturing (or 3D printing) or metal injection moulding. This field is receiving increased attention from various manufacturing sectors including the medical devices sector. It is possible that advanced manufacturing techniques could replace the machining or casting of metal alloys in the manufacture of devices because of associated advantages that include design flexibility, reduced processing costs, reduced waste, and the opportunity to more easily manufacture complex or custom-shaped implants. The emerging advanced manufacturing approaches of metal injection moulding and additive layer manufacturing are receiving particular attention from the implant fabrication industry because they could overcome some of the difficulties associated with traditional implant fabrication techniques such as titanium casting. Using advanced manufacturing, it is also possible to produce more complex porous structures with improved mechanical performance, potentially matching the modulus of elasticity of local bone. While the economic and engineering potential of advanced manufacturing for the manufacture of musculo-skeletal implants is therefore clear, the impact on the biocompatibility of the materials has been less investigated. In this review, the capabilities of advanced powder manufacturing routes in producing components that are suitable for biomedical implant applications are assessed with emphasis placed on surface finishes and porous structures. Given that biocompatibility and host bone response are critical determinants of clinical performance, published studies of in vitro and in vivo research have been considered carefully. The review concludes with a future outlook on advanced Ti production for biomedical implants using powder metallurgy.

Biocompatibility of Advanced Manufactured Titanium Implants—A Review

PubMed Central

Sidambe, Alfred T.

2014-01-01

Titanium (Ti) and its alloys may be processed via advanced powder manufacturing routes such as additive layer manufacturing (or 3D printing) or metal injection moulding. This field is receiving increased attention from various manufacturing sectors including the medical devices sector. It is possible that advanced manufacturing techniques could replace the machining or casting of metal alloys in the manufacture of devices because of associated advantages that include design flexibility, reduced processing costs, reduced waste, and the opportunity to more easily manufacture complex or custom-shaped implants. The emerging advanced manufacturing approaches of metal injection moulding and additive layer manufacturing are receiving particular attention from the implant fabrication industry because they could overcome some of the difficulties associated with traditional implant fabrication techniques such as titanium casting. Using advanced manufacturing, it is also possible to produce more complex porous structures with improved mechanical performance, potentially matching the modulus of elasticity of local bone. While the economic and engineering potential of advanced manufacturing for the manufacture of musculo-skeletal implants is therefore clear, the impact on the biocompatibility of the materials has been less investigated. In this review, the capabilities of advanced powder manufacturing routes in producing components that are suitable for biomedical implant applications are assessed with emphasis placed on surface finishes and porous structures. Given that biocompatibility and host bone response are critical determinants of clinical performance, published studies of in vitro and in vivo research have been considered carefully. The review concludes with a future outlook on advanced Ti production for biomedical implants using powder metallurgy. PMID:28788296

Understanding microstrain anisotropy in yttrium oxide synthesized by sol-gel route

NASA Astrophysics Data System (ADS)

Murugesan, S.; Thirumurugesan, R.; Parameswaran, P.

2018-04-01

Yttrium oxide was synthesized by wet chemical route and calcined at various temperatures. On x-ray diffraction analysis of the material using Williamson-Hall analysis followed by Rietveld analysis indicates that the powder exists in nano crystallite size with lattice strain. The spherical harmonics analysis model of microstrain indicates the presence of strain anisotropy. The change in crystal structure lattice parameter, atomic coordinates of Y, O in yttria and the bond length analysis of the calcined powder reveals the presence of oxygen vacancies in the system.

103. Photocopied 1983, from original drawing (DP49213), Picatinny Arsenal, NOVEMBER ...

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

103. Photocopied 1983, from original drawing (DP-49213), Picatinny Arsenal, NOVEMBER 23, 1945. ROLLED POWDER AREA FINISHING PLANT: FLOW DIAGRAM.' - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Spray‐Dried Sodium Zirconate: A Rapid Absorption Powder for CO2 Capture with Enhanced Cyclic Stability

PubMed Central

Bamiduro, Faith; Ji, Guozhao; Brown, Andy P.; Dupont, Valerie A.

2017-01-01

Abstract Improved powders for capturing CO2 at high temperatures are required for H2 production using sorption‐enhanced steam reforming. Here, we examine the relationship between particle structure and carbonation rate for two types of Na2ZrO3 powders. Hollow spray‐dried microgranules with a wall thickness of 100–300 nm corresponding to the dimensions of the primary acetate‐derived particles gave about 75 wt % theoretical CO2 conversion after a process‐relevant 5 min exposure to 15 vol % CO2. A conventional powder prepared by solid‐state reaction carbonated more slowly, achieving only 50 % conversion owing to a greater proportion of the reaction requiring bulk diffusion through the densely agglomerated particles. The hollow granular structure of the spray‐dried powder was retained postcarbonation but chemical segregation resulted in islands of an amorphous Na‐rich phase (Na2CO3) within a crystalline ZrO2 particle matrix. Despite this phase separation, the reverse reaction to re‐form Na2ZrO3 could be achieved by heating each powder to 900 °C in N2 (no dwell time). This resulted in a very stable multicycle performance in 40 cycle tests using thermogravimetric analysis for both powders. Kinetic analysis of thermogravimetric data showed the carbonation process fits an Avrami–Erofeyev 2 D nucleation and nuclei growth model, consistent with microstructural evidence of a surface‐driven transformation. Thus, we demonstrate that spray drying is a viable processing route to enhance the carbon capture performance of Na2ZrO3 powder. PMID:28371521

Wet powder processing of sol-gel derived mesoporous silica-hydroxyapatite hybrid powders.

PubMed

Andersson, Jenny; Johannessen, Espen; Areva, Sami; Järn, Mikael; Lindén, Mika

2006-08-01

This paper describes a method by which a porous silica coating layer can be obtained on different apatite particles through a simple sol-gel synthesis route. Sol-gel derived powders of hydroxyapatite (HAP) and beta tricalciumphosphate (beta-TCP) were coated with a mesoporous silica using C16TAB (hexadecyltrimethylammonium bromide) as a template in order to induce mesophase formation. Further calcination of the material removes the template from the mesophase and leaves a highly ordered hexagonal arranged mesoporous silica structure with a core of HAP/beta-TCP. The phase purity of the SiO2/apatite composites has been thoroughly investigated by the means of FT-IR, XRD, and solid state 31P MAS NMR. The phase purity of these materials is shown to be dependent on the solubility properties of the used apatites. The hybrid materials are suitable as a multifunctional biomaterial where osteoconductive properties can be combined with drug delivery.

Effect of Annealing on Mechanical Properties and Formability of Cold Rolled Thin Sheets of Fe-P P/M Alloys

NASA Astrophysics Data System (ADS)

Trivedi, Shefali; Ravi Kumar, D.; Aravindan, S.

2016-10-01

Phosphorus in steel is known to increase strength and hardness and decrease ductility. Higher phosphorus content (more than 0.05%), however, promotes brittle behavior due to segregation of Fe3P along the grain boundaries which makes further mechanical working of these alloys difficult. In this work, thin sheets of Fe-P alloys (with phosphorus in range of 0.1-0.35%) have been developed through processing by powder metallurgy followed by hot rolling and cold rolling. The effect of phosphorus content and annealing parameters (temperature and time) on microstructure, mechanical properties, formability in biaxial stretching and fracture behavior of the cold rolled and annealed sheets has been studied. A comparison has also been made between the properties of the sheets made through P/M route and the conventional cast route with similar phosphorus content. It has been shown that thin sheets of Fe-P alloys with phosphorous up to 0.35% possessing a good combination of strength and formability can be produced through rolling of billets of these alloys made through powder metallurgy technique without the problem of segregation.

Effect of freeze-drying and self-ignition process on the microstructural and electrochemical properties of Li{sub 4}Ti{sub 5}O{sub 12}

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

Jamin, Claire; Traina, Karl; APTIS, Department of Physics, B5a, University of Liège, Sart-Tilman, 4000 Liège

2013-11-15

Graphical abstract: - Highlights: • Li{sub 4}Ti{sub 5}O{sub 12} is prepared by a method involving self-ignition of a freeze-dried gel. • Addition of NH{sub 4}NO{sub 3} modifies the self-ignition propagation mode. • Well-crystallized Li{sub 4}Ti{sub 5}O{sub 12} phase is obtained after only 2 h at 800 °C. • Li{sub 4}Ti{sub 5}O{sub 12} powder has 161 mAh g{sup −1} capacity and good retention at C/4 rate. - Abstract: Crystalline Li{sub 4}Ti{sub 5}O{sub 12} is synthesized by a method involving the freeze-drying and self-ignition of a gel prepared from titanium isopropoxide, lithium nitrate and hydroxypropylmethylcellulose (HPMC). This synthesis route yields crystalline Li{submore » 4}Ti{sub 5}O{sub 12} particles after calcination at 800 °C for 2 h. In an alternative route, addition of ammonium nitrate shifts the self-ignition mode from wave-like propagation to simultaneous. Powders with different microstructures are thereby obtained. Electrochemical characterization shows that the best results for Li{sup +} intercalation/desintercalation are obtained for the powder prepared without ammonium nitrate addition. These results highlight the necessity for a control of the self-ignition mode to obtain adequate properties.« less

Influence of sintering temperature on the phases and photoelectric characteristics of BiOCl/ZnO composite powders

NASA Astrophysics Data System (ADS)

Chen, Song; Zhu, De-gui

2017-12-01

Zinc oxide is a typical functional oxide that has been widely researched for various industry applications due to its peculiar physical characteristics. However, to achieve its potential in promising applications, much work has been diligently performed to improve the physical properties of ZnO. In this work, an aqueous suspension route was used to prepare BiOCl/ZnO composite powders, and sintering processes were applied to investigate the influence of sintering temperature on the phase evolutions, microstructures, and photoelectric characteristics of BiOCl/ZnO composite powders. The results indicated that the photoelectric properties mainly depend on the relevant content of BiOCl in the composite powders and the sintering temperature. The photoelectric measurements in K2SO4 solutions show that the photoelectric properties of the samples with the appropriate BiOCl content (0.3mol% and 2.0mol%) are better than those of ZnO and commercial TiO2 (P25) powders, but the photoelectric measurements in NaOH solutions indicate that the photoelectric characteristics of the as-sintered samples are only better than those of P25.

Synthesis of nanocrystalline Ni/Ce-YSZ powder via a polymerization route

NASA Astrophysics Data System (ADS)

Abolghasemi, Z.; Tamizifar, M.; Arzani, K.; Nemati, A.; Khanfekr, A.; Bolandi, M.

2013-08-01

Pechini process was used for preparation of three kinds of nanocrystalline powders of yttria-stabilized zirconia (YSZ): doped with 1.5 mol% nickel oxide, doped with 15 mol% ceria, and doped with 1.5 mol% nickel oxide plus 15 mol% ceria. Zirconium chloride, yttrium nitrate, cerium nitrate, nickel nitrate, citric acid and ethylene glycol were polymerized at 80 °C to produce a gel. XRD, SEM and TEM analyses were used to investigate the crystalline phases and microstructures of obtained compounds. The results of XRD revealed the formation of nanocrystalline powder at 900 °C. Morphology of the powder calcined at 900 °C, examined with a scanning electron microscope, showed that the presence of nickel and cerium inhibited the grain growth in the system. The average crystallite size of the material doped with nickel oxide (9.33 nm) was bigger than the one doped with cerium oxide (9.29 nm), while the YSZ doping with the two oxides simultaneously promoted the grain growth with crystallite size of 11.37 nm. Yttria-stabilized zirconia powder with a mean crystallite size of 9.997 nm was prepared successfully by this method.

Effect of annealing on the structural and optical properties of TiO2 powder prepared by sol-gel route

NASA Astrophysics Data System (ADS)

Halder, Nilanjan; Misra, Kamakhya Prakash

2016-05-01

Using titanium isopropoxide as the precursor, Titanium dioxide (TiO2) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO2 samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increase with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO2 nano powder samples.

Development of Cu Reinforced SiC Particulate Composites

NASA Astrophysics Data System (ADS)

Singh, Harshpreet; Kumar, Lailesh; Nasimul Alam, Syed

2015-02-01

This paper presents the results of Cu-SiCp composites developed by powder metallurgy route and an attempt has been made to make a comparison between the composites developed by using unmilled Cu powder and milled Cu powder. SiC particles as reinforcement was blended with unmilled and as-milled Cu powderwith reinforcement contents of 10, 20, 30, 40 vol. % by powder metallurgy route. The mechanical properties of pure Cu and the composites developed were studied after sintering at 900°C for 1 h. Density of the sintered composites were found out based on the Archimedes' principle. X-ray diffraction of all the composites was done in order to determine the various phases in the composites. Scanning electron microscopy (SEM) and EDS (electron diffraction x-ray spectroscopy) was carried out for the microstructural analysis of the composites. Vickers microhardness tester was used to find out the hardness of the samples. Wear properties of the developed composites were also studied.

Solution-Processed Cu2ZnSn(S,Se) 4 Thin-Film Solar Cells Using Elemental Cu, Zn, Sn, S, and Se Powders as Source.

PubMed

Guo, Jing; Pei, Yingli; Zhou, Zhengji; Zhou, Wenhui; Kou, Dongxing; Wu, Sixin

2015-12-01

Solution-processed approach for the deposition of Cu2ZnSn (S,Se)4 (CZTSSe) absorbing layer offers a route for fabricating thin film solar cell that is appealing because of simplified and low-cost manufacturing, large-area coverage, and better compatibility with flexible substrates. In this work, we present a simple solution-based approach for simultaneously dissolving the low-cost elemental Cu, Zn, Sn, S, and Se powder, forming a homogeneous CZTSSe precursor solution in a short time. Dense and compact kesterite CZTSSe thin film with high crystallinity and uniform composition was obtained by selenizing the low-temperature annealed spin-coated precursor film. Standard CZTSSe thin film solar cell based on the selenized CZTSSe thin film was fabricated and an efficiency of 6.4 % was achieved.

The effect of process parameters in Aluminum Metal Matrix Composites with Powder Metallurgy

NASA Astrophysics Data System (ADS)

Vani, Vemula Vijaya; Chak, Sanjay Kumar

2018-06-01

Metal Matrix Composites are developed in recent years as an alternative over conventional engineering materials due to their improved properties. Among all, Aluminium Matrix Composites (AMCs) are increasing their demand due to low density, high strength-to-weight ratio, high toughness, corrosion resistance, higher stiffness, improved wear resistance, increased creep resistance, low co-efficient of thermal expansion, improved high temperature properties. Major applications of these materials have been in aerospace, automobile, military. There are different processing techniques for the fabrication of AMCs. Powder metallurgy is a one of the most promising and versatile routes for fabrication of particle reinforced AMCs as compared to other manufacturing methods. This method ensures the good wettability between matrix and reinforcement, homogeneous microstructure of the fabricated MMC, and prevents the formation of any undesirable phases. This article addresses mainly on the effect of process parameters like sintering time, temperature and particle size on the microstructure of aluminum metal matrix composites.

15. BUILDING NO. 445, PHYSICS LAB (FORMERLY GUN BAG LOADING), ...

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

15. BUILDING NO. 445, PHYSICS LAB (FORMERLY GUN BAG LOADING), INTERIOR, FOURTH LEVEL. POWDER HOPPER AT TOP OF ELEVATOR SHAFT. POWDER DISTRIBUTED FROM HERE TO LOADING ROOMS BY TUBES. - Picatinny Arsenal, 400 Area, Gun Bag Loading District, State Route 15 near I-80, Dover, Morris County, NJ

Low cost synthesis of TiO2-C nanocomposite powder for high efficiency visible light photocatalysis

NASA Astrophysics Data System (ADS)

Mohapatra, A. K.; Nayak, J.

2018-04-01

Titanium dioxide-carbon nanocomposite powder was synthesized via a low cost chemical route using oleic acid and titanium tetra-isopropoxide. Since the carbon remained mainly on the surface of the TiO2 nanoparticles, the powder had black color. The composition of the powder was analyzed by X-ray photoelectron spectroscopy and the structure was studied with X-ray diffraction and transmission electron microscopy. The visible photocatalytic activity of the black TiO2 powder was investigated by studying the photo-bleaching of methylene blue under visible light. Our experimental observation showed that the black-TiO2 powder had a higher visible photocatalytic activity compared to the commercial TiO2 powder (P25 Degussa).

The influence of surface active l-leucine and 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC) in the improvement of aerosolization of pyrazinamide and moxifloxacin co-spray dried powders.

PubMed

Eedara, Basanth Babu; Rangnekar, Bhamini; Doyle, Colin; Cavallaro, Alex; Das, Shyamal C

2018-05-05

Pharmacotherapy of tuberculosis is potentially more efficient when delivered by the inhaled route than by the current oral and/or parenteral routes due to the higher concentration of drug reaching the primary region of infection in the lungs. This study investigated the influence of the amino acid l-leucine alone and in combination with the phospholipid, 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC), on the aerosolization behaviour of the anti-TB drugs, pyrazinamide and moxifloxacin HCl. Spray dried powders of pyrazinamide (P), moxifloxacin (M) alone and in combination with 10% l-leucine (PL and ML) and 10% DPPC (PLD and MLD) were produced. The particle sizes of all powders except P were in the inhalable size range (<5 µm) but differ in their morphology in presence of the excipients. X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) revealed the migration of surface active l-leucine and DPPC onto the surface of the particles during the spray drying process. The aerosolization from a dry powder inhaler, Aerolizer ® , using a Next Generation Impactor revealed fine particle fraction (FPF) values for P, PL and PLD of 18.7 ± 3.4%, 53.0 ± 3.2% and 74.5 ± 5.3% respectively while FPF values for M, ML and MLD were 55.6 ± 3.3%, 74.7 ± 4.7% and 74.1 ± 1.3% respectively. In conclusion, the differences in the aerosolization behaviours of the pyrazinamide and moxifloxacin spray dried powders with and without excipients was a combination of difference in the surface morphology and surface composition. Copyright © 2018 Elsevier B.V. All rights reserved.

Mechanisms of Precipitation of Different Generations of Gamma-Prime Precipitates During Continuous Cooling of a Nickel Base Superalloy (PREPRINT)

DTIC Science & Technology

2012-08-01

processed through the powder metallurgy route and develops a polycrystalline microstructure consisting of γ grains with nanoscale γ’ precipitates...on the cooling rate employed. Faster cooling rates, such as those encountered during water quenching the alloy from the high temperature single γ...and the first generation γ’ precipitates. Subsequently on quenching to a lower temperature a second generation of γ’ precipitates are formed that are

Direct and continuous synthesis of VO2 nanoparticles

NASA Astrophysics Data System (ADS)

Powell, M. J.; Marchand, P.; Denis, C. J.; Bear, J. C.; Darr, J. A.; Parkin, I. P.

2015-11-01

Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.

Direct and continuous synthesis of VO2 nanoparticles.

PubMed

Powell, M J; Marchand, P; Denis, C J; Bear, J C; Darr, J A; Parkin, I P

2015-11-28

Monoclinic VO2 nanoparticles are of interest due to the material's thermochromic properties, however, direct synthesis routes to VO2 nanoparticles are often inaccessible due to the high synthesis temperatures or long reaction times required. Herein, we present a two-step synthesis route for the preparation of monoclinic VO2 nanoparticles using Continuous Hydrothermal Flow Synthesis (CHFS) followed by a short post heat treatment step. A range of particle sizes, dependent on synthesis conditions, were produced from 50 to 200 nm by varying reaction temperatures and the residence times in the process. The nanoparticles were characterised by powder X-ray diffraction, Raman and UV/Vis spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The nanoparticles were highly crystalline with rod and sphere-like morphologies present in TEM micrographs, with the size of both the rod and spherical particles being highly dependent on both reaction temperature and residence time. SEM micrographs showed the surface of the powders produced from the CHFS process to be highly uniform. The samples were given a short post synthesis heat treatment to ensure that they were phase pure monoclinic VO2, which led to them exhibiting a large and reversible switch in optical properties (at near-IR wavelengths), which suggests that if such materials can be incorporated into coatings or in composites, they could be used for fenestration in architectural applications.

Chromium Extraction via Chemical Processing of Fe-Cr Alloys Fine Powder with High Carbon Content

NASA Astrophysics Data System (ADS)

Torres, D. M.; Navarro, R. C. S.; Souza, R. F. M.; Brocchi, E. A.

2017-06-01

Ferrous alloys are important raw materials for special steel production. In this context, alloys from the Fe-Cr system, with typical Cr weight fraction ranging from 0.45 to 0.95, are prominent, particularly for the stainless steel industry. During the process in which these alloys are obtained, there is considerable production of fine powder, which could be reused after suitable chemical treatment, for example, through coupling pyrometallurgical and hydrometallurgical processes. In the present study, the extraction of chromium from fine powder generated during the production of a Fe-Cr alloy with high C content was investigated. Roasting reactions were performed at 1073 K, 1173 K, and 1273 K (800 °C, 900 °C, and 1000 °C) with 300 pct (w/w) excess NaOH in an oxidizing atmosphere (air), followed by solubilization in deionized water, selective precipitation, and subsequent calcination at 1173 K (900 °C) in order to convert the obtained chromium hydroxide to Cr2O3. The maximum achieved Cr recovery was around 86 pct, suggesting that the proposed chemical route was satisfactory regarding the extraction of the chromium initially present. Moreover, after X-ray diffraction analysis, the final produced oxide has proven to be pure Cr2O3 with a mean crystallite size of 200 nm.

Synthesis of nano-titanium dioxide by sol-gel route

NASA Astrophysics Data System (ADS)

Kaler, Vandana; Duchaniya, R. K.; Pandel, U.

2016-04-01

Nanosized titanium dioxide powder was synthesised via sol-gel route by hydrolysis of titanium tetraisopropoxide with ethanol and water mixture in high acidic medium. The synthesized nanopowder was further characterized by X-ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and Ultraviolet Visible Spectroscopy in order to determine size, morphology and crystalline structure of the material. The synthesis of nano-TiO2 powder in anatase phase was realized by XRD. The optical studies of nano-TiO2 powder was carried out by UV-Vis spectroscopy and band gap was calculated as 3.5eV, The SEM results with EDAX confirmed that prepared nano-TiO2 particles were in nanometer range with irregular morphology. The FTIR analysis showed that only desired functional groups were present in sample. These nano-TiO2 particles have applications in solar cells, chemical sensors and paints, which are thrust areas these days.

Powder Injection Molding for mass production of He-cooled divertor parts

NASA Astrophysics Data System (ADS)

Antusch, S.; Norajitra, P.; Piotter, V.; Ritzhaupt-Kleissl, H.-J.

2011-10-01

A He-cooled divertor for future fusion power plants has been developed at KIT. Tungsten and tungsten alloys are presently considered the most promising materials for functional and structural divertor components. The advantages of tungsten materials lie, e.g. in the high melting point, and low activation, the disadvantages are high hardness and brittleness. The machinig of tungsten, e.g. milling, is very complex and cost-intensive. Powder Injection Molding (PIM) is a method for cost effective mass production of near-net-shape parts with high precision. The complete W-PIM process route is outlined and, results of product examination discussed. A binary tungsten powder feedstock with a grain size distribution in the range 0.7-1.7 μm FSSS, and a solid load of 50 vol.% was developed. After heat treatment, the successfully finished samples showed promising results, i.e. 97.6% theoretical density, a grain size of approximately 5 μm, and a hardness of 457 HV0.1.

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

Ay, H.; Özyurek, D.; Yıldırım, M., E-mail: musayildirim@karabuk.edu.tr

In this study, the wear properties of in-situ 7075 Al-Ti composites produced by powder metallurgy route were investigated. Different amount of Ti (2, 4, 6 %) added to gas atomized 7075 Al alloy powders and they were mixed in turbula with 47rpm for 45 minutes. Then the mixed powders were pre-shaped by press under 600 MPa pressure. The samples were cooled in the furnace after sintered at 580 °C for 4 hours in the atmosphere controlled furnace. Standard metallographic process such as grinding, polishing and etching were applied to sintered samples. The hardness values were measured. Scanning Electron Microscope (SEM), X-Raymore » Diffraction (XRD) examines were carried out. The wear tests were performed in a pin-on disc type wear apparatus with 1 ms{sup −1} sliding speed at six different sliding distance (500-3000 m) under 30 N loads. As a result of studies, hardness values were increased with increasing Ti content, in addition the weight losses were decreased with increasing Ti amount.« less

The Coast Artillery Journal. Volume 58, Number 2, February 1923

DTIC Science & Technology

1923-02-01

firing mechanism block with a fresh primer in place. No.5 acted as a powder runner between the powder pit and No.2. Nos. 6 and 7 carried the loading...obstruct these routes. Xumerous passive obstructions have been conceived: metallic cables raised and maintained in the air by kites ; cables shot into the

Effect of annealing on the structural and optical properties of TiO{sub 2} powder prepared by sol-gel route

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

Halder, Nilanjan; Misra, Kamakhya Prakash

2016-05-06

Using titanium isopropoxide as the precursor, Titanium dioxide (TiO{sub 2}) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO{sub 2} samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increasemore » with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO{sub 2} nano powder samples.« less

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering.

PubMed

Musa, Clara; Licheri, Roberta; Orrù, Roberto; Cao, Giacomo; Sciti, Diletta; Silvestroni, Laura; Zoli, Luca; Balbo, Andrea; Mercatelli, Luca; Meucci, Marco; Sani, Elisa

2016-06-18

In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS) after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS) followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa) is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C) could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1-2.4) in the 1000-1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers.

Alterations of thorium oxalate morphology by changing elementary precipitation conditions

NASA Astrophysics Data System (ADS)

Tyrpekl, V.; Beliš, M.; Wangle, T.; Vleugels, J.; Verwerft, M.

2017-09-01

Oxalates of actinide elements are widely used in research and industry mainly due to their low solubility in aqueous solution and easy conversion to oxide. Although thorium oxide is worldwide mostly produced by the oxalate precipitation and conversion route, the powder morphology obtained through this process is known to inhibit the packing and sintering step of the pellet production. The presented work investigates the effects of oxalate precipitation conditions on the final powder morphology. Among the precipitation conditions considered are: pH of the thorium feed solution, concentration, temperature and the order of addition (thorium solution in oxalic acid solution and vice versa) known as reverse/direct strike. Herein, we show that the morphology of the final oxalate depends significantly on the above mentioned precipitation parameters.

One-Step Hydrothermal-Electrochemical Route to Carbon-Stabilized Anatase Powders

NASA Astrophysics Data System (ADS)

Tao, Ying; Yi, Danqing; Zhu, Baojun

2013-04-01

Black carbon-stabilized anatase particles were prepared by a simple one-step hydrothermal-electrochemical method using glucose and titanium citrate as the carbon and titanium source, respectively. Morphological, chemical, structural, and electrochemical characterizations of these powders were carried out by Raman spectroscopy, Fourier-transform infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and cyclic voltammetry. It was revealed that 200-nm carbon/anatase TiO2 was homogeneously dispersed, and the powders exhibited excellent cyclic performance at high current rates of 0.05 V/s. The powders are interesting potential materials that could be used as anodes for lithium-ion batteries.

Development of Ceramic Systems for High temperature Coatings

NASA Technical Reports Server (NTRS)

Eslamloo-Grami, Maryame

2003-01-01

Professor Eslamloo-Grami will synthesize ceramic powders of various compositions based on pyrochlore, perovskite, and magnetoplumbite structures by doping with various oxides. Sol-gel and combustion synthesis routes will be used for powder syntheses. The powders will be characterized for particle size, surface area, microstructure, sintering etc. Thermal conductivity of the hot pressed specimens will also be measured at various temperatures. At the end, a project report will be prepared describing in details the experimental methods, results, discussion, and future research.

62. BUILDING NO. 1301, ORDNANCE FACILITY (MORTAR POWDER BUILDING), LOOKING ...

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

62. BUILDING NO. 1301, ORDNANCE FACILITY (MORTAR POWDER BUILDING), LOOKING AT NORTHWEST FACADE. ACCESS TO ROOF ALLOWS MAINTENANCE OF VENTILATION EQUIPMENT WHICH IS PLACED OUTSIDE BUILDING TO MINIMIZE EXPLOSION HAZARD. NO. 2 VISIBLE ON WALL OF BUILDING STANDS FOR EXPLOSION HAZARD WITH FRAGMENTATION. - Picatinny Arsenal, State Route 15 near I-80, Dover, Morris County, NJ

Y-TZP ceramic processing from coprecipitated powders: a comparative study with three commercial dental ceramics.

PubMed

Lazar, Dolores R R; Bottino, Marco C; Ozcan, Mutlu; Valandro, Luiz Felipe; Amaral, Regina; Ussui, Valter; Bressiani, Ana H A

2008-12-01

(1) To synthesize 3mol% yttria-stabilized zirconia (3Y-TZP) powders via coprecipitation route, (2) to obtain zirconia ceramic specimens, analyze surface characteristics, and mechanical properties, and (3) to compare the processed material with three reinforced dental ceramics. A coprecipitation route was used to synthesize a 3mol% yttria-stabilized zirconia ceramic processed by uniaxial compaction and pressureless sintering. Commercially available alumina or alumina/zirconia ceramics, namely Procera AllCeram (PA), In-Ceram Zirconia Block (CAZ) and In-Ceram Zirconia (IZ) were chosen for comparison. All specimens (6mmx5mmx5mm) were polished and ultrasonically cleaned. Qualitative phase analysis was performed by XRD and apparent densities were measured on the basis of Archimedes principle. Ceramics were also characterized using SEM, TEM and EDS. The hardness measurements were made employing Vickers hardness test. Fracture toughness (K(IC)) was calculated. Data were analyzed using one-way analysis of variance (ANOVA) and Tukey's test (alpha=0.05). ANOVA revealed that the Vickers hardness (p<0.0001) and fracture toughness (p<0.0001) were affected by the ceramic materials composition. It was confirmed that the PA ceramic was constituted of a rhombohedral alumina matrix, so-called alpha-alumina. Both CAZ and IZ ceramics presented tetragonal zirconia and alpha-alumina mixture of phases. The SEM/EDS analysis confirmed the presence of aluminum in PA ceramic. In the IZ and CAZ ceramics aluminum, zirconium and cerium in grains involved by a second phase containing aluminum, silicon and lanthanum were identified. PA showed significantly higher mean Vickers hardness values (H(V)) (18.4+/-0.5GPa) compared to vitreous CAZ (10.3+/-0.2GPa) and IZ (10.6+/-0.4GPa) ceramics. Experimental Y-TZP showed significantly lower results than that of the other monophased ceramic (PA) (p<0.05) but it showed significantly higher fracture toughness (6.0+/-0.2MPam(1/2)) values when compared to the other tested ceramics (p<0.05). The coprecipitation method used to synthesize zirconia powders and the adopted ceramic processing conditions led to ceramics with mechanical properties comparable to commercially available reinforced ceramic materials.

Additive Manufacturing of Advanced High Temperature Masking Fixtures for EBPVD TBC Coating

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

List, III, Frederick Alyious; Feuerstein, Albert; Dehoff, Ryan

2016-03-30

The purpose of this Manufacturing Demonstration Facility (MDF) technical collaboration project between Praxair Surface Technologies, Inc. (PST) and Oak Ridge National Laboratory (ORNL) was to develop an additive manufacturing process to fabricate next generation high temperature masking fixtures for coating of turbine airfoils with ceramic Thermal Barrier Coatings (TBC) by the Electron Beam Physical Vapor Deposition (EBPVD) process. Typical masking fixtures are sophisticated designs and require complex part manipulation in order to achieve the desired coating distribution. Fixtures are typically fabricated from high temperature nickel (Ni) based superalloys. The fixtures are fabricated from conventional processes by welding of thin sheetmore » material into a complex geometry, to decrease the weight load for the manipulator and to reduce the thermal mass of the fixture. Recent attempts have been made in order to fabricate the fixtures through casting, but thin walled sections are difficult to cast and have high scrap rates. This project focused on understanding the potential for fabricating high temperature Ni based superalloy fixtures through additive manufacturing. Two different deposition processes; electron beam melting (EBM) and laser powder bed fusion were evaluated to determine the ideal processing route of these materials. Two different high temperature materials were evaluated. The high temperature materials evaluated were Inconel 718 and another Ni base alloy, designated throughout the remainder of this document as Alloy X, as the alloy composition is sensitive. Inconel 718 is a more widely utilized material for additive manufacturing although it is not currently the material utilized for current fixtures. Alloy X is the alloy currently used for the fixtures, but is not a commercially available alloy for additive manufacturing. Praxair determined it was possible to build the fixture using laser powder bed technology from Inconel 718. ORNL fabricated the fixture geometry using the EBM technology in order to compare deposition features such as surface roughness, geometric accuracy, deposition rate, surface and subsurface porosity, and material quality. It was determined that the laser powder bed technology was ideal for the geometry and requirements of the fixture set by Praxair, and Praxair moved forward with the purchase of a laser powder bed system. The subsequent portion of the project focused on determining the ideal processing parameters for alloy X for the laser powder bed system using ORNL’s Renishaw laser powder bed system. Praxair supplied gas atomized powders of alloy X material with properties specified by ORNL. ORNL printed text cube arrays in order to determine the ideal combination of laser powder and laser travel speed in order to maximize material density, improve surface quality, and maintain geometric accuracy. Additional powder supplied by Praxair was used to fabricate a full-scale fixture component.« less

Evaluation of effects of geometrical parameters on density distribution in compaction of PM gears

NASA Astrophysics Data System (ADS)

Khodaee, Alireza; Melander, Arne

2017-10-01

The usage of powder metallurgy (PM) for manufacturing of transmission components in automotive industries has been studied by many researchers. PM components have become of interest in recent years due to advancements in post processing possibilities such as hot isostatic pressing (HIP). Still in many of the forming process routes for making components from PM materials, the compaction of the powder into green component is the first step. Compaction is required to put the powder into the near net shape of the desired component and it causes a density gradient in the body of the green component. Basically the friction between powder particles and between the powder particles and die walls are the well-known roots for such density gradients in the compacted component. Looking at forming of PM gears, the gradient in density is one of the most important roots of problems in the processing of PM gears as well. That is because making a gear with full density and no pores will be very costly if large density gradients exist in the green component. The purpose of this study is to find the possible relations between the gear geometry and the density gradients in the green component after compaction in addition to the friction effects. For this purpose several gears should be tested. To reduce the research costs, the finite element (FE) method is used. First a FE model of the compaction process is developed and verified. To investigate the relations between the density gradients and the gear parameters such as addendum diameter (da) and the face width (b) several gear geometries have been studied. The compaction of selected gears is simulated using the FE model. The simulations results which are the distribution of density in the green component are evaluated and discussed and conclusion are made based on them.

Sulvanite (Cu 3VS 4) nanocrystals for printable thin film photovoltaics

DOE PAGES

Chen, Ching -Chin; Stone, Kevin H.; Lai, Cheng -Yu; ...

2017-09-21

Copper Vanadium Sulfide (Cu 3VS 4), also known as sulvanite, has recently emerged as a suitable absorber material for thin film photovoltaics. The synthesis of Cu 3VS 4 nanocrystals via a rapid solvothermal route is reported for the first time. The phase purity of the Cu 3VS 4 nanocrystals has been confirmed by X-ray powder diffraction (XRD) and Raman spectroscopy, while the nanoparticle size, of about 10 nm, was evaluated by transmission electron microscopy (TEM). Successful ligand exchange with sulfide, an inorganic ligand, demonstrated that the nanoparticles are amenable to surface modifications, key element in solution processing. Further annealing ofmore » as-synthesized nanocrystals under a sulfur/argon atmosphere at 600 °C, rendered highly crystalline Cu 3VS 4 powders exhibiting an impurity that could be potentially mitigated by annealing temperature optimization. Furthermore, Cu 3VS 4, formed solely from Earth-abundant elements, could provide an inexpensive, reliable approach to fabricating solution processed thin film photovoltaic absorbers.« less

Sulvanite (Cu 3VS 4) nanocrystals for printable thin film photovoltaics

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

Chen, Ching -Chin; Stone, Kevin H.; Lai, Cheng -Yu

Copper Vanadium Sulfide (Cu 3VS 4), also known as sulvanite, has recently emerged as a suitable absorber material for thin film photovoltaics. The synthesis of Cu 3VS 4 nanocrystals via a rapid solvothermal route is reported for the first time. The phase purity of the Cu 3VS 4 nanocrystals has been confirmed by X-ray powder diffraction (XRD) and Raman spectroscopy, while the nanoparticle size, of about 10 nm, was evaluated by transmission electron microscopy (TEM). Successful ligand exchange with sulfide, an inorganic ligand, demonstrated that the nanoparticles are amenable to surface modifications, key element in solution processing. Further annealing ofmore » as-synthesized nanocrystals under a sulfur/argon atmosphere at 600 °C, rendered highly crystalline Cu 3VS 4 powders exhibiting an impurity that could be potentially mitigated by annealing temperature optimization. Furthermore, Cu 3VS 4, formed solely from Earth-abundant elements, could provide an inexpensive, reliable approach to fabricating solution processed thin film photovoltaic absorbers.« less

Kinetic study of isothermal crystallization process of Gd2Ti2O7 precursor's powder prepared through the Pechini synthetic approach

NASA Astrophysics Data System (ADS)

Janković, Bojan; Marinović-Cincović, Milena; Dramićanin, Miroslav

2015-10-01

Crystallization process of Gd2Ti2O7 precursor's powder prepared by Pechini-type polymerized complex route has been studied under isothermal experimental conditions in an air atmosphere. It was found that the crystallization proceeds through two-parameter Šesták-Berggren (SB) autocatalytic model, in the operating temperature range of 550 °C≤T≤750 °C. Based on the behavior of SB parameters (M, N), it was found that in the lower operating temperature range, the crystallites with relatively low compactness exist, which probably disclosed low dimensionality of crystal growth from numerous nucleation sites, where the amorphous solid is produced. In the higher operating temperature region (above 750 °C), it was established that a morphological well-defined and high-dimensional particles of the formed pyrochlore phase can be expected. It was found that at T=850 °C, there is a change in the rate-determining reaction step, from autocatalytic into the contracting volume mechanism.

Preparation of core-shell Ti-Nb oxide nanocrystals

NASA Astrophysics Data System (ADS)

Simakov, David S. A.; Tsur, Yoed

2008-01-01

Nanosized powders of Ti-Nb oxide core-shell nanocrystals with atomic ratios of Nb/Ti = 0.11, 0.25, and 0.38 have been prepared by two preparation routes. The first route was co-precipitation, followed by␣annealing, using NbCl5 as a source of Nb. The second route was coating of pure TiO2 nanocrystals by Nb-isopropoxide in liquid medium, followed by impregnation of the Nb into the nanoparticles by annealing. Both methods yielded anatase nanocrystals with a Nb-rich shell and a core, which had much lower Nb loadings. The anatase structure solid solution (with Nb incorporated) was stable under annealing up to 760°C. The particle size remained within the nanometric scale ( <50 nm) under heat-treatment up to 760°C. It has been shown that the fabricated powders can be redispersed in aqueous media by simple ultrasound treatment, resulting in nanosized dispersions. Using a variety of analytical techniques, including depth profiling of single nanocrystallites by AES combined with sputtering by Ar ions, the mechanism of the core-shell structure creation was studied. It is proposed that the formation of the core-shell structure is governed by solubility limitations in the co-precipitation route and by solubility and diffusion limitations in the coating-incorporation route.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Oxalate co-precipitation synthesis of calcium zirconate and calcium titanate powders.

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

Hernandez-Sanchez, Bernadette A.; Tuttle, Bruce Andrew

2009-06-01

Fine powders of calcium zirconate (CaZrO{sub 3}, CZ) and calcium titanate (CaTiO{sub 3}, CT) were synthesized using a nonaqueous oxalate co-precipitation route from Ca(NO{sub 3}){sub 2}{center_dot}4 H{sub 2}O and group(IV) n-butoxides (Ti(OBu{sup n}){sub 4} or Zr(OBu{sup n}){sub 4}). Several reaction conditions and batch sizes (2-35 g) were explored to determine their influence on final particle size, morphology, and phase. Characterization of the as-prepared oxalate precursors, oven dried oxalate precursors (60-90 C), and calcined powders (635-900 C) were analyzed with TGA/DTA, XRD, TEM, and SEM. Densification and sintering studies on pressed CZ pellets at 1375 and 1400 C were also performed.more » Through the developed oxalate co-precipitation route, densification temperatures for CZ were lowered by 125 C from the 1500 C firing temperature required for conventional mixed oxide powders. Low field electrical tests of the CZ pellets indicated excellent dielectric properties with dielectric constants of {approx}30 and a dissipation factor of 0.0004 were measured at 1 kHz.« less

Enhancement of exchange coupling interaction of NdFeB/MnBi hybrid magnets

NASA Astrophysics Data System (ADS)

Nguyen, Truong Xuan; Nguyen, Khanh Van; Nguyen, Vuong Van

2018-03-01

MnBi ribbons were fabricated by melt - spinning with subsequent annealing. The MnBi ribbons were ground and mixed with NdFeB commercial Magnequench powders (MQA). The hybrid powder mixtures were subjected thrice to the annealing and ball-milling route. The hybrid magnets (100 - x)NdFeB/xMnBi, x=0, 30, 40, 50 and 100 wt% were in-mold aligned in an 18 kOe magnetic field and warm compacted at 290 °C by 2000 psi uniaxial pressure for 10 min. An enhancement of the exchange coupling of NdFeB/MnBi hybrid magnets was obtained by optimizing the magnets' microstructures via annealing and ball-milling processes. The magnetic properties of prepared NdFeB/MnBi hybrid magnets were studied and discussed in details.

On the phase evolution of AlCoCrCuFeMnSix high entropy alloys prepared by mechanical alloying and arc melting route

NASA Astrophysics Data System (ADS)

Kumar, Anil; Chopkar, Manoj

2018-05-01

Effect of Si addition on phase formation of AlCoCrCuFeMnSix (x=0, 0.3, 0.6 and 0.9) high entropy alloy have been investigated in this work. The alloys are prepared by mechanical alloying and vacuum arc melting technique. The X-ray diffraction results reveals the formation of mixture of face centered and body centered cubic solid solution phases in milled powders. The addition of Si favours body centered cubic structure formation during milling process. Whereas, after melting the milled powders, body centered phases formed during milling is partial transformed into sigma phases. XRD results were also correlated with the SEM elemental mapping of as casted samples. Addition of Si favours σ phase formation in the as cast samples.

Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.

PubMed

Prakash, B Shri; Varma, K B R

2008-11-01

Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.

Powder bed binder jet 3D printing of Inconel 718: Densification, microstructural evolution and challenges

DOE PAGES

Nandwana, Peeyush; Elliott, Amy M.; Siddel, Derek; ...

2017-01-03

Traditional manufacturing of Inconel 718 components from castings and thermomechanical processing routes involve extensive post processing and machining to attain the desired geometry. Additive manufacturing (AM) technologies including direct energy deposition (DED), selective laser melting (SLM), electron beam melting (EBM) and binder jet 3D printing (BJ3DP) can minimize scrap generation and reduce lead times. While there is extensive literature on the use of melting and solidification based AM technologies, there has been limited research on the use of binder jet 3D printing. In this paper, a brief review on binder jet additive manufacturing of Inconel 718 is presented. In addition,more » existing knowledge on sintering of Inconel 718 has been extended to binder jet 3D printing. We found that supersolidus liquid phase sintering (SLPS) is necessary to achieve full densification of Inconel 718. SLPS is sensitive to the feedstock chemistry that has a strong influence on the liquid volume fraction at the processing temperature. Based on these results, we discuss an empirical framework to determine the role of powder particle size and liquid volume fraction on sintering kinetics. In conclusion, the role of powder packing factor and binder saturation on microstructural evolution is discussed. The current challenges in the use of BJ3DP for fabrication of Inconel 718, as well as, extension to other metal systems, are presented.« less

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

Rounaghi, S.A., E-mail: s.a.rounaghi@gmail.com; Kiani Rashid, A.R.; Eshghi, H., E-mail: heshghi@ferdowsi.um.ac.ir

Decomposition of melamine was studied by solid state reaction of melamine and aluminum powders during high energy ball-milling. The milling procedure performed for both pure melamine and melamine/Al mixed powders as the starting materials for various times up to 48 h under ambient atmosphere. The products were characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The results revealed that Al causes melamine deammoniation at the first stages of milling and further milling process leads to the s-triazine ring degradation while nano-crystallite hexagonal aluminum nitride (h-AlN) was the main solid product. Comparison to milling process, the possibility ofmore » the reaction of melamine with Al was also investigated by thermal treatment method using differential scanning calorimeter (DSC) and thermo gravimetric analyzer (TGA). Melamine decomposition occurred by thermal treatment in the range of 270-370 Degree-Sign C, but no reaction between melamine and aluminum was observed. - Graphical Abstract: Mechanochemical reaction of melamine with Al resulted in the formation of nanocrystalline AlN after 7 h milling time Highlights: Black-Right-Pointing-Pointer High energy ball milling of melamine and aluminum results decomposition of melamine with elimination of ammonia. Black-Right-Pointing-Pointer Nano-crystalline AlN was synthesized by the mechanochemical route. Black-Right-Pointing-Pointer Milling process has no conspicuous effect on pure melamine degradation. Black-Right-Pointing-Pointer No reaction takes place by heating melamine and aluminum powder mixture in argon.« less

Synthesis of nano-titanium dioxide by sol-gel route

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

Kaler, Vandana, E-mail: vandana.kaler@gmail.com; Duchaniya, R. K.; Pandel, U.

Nanosized titanium dioxide powder was synthesised via sol-gel route by hydrolysis of titanium tetraisopropoxide with ethanol and water mixture in high acidic medium. The synthesized nanopowder was further characterized by X-ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and Ultraviolet Visible Spectroscopy in order to determine size, morphology and crystalline structure of the material. The synthesis of nano-TiO{sub 2} powder in anatase phase was realized by XRD. The optical studies of nano-TiO{sub 2} powder was carried out by UV-Vis spectroscopy and band gap was calculated as 3.5eV, The SEM results with EDAX confirmed that prepared nano-TiO{sub 2} particles weremore » in nanometer range with irregular morphology. The FTIR analysis showed that only desired functional groups were present in sample. These nano-TiO{sub 2} particles have applications in solar cells, chemical sensors and paints, which are thrust areas these days.« less

Influence of hydration and annealing on structure, PSL yield and spatial resolution of pressed powder imaging plates of the X-ray storage phosphor CsBr:Eu2+

NASA Astrophysics Data System (ADS)

Kersting, E.; von Seggern, H.

2017-08-01

A new production route for europium doped cesium bromide (CsBr:Eu2+) imaging plates has been developed, synthesizing CsBr:Eu2+ powder from a precipitation reaction of aqueous CsBr solution with ethanol. This new route allows the control of features like homogeneous grain size and grain shape of the obtained powder. After drying and subsequent compacting the powder, disk-like samples were fabricated, and their resulting photostimulated luminescence (PSL) properties like yield and spatial resolution were determined. It will be shown that hydration of such disks causes the CsBr:Eu2+ powder to recrystallize starting from the humidity exposed surfaces to the sample interior up to a completely polycrystalline sample resulting in a decreasing PSL yield and an increasing resolution. Subsequent annealing leads to grain refinement combined with a large PSL yield increment and a minor effect on the spatial resolution. By first annealing the "as made" disk, one observes a strong increment of the PSL yield and almost no effect on the spatial resolution. During subsequent hydration, the recrystallization is hindered by minor structural changes of the grains. The related PSL yield drops slightly with increasing hydration time, and the spatial resolution drops considerably. The obtained PSL properties with respect to structure will be discussed with a simple model.

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering

PubMed Central

Musa, Clara; Licheri, Roberta; Orrù, Roberto; Cao, Giacomo; Sciti, Diletta; Silvestroni, Laura; Zoli, Luca; Balbo, Andrea; Mercatelli, Luca; Meucci, Marco; Sani, Elisa

2016-01-01

In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS) after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS) followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa) is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C) could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1–2.4) in the 1000–1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers. PMID:28773611

Bacteria-assisted preparation of nano α-Fe2O3 red pigment powders from waste ferrous sulfate.

PubMed

Li, Xiang; Wang, Chuankai; Zeng, Yu; Li, Panyu; Xie, Tonghui; Zhang, Yongkui

2016-11-05

Massive ferrous sulfate with excess sulfuric acid is produced in titanium dioxide industry each year, ending up stockpiled or in landfills as solid waste, which is hazardous to environment and in urgent demand to be recycled. In this study, waste ferrous sulfate was used as a second raw material to synthesize nano α-Fe2O3 red pigment powders with a bacteria-assisted oxidation process by Acidithiobacillus ferrooxidans. The synthesis route, mainly consisting of bio-oxidation, precipitation and calcination, was investigated by means of titration, thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscope (SEM) and X-ray fluorescence (XRF) to obtain optimum conditions. Under the optimum conditions, nano α-Fe2O3 red pigment powders contained 98.24wt.% of Fe2O3 were successfully prepared, with a morphology of spheroidal and particle size ranged from 22nm to 86nm and averaged at 45nm. Moreover, the resulting product fulfilled ISO 1248-2006, the standards of iron oxide pigments. Copyright © 2016 Elsevier B.V. All rights reserved.

Time cycle analysis and simulation of material flow in MOX process layout

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

Chakraborty, S.; Saraswat, A.; Danny, K.M.

The (U,Pu)O{sub 2} MOX fuel is the driver fuel for the upcoming PFBR (Prototype Fast Breeder Reactor). The fuel has around 30% PuO{sub 2}. The presence of high percentages of reprocessed PuO{sub 2} necessitates the design of optimized fuel fabrication process line which will address both production need as well as meet regulatory norms regarding radiological safety criteria. The powder pellet route has highly unbalanced time cycle. This difficulty can be overcome by optimizing process layout in terms of equipment redundancy and scheduling of input powder batches. Different schemes are tested before implementing in the process line with the helpmore » of a software. This software simulates the material movement through the optimized process layout. The different material processing schemes have been devised and validity of the schemes are tested with the software. Schemes in which production batches are meeting at any glove box location are considered invalid. A valid scheme ensures adequate spacing between the production batches and at the same time it meets the production target. This software can be further improved by accurately calculating material movement time through glove box train. One important factor is considering material handling time with automation systems in place.« less

Effect of synthesizing method on the properties of LiFePO4/C composite for rechargeable lithium-ion batteries

NASA Astrophysics Data System (ADS)

Yoon, Man-Soon; Islam, Mobinul; Park, Young Min; Ur, Soon-Chul

2013-03-01

Olivine-type LiFePO4/C cathode materials are fabricated with FePO4 powders that are pre-synthesized by two different processes from iron chloride solution. Process I is a modified precipitation method which is implemented by the pH control of a solution using NH4OH to form FePO4 precipitates at room temperature. Process II is a conventional precipitation method, of which H3PO4 (85%) solution is gradually added to a FeCl3 solution during the process to maintain a designated mole ratio. The solution is subsequently aged at 90°C in a water bath until FePO4 precipitates appear. In order to synthesize LiFePO4/C composites, each batch of FePO4 powders is then mixed with pre-milled lithium carbonate and glucose (8 wt. %) as a carbon source in a ball-mill. The structural characteristics of both LiFePO4/C composites fabricated using iron phospates from two different routes have been examined employing XRD and SEM. The modified precipitation process is considered to be a relatively simple and effective process for the preparation of LiFePO4/C composites owing to their excellent electrochemical properties and rate capabilities.

Aqueous Combustion Synthesis and Characterization of Nanosized Tetragonal Zirconia Single Crystals

NASA Astrophysics Data System (ADS)

Reddy, B. S. B.; Mal, Indrajit; Tewari, Shanideep; Das, Karabi; Das, Siddhartha

2007-08-01

Nanocrystalline zirconia powder has been synthesized by an aqueous combustion synthesis route using glycine as fuel and nitrate as oxidizer. The powders have been prepared by using different glycine to zirconyl nitrate molar ratios (G/N). The powders produced with different G/N ratios have been characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) to determine the parameters resulting from powder with attractive properties. The theoretical combustion temperature (T ad ) has been calculated for different G/N ratios, and it is correlated with powder characteristics. An attempt is also made to explain the stability of tetragonal zirconia on the basis of extrinsic factors such as the morphology of nanocrystallites. Nanocrystalline metastable tetragonal zirconia (˜25 nm) powder (TZ) with disc-shaped morphology has been produced with a weak agglomeration in fuel deficient mixtures.

Synthesis of Al4SiC4 powders from kaolin grog, aluminum and carbon black by carbothermal reaction

NASA Astrophysics Data System (ADS)

Yuan, Wenjie; Yu, Chao; Deng, Chengji; Zhu, Hongxi

2013-12-01

In this paper, the synthesis of Al4SiC4 used as natural oxide materials by carbothermal reduction was investigated in order to explore the synthesis route with low costs. The samples were calcined by using kaolin grog, aluminum and carbon black as raw materials with the selected proportion at the temperature from 1500 to 1800 ° C for 2 hours under flow argon atmosphere. The phase composition of reaction products were determined by X-ray diffraction. The microstructure and elemental composition of different phases were observed and identified by scanning electron microscopy and energy dispersive spectroscopy. The mechanism of reaction processing was discussed. The results show that Al4SiC4 powders composed of hexagonal plate-like particulates with various sizes and the thickness of less than 20 μm are obtained when the temperature reaches 1800 °C.

Metal release from stainless steel powders and massive sheets--comparison and implication for risk assessment of alloys.

PubMed

Hedberg, Yolanda; Mazinanian, Neda; Odnevall Wallinder, Inger

2013-02-01

Industries that place metal and alloy products on the market are required to demonstrate that they are safe for all intended uses, and that any risks to humans, animals or the environment are adequately controlled. This requires reliable and robust in vitro test procedures. The aim of this study is to compare the release of alloy constituents from stainless steel powders of different grades (focus on AISI 316L) and production routes into synthetic body fluids with the release of the same metals from massive sheets in relation to material and surface characteristics. The comparison is justified by the fact that the difference between massive surfaces and powders from a metal release/dissolution and surface perspective is not clearly elucidated within current legislations. Powders and abraded and aged (24 h) massive sheets were exposed to synthetic solutions of relevance for biological settings and human exposure routes, for periods of up to one week. Concentrations of released iron, chromium, nickel, and manganese in solution were measured, and the effect of solution pH, acidity, complexation capacity, and proteins elucidated in relation to surface oxide composition and its properties. Implications for risk assessments based on in vitro metal release data from alloys are elucidated.

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

NASA Technical Reports Server (NTRS)

Sun, Z.; Huertas, J. I.; Axelbaum, R. L.

1999-01-01

Two critical challenges facing the application of flames for synthesis of nanopowder materials are: (1) overcoming formation of agglomerates and (2) ensuring that the highly reactive nanopowders that are synthesized in flames can be produced in such a manner that their purity is maintained during subsequent processing. Agglomerates are produced in flames because particle formation occurs in a high temperature and high number density environment. They are undesirable in most advanced applications of powders. For example, agglomerates have a deleterious effect on compaction density, leading to voids when nanopowders are consolidated. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Powder purity must also be maintained during subsequent handling of nanopowders and this poses a significant challenge for any synthesis route because nanopowders, particularly metals and non-oxide ceramic powders, are inherently reactive. Impurities acquired during handling of nanopowders have slowed the advancement of the nanostructured materials industry. One promising approach that has been proposed to address these problems is nano-encapsulation. In this approach, the core particles are encapsulated in a removable material while they are within the flame but before excessive agglomeration has occurred. Condensation can be very rapid so that core particles are trapped within the condensed material and agglomeration is limited. Nano-encapsulation also addresses the handling concerns for post-synthesis processing. Results have shown that when nano-encapsulated powders are exposed to atmosphere the core particles are protected from oxidation and/or hydrolysis. Thus, handling of the powders does not require extreme care. If, for example, at the time of consolidation the encapsulation material is removed by vacuum annealing, the resulting powder remains unagglomerated and free of impurities. In this work, we described a novel aerosol model that has been developed to simulate particle encapsulation in flames. The model will ultimately be coupled to a one-dimensional spherical flame code and compared to results from microgravity flame experiments.

Conduction and Narrow Escape in Dense, Disordered, Particulate-based Heterogeneous Materials

NASA Astrophysics Data System (ADS)

Lechman, Jeremy

For optimal and reliable performance, many technological devices rely on complex, disordered heterogeneous or composite materials and their associated manufacturing processes. Examples include many powder and particulate-based materials found in phyrotechnic devices for car airbags, electrodes in energy storage devices, and various advanced composite materials. Due to their technological importance and complex structure, these materials have been the subject of much research in a number of fields. Moreover, the advent of new manufacturing techniques based on powder bed and particulate process routes, the potential of functional nano-structured materials, and the additional recognition of persistent shortcomings in predicting reliable performance of high consequence applications; leading to ballooning costs of fielding and maintaining advanced technologies, should motivate renewed efforts in understanding, predicting and controlling these materials' fabrication and behavior. Our particular effort seeks to understand the link between the top-down control presented in specific non-equilibrium processes routes (i.e., manufacturing processes) and the variability and uncertainty of the end product performance. Our ultimate aim is to quantify the variability inherent in these constrained dynamical or random processes and to use it to optimize and predict resulting material properties/performance and to inform component design with precise margins. In fact, this raises a set of deep and broad-ranging issues that have been recognized and as touching the core of a major research challenge at Sandia National Laboratories. In this talk, we will give an overview of recent efforts to address aspects of this vision. In particular the case of conductive properties of packed particulate materials will be highlighted. Combining a number of existing approaches we will discuss new insights and potential directions for further development toward the stated goal. Sandia National Laboratories is a multiprogram laboratory managed and operated by Sandia Corporation, a Lockheed-Martin Company, for the U. S. Department of Energy's National Nuclear Security Administration under Contract No. DE-AC04-94AL85000.

Feasibility study of the production of biomedical Ti-6Al-4V alloy by powder metallurgy.

PubMed

Bolzoni, L; Ruiz-Navas, E M; Gordo, E

2015-04-01

Titanium and its alloys are characterized by an exceptional combination of properties like high strength, good corrosion resistance and biocompatibility which makes them suitable materials for biomedical prosthesis and devices. The wrought Ti-6Al-4V alloy is generally favored in comparison to other metallic biomaterials due to its relatively low elastic modulus and it has been long used to obtain products for biomedical applications. In this work an alternative route to fabricate biomedical implants made out of the Ti-6Al-4V alloy is investigated. Specifically, the feasibility of the conventional powder metallurgy route of cold uniaxial pressing and sintering is addressed by considering two types of powders (i.e. blended elemental and prealloyed). The characterization of physical properties, chemical analysis, mechanical behavior and microstructural analysis is carried out in-depth and the properties are correlated among them. On the base of the results found, the produced alloys are promising materials for biomedical applications as well as cheaper surgical devices and tools. Copyright © 2015 Elsevier B.V. All rights reserved.

Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

NASA Astrophysics Data System (ADS)

He, Feng

The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single phase and heterogeneous diphasic mullite gels from same starting chemicals. Amorphous powders were obtained after optimized calcinations. Their different crystallization routes and sintering behavior were investigated and correlated with the different homogeneities of precursor gels. Structurally stable open, porous ceramics (up to 80% porosity) were produced from the single-phase gel derived powder, where gases exsolved during calcination caused foaming coincident with sintering. Translucent, dense glass ceramic was made from the calcined diphasic gel by hot-pressing.

A controlled wet-spinning and dip-coating process for preparation of high-permeable TiO2 hollow fiber membranes.

PubMed

Zhang, Qi; Wang, Hua; Fan, Xinfei; Chen, Shuo; Yu, Hongtao; Quan, Xie

2016-01-01

In order to improve the permeate flux of photocatalytic membranes, we present an approach for coupling TiO2 with ceramic hollow fiber membranes. The ceramic hollow fiber membranes with high permeate flux were fabricated by a controlled wet-spinning process using polyethersulfone (PESf) and ceramic powder as precursors and 1-methyl-2-pyrrolidinone as solvent, and the subsequent TiO2 coating was performed by a dip-coating process using tetra-n-butyl titanate as precursor. It has been found that the PESf/ceramic powder ratio could influence the structure of the membranes. Here the as-prepared TiO2 hollow fiber membranes had a pure water flux of 4,450 L/(m(2)·h). The performance of the TiO2 hollow fiber membrane was evaluated using humic acid (HA) as a test substance. The results demonstrated that this membrane exhibited a higher permeate flux under UV irradiation than in the dark and the HA removal efficiency was enhanced. The approach described here provides an operable route to the development of high-permeable photocatalytic membranes for water treatment.

Silica coating of nanoparticles by the sonogel process.

PubMed

Chen, Quan; Boothroyd, Chris; Tan, Gim Hong; Sutanto, Nelvi; Soutar, Andrew McIntosh; Zeng, Xian Ting

2008-02-05

A modified aqueous sol-gel route was developed using ultrasonic power for the silica coating of indium tin oxide (ITO) nanoparticles. In this approach, organosilane with an amino functional group was first used to cover the surface of as-received nanoparticles. Subsequent silica coating was initiated and sustained under power ultrasound irradiation in an aqueous mixture of surface-treated particles and epoxy silane. This process resulted in a thin but homogeneous coverage of silica on the particle surface. Particles coated with a layer of silica show better dispersability in aqueous and organic media compared with the untreated powder. Samples were characterized by high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and the zeta potential.

Anthrax Vaccine Powder Formulations for Nasal Mucosal Delivery

DTIC Science & Technology

2005-08-04

inhalational anthrax can be achieved in a rabbit model, by intranasal delivery of a powder rPA formulation. Here we describe the preformulation and...fluorescence. Based on these stability profiles, spray freeze-dried (SFD) formulations were prepared at pH 7–8 using trehalose as stabilizer and a CpG...gas- trointestinal, and pulmonary routes. The inhaled form is of particular concern considering its de- monstrated use as a bioweapon.1–4 Inhalational

Recovery of zinc and manganese from spent alkaline batteries by liquid-liquid extraction with Cyanex 272

NASA Astrophysics Data System (ADS)

Salgado, Aline L.; Veloso, Aline M. O.; Pereira, Daniel D.; Gontijo, Glayson S.; Salum, Adriane; Mansur, Marcelo B.

A hydrometallurgical route based on the liquid-liquid extraction technique using Cyanex 272 as extractant is investigated for the selective separation of metal values, in particular, zinc and manganese from spent alkaline batteries. The recycling route consists of following steps: (1) cryogenic dismantling of the spent batteries, (2) pre-treatment of the internal material consisting of drying, grinding and screening steps in order to produce a dry homogeneous powder, (3) leaching of the powder with sulphuric acid and (4) metal separation by liquid-liquid extraction. Bench scale experiments have shown that zinc and manganese are easily separated (ΔpH 1/2≈2.0) using 20% (v/v) Cyanex 272 dissolved in Escaid 110 at 50 °C. Therefore, the proposed route can treat residues from both zinc-carbon and alkaline batteries because metal composition of these batteries is quite similar. The metal content of other batteries such as Ni-Cd and nickel-metal hydride (NiMH) has been also determined in order to include them in future investigations.

51. BUILDING NO. 533, SOLVENT RECOVERY BUILDING, LOOKING WEST AT ...

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

51. BUILDING NO. 533, SOLVENT RECOVERY BUILDING, LOOKING WEST AT SOUTHEAST (REAR) ELEVATION. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Effect of Alloying Type and Lean Sintering Atmosphere on the Performance of PM Components

NASA Astrophysics Data System (ADS)

Sundaram, M. Vattur; Shvab, R.; Millot, S.; Hryha, E.; Nyborg, L.

2017-12-01

In order to be cost effective and to meet increasing performance demands, powder metallurgy steel components require continuous improvement in terms of materials and process development. This study demonstrates the feasibility of manufacturing structural components using two different alloys systems, i.e. lean Cr-prealloyed and diffusion bonded water atomised powders with different processing conditions. The components were sintered at two different temperatures, i.e. 1120 and 1250 °C for 30 minutes in three different atmospheres: vacuum, N2- 10%H2 atmosphere as well as lean N2-5%H2-0.5%CO-(0.1-0.4)%CH4 sintering atmosphere. Components after sintering were further processed by either low pressure carburizing, sinterhardening or case hardening. All trials were performed in the industrial furnaces to simulate the actual production of the components. Microstructure, fractography, apparent and micro hardness analyses were performed close to the surface and in the middle of the sample to characterize the degree of sintering (temperature and atmosphere) and the effect of heat treatment. In all cases, components possess mostly martensitic microstructure with a few bainitic regions. The fracture surface shows well developed sinter necks. Inter- and trans-granular ductile and cleavage fracture modes are dominant and their fraction is determined by the alloy and processing route.

Solvent-Based Synthesis of Nano-Bi0.85Sb0.15 for Low-Temperature Thermoelectric Applications

NASA Astrophysics Data System (ADS)

Kaspar, K.; Fritsch, K.; Habicht, K.; Willenberg, B.; Hillebrecht, H.

2017-01-01

In this study we show a preparation method for nanostructured Bi0.85Sb0.15 powders via a chemical reduction route in a polyol medium, yielding material with particle sizes of 20-150 nm in scalable amounts. The powders were consolidated by spark plasma sintering (SPS) in order to maintain the nanostructure. To investigate influence of the sinter process, the powders were characterized by x-ray diffraction (XRD), energy dispersive x-ray spectroscopy (EDX), and scanning electron microscopy (SEM) measurements before and after SPS. Transport properties, Seebeck effect, and thermal conductivity were determined in the low temperature range below 300 K. The samples showed excellent thermal conductivity of 2.3-2.6 W/m × K at 300 K and Seebeck coefficients from -97 μV/K to -107 μV/K at 300 K with a maximum of -141 μV/K at 110 K, thus leading to ZT values of up to 0.31 at room temperature. The results show that Bi-Sb-alloys are promising materials for low-temperature applications. Our wet chemical approach gives access to scalable amounts of nano-material with increased homogeneity and good thermoelectric properties after SPS.

FY-12 INL KR CAPTURE ACTIVITIES SUPPORTING THE OFF-GAS SIGMA TEAM

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

Troy G. Garn; Mitchell R. Greenhalgh; Jack D Law

2012-08-01

Tasks performed this year by INL Kr capture off-gas team members can be segregated into three separate task sub-sections which include: 1) The development and testing of a new engineered form sorbent, 2) An initial NDA gamma scan effort performed on the drum containing the Legacy Kr-85 sample materials, and 3) Collaborative research efforts with PNNL involving the testing of the Ni-DOBDC MOF and an initial attempt to make powdered chalcogel material into an engineered form using our binding process. This document describes the routes to success for the three task sub-sections.

High-fraction brookite films from amorphous precursors.

PubMed

Haggerty, James E S; Schelhas, Laura T; Kitchaev, Daniil A; Mangum, John S; Garten, Lauren M; Sun, Wenhao; Stone, Kevin H; Perkins, John D; Toney, Michael F; Ceder, Gerbrand; Ginley, David S; Gorman, Brian P; Tate, Janet

2017-11-09

Structure-specific synthesis processes are of key importance to the growth of polymorphic functional compounds such as TiO 2 , where material properties strongly depend on structure as well as chemistry. The robust growth of the brookite polymorph of TiO 2 , a promising photocatalyst, has been difficult in both powder and thin-film forms due to the disparity of reported synthesis techniques, their highly specific nature, and lack of mechanistic understanding. In this work, we report the growth of high-fraction (~95%) brookite thin films prepared by annealing amorphous titania precursor films deposited by pulsed laser deposition. We characterize the crystallization process, eliminating the previously suggested roles of substrate templating and Na helper ions in driving brookite formation. Instead, we link phase selection directly to film thickness, offering a novel, generalizable route to brookite growth that does not rely on the presence of extraneous elements or particular lattice-matched substrates. In addition to providing a new synthesis route to brookite thin films, our results take a step towards resolving the problem of phase selection in TiO 2 growth, contributing to the further development of this promising functional material.

Pharmacological and toxicological assessment of innovative self-assembled polymeric micelles as powders for insulin pulmonary delivery.

PubMed

Andrade, Fernanda; Fonte, Pedro; Costa, Ana; Reis, Cassilda Cunha; Nunes, Rute; Almeida, Andreia; Ferreira, Domingos; Oliva, Mireia; Sarmento, Bruno

2016-09-01

Explore the use of polymeric micelles in the development of powders intended for pulmonary delivery of biopharmaceuticals, using insulin as a model protein. Formulations were assessed in vitro for aerosolization properties and in vivo for efficacy and safety using a streptozotocin-induced diabetic rat model. Powders presented good aerosolization properties like fine particle fraction superior to 40% and a mass median aerodynamic diameter inferior of 6 μm. Endotracheally instilled powders have shown a faster onset of action than subcutaneous administration of insulin at a dose of 10 IU/kg, with pharmacological availabilities up to 32.5% of those achieved by subcutaneous route. Additionally, micelles improved the hypoglycemic effect of insulin. Bronchoalveolar lavage screening for toxicity markers (e.g., lactate dehydrogenase, cytokines) revealed no signs of lung inflammation and cytotoxicity 14 days postadministration. Developed powders showed promising safety and efficacy characteristics for the systemic delivery of insulin by pulmonary administration.

28. BUILDING NO. 527, DEHYDRATING HOUSE, LOOKING SOUTH AT NORTH ...

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

28. BUILDING NO. 527, DEHYDRATING HOUSE, LOOKING SOUTH AT NORTH (REAR) ELEVATION OF PRELIMINARY SOLVENT RECOVERY WING. RAILS LEADING FROM DOORS CARRIED STANDARD GUAGE R.R. CARTS ONTO SMALL FLATCARS RIDING IN TRACKS IN FOREGROUND. FROM HERE THE CARS WERE TAKEN TO BUILDING NO. 533, SOLVENT RECOVERY. BUILDING NO. 540, LOADING DOCK (STORAGE FOR POWDER BUGGIES) IN BACKGROUND LEFT. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

25. BUILDING NO. 527, DEHYDRATING HOUSE, DETAIL OF SOLVENT RECOVERY ...

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

25. BUILDING NO. 527, DEHYDRATING HOUSE, DETAIL OF SOLVENT RECOVERY DUCTS. SOUTH SIDE OF BUILDING. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Investigations on Bi{sub 25}FeO{sub 40} powders synthesized by hydrothermal and combustion-like processes

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

Köferstein, Roberto, E-mail: roberto.koeferstein@chemie.uni-halle.de; Buttlar, Toni; Ebbinghaus, Stefan G.

2014-09-15

The syntheses of phase-pure and stoichiometric iron sillenite (Bi{sub 25}FeO{sub 40}) powders by a hydrothermal (at ambient pressure) and a combustion-like process are described. Phase-pure samples were obtained in the hydrothermal reaction at 100 °C (1), whereas the combustion-like process leads to pure Bi{sub 25}FeO{sub 40} after calcination at 750 °C for 2 h (2a). The activation energy of the crystallite growth process of hydrothermally synthesized Bi{sub 25}FeO{sub 40} was calculated as 48(9) kJ mol{sup −1}. The peritectic point was determined as 797(1) °C. The optical band gaps of the samples are between 2.70(7) eV and 2.81(6) eV. Temperature andmore » field-depending magnetization measurements (5−300 K) show a paramagnetic behaviour with a Curie constant of 55.66×10{sup −6} m{sup 3} K mol{sup −1} for sample 1 and C=57.82×10{sup −6} m{sup 3} K mol{sup −1} for sample 2a resulting in magnetic moments of µ{sub mag}=5.95(8) µ{sub B} mol{sup −1} and µ{sub mag}=6.07(4) µ{sub B} mol{sup −1}. The influence of amorphous iron-oxide as a result of non-stoichiometric Bi/Fe ratios in hydrothermal syntheses on the magnetic behaviour was additionally investigated. - Graphical abstract: Bi{sub 25}FeO{sub 40} powders were prepared by a hydrothermal method and a combustion process. The optical band gaps and the peritectic point were determined. The magnetic behaviour was investigated depending on the synthesis and the initial Bi/Fe ratios. The influence of amorphous iron-oxide on the magnetic properties was examined. - Highlights: • Two simple syntheses routes for stoichiometric Bi{sub 25}FeO{sub 40} powders using starch as polymerization agent. • Monitoring the phase evolution and crystallite growth kinetics during the syntheses. • Determination of the optical band gap and melting point. • Investigations of the magnetic behaviour of Bi{sub 25}FeO{sub 40} powders. • Influence of amorphous iron oxide and a non-stoichiometric Bi/Fe ratio on the magnetic behaviour.« less

Towards long lasting zirconia-based composites for dental implants. Part I: innovative synthesis, microstructural characterization and in vitro stability.

PubMed

Palmero, Paola; Fornabaio, Marta; Montanaro, Laura; Reveron, Helen; Esnouf, Claude; Chevalier, Jérôme

2015-05-01

In order to fulfill the clinical requirements for strong, tough and stable ceramics used in dental applications, we designed and developed innovative zirconia-based composites, in which equiaxial α-Al2O3 and elongated SrAl12O19 phases are dispersed in a ceria-stabilized zirconia matrix. The composite powders were prepared by an innovative surface coating route, in which commercial zirconia powders were coated by inorganic precursors of the second phases, which crystallize on the zirconia particles surface under proper thermal treatment. Samples containing four different ceria contents (in the range 10.0-11.5 mol%) were prepared by carefully tailoring the amount of the cerium precursor during the elaboration process. Slip cast green bodies were sintered at 1450 °C for 1 h, leading to fully dense materials. Characterization of composites by SEM and TEM analyses showed highly homogeneous microstructures with an even distribution of both equiaxial and elongated-shape grains inside a very fine zirconia matrix. Ce content plays a major role on aging kinetics, and should be carefully controlled: sample with 10 mol% of ceria were transformable, whereas above 10.5 mol% there is negligible or no transformation during autoclave treatment. Thus, in this paper we show the potential of the innovative surface coating route, which allows a perfect tailoring of the microstructural, morphological and compositional features of the composites; moreover, its processing costs and environmental impacts are limited, which is beneficial for further scale-up and real use in the biomedical field. Copyright © 2015 Elsevier Ltd. All rights reserved.

Particle engineering of materials for oral inhalation by dry powder inhalers. I-Particles of sugar excipients (trehalose and raffinose) for protein delivery.

PubMed

Ogáin, Orla Ní; Li, Jianhe; Tajber, Lidia; Corrigan, Owen I; Healy, Anne Marie

2011-02-28

The pulmonary route of delivery offers a potential alternative to parenteral administration of peptides and proteins. Protection of protein structure is essential in both processing and storage of the final formulation. Sugars, such as trehalose and raffinose, have been employed to act as protein stabilisers. Optimisation of the aerodynamic characteristics of microparticles in dry powder inhaler formulations is critical to ensure optimum deposition of the formulation into the respiratory tract. In the present study we examine the adaptation to hydrophilic materials, specifically the disaccharide, trehalose and the trisaccharide, raffinose, of a previously reported spray drying process for producing nanoporous microparticles (NPMPs). We also investigate the feasibility of incorporating a model protein, lysozyme, into these sugar-based NPMPs. While spray drying raffinose or trehalose from aqueous solution or ethanol:water solutions resulted in non-porous microspheres, spray drying from a methanol:n-butyl acetate mixed solvent system resulted in microparticles which appeared to consist of an agglomeration of individual nanoparticles, i.e. nanoporous/nanoparticulate microparticles. NPMPs of trehalose and raffinose were amorphous, with glass transition temperatures (Tgs) that were sufficiently high (124°C and ∼120°C for trehalose and raffinose, respectively) to suggest good physical stability at room temperature and good potential to act as protein carriers and/or stabilisers. NPMPs demonstrated improved aerosolisation properties compared to spray dried non-porous particles. The successful incorporation of lysozyme into these NPMPs at a sugar to protein weight ratio of 1:4 demonstrated the potential of these systems to act as carriers for peptide or protein drugs which could be delivered via the pulmonary route. Copyright © 2010 Elsevier B.V. All rights reserved.

36. BUILDINGS NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, AND ...

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

36. BUILDINGS NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, AND NO. 523, REFRIGERATION PLANT BUILDING, LOOKING EAST. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

An Innovative Method for Manufacturing Gamma-TiAl Foil

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Saqib, Mohammad; Alexa, Joel A.

2003-01-01

The manufacture and entrance into service of thin gage gamma-TiAl product has been hampered by the inherent low room temperature ductility of the material. In the present study a new approach was explored for the efficient manufacture of gamma-TiAl foil with improved ductility. The objective was to produce a very clean material (low interstitial content) with a highly refined, homogeneous microstructure placed in a fully lamellar condition. The processing route involved the use of RF plasma spray deposition of pre-alloyed powders, followed by consolidation via vacuum hot pressing and heat treatment. The approach took advantage of a deposition process which included no electrodes, no binders and high cooling rates. Results and discussion of the work performed to date are presented.

Novel Route to Transition Metal Isothiocyanate Complexes Using Metal Powders and Thiourea

NASA Technical Reports Server (NTRS)

Harris, Jerry D.; Eckles, William E.; Hepp, Aloysius F.; Duraj, Stan A.; Hehemann, David G.; Fanwick, Phillip E.; Richardson, John

2003-01-01

A new synthetic route to isothiocyanate-containing materials is presented. Eight isothiocyanate- 4-methylpyridine (y-picoline) compounds were prepared by refluxing metal powders (Mn, Fe, Co, Ni, and Cu) with thiourea in y-picoline. With the exception of compound 5,prepared with Co, the isothiocyanate ligand was generated in situ by the isomerization of thiourea to NH4+SCN- at reflux temperatures. The complexes were characterized by x-ray crystallography. Compounds 1,2, and 8 are the first isothiocyanate- 4-methylpyridine anionic compounds ever prepared and structurally characterized. Compounds 1 and 2 are isostructural with four equatorially bound isothiocyanate ligands and two axially bound y-picoline molecules. Compound 8 is a five-coordinate copper(II) molecule with a distorted square-pyramidal geometry. Coordinated picoline and two isothiocyanates form the basal plane and the remaining isothiocyanate is bound at the apex. Structural data are presented for all compounds.

Elaboration of austenitic stainless steel samples with bimodal grain size distributions and investigation of their mechanical behavior

NASA Astrophysics Data System (ADS)

Flipon, B.; de la Cruz, L. Garcia; Hug, E.; Keller, C.; Barbe, F.

2017-10-01

Samples of 316L austenitic stainless steel with bimodal grain size distributions are elaborated using two distinct routes. The first one is based on powder metallurgy using spark plasma sintering of two powders with different particle sizes. The second route applies the reverse-annealing method: it consists in inducing martensitic phase transformation by plastic strain and further annealing in order to obtain two austenitic grain populations with different sizes. Microstructural analy ses reveal that both methods are suitable to generate significative grain size contrast and to control this contrast according to the elaboration conditions. Mechanical properties under tension are then characterized for different grain size distributions. Crystal plasticity finite element modelling is further applied in a configuration of bimodal distribution to analyse the role played by coarse grains within a matrix of fine grains, considering not only their volume fraction but also their spatial arrangement.

Enhanced Sintering of TiNi Shape Memory Foams under Mg Vapor Atmosphere

NASA Astrophysics Data System (ADS)

Aydoğmuş, Tarik; Bor, Şakir

2012-12-01

TiNi alloy foams are promising candidates for biomaterials to be used as artificial orthopedic implant materials for bone replacement applications in biomedical sector. However, certain problems exist in their processing routes, such as formation of unwanted secondary intermetallic phases leading to brittleness and deterioration of shape memory and superelasticity characteristics; and the contamination during processing resulting in oxides and carbonitrides which affect mechanical properties negatively. Moreover, the eutectic reaction present in Ti-Ni binary system at 1391 K (1118 °C) prevents employment of higher sintering temperatures (and higher mechanical properties) even when equiatomic prealloyed powders are used because of Ni enrichment of TiNi matrix as a result of oxidation. It is essential to prevent oxidation of TiNi powders during processing for high-temperature (>1391 K i.e., 1118 °C) sintering practices. In the current study, magnesium powders were used as space holder material to produce TiNi foams with the porosities in the range of 40 to 65 pct. It has been found that magnesium prevents secondary phase formation and contamination. It also prevents liquid phase formation while enabling employment of higher sintering temperatures by two-step sintering processing: holding the sample at 1373 K (1100 °C) for 30 minutes, and subsequently sintering at temperatures higher than the eutectic temperature, 1391 K (1118 °C). By this procedure, magnesium may allow sintering up to temperatures close to the melting point of TiNi. TiNi foams produced with porosities in the range of 40 to 55 pct were found to be acceptable as implant materials in the light of their favorable mechanical properties.

Application of pulsed-field gel electrophoresis to characterise and trace the prevalence of Enterobacter sakazakii in an infant formula processing facility.

PubMed

Mullane, N R; Whyte, P; Wall, P G; Quinn, T; Fanning, S

2007-05-01

Enterobacter sakazakii (E. sakazakii) contamination of powdered infant formula (PIF) and its processing environment was monitored between April 2005 and March 2006. The purpose of the monitoring programme was to locate points of contamination, investigate clonal persistence, and identify possible dissemination routes along the processing chain. A total of 80 E. sakazakii isolates were recovered from the manufacturing facility. The overall frequency of isolation of E. sakazakii in intermediate and final product was 2.5%, while specific locations in the processing environment were contaminated at frequencies up to 31%. All E. sakazakii isolates were characterised by pulsed-field gel electrophoresis (PFGE). XbaI macrorestriction digests yielded 19 unique pulse-types that could be grouped into 6 clusters of between 5 and 32 isolates. The formation of large clusters was consistent with the presence of a number of clones in the manufacturing environment. While the majority of isolates were of environmental origin (72.5%), no cluster was confined to one specific location and indistinguishable PFGE profiles were generated from isolates cultured from the manufacturing environment, sampling points along the processing chain and from intermediate and final product. These findings suggest that the manufacturing environment serves as a key route for sporadic contamination of PIF. These data will support the development of efficient intervention measures contributing to the reduction of E. sakazakii in the PIF processing chain.

Large grained perovskite solar cells derived from single-crystal perovskite powders with enhanced ambient stability

DOE PAGES

Yen, Hung -Ju; Liang, Po -Wei; Chueh, Chu -Chen; ...

2016-05-25

In this study, we demonstrate the large grained perovskite solar cells prepared from precursor solution comprising single-crystal perovskite powders for the first time. Here, the resultant large grained perovskite thin film possesses negligible physical (structural) gap between each large grain and are highly crystalline as evidenced by its fan-shaped birefringence observed under polarized light, which is very different to the thin film prepared from the typical precursor route (MAI + PbI 2).

Preparation and Properties of New Inorganic Glasses and Gel-Derived Solids

DTIC Science & Technology

1991-04-01

route were examined, including the use of SiC and diamond powder as fillers and some triphasic , solids. Many ferroelectnic thin films were prepared...use of SiC and diamond powder as fillers and some triphasic solids. Many ferroelectric thin films were prepared and their properties measured. An...Exit Filter Mmrn Holder Filter He Gas Perforated Pyrolysis Reactor 00 0 00 00 00 00 0 0 0 0 Soutolution asWe Fi.8.Shmai darm fepeiena0yses I I I ci

Synthesis and characterization of nano-sized zirconia powder synthesized by single emulsion-assisted direct precipitation.

PubMed

Chandra, Navin; Singh, Deepesh Kumar; Sharma, Meenakshi; Upadhyay, Ravi Kant; Amritphale, S S; Sanghi, S K

2010-02-15

For the first time, single reverse microemulsion-assisted direct precipitation route has been successfully used to synthesize tetragonal zirconia nanoparticles in narrow size range. The synthesized powder was characterized using FT-IR, XRD and HRTEM techniques. The zirconia nanoparticles obtained were spherical in shape and has narrow particle size distribution in the range of 13-31nm and crystallite size in the range of 13-23nm. Copyright 2009 Elsevier Inc. All rights reserved.

The Heterogeneous Photocatalytic Decomposition of Benzoic Acid and Adipic Acid on Platinized TiO2 Powder. The Photo-Kolbe Decarboxylative Route to the Breakdown of the Benzene Ring and to the Production to Butane.

DTIC Science & Technology

1980-10-29

adsorbed oxygen on powders. 23. Jaeger, C.D.; Bard, A.J. J. Ph s. Chem. 1979, 83, 3746. 24. Izumi, I; Dunn, W. W.; Wilbourn , K. 0.; Fan, F-R. F.; Bard, A... Joseph Singer, Code 302-1 Electrochimica Corporation NASA-Lewis Attention: Technical Library 21000 BrookDark Road 2485 Charleston Poad Cleveland, Ohio

An efficient process for lactic acid production from wheat straw by a newly isolated Bacillus coagulans strain IPE22.

PubMed

Zhang, Yuming; Chen, Xiangrong; Luo, Jianquan; Qi, Benkun; Wan, Yinhua

2014-04-01

A thermophilic lactic acid (LA) producer was isolated and identified as Bacillus coagulans strain IPE22. The strain showed remarkable capability to ferment pentose, hexose and cellobiose, and was also resistant to inhibitors from lignocellulosic hydrolysates. Based on the strain's promising features, an efficient process was developed to produce LA from wheat straw. The process consisted of biomass pretreatment by dilute sulfuric acid and subsequent SSCF (simultaneous saccharification and co-fermentation), while the operations of solid-liquid separation and detoxification were avoided. Using this process, 46.12 g LA could be produced from 100g dry wheat straw with a supplement of 10 g/L corn steep liquid powder at the cellulase loading of 20 FPU (filter paper activity units)/g cellulose. The process by B. coagulans IPE22 provides an economical route to produce LA from lignocellulose. Copyright © 2014 Elsevier Ltd. All rights reserved.

NanoClusters Enhance Drug Delivery in Mechanical Ventilation

NASA Astrophysics Data System (ADS)

Pornputtapitak, Warangkana

The overall goal of this thesis was to develop a dry powder delivery system for patients on mechanical ventilation. The studies were divided into two parts: the formulation development and the device design. The pulmonary system is an attractive route for drug delivery since the lungs have a large accessible surface area for treatment or drug absorption. For ventilated patients, inhaled drugs have to successfully navigate ventilator tubing and an endotracheal tube. Agglomerates of drug nanoparticles (also known as 'NanoClusters') are fine dry powder aerosols that were hypothesized to enable drug delivery through ventilator circuits. This Thesis systematically investigated formulations of NanoClusters and their aerosol performance in a conventional inhaler and a device designed for use during mechanical ventilation. These engineered powders of budesonide (NC-Bud) were delivered via a MonodoseRTM inhaler or a novel device through commercial endotracheal tubes, and analyzed by cascade impaction. NC-Bud had a higher efficiency of aerosol delivery compared to micronized stock budesonide. The delivery efficiency was independent of ventilator parameters such as inspiration patterns, inspiration volumes, and inspiration flow rates. A novel device designed to fit directly to the ventilator and endotracheal tubing connections and the MonodoseRTM inhaler showed the same efficiency of drug delivery. The new device combined with NanoCluster formulation technology, therefore, allowed convenient and efficient drug delivery through endotracheal tubes. Furthermore, itraconazole (ITZ), a triazole antifungal agent, was formulated as a NanoCluster powder via milling (top-down process) or precipitation (bottom-up process) without using any excipients. ITZ NanoClusters prepared by wet milling showed better aerosol performance compared to micronized stock ITZ and ITZ NanoClusters prepared by precipitation. ITZ NanoClusters prepared by precipitation methods also showed an amorphous state while milled ITZ NanoClusters maintained the crystalline character. Overall, NanoClusters prepared by various processes represent a potential engineered drug particle approach for inhalation therapy since they provide effective aerosol properties and stability due to the crystalline state of the drug powders. Future work will continue to explore formulation and delivery performance in vitro and in vivo..

Oxidation and particle deposition modeling in plasma spraying of Ti-6Al-4V/SiC fiber composites

NASA Astrophysics Data System (ADS)

Cochelin, E.; Borit, F.; Frot, G.; Jeandin, M.; Decker, L.; Jeulin, D.; Taweel, B. Al; Michaud, V.; Noël, P.

1999-03-01

Plasma spraying is known to be a promising process for the manufacturing of Ti/SiC long-fiber composites. However, some improvements remain for this process to be applied in an industrial route. These include: oxygen contamination of the sprayed material through that of titanium particles before and during spraying, damage to fibers due to a high level of thermal stresses induced at the spraying stage, adequate deposition of titanium-base powder to achieve a low-porosity matrix and good impregnation of the fiber array. This article deals with work that resulted in a threefold study of the process. Oxidation was studied using electron microprobe analysis of elementary particles quenched and trapped into a closed box at various given flight distances. Oxygen diffusion phenomena within the particles are discussed from a preliminary theoretical approach coupled with experimental data. Isothermal and thermomechanical calculations were made using the ABAQUS code to determine stresses arising from contact of a liquid Ti-6Al-4V particle onto a SiC fiber. On the scale of the sprayed powder flow, a two-dimensional new type of model simulating the deposition of droplets onto a substrate was developed. This new type of model is based on a lattice-gas automaton that reproduces the hydrodynamical behavior of fluids.

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

Nandwana, Peeyush; Elliott, Amy M.; Siddel, Derek

Traditional manufacturing of Inconel 718 components from castings and thermomechanical processing routes involve extensive post processing and machining to attain the desired geometry. Additive manufacturing (AM) technologies including direct energy deposition (DED), selective laser melting (SLM), electron beam melting (EBM) and binder jet 3D printing (BJ3DP) can minimize scrap generation and reduce lead times. While there is extensive literature on the use of melting and solidification based AM technologies, there has been limited research on the use of binder jet 3D printing. In this paper, a brief review on binder jet additive manufacturing of Inconel 718 is presented. In addition,more » existing knowledge on sintering of Inconel 718 has been extended to binder jet 3D printing. We found that supersolidus liquid phase sintering (SLPS) is necessary to achieve full densification of Inconel 718. SLPS is sensitive to the feedstock chemistry that has a strong influence on the liquid volume fraction at the processing temperature. Based on these results, we discuss an empirical framework to determine the role of powder particle size and liquid volume fraction on sintering kinetics. In conclusion, the role of powder packing factor and binder saturation on microstructural evolution is discussed. The current challenges in the use of BJ3DP for fabrication of Inconel 718, as well as, extension to other metal systems, are presented.« less

44. BUILDING NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, INTERIOR, ...

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

44. BUILDING NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, INTERIOR, LOOKING UP DISTILLATION TOWER FROM 2ND LEVEL. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Microwave synthesis of noncentrosymmetric BaTiO3 truncated nanocubes for charge storage applications.

PubMed

Swaminathan, V; Pramana, Stevin S; White, T J; Chen, L; Chukka, Rami; Ramanujan, R V

2010-11-01

Truncated nanocubes of barium titanate (BT) were synthesized using a rapid, facile microwave-assisted hydrothermal route. Stoichiometric composition of pellets of nanocube BT powders was prepared by two-stage microwave process. Characterization by powder XRD, Rietveld refinement, SEM, TEM, and dielectric and polarization measurements was performed. X-ray diffraction revealed a polymorphic transformation from cubic Pm3̅m to tetragonal P4mm after 15 min of microwave irradiation, arising from titanium displacement along the c-axis. Secondary electron images were examined for nanocube BT synthesis and annealed at different timings. Transmission electron microscopy showed a narrow particle size distribution with an average size of 70 ± 9 nm. The remanence and saturation polarization were 15.5 ± 1.6 and 19.3 ± 1.2 μC/cm(2), respectively. A charge storage density of 925 ± 47 nF/cm(2) was obtained; Pt/BT/Pt multilayer ceramic capacitor stack had an average leakage current density of 5.78 ± 0.46 × 10(-8) A/cm(2) at ±2 V. The significance of this study shows an inexpensive and facile processing platform for synthesis of high-k dielectric for charge storage applications.

Alternative route for the preparation of CoSb{sub 3} and Mg{sub 2}Si derivatives

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

Godlewska, E., E-mail: godlewsk@agh.edu.pl; Mars, K.; Zawadzka, K.

2012-09-15

An alternative manufacturing route has been developed for cobalt triantimonide and magnesium disilicide derivatives. Elemental powders were mixed in stoichiometric proportions, cold pressed into cylindrical preforms and heated in oxygen-free environment to initiate the exothermic reaction. According to DTA/TG measurements and observations under high-temperature microscope, the onset of reaction occurred at a temperature not exceeding the melting point of the more volatile component, i.e. antimony in the case of CoSb{sub 3} and magnesium in the case of Mg{sub 2}Si. The reaction products were additionally heat treated to secure homogenization. Dense sinters were obtained by hot uniaxial pressing of the obtainedmore » powders in moderate temperature-and-pressure conditions. Several advantages were identified in the proposed technology: absence of liquid phases, relatively short time of the synthesis, possibility of in-situ or ex-situ doping and grain size control. - Graphical abstract: (1) Manufacturing flow sheet for CoSb{sub 3} (milling included) and Mg{sub 2}Si (no milling). (2) Micrographs of CoSb{sub 3} product. (3) Micrographs of Mg{sub 2}Si product. Highlights: Black-Right-Pointing-Pointer The combustion synthesis followed by HP was used for the manufacturing of CoSb{sub 3} or Mg{sub 2}Si. Black-Right-Pointing-Pointer The time of reaction is shorter compared with many other synthesis methods. Black-Right-Pointing-Pointer The process is scalable and practically wasteless.« less

Concurrent crack and powder cocaine users from Sao Paulo: Do they represent a different group?

PubMed Central

Guindalini, Camila; Vallada, Homero; Breen, Gerome; Laranjeira, Ronaldo

2006-01-01

Background Cocaine abuse is a serious and socially damaging illegal drug problem. Different routes of administration are associated with a specific progression of use, different degrees of abuse liability, propensity for dependence and treatment response. There have been relatively few studies comparing different cocaine users groups and no studies into the characterization of the group of individuals reporting concurrent use of powder cocaine and crack cocaine. Methods Six hundred and ninety-nine cocaine users were assessed during the period August 1997 to October 1998 in one outpatient and six inpatient clinics located in the São Paulo, Brazil. Patients were interviewed using a structured questionnaire schedule in Portuguese, designed specifically for the Brazilian population. The statistical analyses were performed using either ANOVA or a chi-squared test and focusing on their preferred form of use/route of administration and other variables. Results For 83% of the variables tested in this study, the Dual Users subgroup (using both powder and crack cocaine) demonstrated statistical differences from the single drug user subgroups. Those differences include the initiation of cocaine, the abuse of other illicit drugs, and rates of criminal history. Conclusion These data suggest cocaine-dependent individuals who report use of both powder and crack cocaine are an at least partially, distinct subgroup. However, further studies will be necessary to confirm this and to determine if they also show a different treatment response. PMID:16426451

Structural, electrical and dielectric properties of spinel nickel ferrite prepared by soft mechanochemical synthesis

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

Lazarević, Zorica Ž., E-mail: lzorica@yahoo.com; Jovalekić, Čedomir; Sekulić, Dalibor L.

2013-10-15

Graphical abstract: - Highlights: • Sintered NiFe{sub 2}O{sub 4} was prepared by a soft mechanochemical route from mixture powders. • XRD and Raman measurements indicate that the prepared samples have spinel structure. • The activation energy ΔE are 0.653 and 0.452 eV for NiFe{sub 2}O{sub 4} samples. • Ferrite from Ni(OH){sub 2}/Fe{sub 2}O{sub 3} has lower DC conductivity than from Ni(OH){sub 2}/Fe(OH){sub 3} powders. • The values of dielectric constant of samples NiFe{sub 2}O{sub 4} are 70 and 200, respectively. - Abstract: Nickel ferrite, NiFe{sub 2}O{sub 4} was prepared by a soft mechanochemical route from a mixture of (1) Ni(OH){submore » 2} and α-Fe{sub 2}O{sub 3} and (2) Ni(OH){sub 2} and Fe(OH){sub 3} powders in a planetary ball mill for 25 h. The powder samples were sintered at 1100 °C for 2 h and were characterized by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). Impedance spectroscopy techniques were used to study the effect of grain and grain boundary on the electrical properties of the prepared samples. A difference in dielectric constant (ε) and dielectric loss tangent (tan δ) of NiFe{sub 2}O{sub 4} samples obtained by the same methods but starting from different initial components was observed.« less

Surface segregation of additives on SnO 2 based powders and their relationship with macroscopic properties

NASA Astrophysics Data System (ADS)

Pereira, Gilberto J.; Castro, Ricardo H. R.; Hidalgo, Pilar; Gouvêa, Douglas

2002-07-01

Surface properties of ceramic powders frequently play an important role in producing high-quality, high-performance, and reliable ceramic products. These properties are related to the surface bond types and interactions with the surroundings. Oxide surfaces generally contain adsorbed hydroxyl groups and modifications in the chemical composition of the surface may be studied by infrared spectroscopy. In this work, we prepared SnO 2 containing Fe or Mg ions by organic chemical route derived from Pechini's method. The prepared powders were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), dynamic electrophoretic mobility and surface area determination. Results demonstrated that the studied additives segregate onto the oxide surface and modify the hydroxyl IR bands of the adsorbed hydroxyl groups. These surface modifications change some macroscopic properties of the powder such as the isoelectric point (IEP) in aqueous suspensions and the final specific surface area. The increase of the surface area with additive concentration is supposedly due to the reduction of surface energy of the powders when additives segregate on the powder surface.

High yttria ferritic ODS steels through powder forging

NASA Astrophysics Data System (ADS)

Kumar, Deepak; Prakash, Ujjwal; Dabhade, Vikram V.; Laha, K.; Sakthivel, T.

2017-05-01

Oxide dispersion strengthened (ODS) steels are being developed for future nuclear reactors. ODS Fe-18%Cr-2%W-0.2%Ti steels with 0, 0.35, 0.5, 1 and 1.5% Y2O3 (all compositions in weight%) dispersion were fabricated by mechanical alloying of elemental powders. The powders were placed in a mild steel can and forged in a stream of hydrogen gas at 1473 K. The steels were forged again to final density. The strength of ODS steel increased with yttria content. Though this was accompanied by a decrease in tensile elongation, all the steels showed significant ductility. The ductility in high yttria alloys may be attributed to improved inter-particle bonding between milled powders due to reduction of surface oxides by hydrogen. This may permit development of ODS steels with yttria contents higher than the conventional limit of 0.5%. It is suggested that powder forging is a promising route to fabricate ODS steels with high yttria contents and improved ductility.

Toughened and machinable glass matrix composites reinforced with graphene and graphene-oxide nano platelets

NASA Astrophysics Data System (ADS)

Porwal, Harshit; Tatarko, Peter; Grasso, Salvatore; Hu, Chunfeng; Boccaccini, Aldo R.; Dlouhý, Ivo; Reece, Mike J.

2013-10-01

The processing conditions for preparing well dispersed silica-graphene nanoplatelets and silica-graphene oxide nanoplatelets (GONP) composites were optimized using powder and colloidal processing routes. Fully dense silica-GONP composites with up to 2.5 vol% loading were consolidated using spark plasma sintering. The GONP aligned perpendicularly to the applied pressure during sintering. The fracture toughness of the composites increased linearly with increasing concentration of GONP and reached a value of ˜0.9 MPa m1/2 for 2.5 vol% loading. Various toughening mechanisms including GONP necking, GONP pull-out, crack bridging, crack deflection and crack branching were observed. GONP decreased the hardness and brittleness index (BI) of the composites by ˜30 and ˜50% respectively. The decrease in BI makes silica-GONP composites machinable compared to pure silica. When compared to silica-Carbon nanotube composites, silica-GONP composites show better process-ability and enhanced mechanical properties.

Toughened and machinable glass matrix composites reinforced with graphene and graphene-oxide nano platelets

PubMed Central

Porwal, Harshit; Tatarko, Peter; Grasso, Salvatore; Hu, Chunfeng; Boccaccini, Aldo R; Dlouhý, Ivo; Reece, Mike J

2013-01-01

The processing conditions for preparing well dispersed silica–graphene nanoplatelets and silica–graphene oxide nanoplatelets (GONP) composites were optimized using powder and colloidal processing routes. Fully dense silica–GONP composites with up to 2.5 vol% loading were consolidated using spark plasma sintering. The GONP aligned perpendicularly to the applied pressure during sintering. The fracture toughness of the composites increased linearly with increasing concentration of GONP and reached a value of ∼0.9 MPa m1/2 for 2.5 vol% loading. Various toughening mechanisms including GONP necking, GONP pull-out, crack bridging, crack deflection and crack branching were observed. GONP decreased the hardness and brittleness index (BI) of the composites by ∼30 and ∼50% respectively. The decrease in BI makes silica–GONP composites machinable compared to pure silica. When compared to silica–Carbon nanotube composites, silica–GONP composites show better process-ability and enhanced mechanical properties. PMID:27877614

Single step, phase controlled, large scale synthesis of ferrimagnetic iron oxide polymorph nanoparticles by thermal plasma route and their rheological properties

NASA Astrophysics Data System (ADS)

Raut, Suyog A.; Mutadak, Pallavi R.; Kumar, Shiv; Kanhe, Nilesh S.; Huprikar, Sameer; Pol, Harshawardhan V.; Phase, Deodatta M.; Bhoraskar, Sudha V.; Mathe, Vikas L.

2018-03-01

In this paper we report single step large scale synthesis of highly crystalline iron oxide nanoparticles viz. magnetite (Fe3O4) and maghemite (γ-Fe2O3) via gas phase condensation process, where micron sized iron metal powder was used as a precursor. Selective phases of iron oxide were obtained by variation of gas flow rate of oxygen and hence partial pressure of oxygen inside the plasma reactor. Most of the particles were found to possesses average crystallite size of about 20-30 nm. The DC magnetization curves recorded indicate almost super-paramagnetic nature of the iron oxide magnetic nanoparticles. Further, iron oxide nanoparticles were analyzed using Raman spectroscopy, X-ray photoelectron spectroscopy and Mossbauer spectroscopy. In order to explore the feasibility of these nanoparticles for magnetic damper application, rheological studies have been carried out and compared with commercially available Carbonyl Iron (CI) particles. The nanoparticles obtained by thermal plasma route show improved dispersion which is useful for rheological applications.

Nanoscale contact resistance of V2O5 xerogel films developed by nanostructured powder

NASA Astrophysics Data System (ADS)

Bera, Biswajit; Sekhar Das, Pradip; Bhattacharya, Manjima; Ghosh, Swapankumar; Mukhopadhyay, Anoop Kumar; Dey, Arjun

2016-03-01

Here we report the synthesis of V2O5 nanostructures by a fast, simple, cost-effective, low-temperature chemical process; followed by the deposition of V2O5 xerogel thin films on a glass substrate by a sol-gel route. Phase analysis, phase transition, microstructural and electronic characterization studies are carried out by x-ray diffraction, texture coefficient analysis, field emission scanning electron microscopy, transmission electron microscopy (TEM), related selected area electron diffraction pattern (SAED) analysis, Fourier transform infrared spectroscopy, thermogravimetry and differential thermal analysis, differential scanning calorimetry, and x-ray photoelectron spectroscopy techniques. Confirmatory TEM and SAED data analysis prove further that in this polycrystalline powder there is a unique localized existence of purely single crystalline V2O5 powder with a preferred orientation in the (0 1 0) direction. The most interesting result obtained in the present work is that the xerogel thin films exhibit an inherent capability to enhance the intrinsic resistance against contact induced deformations as more external load is applied during the nanoindentation experiments. In addition, both the nanohardness and Young’s modulus of the films are found to be insensitive to load variations (e.g. 1 to 7 mN). These results are explained in terms of microstructural parameters, e.g. porosity and structural configuration.

Suppressing the Photocatalytic Activity of TiO2 Nanoparticles by Extremely Thin Al2O3 Films Grown by Gas-Phase Deposition at Ambient Conditions

PubMed Central

Guo, Jing; Valdesueiro, David; Yuan, Shaojun; Liang, Bin; van Ommen, J. Ruud

2018-01-01

This work investigated the suppression of photocatalytic activity of titanium dioxide (TiO2) pigment powders by extremely thin aluminum oxide (Al2O3) films deposited via an atomic-layer-deposition-type process using trimethylaluminum (TMA) and H2O as precursors. The deposition was performed on multiple grams of TiO2 powder at room temperature and atmospheric pressure in a fluidized bed reactor, resulting in the growth of uniform and conformal Al2O3 films with thickness control at sub-nanometer level. The as-deposited Al2O3 films exhibited excellent photocatalytic suppression ability. Accordingly, an Al2O3 layer with a thickness of 1 nm could efficiently suppress the photocatalytic activities of rutile, anatase, and P25 TiO2 nanoparticles without affecting their bulk optical properties. In addition, the influence of high-temperature annealing on the properties of the Al2O3 layers was investigated, revealing the possibility of achieving porous Al2O3 layers. Our approach demonstrated a fast, efficient, and simple route to coating Al2O3 films on TiO2 pigment powders at the multigram scale, and showed great potential for large-scale production development. PMID:29364840

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

Cook, John B.; Detsi, Eric; Liu, Yijin

Next generation Li-ion batteries will require negative electrode materials with energy densities many-fold higher than that found in the graphitic carbon currently used in commercial Li-ion batteries. While various nanostructured alloying-type anode materials may satisfy that requirement, such materials do not always exhibit long cycle lifetimes and/or their processing routes are not always suitable for large-scale synthesis. Here, we report on a high-performance anode material for next generation Li-ion batteries made of nanoporous Sn powders with hierarchical ligament morphology. This material system combines both long cycle lifetimes (more than 72% capacity retention after 350 cycles), high capacity (693 mAh/g, nearlymore » twice that of commercial graphitic carbon), good charging/discharging capabilities (545 mAh/g at 1 A/g, 1.5C), and a scalable processing route that involves selective alloy corrosion. The good cycling performance of this system is attributed to its nanoporous architecture and its unique hierarchical ligament morphology, which accommodates the large volume changes taking place during lithiation, as confirmed by synchrotron-based ex-situ X-ray 3D tomography analysis. In conclusion, our findings are an important step for the development of high-performance Li-ion batteries.« less

High-fraction brookite films from amorphous precursors

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

Haggerty, James E. S.; Schelhas, Laura T.; Kitchaev, Daniil A.

2017-11-09

Structure-specific synthesis processes are of key importance to the growth of polymorphic functional compounds such as TiO 2, where material properties strongly depend on structure as well as chemistry. The robust growth of the brookite polymorph of TiO 2, a promising photocatalyst, has been difficult in both powder and thin-film forms due to the disparity of reported synthesis techniques, their highly specific nature, and lack of mechanistic understanding. In this work, we report the growth of high-fraction (~95%) brookite thin films prepared by annealing amorphous titania precursor films deposited by pulsed laser deposition. We characterize the crystallization process, eliminating themore » previously suggested roles of substrate templating and Na helper ions in driving brookite formation. Instead, we link phase selection directly to film thickness, offering a novel, generalizable route to brookite growth that does not rely on the presence of extraneous elements or particular lattice-matched substrates. In addition to providing a new synthesis route to brookite thin films, our results take a step towards resolving the problem of phase selection in TiO 2 growth, contributing to the further development of this promising functional material.« less

Corrosion Issues for Ceramics in Gas Turbines

NASA Technical Reports Server (NTRS)

Jacobson, Nathan S.; Fox, Dennis S.; Smialek, James L.; Opila, Elizabeth J.; Tortorelli, Peter F.; More, Karren L.; Nickel, Klaus G.; Hirata, Takehiko; Yoshida, Makoto; Yuri, Isao

2000-01-01

The requirements for hot-gas-path materials in gas turbine engines are demanding. These materials must maintain high strength and creep resistance in a particularly aggressive environment. A typical gas turbine environment involves high temperatures, rapid gas flow rates, high pressures, and a complex mixture of aggressive gases. Figure 26.1 illustrates the requirements for components of an aircraft engine and critical issues [1]. Currently, heat engines are constructed of metal alloys, which meet these requirements within strict temperature limits. In order to extend these temperature limits, ceramic materials have been considered as potential engine materials, due to their high melting points and stability at high temperatures. These materials include oxides, carbides, borides, and nitrides. Interest in using these materials in engines appears to have begun in the 1940s with BeO-based porcelains [2]. During the 1950s, the efforts shifted to cermets. These were carbide-based materials intended to exploit the best properties of metals and ceramics. During the 1960s and 1970s, the silicon-based ceramics silicon carbide (SiC) and silicon nitride (Si3N4) were extensively developed. Although the desirable high-temperature properties of SiC and Si3N4 had long been known, consolidation of powders into component-sized bodies required the development of a series of specialized processing routes [3]. For SiC, the major consolidation routes are reaction bonding, hot-pressing, and sintering. The use of boron and carbon as additives which enable sintering was a particularly noteworthy advance [4]. For Si3N4 the major consolidation routes are reaction bonding and hot pressing [5]. Reaction-bonding involves nitridation of silicon powder. Hot pressing involves addition of various refractory oxides, such as magnesia (MgO), alumina (Al2O3), and yttria (y2O3). Variations on these processes include a number of routes including Hot Isostatic Pressing (HIP), gas-pressure sintering, sinter-HIPing, and Encapsulation-HIPing. It is important to note that each process involves the addition of secondary elements, which later were shown to dramatically influence oxidation and corrosion behavior. As dense bodies of silicon-based ceramics became more readily available, their desirable high temperature properties were confirmed. These materials retained strength to very high temperatures (i.e. 1300-1400 C). Further, they were lightweight and made from abundant materials. SiC and Si3N4 therefore emerged as leading ceramic candidates for components in heat engines, designed to operate at higher temperatures for better performance and fuel efficiency. The first US programs for ceramics in heat engines have been reviewed [6]. Selected programs on ceramic engine parts are summarized here in regard to their contributions to understanding the corrosion behavior of a heat engine environment.

Scalable graphene production from ethanol decomposition by microwave argon plasma torch

NASA Astrophysics Data System (ADS)

Melero, C.; Rincón, R.; Muñoz, J.; Zhang, G.; Sun, S.; Perez, A.; Royuela, O.; González-Gago, C.; Calzada, M. D.

2018-01-01

A fast, efficient and simple method is presented for the production of high quality graphene on a large scale by using an atmospheric pressure plasma-based technique. This technique allows to obtain high quality graphene in powder in just one step, without the use of neither metal catalysts and nor specific substrate during the process. Moreover, the cost for graphene production is significantly reduced since the ethanol used as carbon source can be obtained from the fermentation of agricultural industries. The process provides an additional benefit contributing to the revalorization of waste in the production of a high-value added product like graphene. Thus, this work demonstrates the features of plasma technology as a low cost, efficient, clean and environmentally friendly route for production of high-quality graphene.

Direct metal writing: Controlling the rheology through microstructure

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

Chen, Wen; Thornley, Luke; Coe, Hannah G.

Most metal additive manufacturing approaches are based on powder-bed melting techniques such as laser selective melting or electron beam melting, which often yield uncontrolled microstructures with defects (e.g., pores or microcracks) and residual stresses. Here, we introduce a proof-of-concept prototype of a 3D metal freeform fabrication process by direct writing of metallic alloys in the semi-solid regime. This process is achieved through controlling the particular microstructure and the rheological behavior of semi-solid alloy slurries, which demonstrate a well suited viscosity and a shear thinning property to retain the shape upon printing. Furthermore, the ability to control the microstructure through thismore » method yields a flexible manufacturing route to fabricating 3D metal parts with full density and complex geometries.« less

Direct metal writing: Controlling the rheology through microstructure

DOE PAGES

Chen, Wen; Thornley, Luke; Coe, Hannah G.; ...

2017-02-27

Most metal additive manufacturing approaches are based on powder-bed melting techniques such as laser selective melting or electron beam melting, which often yield uncontrolled microstructures with defects (e.g., pores or microcracks) and residual stresses. Here, we introduce a proof-of-concept prototype of a 3D metal freeform fabrication process by direct writing of metallic alloys in the semi-solid regime. This process is achieved through controlling the particular microstructure and the rheological behavior of semi-solid alloy slurries, which demonstrate a well suited viscosity and a shear thinning property to retain the shape upon printing. Furthermore, the ability to control the microstructure through thismore » method yields a flexible manufacturing route to fabricating 3D metal parts with full density and complex geometries.« less

47. BUILDING NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, INTERIOR, ...

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

47. BUILDING NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, INTERIOR, 4TH LEVEL, LOOKING NORTH AT TOPS OF ALCOHOL AND ETHER DISTILLATION TOWERS. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

77 FR 64592 - Tongue River Railroad Company, Inc.-Rail Construction and Operation-in Custer, Powder River and...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-10-22

.... Colstrip Alternative--This route would leave the existing Cow Creek branch of BNSF at Colstrip, crossing Cow Creek and Rosebud Creek as it heads south and east, following the Greenleaf Creek valley to the...

Rapid Processing of Net-Shape Thermoplastic Planar-Random Composite Preforms

NASA Astrophysics Data System (ADS)

Jespersen, S. T.; Baudry, F.; Schmäh, D.; Wakeman, M. D.; Michaud, V.; Blanchard, P.; Norris, R. E.; Månson, J.-A. E.

2009-02-01

A novel thermoplastic composite preforming and moulding process is investigated to target cost issues in textile composite processing associated with trim waste, and the limited mechanical properties of current bulk flow-moulding composites. The thermoplastic programmable powdered preforming process (TP-P4) uses commingled glass and polypropylene yarns, which are cut to length before air assisted deposition onto a vacuum screen, enabling local preform areal weight tailoring. The as-placed fibres are heat-set for improved handling before an optional preconsolidation stage. The preforms are then preheated and press formed to obtain the final part. The process stages are examined to optimize part quality and throughput versus processing parameters. A viable processing route is proposed with typical cycle times below 40 s (for a plate 0.5 × 0.5 m2, weighing 2 kg), enabling high production capacity from one line. The mechanical performance is shown to surpass that of 40 wt.% GMT and has properties equivalent to those of 40 wt.% GMTex at both 20°C and 80°C.

Powder treatment process

DOEpatents

Weyand, J.D.

1988-02-09

Disclosed are: (1) a process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder. 2 figs.

Powder treatment process

DOEpatents

Weyand, John D.

1988-01-01

(1) A process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder.

16. BUILDING NO. 445, PHYSICS LAB (FORMERLY GUN BAG LOADING), ...

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

16. BUILDING NO. 445, PHYSICS LAB (FORMERLY GUN BAG LOADING), INTERIOR, SECOND LEVEL. LOOKING UP AT POWDER AND DISTRIBUTION TUBES. ELEVATOR SHAFT ON LEFT. - Picatinny Arsenal, 400 Area, Gun Bag Loading District, State Route 15 near I-80, Dover, Morris County, NJ

DEXTRON TEMPLATED MICROWAVE-ASSISTED SYNTHESIS OF POROUS TITANIUM DIOXIDE

EPA Science Inventory

An alternative route to the preparation and formation of porous titania powders and carbon coated titania using microwave radiation is described. Inexpensive dextrose was chosen as capping agent or template in view of its high water solubility when compared to other sugar templat...

Preparation and Characteristics of Porous Ceramics by a foaming Technology at Low Temperature

NASA Astrophysics Data System (ADS)

Zhang, H. Q.; Wang, S. P.; Wen, J.; Wu, N.; Xu, S. H.

2017-12-01

Recycling and converting coal gangue and red mud into porous ceramics with good performance is a feasible disposal route. In this present work, porous foam ceramics was prepared using coal gangue and red mud as main raw materials at low sintering temperature, The amount of coal gangue and red mud were up to 70 wt%. To regulate the forming and sintering performance of the product, quartz sands and clay material were added to the formula. The green body was formed by a foaming technology using aluminum powders as foaming agents at room temperature. After foamed, the specimens were dried at 60-80 °C, and then calcined at 1060°C. Effects of concentration of NaOH and amount of aluminum powders on the phase, mechanical properties and microstructure were investigated here. Such study is expected to provide a new utilization route of the coal gangue and red mud, and brings both intensive environmental and economic benefits.

Mechanochemical synthesis of nanostructured Sr(Ti{sub 1-x}Fe{sub x})O{sub 3-{delta}} solid-solution powders and their surface photovoltage responses

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

Chen Xiaofeng; Luo Qiong; GlobalFoundries Singapore Pte Ltd, 60 Woodlands Industrial Park D Street 2, Singapore 738406

2012-05-15

A series of nanostructure Sr(Ti{sub 1-x}Fe{sub x})O{sub 3-{delta}} (STFx, x=0.4, 0.6, 0.8) solid-solution powders were synthesized by mechanochemical approach milling from the mixture of SrO, Fe{sub 2}O{sub 3} and TiO{sub 2} metal oxides at room temperature. The XRD results revealed that the perovskite STFx nanoparticles were finally formed with few residual {alpha}-Fe{sub 2}O{sub 3} detected dependent on the milling conditions. The structure evolution suggested that the mechanochemical synthesis underwent via a solid-state reaction route to initially form Ti-rich perovskite and then incorporate with the residual {alpha}-Fe{sub 2}O{sub 3} to achieve the estimated composition. The synthesized STF08 powders exhibited the significantmore » Surface Photovoltage (SPV) spectrum response both in UV and in visible-light region with p-type semiconductor behavior. This finding suggested that the synthesized STF nanopowders could potentially utilize more solar spectrum energy effectively for photo-oxidation and photo-catalysis applications. - Graphical abstract: It is demonstrated that Sr(Ti{sub 1-x}Fe{sub x})O{sub 3-{delta}} perovskite nanopowders were successfully synthesized by mechanochemical reaction approach at room temerpature, and the synthesized STF08 powders showed the significant SPV response in UV-VIS region with p-type semiconductor behaviors. Highlights: Black-Right-Pointing-Pointer Sr(Ti{sub 1-x}Fe{sub x})O{sub 3-{delta}} nanopowders synthesized by mechanochemical reaction approach. Black-Right-Pointing-Pointer The reaction process was shorten by introduce high impact energy. Black-Right-Pointing-Pointer Synthesized STF08 powders show the significant SPV response in UV-VIS region. Black-Right-Pointing-Pointer Synthesized STFx powders show p-type semiconductor behaviors.« less

Effect of synthesis conditions on the nanopowder properties of Ce{sub 0.9}Zr{sub 0.1}O{sub 2}

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

Zimicz, M.G.; Fabregas, I.O.; Lamas, D.G.

Graphical abstract: . The synthesis of nanocrystalline Ce{sub 0.9}Zr{sub 0.1}O{sub 2} powders via the gel-combustion method, using different fuels, and following either stoichiometric or non-stoichiometric pH-controlled routes is investigated. Research highlights: {yields} All samples exhibited the fluorite-type crystal structure, nanometric average crystallite size and negligible carbon content. {yields} Synthesis conditions strongly affect the average crystallite size, the degree of agglomeration, the specific surface area and the pore volume. {yields} Our results indicate that, by controlling the synthesis conditions it is possible to obtain solids with custom-made morphological properties. -- Abstract: In this work, the synthesis of nanocrystalline Ce{sub 0.9}Zr{sub 0.1}O{submore » 2} powders via the gel-combustion method, using different fuels, and following either stoichiometric or non-stoichiometric pH-controlled routes is investigated. The objective is to evaluate the effect of synthesis conditions on the textural and morphological properties, and the crystal structure of the synthesized materials. The solids were characterized by nitrogen physisorption, Scanning Electron Microscopy (SEM), X-ray powder diffraction (XPD), and Carbon-Hydrogen-Nitrogen Elemental Analysis (CHN). All the powders exhibited nanometric crystallite size, fluorite-type structure and negligible carbon content. Synthesis conditions strongly affect the average crystallite size, the degree of agglomeration, the specific surface area and the pore volume. Our results indicate that, by controlling the synthesis conditions it is possible to obtain solids with custom-made morphological properties.« less

Dual mechanisms of grain refinement in a FeCoCrNi high-entropy alloy processed by high-pressure torsion

PubMed Central

Wu, Wenqian; Song, Min; Ni, Song; Wang, Jingshi; Liu, Yong; Liu, Bin; Liao, Xiaozhou

2017-01-01

An equiatomic FeCoCrNi high-entropy alloy with a face-centered cubic structure was fabricated by a powder metallurgy route, and then processed by high-pressure torsion. Detailed microscopy investigations revealed that grain refinement from coarse grains to nanocrystalline grains occurred mainly via concurrent nanoband (NB) subdivision and deformation twinning. NB–NB, twin–NB and twin–twin interactions contributed to the deformation process. The twin–twin interactions resulted in severe lattice distortion and accumulation of high densities of dislocations in the interaction areas. With increasing strain, NB subdivision and interactions between primary twins and inclined secondary stacking faults (SFs)/nanotwins occurred. Secondary nanotwins divided the primary twins into many equiaxed parts, leading to further grain refinement. The interactions between secondary SFs/nanotwins associated with the presence of Shockley partials and primary twins also transformed the primary twin boundaries into incoherent high-angle grain boundaries. PMID:28429759

The role of nano-particles in the field of thermal spray coating technology

NASA Astrophysics Data System (ADS)

Siegmann, Stephan; Leparoux, Marc; Rohr, Lukas

2005-06-01

Nano-particles play not only a key role in recent research fields, but also in the public discussions about health and safety in nanotechnology. Nevertheless, the worldwide activities in nano-particles research increased dramatically during the last 5 to 10 years. There are different potential routes for the future production of nano-particles at large scale. The main directions envisaged are mechanical milling, wet chemical reactions or gas phase processes. Each of the processes has its specific advantages and limitations. Mechanical milling and wet chemical reactions are typically time intensive and batch processes, whereas gas phase productions by flames or plasma can be carried out continuously. Materials of interest are mainly oxide ceramics, carbides, nitrides, and pure metals. Nano-ceramics are interesting candidates for coating technologies due to expected higher coating toughness, better thermal shock and wear resistance. Especially embedded nano-carbides and-nitrides offer homogenously distributed hard phases, which enhance coatings hardness. Thermal spraying, a nearly 100 years old and world wide established coating technology, gets new possibilities thanks to optimized, nano-sized and/or nano-structured powders. Latest coating system developments like high velocity flame spraying (HVOF), cold gas deposition or liquid suspension spraying in combination with new powder qualities may open new applications and markets. This article gives an overview on the latest activities in nano-particle research and production in special relation to thermal spray coating technology.

8. Photocopied 1983, from original drawing (DP14261), Picatinny Arsenal, August ...

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

8. Photocopied 1983, from original drawing (DP-14261), Picatinny Arsenal, August 14, 1931. BUILDING NO. 511, 'NITRATING HOUSE - BUILDING 511 ALTERATIONS AND ADDITIONS TO EQUIPMENT - SECTIONS,'. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

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

Ranieri, M.G.A., E-mail: gabi.ranieri@ig.com.br; Aguiar, E.C.; Cilense, M.

Highlights: • Bi{sub 4}Ti{sub 3}O{sub 12} thick films were obtained by SSR and PPM methods. • Both systems crystallize in an orthorhombic structure. • Textured characteristics were evidenced. • Grain morphology affects the P–E loops. - Abstract: Bismuth titanate powders (Bi{sub 4}Ti{sub 3}O{sub 12}-BIT) were fabricated by solid state reaction (SSR) and polymeric precursor method (PPM). From these powders, Bi{sub 4}Ti{sub 3}O{sub 12} pellets were obtained by tape-casting using plate-like templates particles prepared by a molten salt method. The BIT phase crystallizes in an orthorhombic structure type with space group Fmmm. Agglomeration of the particles, which affects the densification ofmore » the ceramic, electrical conduction and leakage current at high electric fields, was monitored by transmission electronic microscopy (TEM) analyses. FEG-SEM indicated that different shape of grains of BIT ceramics was influenced by the processing route. Both SSR and PPM methods lead to unsaturated P–E loops of BIT ceramics originating from the highly c-axis orientation and high conductivity which was affected by charge carriers flowing normally to the grain boundary of the crystal lattice.« less

Copper-containing ceramic precursor synthesis: Solid-state transformations and materials technology

NASA Technical Reports Server (NTRS)

Hepp, Aloysius F.; Eckles, William E.; Duraj, Stan A.; Andras, Maria T.; Fanwick, Phillip E.; Richman, Robert M.; Sabat, Michael L.; Power, Michael B.; Gordon, Edward M.; Barron, Andrew

1994-01-01

Three copper systems with relevance to materials technology are discussed. In the first, a CuS precursor, Cu4S1O (4-methylpyridine)(sub 4)- (4-MePy), was prepared by three routes: reaction of Cu2S, reaction of CuBr-SMe2, and oxidation of copper powder with excess sulfur in 4-methylpyridine by sulfur. In the second, copper powder was found to react with excess thiourea (H2NC(S)NH2) in 4-methylpyridine to produce thiocyanate (NCS(-)) complexes. Three isolated and characterized compounds are: Cu(NCS)(4-MePy)(sub 2), a polymer, (4-MePy-H)(Cu(NCS)(sub 3)(4-MePy)(sub 2)), a salt, and t-Cu(NCS)(sub 2)(4-MePy)(sub 4). Finally, an attempt to produce a mixed-metal sulfide precursor of Cu and Ga in N-methylimidazole (N-MeIm) resulted in the synthesis of a Cu-containing polymer, Cu(SO4)(N-MeIm). The structures are presented; the chemistry will be briefly discussed in the context of preparation and processing of copper-containing materials for aerospace applications.

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

NASA Technical Reports Server (NTRS)

Sun, Z.; Huertas, J. I.; Axelbaum, R. L.

1999-01-01

Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.

Alternative products to treat allergic rhinitis and alternative routes for allergy immunotherapy.

PubMed

Ipci, Kagan; Oktemer, Tugba; Muluk, Nuray Bayar; Şahin, Ethem; Altıntoprak, Niyazi; Bafaqeeh, Sameer Ali; Kurt, Yasemin; Mladina, Ranko; Šubarić, Marin; Cingi, Cemal

2016-09-01

Some alternative products instead of immunotherapy are used in patients with allergic rhinitis (AR). In this paper, alternative products to treat allergic rhinitis and alternative routes for allergy immunotherapy are reviewed. Alternative products and methods used instead of immunotherapy are tea therapy, acupuncture, Nigella sativa, cinnamon bark, Spanish needle, acerola, capsaicin (Capsicum annum), allergen-absorbing ointment, and cellulose powder. N. sativa has been used in AR treatment due to its anti-inflammatory effects. N. sativa oil also inhibits the cyclooxygenase and 5-lipoxygenase pathways of arachidonic acid metabolism. The beneficial effects of N. sativa seed supplementation on the symptoms of AR may be due to its antihistaminic properties. To improve the efficacy of immunotherapy, some measures are taken regarding known immunotherapy applications and alternative routes of intralymphatic immunotherapy and epicutaneous immunotherapy are used. There are alternative routes and products to improve the efficacy of immunotherapy.

Nanometrization of Lanthanide-Based Coordination Polymers.

PubMed

Neaime, Chrystelle; Daiguebonne, Carole; Calvez, Guillaume; Freslon, Stéphane; Bernot, Kevin; Grasset, Fabien; Cordier, Stéphane; Guillou, Olivier

2015-11-23

Heteronuclear lanthanide-based coordination polymers are microcrystalline powders, the luminescence properties of which can be precisely tuned by judicious choice of the rare-earth ions. In this study, we demonstrate that such materials can also be obtained as stable solutions of nanoparticles in non-toxic polyols. Bulk powders of the formula [Ln2-2x Ln'2x (bdc)3 ⋅4 H2 O]∞ (where H2 bdc denotes 1,4-benzene-dicarboxylic acid, 0≤x≤1, and Ln and Ln' denote lanthanide ions of the series La to Tm plus Y) afford nanoparticles that have been characterized by dynamic light-scattering (DLS) and transmission electron microscopy (TEM) measurements. Their luminescence properties are similar to those of the bulk materials. Stabilities versus time and versus dilution with another solvent have been studied. This study has revealed that it is possible to tune the size of the nanoparticles. This process offers a reliable means of synthesizing suspensions of nanoparticles with tunable luminescence properties and tunable size distributions in a green solvent (glycerol). The process is also extendable to other coordination polymers and other solvents (ethylene glycol, for example). It constitutes a new route for the facile solubilization of lanthanide-based coordination polymers. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Experimental study of the Er-Zr-O ternary system at 800 °C and 1100 °C

NASA Astrophysics Data System (ADS)

Mascaro, A.; Jourdan, J.; Toffolon-Masclet, C.; Joubert, J.-M.

2012-08-01

The Er-O-Zr ternary system has been investigated experimentally along two isothermal sections at 800 °C and 1100 °C. In order to obtain pure and homogeneous samples, powder metallurgy has been used. The samples have been synthesized using pure Er and Zr powder obtained by the hydride route. The study has been focused on the Zr rich corner and the results allow defining the co-solubility domains at both temperatures and the nature of the phases in equilibrium with αZr and βZr.

Speciation of residual carbon contained in UO{sub 2}

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

Ziouane, Yannis; Arab-Chapelet, Bénédicte; Tamain, Christelle

2016-12-15

UO{sub 2} powders were synthesized thanks to oxalic precipitation (platelet morphology) and sol-gel route and completely characterized. A secondary phase was found depending on the calcination atmospheres. This phase has been identified by Raman spectroscopy as graphitic material (i.e. carbon-based secondary compound) and quantified by thermogravimetric analyses. Its amount varies with the calcination atmosphere. The presence of this secondary phase has no significant effect on the lattice parameter and its specific surface area. - Graphical abstract: Figure 2: Raman spectroscopy of the three UO{sub 2} powders and of the dissolution residues.

High coercivity, anisotropic, heavy rare earth-free Nd-Fe-B by Flash Spark Plasma Sintering.

PubMed

Castle, Elinor; Sheridan, Richard; Zhou, Wei; Grasso, Salvatore; Walton, Allan; Reece, Michael J

2017-09-11

In the drive to reduce the critical Heavy Rare Earth (HRE) content of magnets for green technologies, HRE-free Nd-Fe-B has become an attractive option. HRE is added to Nd-Fe-B to enhance the high temperature performance of the magnets. To produce similar high temperature properties without HRE, a crystallographically textured nanoscale grain structure is ideal; and this conventionally requires expensive "die upset" processing routes. Here, a Flash Spark Plasma Sintering (FSPS) process has been applied to a Dy-free Nd 30.0 Fe 61.8 Co 5.8 Ga 0.6 Al 0.1 B 0.9 melt spun powder (MQU-F, neo Magnequench). Rapid sinter-forging of a green compact to near theoretical density was achieved during the 10 s process, and therefore represents a quick and efficient means of producing die-upset Nd-Fe-B material. The microstructure of the FSPS samples was investigated by SEM and TEM imaging, and the observations were used to guide the optimisation of the process. The most optimal sample is compared directly to commercially die-upset forged (MQIII-F) material made from the same MQU-F powder. It is shown that the grain size of the FSPS material is halved in comparison to the MQIII-F material, leading to a 14% increase in coercivity (1438 kA m -1 ) and matched remanence (1.16 T) giving a BH max of 230 kJ m -3 .

Data on the impact of increasing the W amount on the mass density and compressive properties of Ni-W alloys processed by spark plasma sintering.

PubMed

Sadat, T; Hocini, A; Lilensten, L; Faurie, D; Tingaud, D; Dirras, G

2016-06-01

Bulk Ni-W alloys having composite-like microstructures are processed by spark plasma sintering (SPS) route of Ni and W powder blends as reported in a recent study of Sadat et al. (2016) (DOI of original article: doi:10.1016/j.matdes.2015.10.083) [1]. The present dataset deals with determination of mass density and evaluation of room temperature compressive mechanical properties as function of the amount of W (%wt. basis). The presented data concern: (i) measurement of the mass of each investigated Ni-W alloy which is subsequently used to compute the mass density of the alloy and (ii) the raw (stress (MPa) and strain ([Formula: see text])) data, which can be subsequently used for stress/ strain plots.

Data on the impact of increasing the W amount on the mass density and compressive properties of Ni–W alloys processed by spark plasma sintering

PubMed Central

Sadat, T.; Hocini, A.; Lilensten, L.; Faurie, D.; Tingaud, D.; Dirras, G.

2016-01-01

Bulk Ni–W alloys having composite-like microstructures are processed by spark plasma sintering (SPS) route of Ni and W powder blends as reported in a recent study of Sadat et al. (2016) (DOI of original article: doi:10.1016/j.matdes.2015.10.083) [1]. The present dataset deals with determination of mass density and evaluation of room temperature compressive mechanical properties as function of the amount of W (%wt. basis). The presented data concern: (i) measurement of the mass of each investigated Ni–W alloy which is subsequently used to compute the mass density of the alloy and (ii) the raw (stress (MPa) and strain (ΔLL0)) data, which can be subsequently used for stress/ strain plots. PMID:27158658

Continuous Polyol Synthesis of Metal and Metal Oxide Nanoparticles Using a Segmented Flow Tubular Reactor (SFTR).

PubMed

Testino, Andrea; Pilger, Frank; Lucchini, Mattia Alberto; Quinsaat, Jose Enrico Q; Stähli, Christoph; Bowen, Paul

2015-06-08

Over the last years a new type of tubular plug flow reactor, the segmented flow tubular reactor (SFTR), has proven its versatility and robustness through the water-based synthesis of precipitates as varied as CaCO3, BaTiO3, Mn(1-x)NixC2O4·2H2O, YBa oxalates, copper oxalate, ZnS, ZnO, iron oxides, and TiO2 produced with a high powder quality (phase composition, particle size, and shape) and high reproducibility. The SFTR has been developed to overcome the classical problems of powder production scale-up from batch processes, which are mainly linked with mass and heat transfer. Recently, the SFTR concept has been further developed and applied for the synthesis of metals, metal oxides, and salts in form of nano- or micro-particles in organic solvents. This has been done by increasing the working temperature and modifying the particle carrying solvent. In this paper we summarize the experimental results for four materials prepared according to the polyol synthesis route combined with the SFTR. CeO2, Ni, Ag, and Ca3(PO4)2 nanoparticles (NPs) can be obtained with a production rate of about 1-10 g per h. The production was carried out for several hours with constant product quality. These findings further corroborate the reliability and versatility of the SFTR for high throughput powder production.

Pulmonary delivery of a GLP-1 receptor agonist, BMS-686117.

PubMed

Qian, Feng; Mathias, Neil; Moench, Paul; Chi, Cecilia; Desikan, Sridhar; Hussain, Munir; Smith, Ronald L

2009-01-21

Alternate delivery route of therapeutic peptides is an attractive non-invasive option to patients who must chronically self-administer their medication through injections. In recent years, much attention has centered on pulmonary peptide delivery of peptide drugs such as insulin and GLP-1 mimetic peptides in the treatment of type II diabetes. In this study, we assessed the feasibility of delivering BMS-686117, an 11-mer GLP-1 receptor peptide agonist, to the lung in rats via intratracheal administration. The pharmacokinetic profiles of three spray-dried, prototype inhaled powder formulations, 80/20 BMS-686117/trehalose (I), 100% BMS-686117 (II), and 20/80 BMS-686117/mannitol (III), as well as a lyophilized BMS-686117 powder, were compared with intravenously and subcutaneously administered peptide. The spray-dried formulations were mostly spherical particles with narrow particle size distribution between 2 to 10 microm, which are better suited for inhalation delivery than the lyophilized, irregular shape powder with a wide particle size distribution between 2 to 100 microm. Prototype III exhibited the best physical characteristics and in vivo performance, with bioavailability of 45% relative to subcutaneous administration. The T(max) for lung delivered peptide formulations were almost twice as fast as subcutaneous injection, suggesting potential for rapid absorption and onset of action. This study demonstrated that pulmonary delivery is a promising, non-invasive route for the administration of BMS-686117.

Redox reaction between graphene oxide and In powder to prepare In2O3/reduced graphene oxide hybrids for supercapacitors

NASA Astrophysics Data System (ADS)

Xu, Xiaoyang; Wu, Tao; Xia, Fengling; Li, Yi; Zhang, Congcong; Zhang, Lei; Chen, Mingxi; Li, Xichuan; Zhang, Li; Liu, Yu; Gao, Jianping

2014-11-01

A facile and quick route for the chemical reduction of graphene oxide (GO) using In powder as a reductant has been established. The reduction of GO by In powder is traced by UV-visible absorption spectroscopy, and the obtained reduced graphene oxide (rGO) is analyzed. The In3+ ions produced during the reaction between the GO and the In powder are chemically transformed to In2O3 and then form In2O3/rGO hybrids. The In2O3/rGO hybrids are used as electrode materials and their electrochemical performance are studied using cyclic voltammetry and galvanostatic charge/discharge. The In2O3/rGO hybrids demonstrate excellent electrochemical performance and their highest specific capacitance is 178.8 F g-1 which is much higher than that of either In2O3 or rGO. In addition, the In2O3/rGO hybrids are also very stable.

Mechanical behaviour of pressed and sintered titanium alloys obtained from prealloyed and blended elemental powders.

PubMed

Bolzoni, L; Esteban, P G; Ruiz-Navas, E M; Gordo, E

2012-10-01

The applicability of irregular prealloyed Ti-6Al-4V powder for the fabrication of titanium products by pressing and sintering and its employment as a master alloy to obtain the Ti-3Al-2.5V alloy was studied. To this end, the starting powders were characterised by dilatometry, differential thermal analysis and XRD. Green samples were obtained by cold uniaxial pressing, and the evolution of the microstructure over the sintering temperature range 900-1400°C was studied. The variation of the final density and mechanical properties with the sintering temperature was considered. Based on the study carried out, it can be stated that more reliable powders are needed to open the titanium market to new applications. A relative density of 95% and diverse microstructural features and mechanical properties equivalent to those of biomedical devices can be obtained by the pressing and sintering route. Copyright © 2012 Elsevier Ltd. All rights reserved.

Microwave assisted synthesis and characterization of barium titanate nanoparticles for multi layered ceramic capacitor applications.

PubMed

Thirumalai, Sundararajan; Shanmugavel, Balasivanandha Prabu

2011-01-01

Barium titanate is a common ferroelectric electro-ceramic material having high dielectric constant, with photorefractive effect and piezoelectric properties. In this research work, nano-scale barium titanate powders were synthesized by microwave assisted mechano-chemical route. Suitable precursors were ball milled for 20 hours. TGA studies were performed to study the thermal stability of the powders. The powders were characterized by XRD, SEM and EDX Analysis. Microwave and Conventional heating were performed at 1000 degrees C. The overall heating schedule was reduced by 8 hours in microwave heating thereby reducing the energy and time requirement. The nano-scale, impurity-free and defect-free microstructure was clearly evident from the SEM micrograph and EDX patterns. LCR meter was used to measure the dielectric constant and dielectric loss values at various frequencies. Microwave heated powders showed superior dielectric constant value with low dielectric loss which is highly essential for the fabrication of Multi Layered Ceramic Capacitors.

Microstructural and Mechanical Characterization of Ti-12Mo-6Zr Biomaterials Fabricated by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Daoush, Walid Mohamed Rashad Mohamed; Park, Hee Sup; Inam, Fawad; Lim, Byung Kyu; Hong, Soon Hyung

2015-03-01

Ti-12Mo-6Zr/Al2O3 (titanium biomaterial) was prepared by a powder metallurgy route using Spark Plasma Sintering (SPS). Ti, Mo, and Zr powders were mixed by wet milling with different content of alumina nanoparticles (up to 5 wt pct) as an oxide dispersion strengthening phase. Composite powder mixtures were SPSed at 1273 K (1000 °C) followed by heat treatment and quenching. Composite powders, sintered materials, and heat-treated materials were examined using optical and high-resolution electronic microscopy (scanning and transmission) and X-ray diffraction to characterize particle size, surface morphology, and phase identifications for each composition. All sintered materials were evaluated by measuring density, Vickers hardness, and tensile properties. Fully dense sintered materials were produced by SPS and mechanical properties were found to be improved by subsequent heat treatment. The tensile properties as well as the hardness were increased by increasing the content of Al2O3 nanoparticles in the Ti-12Mo-6Zr matrix.

Development of steel foam processing methods and characterization of metal foam

NASA Astrophysics Data System (ADS)

Park, Chanman

2000-10-01

Steel foam was synthesized by a powder metallurgical route, resulting in densities less than half that of steel. Process parameters for foam synthesis were investigated, and two standard powder formulations were selected consisting of Fe-2.5% C and 0.2 wt% foaming agent (either MgCO3 or SrCO3). Compression tests were performed on annealed and pre-annealed foam samples of different density to determine mechanical response and energy absorption behavior. The stress-strain response was strongly affected by annealing, which reduced the carbon content and converted much of the pearlitic structure to ferrite. Different powder blending methods and melting times were employed and the effects on the geometric structure of steel foam were examined. Dispersion of the foaming agent affected the pore size distribution of the expanded foams. With increasing melt time, pores coalesced, leading to the eventual collapse of the foam. Inserting interlayer membranes in the powder compacts inhibited coalescence of pores and produced foams with more uniform cell size and distribution. The closed-cell foam samples exhibited anisotropy in compression, a phenomenon that was caused primarily by the ellipsoidal cell shapes within the foam. Yield strengths were 3x higher in the transverse direction than in the longitudinal direction. Yield strength also showed a power-law dependence on relative density (n ≅ 1.8). Compressive strain was highly localized and occurred in discrete bands that extended transverse to the loading direction. The yield strength of foam samples showed stronger strain rate dependence at higher strain rates. The increased strain rate dependence was attributed to microinertial hardening. Energy absorption was also observed to increase with strain rate. Measurements of cell wall curvature showed that an increased mean curvature correlated with a reduced yield strength, and foam strengths generally fell below predictions of Gibson-Ashby theory. Morphological defects reduced yield strength and altered the dependence on density. Microstructural analysis was performed on a porous Mg and AZ31 Mg alloy synthesized by the GASAR process. The pore distribution depended on the distance from the chill end of ingots. TEM observations revealed apparent gas tracks neat the pores and ternary intermetallic phases in the alloy.

Bioleaching of valuable metals from spent lithium-ion mobile phone batteries using Aspergillus niger

NASA Astrophysics Data System (ADS)

Horeh, N. Bahaloo; Mousavi, S. M.; Shojaosadati, S. A.

2016-07-01

In this paper, a bio-hydrometallurgical route based on fungal activity of Aspergillus niger was evaluated for the detoxification and recovery of Cu, Li, Mn, Al, Co and Ni metals from spent lithium-ion phone mobile batteries under various conditions (one-step, two-step and spent medium bioleaching). The maximum recovery efficiency of 100% for Cu, 95% for Li, 70% for Mn, 65% for Al, 45% for Co, and 38% for Ni was obtained at a pulp density of 1% in spent medium bioleaching. The HPLC results indicated that citric acid in comparison with other detected organic acids (gluconic, oxalic and malic acid) had an important role in the effectiveness of bioleaching using A. niger. The results of FTIR, XRD and FE-SEM analysis of battery powder before and after bioleaching process confirmed that the fungal activities were quite effective. In addition, bioleaching achieved higher removal efficiency for heavy metals than the chemical leaching. This research demonstrated the great potential of bio-hydrometallurgical route to recover heavy metals from spent lithium-ion mobile phone batteries.

Surface passivity largely governs the bioaccessibility of nickel-based powder particles at human exposure conditions.

PubMed

Hedberg, Yolanda S; Herting, Gunilla; Latvala, Siiri; Elihn, Karine; Karlsson, Hanna L; Odnevall Wallinder, Inger

2016-11-01

The European chemical framework REACH requires that hazards and risks posed by chemicals, including alloys and metals, are identified and proven safe for humans and the environment. Therefore, differences in bioaccessibility in terms of released metals in synthetic biological fluids (different pH (1.5-7.4) and composition) that are relevant for different human exposure routes (inhalation, ingestion, and dermal contact) have been assessed for powder particles of an alloy containing high levels of nickel (Inconel 718, 57 wt% nickel). This powder is compared with the bioaccessibility of two nickel-containing stainless steel powders (AISI 316L, 10-12% nickel) and with powders representing their main pure alloy constituents: two nickel metal powders (100% nickel), two iron metal powders and two chromium metal powders. X-ray photoelectron spectroscopy, microscopy, light scattering, and nitrogen absorption were employed for the particle and surface oxide characterization. Atomic absorption spectroscopy was used to quantify released amounts of metals in solution. Cytotoxicity (Alamar blue assay) and DNA damage (comet assay) of the Inconel powder were assessed following exposure of the human lung cell line A549, as well as its ability to generate reactive oxygen species (DCFH-DA assay). Despite its high nickel content, the Inconel alloy powder did not release any significant amounts of metals and did not induce any toxic response. It is concluded, that this is related to the high surface passivity of the Inconel powder governed by its chromium-rich surface oxide. Read-across from the pure metal constituents is hence not recommended either for this or any other passive alloy. Copyright © 2016 The Author(s). Published by Elsevier Inc. All rights reserved.

Nanoporous Tin with a Granular Hierarchical Ligament Morphology as a Highly Stable Li-Ion Battery Anode

DOE PAGES

Cook, John B.; Detsi, Eric; Liu, Yijin; ...

2016-12-07

Next generation Li-ion batteries will require negative electrode materials with energy densities many-fold higher than that found in the graphitic carbon currently used in commercial Li-ion batteries. While various nanostructured alloying-type anode materials may satisfy that requirement, such materials do not always exhibit long cycle lifetimes and/or their processing routes are not always suitable for large-scale synthesis. Here, we report on a high-performance anode material for next generation Li-ion batteries made of nanoporous Sn powders with hierarchical ligament morphology. This material system combines both long cycle lifetimes (more than 72% capacity retention after 350 cycles), high capacity (693 mAh/g, nearlymore » twice that of commercial graphitic carbon), good charging/discharging capabilities (545 mAh/g at 1 A/g, 1.5C), and a scalable processing route that involves selective alloy corrosion. The good cycling performance of this system is attributed to its nanoporous architecture and its unique hierarchical ligament morphology, which accommodates the large volume changes taking place during lithiation, as confirmed by synchrotron-based ex-situ X-ray 3D tomography analysis. In conclusion, our findings are an important step for the development of high-performance Li-ion batteries.« less

The role of processing route on the microstructure of 14YWT nanostructured ferritic alloy

DOE PAGES

Mazumder, B.; Parish, C. M.; Bei, H.; ...

2015-06-03

Nanostructured ferritic alloys (NFAs) have outstanding high temperature creep properties and extreme tolerance to radiation damage. To achieve these properties, NFAs are fabricated by mechanical alloying of metallic and yttria powders. Atom probe tomography has demonstrated that milling times of at least 40 h are required to produce a uniform distribution of solutes in the flakes. After milling and hot extrusion, the microstructure consists of -Fe, high number densities of Ti-Y-O-vacancy-enriched nanoclusters, and coarse Y2Ti2O7 and Ti(O,C,N) precipitates on the grain boundaries. In contrast, the as-cast condition consists of -Fe with 50-100 m irregularly-shaped Y2Ti2O7 pyrochlore precipitates with smaller embeddedmore » precipitates with the Al5Y3O12 (yttrium-aluminum garnet) crystal structure indicating that this traditional processing route is not a viable approach to achieve the desired microstructure. The nano-hardnesses were also substantially different, i.e., 4 and 8 GPa for the as-cast and as-extruded conditions, respectively. These differences can be explained by the differences in the microstructure and the effects of the high vacancy content introduced by mechanical alloying, and the strong binding energy of vacancies with O, Ti, and Y atoms retarding diffusion.« less

The role of processing route on the microstructure of 14YWT nanostructured ferritic alloy

NASA Astrophysics Data System (ADS)

Mazumder, B.; Parish, C. M.; Bei, H.; Miller, M. K.

2015-10-01

Nanostructured ferritic alloys have outstanding high temperature creep properties and enhanced tolerance to radiation damage over conventional ferritic alloys. To achieve these properties, NFAs are fabricated by mechanical alloying of metallic and yttria powders. Atom probe tomography has demonstrated that milling times of at least 40 h are required to produce a uniform distribution of solutes in the flakes. After milling and hot extrusion, the microstructure consists of α-Fe, high number densities of Ti-Y-O-vacancy-enriched nanoclusters, and coarse Y2Ti2O7 and Ti(O,C,N) precipitates on the grain boundaries. In contrast, the as-cast condition consists of α-Fe with 50-100 μm irregularly-shaped Y2Ti2O7 pyrochlore precipitates with smaller embedded precipitates with the Y3Al5O12 (yttrium-aluminum garnet) crystal structure indicating that this traditional processing route is not a viable approach to achieve the desired microstructure. The nano-hardnesses were also substantially different, i.e., 4 and 8 GPa for the as-cast and as-extruded conditions, respectively. These variances can be explained by the microstructural differences and the effects of the high vacancy content introduced by mechanical alloying, and the strong binding energy of vacancies with O, Ti, and Y atoms that retard diffusion.

Luminescence properties of Sm3+-doped alkaline earth ortho-stannates

NASA Astrophysics Data System (ADS)

Stanulis, Andrius; Katelnikovas, Artūras; Enseling, David; Dutczak, Danuta; Šakirzanovas, Simas; Bael, Marlies Van; Hardy, An; Kareiva, Aivaras; Jüstel, Thomas

2014-05-01

A series of Sm3+ doped M2SnO4 (M = Ca, Sr and Ba) samples were prepared by a conventional high temperature solid-state reaction route. All samples were characterized by powder X-ray diffraction (XRD) analysis, photoluminescence (PL), photoluminescence thermal quenching (TQ) and fluorescence lifetime (FL) measurements. The morphology of synthesized phosphor powders was examined by scanning electron microscopy (SEM). Moreover, luminous efficacies (LE) and color points of the CIE 1931 color space diagram were calculated and discussed. Synthesized powders showed bright orange-red emission under UV excitation. Based on the results obtained we demonstrate that Sm3+ ions occupy Ca and Sr sites in the Ca2SnO4 and Sr2SnO4 ortho-stannate structures, respectively. In contrast, Sm3+ substitutes Sn in the barium ortho-stannate Ba2SnO4 structure.

Powder Bed Layer Characteristics: The Overseen First-Order Process Input

NASA Astrophysics Data System (ADS)

Mindt, H. W.; Megahed, M.; Lavery, N. P.; Holmes, M. A.; Brown, S. G. R.

2016-08-01

Powder Bed Additive Manufacturing offers unique advantages in terms of manufacturing cost, lot size, and product complexity compared to traditional processes such as casting, where a minimum lot size is mandatory to achieve economic competitiveness. Many studies—both experimental and numerical—are dedicated to the analysis of how process parameters such as heat source power, scan speed, and scan strategy affect the final material properties. Apart from the general urge to increase the build rate using thicker powder layers, the coating process and how the powder is distributed on the processing table has received very little attention to date. This paper focuses on the first step of every powder bed build process: Coating the process table. A numerical study is performed to investigate how powder is transferred from the source to the processing table. A solid coating blade is modeled to spread commercial Ti-6Al-4V powder. The resulting powder layer is analyzed statistically to determine the packing density and its variation across the processing table. The results are compared with literature reports using the so-called "rain" models. A parameter study is performed to identify the influence of process table displacement and wiper velocity on the powder distribution. The achieved packing density and how that affects subsequent heat source interaction with the powder bed is also investigated numerically.

PVC-based composite material containing recycled non-metallic printed circuit board (PCB) powders.

PubMed

Wang, Xinjie; Guo, Yuwen; Liu, Jingyang; Qiao, Qi; Liang, Jijun

2010-12-01

The study is directed to the use of non-metallic powders obtained from comminuted recycled paper-based printed circuit boards (PCBs) as an additive to polyvinyl chloride (PVC) substrate. The physical properties of the non-metallic PCB (NMPCB) powders were measured, and the morphological, mechanical and thermal properties of the NMPCB/PVC composite material were investigated. The results show that recycled NMPCB powders, when added below a threshold, tended to increase the tensile strength and bending strength of PVC. When 20 wt% NMPCB powders (relative to the substrate PVC) of an average diameter of 0.08 mm were added, the composite tensile strength and bending strength reached 22.6 MPa and 39.83 MPa, respectively, representing 107.2% and 123.1% improvement over pure PVC. The elongation at break of the composite material reached 151.94% of that of pure PVC, while the Vicat softening temperature of the composite material did not increase significantly compared to the pure PVC. The above results suggest that paper-based NMPCB powders, when used at appropriate amounts, can be effective for toughening PVC. Thus, this study suggests a new route for reusing paper-based NMPCB, which may have a significant beneficial environmental impact. Copyright © 2010 Elsevier Ltd. All rights reserved.

9. Photocopied 1983, from original drawing (DP27954), Picatinny Arsenal, March ...

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

9. Photocopied 1983, from original drawing (DP-27954), Picatinny Arsenal, March 18, 1940. BUILDING NO. 510, BUILDING NO. 511, 'BUILDINGS NO. 510 AND BUILDING NO. 511 OUTLINE OF COTTON CONVEY'G SYSTEM - NITRATING LINE.' - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

46. BUILDING NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, INTERIOR, ...

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

46. BUILDING NO. 519, ETHER AND ALCOHOL RECOVERY HOUSE, INTERIOR, CONTROL PANEL LEVEL (2ND DECK) OF ETHER AND ALCOHOL STILL BUILDING, LOOKING NORTH, SHOWING TWO ALCOHOL DISTILLATION TOWERS BEHIND 'MIXED SOLVENT UNIT' CONTROL PANEL. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Fabrication and luminescent properties of Al2O3:Cr3 + microspheres via a microwave solvothermal route followed by heat treatment

NASA Astrophysics Data System (ADS)

Zhu, Zhenfeng; Liu, Dianguang; Liu, Hui; Du, Juan; Yu, Hongguang; Deng, Jie

2012-06-01

AlOOH:Cr3 + powders were synthesized via a microwave solvothermal route at 433 K for 30 min and were used as the precursor and template for the preparation of γ-Al2O3:Cr3 + by thermal transformation at 773 K for 2 h in air. The obtained γ-Al2O3 based powders were microspheres with an average diameter about 1.9 μm. Photoluminescence (PL) spectra showed that the Al2O3:Cr3 + particles presented a symmetric broad R band at 696 nm without appreciable splitting when excited at 462 nm. It is shown that the 0.04 mol% of doping concentration of Cr3 + ions in γ-Al2O3:Cr3 + is optimum. According to Dexter's theory, the critical distance between Cr3 + ions for energy transfer was determined to be 47.54 Å. Based on the corresponding PL spectrum, full width at half maximum (FWHM) of Al2O3:Cr3 + (0.04 mol%) was calculated to be 3.35 nm.

New synthesis of nanopowders of proton conducting materials. A route to densified proton ceramics

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

Khani, Zohreh; Taillades-Jacquin, Melanie; Taillades, Gilles

2009-04-15

Low temperature routes have been developed for the preparation of BaCe{sub 0.9}Y{sub 0.1}O{sub 2.95} (BCY10) and BaZr{sub 0.9}Y{sub 0.1}O{sub 2.95} (BZY10) in the form of nanoparticulate powders for use after densification as ceramic membranes for a proton ceramic fuel cell. These methods make use on the one hand of the chelation of metal (II), (III) and (IV) ions by acrylates (hydrogelation route) and on the other of the destabilisation and precipitation of micro-emulsions. Both routes lead to single phase yttrium doped barium cerate or zirconate perovskites, as observed by X-ray diffraction, after thermal treatment at 900 deg. C for 4more » h for BCY10 and 800 deg. C for BZY10. These temperatures, lower than those usually used for preparation of barium cerate or zirconate, lead to oxide nanoparticles of size <40 nm. Dense ceramics (>=95%) are obtained by sintering BCY10 pellets at 1350 deg. C and BZY10 pellets at 1500 deg. C for 10 h. The water uptake of compacted samples at 500 deg. C is 0.14 wt% for BCY10 and 0.26 wt% for BZY10. Total conductivities in the range 300-600 deg. C were determined using impedance spectroscopy in a humidified nitrogen atmosphere. The total conductivity was 1.8x10{sup -2} S/cm for BCY10 and 2x10{sup -3} S/cm for BZY10 at 600 deg. C. The smallest perovskite nanoparticles and highest conductivities were obtained by hydrogelation of precursor barium, zirconium, cerium and yttrium acrylates. - Graphical Abstract: Low temperature hydrogelation and micro-emulsion routes have been developed for the preparation of rare earth doped barium and zirconium cerates in the form of nanoparticulate powders for use after densification as ceramic membranes for a proton ceramic fuel cell.« less

Studies of doped LaMnO3 samples prepared by citrate combustion process

NASA Astrophysics Data System (ADS)

Dimri, M. Chandra; Khanduri, H.; Mere, A.; Stern, R.

2018-04-01

La0.95A0.05MnO3 (where A=Na, Sr, Er, Dy and Ce) powder samples were synthesized by chemical solution route and the magnetic and structural properties are reported in this paper. The pervoskite structure was confirmed from X-ray diffraction patterns and Raman spectra at room temperature in all of these doped samples. Curie transition temperatures in doped LaMnO3 bulk samples were around 250K, which are much higher than the ideal value (˜140 K) in undoped samples. The increase in the magnetic transition temperatures can be related to non-stoichiometry and cation vacancies created due to higher valence substitutions for the univalent La1+ ions.

Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

DOEpatents

Balachandran, Uthamalingam

1996-01-01

A process for the preparation of amorphous precursor powders for Pb-doped Bi.sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains.

Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

DOEpatents

Balachandran, U.

1996-06-04

A process for the preparation of amorphous precursor powders for Pb-doped Bi{sub 2}Sr{sub 2} Ca{sub 2}Cu{sub 3}O{sub x} (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains. 11 figs.

Rapid Solid-State Metathesis Routes to Nanostructured Silicon-Germainum

NASA Technical Reports Server (NTRS)

Rodriguez, Marc (Inventor); Kaner, Richard B. (Inventor); Bux, Sabah K. (Inventor); Fleurial, Jean-Pierre (Inventor)

2014-01-01

Methods for producing nanostructured silicon and silicon-germanium via solid state metathesis (SSM). The method of forming nanostructured silicon comprises the steps of combining a stoichiometric mixture of silicon tetraiodide (SiI4) and an alkaline earth metal silicide into a homogeneous powder, and initating the reaction between the silicon tetraiodide (SiI4) with the alkaline earth metal silicide. The method of forming nanostructured silicon-germanium comprises the steps of combining a stoichiometric mixture of silicon tetraiodide (SiI4) and a germanium based precursor into a homogeneous powder, and initiating the reaction between the silicon tetraiodide (SiI4) with the germanium based precursors.

Lightweight Aluminum/Nano composites for Automotive Drive Train Applications

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

Chelluri, Bhanumathi; Knoth, Edward A.; Schumaker, Edward J.

2012-12-14

During Phase I, we successfully processed air atomized aluminum powders via Dynamic Magnetic Compaction (DMC) pressing and subsequent sintering to produce parts with properties similar to wrought aluminum. We have also showed for the first time that aluminum powders can be processed without lubes via press and sintering to 100 % density. This will preclude a delube cycle in sintering and promote environmentally friendly P/M processing. Processing aluminum powders via press and sintering with minimum shrinkage will enable net shape fabrication. Aluminum powders processed via a conventional powder metallurgy process produce too large a shrinkage. Because of this, sinter partsmore » have to be machined into specific net shape. This results in increased scrap and cost. Fully sintered aluminum alloy under this Phase I project has shown good particle-to-particle bonding and mechanical properties. We have also shown the feasibility of preparing nano composite powders and processing via pressing and sintering. This was accomplished by dispersing nano silicon carbide (SiC) powders into aluminum matrix comprising micron-sized powders (<100 microns) using a proprietary process. These composite powders of Al with nano SiC were processed using DMC press and sinter process to sinter density of 85-90%. The process optimization along with sintering needs to be carried out to produce full density composites.« less

Predictive Simulation of Process Windows for Powder Bed Fusion Additive Manufacturing: Influence of the Powder Bulk Density.

PubMed

Rausch, Alexander M; Küng, Vera E; Pobel, Christoph; Markl, Matthias; Körner, Carolin

2017-09-22

The resulting properties of parts fabricated by powder bed fusion additive manufacturing processes are determined by their porosity, local composition, and microstructure. The objective of this work is to examine the influence of the stochastic powder bed on the process window for dense parts by means of numerical simulation. The investigations demonstrate the unique capability of simulating macroscopic domains in the range of millimeters with a mesoscopic approach, which resolves the powder bed and the hydrodynamics of the melt pool. A simulated process window reveals the influence of the stochastic powder layer. The numerical results are verified with an experimental process window for selective electron beam-melted Ti-6Al-4V. Furthermore, the influence of the powder bulk density is investigated numerically. The simulations predict an increase in porosity and surface roughness for samples produced with lower powder bulk densities. Due to its higher probability for unfavorable powder arrangements, the process stability is also decreased. This shrinks the actual parameter range in a process window for producing dense parts.

Predictive Simulation of Process Windows for Powder Bed Fusion Additive Manufacturing: Influence of the Powder Bulk Density

PubMed Central

Rausch, Alexander M.; Küng, Vera E.; Pobel, Christoph; Körner, Carolin

2017-01-01

The resulting properties of parts fabricated by powder bed fusion additive manufacturing processes are determined by their porosity, local composition, and microstructure. The objective of this work is to examine the influence of the stochastic powder bed on the process window for dense parts by means of numerical simulation. The investigations demonstrate the unique capability of simulating macroscopic domains in the range of millimeters with a mesoscopic approach, which resolves the powder bed and the hydrodynamics of the melt pool. A simulated process window reveals the influence of the stochastic powder layer. The numerical results are verified with an experimental process window for selective electron beam-melted Ti-6Al-4V. Furthermore, the influence of the powder bulk density is investigated numerically. The simulations predict an increase in porosity and surface roughness for samples produced with lower powder bulk densities. Due to its higher probability for unfavorable powder arrangements, the process stability is also decreased. This shrinks the actual parameter range in a process window for producing dense parts. PMID:28937633

Soapnut extract mediated synthesis of nanoscale cobalt substituted NdFeB ferromagnetic materials and their characterization

NASA Astrophysics Data System (ADS)

Rao, G. V. S. Jayapala; Prasad, T. N. V. K. V.; Shameer, Syed; Rao, M. Purnachandra

2018-04-01

Neodymium iron boron (NdFeB) permanent magnets have high energy product with suitable magnetic and physical properties for an array of applications including power generation and motors. However, synthetic routes of NdFeB permanent magnets involve critical procedures with high energy and needs scientific skills. Herein, we report on soapnut extract mediated synthesis of nanoscale cobalt substituted NdFeB (Co-NdFeB) permanent magnetic powders (Nd: 15%, Fe: 77.5%, B: 7.5% and Co with molar ratios: 0.5, 1, 1.5 and 2). A 10 ml of 10% soapnut extract was added to 90 ml of respective chemical composition and heated to 60 °C for 30 min and aged for 24 h. The dried powder was sintered at 500 °C for 1 h. The characterization of the prepared nanoscale Co-NdFeB magnetic powders was done using the techniques such as Dynamic Light Scattering (DLS for size and zeta potential measurements), X-ray diffraction (XRD) for structural determination, Scanning electron microscopy (SEM) with energy dispersion spectroscopy (EDS) for surface morphological and elemental analysis, Fourier transform infrared spectroscopy (FT-IR) for the identification of functional groups associated and hysteresis loop studies to quantify the magnetization. The results revealed that particles were in irregular and tubular shaped and highly stable (Zeta potential: -44.4 mV) with measured size <100 nm. XRD micrographs revealed a tetragonal crystal structure and FTIR showed predominant N-H and O-H stretching indicates the involvement of these functional groups in the reduction and stabilization process of Co-NdFeB magnetic powders. Hysteresis studies signify the effect of an increase in Co concentration.

The Effect of Milling Time on the Microstructural Characteristics and Strengthening Mechanisms of NiMo-SiC Alloys Prepared via Powder Metallurgy.

PubMed

Yang, Chao; Muránsky, Ondrej; Zhu, Hanliang; Thorogood, Gordon J; Avdeev, Maxim; Huang, Hefei; Zhou, Xingtai

2017-04-06

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5-2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni₃Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo₂C particles during sintering. The amount of grain boundaries greatly increases the Hall-Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process.

Impregnation quality of shredded semipreg after compression moulding

NASA Astrophysics Data System (ADS)

Vincent, G.; Balakrishnan, V.; de Bruijn, T. A.; Wijskamp, S.; Abdul Rasheed, M. I.

2017-10-01

Manufacturing of thermoplastic composites (TPC) inherently generates scrap, mainly in the form of offcuts or rejected parts. The growth of TPC over recent decades has now reached a point where developing specific recycling solutions for TPC waste has become crucial. While looking at the various steps during which scrap is produced, the nesting of semipreg or prepreg appears to be critical. This work aims to develop a route for recycling semipreg offcuts, comprising shredding and compression moulding. This article focuses on an experimental study of the compression moulding step of carbon fibres reinforced PPS (C/PPS) to investigate the uniformity and impregnation quality of plates. These plates were realised in a picture frame while varying both the fibre volume content between 30% and 50% and the processing parameters. Visual inspection and cross-sectional microscopy were performed to assess the quality of each plate. As a first step, the influence of the type of added matrix (film, powder, pellets) and the type of pre-impregnation (film, powder) was studied. Stacking of polymer powder with shredded powder-coated semipreg gave the best impregnation quality. It was also shown that longer dwell time at melt leads to better consolidation quality. However, the difficulty in obtaining good impregnation comes from the disentangled shredded material, which is composed of three forms: semipreg flakes, dry bundles and pieces of matrix. When dry bundles reach the mould surfaces during the filling of the mould or when they are packed together, the consolidation cycle hardly impregnates them and they remain dry afterwards. Furthermore, large local variations of fibre fraction were noticed, resulting from a random mould filling. Therefore, the recycling solution for shredded semipreg is feasible when the fibre fraction is reduced but improvements on the part variability still have to be made.

The Effect of Milling Time on the Microstructural Characteristics and Strengthening Mechanisms of NiMo-SiC Alloys Prepared via Powder Metallurgy

PubMed Central

Yang, Chao; Muránsky, Ondrej; Zhu, Hanliang; Thorogood, Gordon J.; Avdeev, Maxim; Huang, Hefei; Zhou, Xingtai

2017-01-01

A new generation of alloys, which rely on a combination of various strengthening mechanisms, has been developed for application in molten salt nuclear reactors. In the current study, a battery of dispersion and precipitation-strengthened (DPS) NiMo-based alloys containing varying amounts of SiC (0.5–2.5 wt %) were prepared from Ni-Mo-SiC powder mixture via a mechanical alloying (MA) route followed by spark plasma sintering (SPS) and rapid cooling. Neutron Powder Diffraction (NPD), Electron Back Scattering Diffraction (EBSD), and Transmission Electron Microscopy (TEM) were employed in the characterization of the microstructural properties of these in-house prepared NiMo-SiC DPS alloys. The study showed that uniformly-dispersed SiC particles provide dispersion strengthening, the precipitation of nano-scale Ni3Si particles provides precipitation strengthening, and the solid-solution of Mo in the Ni matrix provides solid-solution strengthening. It was further shown that the milling time has significant effects on the microstructural characteristics of these alloys. Increased milling time seems to limit the grain growth of the NiMo matrix by producing well-dispersed Mo2C particles during sintering. The amount of grain boundaries greatly increases the Hall–Petch strengthening, resulting in significantly higher strength in the case of 48-h-milled NiMo-SiC DPS alloys compared with the 8-h-milled alloys. However, it was also shown that the total elongation is considerably reduced in the 48-h-milled NiMo-SiC DPS alloy due to high porosity. The porosity is a result of cold welding of the powder mixture during the extended milling process. PMID:28772747

On the thermodynamic path enabling a room-temperature, laser-assisted graphite to nanodiamond transformation

NASA Astrophysics Data System (ADS)

Gorrini, F.; Cazzanelli, M.; Bazzanella, N.; Edla, R.; Gemmi, M.; Cappello, V.; David, J.; Dorigoni, C.; Bifone, A.; Miotello, A.

2016-10-01

Nanodiamonds are the subject of active research for their potential applications in nano-magnetometry, quantum optics, bioimaging and water cleaning processes. Here, we present a novel thermodynamic model that describes a graphite-liquid-diamond route for the synthesis of nanodiamonds. Its robustness is proved via the production of nanodiamonds powders at room-temperature and standard atmospheric pressure by pulsed laser ablation of pyrolytic graphite in water. The aqueous environment provides a confinement mechanism that promotes diamond nucleation and growth, and a biologically compatible medium for suspension of nanodiamonds. Moreover, we introduce a facile physico-chemical method that does not require harsh chemical or temperature conditions to remove the graphitic byproducts of the laser ablation process. A full characterization of the nanodiamonds by electron and Raman spectroscopies is reported. Our model is also corroborated by comparison with experimental data from the literature.

On Intelligent Design and Planning Method of Process Route Based on Gun Breech Machining Process

NASA Astrophysics Data System (ADS)

Hongzhi, Zhao; Jian, Zhang

2018-03-01

The paper states an approach of intelligent design and planning of process route based on gun breech machining process, against several problems, such as complex machining process of gun breech, tedious route design and long period of its traditional unmanageable process route. Based on gun breech machining process, intelligent design and planning system of process route are developed by virtue of DEST and VC++. The system includes two functional modules--process route intelligent design and its planning. The process route intelligent design module, through the analysis of gun breech machining process, summarizes breech process knowledge so as to complete the design of knowledge base and inference engine. And then gun breech process route intelligently output. On the basis of intelligent route design module, the final process route is made, edited and managed in the process route planning module.

Continuum simulation of heat transfer and solidification behavior of AlSi10Mg in Direct Metal Laser Sintering Process

NASA Astrophysics Data System (ADS)

Ojha, Akash; Samantaray, Mihir; Nath Thatoi, Dhirendra; Sahoo, Seshadev

2018-03-01

Direct Metal Laser Sintering (DMLS) process is a laser based additive manufacturing process, which built complex structures from powder materials. Using high intensity laser beam, the process melts and fuse the powder particles makes dense structures. In this process, the laser beam in terms of heat flux strikes the powder bed and instantaneously melts and joins the powder particles. The partial solidification and temperature distribution on the powder bed endows a high cooling rate and rapid solidification which affects the microstructure of the build part. During the interaction of the laser beam with the powder bed, multiple modes of heat transfer takes place in this process, that make the process very complex. In the present research, a comprehensive heat transfer and solidification model of AlSi10Mg in direct metal laser sintering process has been developed on ANSYS 17.1.0 platform. The model helps to understand the flow phenomena, temperature distribution and densification mechanism on the powder bed. The numerical model takes into account the flow, heat transfer and solidification phenomena. Simulations were carried out for sintering of AlSi10Mg powders in the powder bed having dimension 3 mm × 1 mm × 0.08 mm. The solidification phenomena are incorporated by using enthalpy-porosity approach. The simulation results give the fundamental understanding of the densification of powder particles in DMLS process.

Iron's Role in Aluminum: A Powder Metallurgy and Sustainability Approach

NASA Astrophysics Data System (ADS)

Saller, Brandon Dale

The family of Al-Fe alloys is both scientifically and technologically interesting for several reasons. First, the low equilibrium solid solubility (0.03 at.%) and diffusivity of Fe in Al suggest that the alloys containing these two elements should be thermally stable. Many studies have tried to extend this low solubility value via non-equilibrium processing routes. Second, published results suggest that there is a range of intermetallic phases, including the metastable orthorhombic Al6Fe and the equilibrium monoclinic Al13Fe4, for example, the formation of which depends on solidification and subsequent processing conditions. Third, from a sustainability standpoint, both Al and Fe are present in bauxite (aluminum ore), however up to 40 wt.% Fe-oxide present in bauxite is discarded as a waste product, creating red mud pits. In order to understand the multiple facets and implications of iron's role in aluminum, a systematic investigation was performed into the precipitates that form as a function of thermal exposure and their subsequent effect on the tensile behavior of the alloy. In this study, Al-2at.% Fe and Al-5at.% Fe powders were synthesized via helium gas atomization and argon gas atomization, respectively. Cooling rates upwards of 106 K/s were achieved resulting in an intermetallic-free starting structure. Powders were subsequently severely plastically deformed via either cryomilling or high-pressure torsion to obtain nanostructured/ultrafine-grained powder or a consolidated specimen, respectively. Characterization via electron microscopy established a map of the powder microstructure as a function of atomization cooling rate. In addition, electron backscatter diffraction revealed a large number of low-angle grain boundaries, which influenced nucleation and precipitation of the metastable Al6Fe phase. X-ray diffraction and atom probe tomography results provide the most comprehensive evidence to date of forcing of 2at.% Fe into solution with the Al matrix via cryomilling. With respect to the powder, a differential scanning calorimetry and activation energy analysis elucidated the formation and phase transformation temperatures of the relevant intermetallic phases, and the microstructural factors that influenced them. With an understanding of the fundamental science behind the intermetallic formation in the Al-Fe system, the composition of helium atomized Al-2at.% Fe was chosen combined with high-pressure torsion processing to yield a bulk alloy that demonstrated an ultimate tensile strength of 488 MPa. This strength was achieved via a combination of two mechanisms: grain refinement (Hall-Petch) and dislocation-Al6Fe interactions (Orowan strengthening), with notable thermal stability present up until 450°C. Finally, the potential for Al-Fe as a sustainable alloy was studied and a link established between current environmental literature and metallurgy literature on the potential for incorporation of Fe into Al to create a structural alloy.

Chemical route for formation of intermetallic Zn 4Sb 3 phase

NASA Astrophysics Data System (ADS)

Denoix, A.; Solaiappan, A.; Ayral, R. M.; Rouessac, F.; Tedenac, J. C.

2010-05-01

Synthesis of intermetallic zinc antimonide phases via low temperature solution route was investigated. Trial experiments were carried out under inert atmosphere at 70 °C using metallic Zn, SbCl 3 and NaBH 4 as reactants and tetrahydrofuran (THF), dimethylsulfoxide (DMSO) as organic media. Powder X-ray analysis confirmed the nucleation and growth of ZnSb phases in presence of excess Zn. SEM analysis revealed the existence of core-shell structure comprising of Zn core and Sb shell. Such particles get transformed into Zn 4Sb 3 crystalline phases upon thermal treatment at 300 °C/6 h in a silica tube closed under high secondary vacuum.

Particle size, size distribution and morphological evaluation of glass fiber reinforced plastic (GRP) industrial by-product.

PubMed

Mazzoli, Alida; Moriconi, Giacomo

2014-12-01

The waste management of glass fiber reinforced polymer (GRP) materials, in particular those made with thermosetting resins, is a critical issue for the composites industry because these materials cannot be reprocessed. Therefore, most thermosetting GRP waste is presently sent to landfill, in spite of the significant environmental impact caused by their disposal in this way. The limited GRP waste recycling worldwide is mostly due to its intrinsic thermosetting properties, lack of characterization data and unavailability of viable recycling and recovery routes. One of the possibility for re-using GRP industrial by-product is in form of powder as a partial aggregate replacement or filler addition in cement based composites for applications in sustainable construction materials and technologies. However, the feasibility of this kind of reutilization strongly depends on the morphology and particle size distribution of a powder made up of polymer granules and glass fibers. In the present study, the use of image analysis method, based on scanning electron microscopy (SEM) and ImageJ processing program, is proposed in order to evaluate the morphology of the particles and measure the particle size and size distribution of fine GRP waste powder. The obtained results show a great potential of such a method in order to be considered as a standardized method of measurement and analysis in order to characterize the grain size and size distribution of GRP particles before exploiting any compatibility issue for its recycling management. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

Stulikova, Ivana, E-mail: ivana.stulikova@mff.cuni.cz; Smola, Bohumil; Vlach, Martin

Solution treated MgTb3Nd2 alloy (nominal composition in wt.%) (ST) and the alloy prepared by hot extrusion of isostatically pressed powder (PM) were isochronally heat treated and studied by electrical resistivity and hardness measurements and by differential scanning calorimetry. Microstructure development was investigated in transmission electron microscopy. Successive precipitation of transient phases in the sequence β″ (D0{sub 19} plates) → β′(cbco) → β{sub 1} (Mg{sub 3}Gd type, fcc) → β (Mg{sub 5}Gd type, fcc) known from the ST alloy was identified also in the PM alloy. The early precipitation stage (D0{sub 19} clusters) revealed in the ST alloy as well asmore » precipitation of equilibrium β{sub e} phase Mg{sub 41}(Tb,Nd){sub 5} manifest themselves only slightly in the PM alloy. Powder metallurgy route does not change the values of activation energies but shifts the temperature ranges of these processes. Vickers hardness of the as prepared state is higher in the PM alloy and is very resistant against the heat treatment up to 510 °C. Contrary to the ST alloy precipitation due to isochronal annealing does not lead to pronounced hardness changes in the PM alloy. - Highlights: • Powder metallurgy (PM) does not change precipitation sequence in MgTbNd alloy. • Temperature ranges of transient phase precipitations are shifted in PM alloy. • Hardness is resistant against isochronal heat treatment up to 510 °C in the PM alloy. • PM procedure does not change activation energies of precipitation.« less

Structural Ceramic Nanocomposites: A Review of Properties and Powders’ Synthesis Methods

PubMed Central

Palmero, Paola

2015-01-01

Ceramic nanocomposites are attracting growing interest, thanks to new processing methods enabling these materials to go from the research laboratory scale to the commercial level. Today, many different types of nanocomposite structures are proposed in the literature; however, to fully exploit their exceptional properties, a deep understanding of the materials’ behavior across length scales is necessary. In fact, knowing how the nanoscale structure influences the bulk properties enables the design of increasingly performing composite materials. A further key point is the ability of tailoring the desired nanostructured features in the sintered composites, a challenging issue requiring a careful control of all stages of manufacturing, from powder synthesis to sintering. This review is divided into four parts. In the first, classification and general issues of nanostructured ceramics are reported. The second provides basic structure–property relations, highlighting the grain-size dependence of the materials properties. The third describes the role of nanocrystalline second-phases on the mechanical properties of ordinary grain sized ceramics. Finally, the fourth part revises the mainly used synthesis routes to produce nanocomposite ceramic powders, underlining when possible the critical role of the synthesis method on the control of microstructure and properties of the sintered ceramics. PMID:28347029

The synergistic effects of combining the high energy mechanical milling and wet milling on Si negative electrode materials for lithium ion battery

NASA Astrophysics Data System (ADS)

Hou, Shang-Chieh; Su, Yuh-Fan; Chang, Chia-Chin; Hu, Chih-Wei; Chen, Tsan-Yao; Yang, Shun-Min; Huang, Jow-Lay

2017-05-01

The submicro-sized and nanostructured Si aggregated powder is prepared by combinational routes of high energy mechanical milling (HEMM) and wet milling. Milled Si powder is investigated by particle size analyzer, SEM, TEM, XPS and XRD as well as the control ones. Its electrode is also investigated by in situ XRD and electrochemical performance. Morphology reveals that combining the high energy mechanical milling and wet milling not only fracture primary Si particles but also form submicro-sized Si aggregates constructed by amorphous and nanocrystalline phases. Moreover, XPS shows that wet milling in ethanol trigger Sisbnd Osbnd CH2CH3 bonding on Si surface might enhance the SEI formation. In situ XRD analysis shows negative electrode made of submicro-sized Si aggregated powder can effectively suppress formation of crystalline Li15Si4 during lithiation and delithiation due to amorphous and nanocrystalline construction. Thus, the submicro-sized Si powder with synergistic effects combining the high energy mechanical milling and wet milling in ethanol as negative electrode performs better capacity retention.

High surface area nanocrystalline hausmannite synthesized by a solvent-free route

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

Herrera-Miranda, Daniel; Ponrouch, Alexandre; Pons, Josefina

Highlights: ► High surface area Mn{sub 3}O{sub 4} nanoparticles obtained by a solvent-free low temperature route. ► 3,6,9-Trioxadecanoic acid allows to obtain nanocrystalline hausmannite. ► Tape casted electrodes show up to 300 mAh g{sup −1} capacity after more than 40 cycles at a C/3 rate. ► Upper cut off voltage strongly influences capacity retention upon cycling at high C rates. -- Abstract: Nanocrystalline high surface area Mn{sub 3}O{sub 4} powder was obtained at low temperature by a solvent-free route. The precursor was a mixture of manganese (II) acetate, 3,6,9-trioxadecanoic acid (TODA) and ammonium acetate that were intimately mixed by groundingmore » in an agate mortar. Nanocrystalline Mn{sub 3}O{sub 4} was obtained by thermal treatment at 120 °C. Powder X-ray diffraction, selected area electron diffraction, high resolution transmission electron microscopy, and Fourier transformed infrared characterization confirmed the formation of the hausmannite phase. The as-prepared mesoporous material has high specific surface area (120 m{sup 2} g{sup −1}). The performances of tape casted Mn{sub 3}O{sub 4} nanopowder electrodes were investigated as anode material for lithium ion batteries. High capacity values were achieved at diverse C rates. Capacity fading was found to be dependent on the upper cut off voltage, the presence of a plateau at 2.25 V vs. Li{sup +}/Li being detrimental for long term cyclability.« less

A pilot study using a novel pyrotechnically driven prototype applicator for epidermal powder immunization in piglets.

PubMed

Engert, Julia; Anamur, Cihad; Engelke, Laura; Fellner, Christian; Lell, Peter; Henke, Stefan; Stadler, Julia; Zöls, Susanne; Ritzmann, Mathias; Winter, Gerhard

2018-04-20

Epidermal powder immunization (EPI) is an alternative technique to the classical immunization route using needle and syringe. In this work, we present the results of an in vivo pilot study in piglets using a dried influenza model vaccine which was applied by EPI using a novel pyrotechnically driven applicator. A liquid influenza vaccine (Pandemrix ® ) was first concentrated by tangential flow filtration and hemagglutinin content was determined by RP-HPLC. The liquid formulation was then transformed into a dry powder by collapse freeze-drying and subsequent cryo-milling. The vaccine powder was attached to a membrane of a novel pyrotechnical applicator using oily adjuvant components. Upon actuation of the applicator, particles were accelerated to high speed as determined by a high-speed camera setup. Piglets were immunized twice using either the novel pyrotechnical applicator or classical intramuscular injection. Blood samples of the animals were collected at various time points and analyzed by enzyme-linked immunosorbent assay. Our pilot study shows that acceleration of a dried vaccine powder to supersonic speed using the pyrotechnical applicator is possible and that the speed and impact of the particles is sufficient to breach the stratum corneum of piglet skin. Importantly, the administration of the dry vaccine powder resulted in measurable anti-H1N1 antibody titres in vivo. Copyright © 2018 Elsevier B.V. All rights reserved.

Thermal decomposition behavior of nano/micro bimodal feedstock with different solids loading

NASA Astrophysics Data System (ADS)

Oh, Joo Won; Lee, Won Sik; Park, Seong Jin

2018-01-01

Debinding is one of the most critical processes for powder injection molding. The parts in debinding process are vulnerable to defect formation, and long processing time of debinding decreases production rate of whole process. In order to determine the optimal condition for debinding process, decomposition behavior of feedstock should be understood. Since nano powder affects the decomposition behavior of feedstock, nano powder effect needs to be investigated for nano/micro bimodal feedstock. In this research, nano powder effect on decomposition behavior of nano/micro bimodal feedstock has been studied. Bimodal powders were fabricated with different ratios of nano powder, and the critical solids loading of each powder was measured by torque rheometer. Three different feedstocks were fabricated for each powder depending on solids loading condition. Thermogravimetric analysis (TGA) experiment was carried out to analyze the thermal decomposition behavior of the feedstocks, and decomposition activation energy was calculated. The result indicated nano powder showed limited effect on feedstocks in lower solids loading condition than optimal range. Whereas, it highly influenced the decomposition behavior in optimal solids loading condition by causing polymer chain scission with high viscosity.

Synthesis and electrochemical property of few-layer molybdenum disulfide nanosheets

NASA Astrophysics Data System (ADS)

Fu, Yanjue; Wang, Chunrui; Wang, Linlin; Peng, Xia; Wu, Binhe; Sun, Xingqu; Chen, Xiaoshuang

2016-12-01

Large-scale few-layer MoS2 nanosheets have been fabricated via a simple hydrothermal route using molybdenum powder as precursors. The as-prepared MoS2 samples were characterized by X-ray powder diffraction (XRD) analysis, transmission electron microscopy (TEM), and Raman and photoluminescence (PL) spectral analyses at room temperature. The results confirm that the as-prepared MoS2 displays a sheet-like morphology with a thickness of few (bi- to tri-) layers. Electrochemical measurements showed that the as-prepared few-layer MoS2 exhibited the highest reversible capacity of 1127 mAh g-1 and a stable reversible capacity of 1057 mAh g-1 after 30 cycles.

Shock-induced reaction synthesis of cubic boron nitride

NASA Astrophysics Data System (ADS)

Beason, M. T.; Pauls, J. M.; Gunduz, I. E.; Rouvimov, S.; Manukyan, K. V.; Matouš, K.; Son, S. F.; Mukasyan, A.

2018-04-01

Here, we report ultra-fast (0.1-5 μs) shock-induced reactions in the 3B-TiN system, leading to the direct synthesis of cubic boron nitride, which is extremely rare in nature and is the second hardest material known. Composite powders were produced through high-energy ball milling to provide intimate mixing and subsequently shocked using an explosive charge. High-resolution transmission electron microscopy and X-ray diffraction confirm the formation of nanocrystalline grains of c-BN produced during the metathetical reaction between boron and titanium nitride. Our results illustrate the possibility of rapid reactions enabled by high-energy ball milling possibly occurring in the solid state on incredibly short timescales. This process may provide a route for the discovery and fabrication of advanced compounds.

Atmospheric pressure chemical vapor deposition: an alternative route to large-scale MoS2 and WS2 inorganic fullerene-like nanostructures and nanoflowers.

PubMed

Li, Xiao-Lin; Ge, Jian-Ping; Li, Ya-Dong

2004-11-19

Large-scale MoS2 and WS2 inorganic fullerene-like (IF) nanostructures (onionlike nanoparticles, nanotubes) and elegant three-dimensional nanoflowers (NF) have been selectively prepared through an atmospheric pressure chemical vapor deposition (APCVD) process with the reaction of chlorides and sulfur. The morphologies were controlled by adjusting the deposition position, the deposition temperature, and the flux of the carrier gas. All of the nanostructures have been characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). A reaction mechanism is proposed based on the experimental results. The surface area of MoS2 IF nanoparticles and the field-emission effect of as-prepared WS2 nanoflowers is reported.

Ni Based Powder Reconditioning and Reuse for LMD Process

NASA Astrophysics Data System (ADS)

Renderos, M.; Girot, F.; Lamikiz, A.; Torregaray, A.; Saintier, N.

LMD is an additive manufacturing process based on the injection of metallic powder into a melt-pool created by a heat laser source on a substrate. One of the benefits of this technology is the reduction of the wasted material since it is a near-shape process. Moreover one of the main drawbacks is the relatively low efficiency of the trapped powder, which can be loss than 5% in some cases. The non-trapped powder represents a significant cost in the LMD process, since powder metal material is very expensive and usually is not reused. This article proposes a methodology of the reconditioning and posterior reuse of a nickel base powder commonly used in the aerospace industry, with the main objectives of cost saving, higher environmental cleanup and increase of the overall efficiency in the LMD process. The results are checked by the development of a prototype part built up from reused powder.

Escaping the Tyranny of Carbothermal Reduction: Fumed Silica from Sustainable, Green Sources without First Having to Make SiCl4.

PubMed

Yi, Eongyu; Hyde, Clare E; Sun, Kai; Laine, Richard M

2016-02-12

Fumed silica is produced in 1000 tons per year quantities by combusting SiCl4 in H2 /O2 flames. Given that both SiCl4 and combustion byproduct HCl are corrosive, toxic and polluting, this route to fumed silica requires extensive safeguards that may be obviated if an alternate route were found. Silica, including rice hull ash (RHA) can be directly depolymerized using hindered diols to generate distillable spirocyclic alkoxysilanes or Si(OEt)4 . We report here the use of liquid-feed flame spray pyrolysis (LF-FSP) to combust the aforementioned precursors to produce fumed silica very similar to SiCl4 -derived products. The resulting powders are amorphous, necked, <50 nm average particle sizes, with specific surface areas (SSAs) of 140-230 m(2)  g(-1) . The LF-FSP approach does not require the containment constraints of the SiCl4 process and given that the RHA silica source is produced in million ton per year quantities worldwide, the reported approach represents a sustainable, green and potentially lower-cost alternative. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

From the iron boring scraps to superparamagnetic nanoparticles through an aerobic biological route.

PubMed

Daneshvar, Majid; Hosseini, Mohammad Raouf

2018-06-15

A straightforward, highly efficient, and low-cost biological route was introduced for the synthesis of magnetic nanoparticles. Three urease-positive bacteria namely, Bacillus subtilis, B. pasteurii, and B. licheniformis were used to biosynthesize ammonia and biosurfactants required for the nanoparticle production. Also, the features of the applied biological approach was compared with a chemical co-precipitation method. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), dynamic light scattering (DLS), vibrating-sample magnetometer (VSM), and Fourier transform infrared spectroscopy (FTIR) were applied to characterize the synthesized nanoparticles. Results indicated that the biologically fabricated powders had a single domain structure, and their mean particle size was in the range of 37 to 97 nm. The production capacity of the biological processes was double the chemical method, and the biosynthesized superparamagnetic nanoparticles had higher saturation magnetization up to 132 emu/g. Finally, the removal of Cr(VI) from a synthetic solution was investigated using the four products. The maximum elimination of chromium (over 99%) was achieved by the particles synthesized by B. pasteurii, with the adsorption capacity of 190 mg/g. Copyright © 2018 Elsevier B.V. All rights reserved.

Pulse Check: Trends in Drug Abuse January-June 2002 Reporting Period. Special Topic: A Look at Local Drug Markets.

ERIC Educational Resources Information Center

Meth, Marcia; Chalmers, Rebecca

The report aims to describe chronic drug users, emerging drugs, new routes of administration, varying use patterns, changing demand for treatment, drug-related criminal activity, drug markets, and shifts in supply and distribution patterns. Pulse Check regularly addresses four drugs of serious concern: heroin, crack cocaine/powder cocaine,…

78. BUILDINGS NO. 537, GENERAL STORAGE (DRY HOUSE), NO. 538, ...

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

78. BUILDINGS NO. 537, GENERAL STORAGE (DRY HOUSE), NO. 538, GENERAL STORAGE (GRAPHITING & SORTING HOUSE), LOOKING SOUTHEAST AT NORTHWEST AND SOUTHWEST SIDES. BUILDING NO. 537 WAS ONCE USED AS A DRY HOUSE, AND BUILDING NO. 538 AS A GLAZING (GRAPHITING) AND SORTING HOUSE. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

7. Photocopied 1983, from original drawing (DP14260), Picatinny Arsenal, August ...

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

7. Photocopied 1983, from original drawing (DP-14260), Picatinny Arsenal, August 14, 1931. BUILDING NO. 511, 'NITRATING HOUSE - BUILDING 511 ALTERATIONS AND ADDITIONS TO EQUIPMENT - PLANS'. THIS DRAWING ALSO CONTAINS A SMALL SKETCH MAP SHOWING BUILDING NO.S 508 to 514. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Microwave mediated synthesis of ZnS spherical nanoparticles for IR optical ceramics

NASA Astrophysics Data System (ADS)

Ravichandran, D.; Wharton, T.; Devan, B.; Korenstein, R.; Tustison, R.; Komarneni, S.

2011-06-01

The existing material choice for long-wave infrared (LWIR) and semi-active laser domes is multispectral zinc sulfide (ZnS), made by chemical vapor deposition. An alternative route to make more erosion-resistant ZnS could be through hot pressing ZnS nanoparticles into small-grain material. We have attempted to produce ZnS nanoparticles both by microwave and microwave-hydrothermal methods. Microwave route produced ultrahigh purity, homogeneous, well dispersed, and uniformly spherical ZnS nanoparticles. Microwave-hydrothermal route produced equiaxed cubic-faceted nanoparticles. The powder X-ray diffraction patterns of ZnS shows the presence of broad reflections corresponding to the (1 1 1), (2 2 0), and (3 1 1) planes of the cubic crystalline ZnS material. The domain size of the particles estimated from the Debye-Scherrer formula for the main reflection (111) gives a value of 2.9 and 2.5 for the microwave and microwave-hydrothermal methods respectively.

A polyethylene glycol-assisted route to synthesize Pb(Ni 1/3Nb 2/3)O 3-PbTiO 3with improved electric properties

NASA Astrophysics Data System (ADS)

Ye, Yin; Yu, Shuhui; Huang, Haitao; Zhou, Limin

2007-07-01

Polyethylene glycol (PEG)-assisted solid state reaction route is employed to prepare the relaxor-type ferroelectric powders and ceramics of (1-x)Pb(Ni 1/3Nb 2/3)O 3-xPbTiO 3 (PNN-PT) with the morphotropic phase boundary (MPB) composition at x=0.36 (0.64PNN-0.36PT). PEG additive with the molecular weight of 200 is introduced into PNN-PT oxide precursors in order to obtain the perovskite phase. The XRD and TG/DSC results demonstrate that the interactions between PbO and PEG favor the transformation from the lead-rich pyrochlore to the lead-deficient pyrochlore, thus facilitating the formation of the perovskite. Consequently, nearly pure perovskite 0.64PNN-0.36PT powders are synthesized at a relatively low temperature of 850 °C. A significant improvement of electric properties of the ceramics sintered at 1200 °C is achieved by PEG modification. The dielectric constant at room temperature and the maximum dielectric constant at T c reach 4987 and 24307, respectively, at a frequency of 1 kHz. The piezoelectric constant d 33 is 460 pC/N.

Consumer acceptance and aroma characterization of navy bean (Phaseolus vulgaris) powders prepared by extrusion and conventional processing methods.

PubMed

Szczygiel, Edward J; Harte, Janice B; Strasburg, Gale M; Cho, Sungeun

2017-09-01

Food products produced with bean ingredients are gaining in popularity among consumers due to the reported health benefits. Navy bean (Phaseolus vulgaris) powder produced through extrusion can be considered as a resource-efficient alternative to conventional methods, which often involve high water inputs. Therefore, navy bean powders produced with extrusion and conventional methods were assessed for the impact of processing on consumer liking in end-use products and odor-active compounds. Consumer acceptance results reveal significant differences in flavor, texture and overall acceptance scores of several products produced with navy bean powder. Crackers produced with extruded navy bean powder received higher hedonic flavor ratings than those produced with commercial navy bean powder (P < 0.001). GC-O data showed that the commercial powder produced through conventional processing had much greater contents of several aliphatic aldehydes commonly formed via lipid oxidation, such as hexanal, octanal and nonanal with descriptors of 'grassy', 'nutty', 'fruity', 'dusty', and 'cleaner', compared to the extruded powder. Extrusion processed navy bean powders were preferred over commercial powders for certain navy bean powder applications. This is best explained by substantial differences in aroma profiles of the two powders that may have been caused by lipid oxidation. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

High-performance perovskite CH3NH3PbI3 thin films for solar cells prepared by single-source physical vapour deposition

PubMed Central

Fan, Ping; Gu, Di; Liang, Guang-Xing; Luo, Jing-Ting; Chen, Ju-Long; Zheng, Zhuang-Hao; Zhang, Dong-Ping

2016-01-01

In this work, an alternative route to fabricating high-quality CH3NH3PbI3 thin films is proposed. Single-source physical vapour deposition (SSPVD) without a post-heat-treating process was used to prepare CH3NH3PbI3 thin films at room temperature. This new process enabled complete surface coverage and moisture stability in a non-vacuum solution. Moreover, the challenges of simultaneously controlling evaporation processes of the organic and inorganic sources via dual-source vapour evaporation and the heating process required to obtain high crystallization were avoided. Excellent composition with stoichiometry transferred from the powder material, a high level of tetragonal phase-purity, full surface coverage, well-defined grain structure, high crystallization and reproducibility were obtained. A PCE of approximately 10.90% was obtained with a device based on SSPVD CH3NH3PbI3. These initial results suggest that SSPVD is a promising method to significantly optimize perovskite CH3NH3PbI3 solar cell efficiency. PMID:27426686

Improved silicon carbide for advanced heat engines

NASA Technical Reports Server (NTRS)

Whalen, Thomas J.; Mangels, J. A.

1986-01-01

The development of silicon carbide materials of high strength was initiated and components of complex shape and high reliability were formed. The approach was to adapt a beta-SiC powder and binder system to the injection molding process and to develop procedures and process parameters capable of providing a sintered silicon carbide material with improved properties. The initial effort was to characterize the baseline precursor materials, develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures were performed in order to distinguish process routes for improving material properties. A total of 276 modulus-of-rupture (MOR) bars of the baseline material was molded, and 122 bars were fully processed to a sinter density of approximately 95 percent. Fluid mixing techniques were developed which significantly reduced flaw size and improved the strength of the material. Initial MOR tests indicated that strength of the fluid-mixed material exceeds the baseline property by more than 33 percent. the baseline property by more than 33 percent.

Evaluation of lead recovery efficiency from waste CRT funnel glass by chlorinating volatilization process.

PubMed

Erzat, Aris; Zhang, Fu-Shen

2014-01-01

The current study was carried out to develop a novel process, namely chloride volatilization procedure for lead recovery from waste cathode ray tube (CRT) funnel glass. In the recovery system, the glass powder was first compressed into cylindrical pellet homogeneously with chlorinating agents, and then subjected to thermal treatment for solid-phase reaction. In this case, lead could be easily released from the silicon oxide network of the glass and it was recovered in the form of PbCl₂. It was found that CaCl2 was the most effective chlorinating agent, and the optimum operation temperature, holding time and system pressure were 1000 °C, 2 h, 600 ± 50 Pa, respectively. The evaporated PbCl₂could be easily recovered by a cooling device. The evaporation ratio of lead from waste CRT was 99.1% and the purity of the recovered PbCl₂product was 97.0%. The reaction routes and lead recovery mechanisms of the process were identified. This study provides an efficient and practical process for waste CRT funnel glass detoxification and recycling.

Spheroidization of molybdenum powder by radio frequency thermal plasma

NASA Astrophysics Data System (ADS)

Liu, Xiao-ping; Wang, Kuai-she; Hu, Ping; Chen, Qiang; Volinsky, Alex A.

2015-11-01

To control the morphology and particle size of dense spherical molybdenum powder prepared by radio frequency (RF) plasma from irregular molybdenum powder as a precursor, plasma process parameters were optimized in this paper. The effects of the carrier gas flow rate and molybdenum powder feeding rate on the shape and size of the final products were studied. The molybdenum powder morphology was examined using high-resolution scanning electron microscopy. The powder phases were analyzed by X-ray diffraction. The tap density and apparent density of the molybdenum powder were investigated using a Hall flow meter and a Scott volumeter. The optimal process parameters for the spherical molybdenum powder preparation are 50 g/min powder feeding rate and 0.6 m3/h carrier gas rate. In addition, pure spherical molybdenum powder can be obtained from irregular powder, and the tap density is enhanced after plasma processing. The average size is reduced from 72 to 62 µm, and the tap density is increased from 2.7 to 6.2 g/cm3. Therefore, RF plasma is a promising method for the preparation of high-density and high-purity spherical powders.

Ceramic oxide powders and the formation thereof

DOEpatents

Katz, Joseph L.; Hung, Cheng-Hung

1993-01-01

Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions.

Influence of Powder Characteristics on Processability of AlSi12 Alloy Fabricated by Selective Laser Melting

PubMed Central

Zherebtsov, Dmitry; Radionova, Ludmila

2018-01-01

Selective laser melting (SLM) is one of the additive manufacturing technologies that allows for the production of parts with complex shapes from either powder feedstock or from wires. Aluminum alloys have a great potential for use in SLM especially in automotive and aerospace fields. This paper studies the influence of starting powder characteristics on the processability of SLM fabricated AlSi12 alloy. Three different batches of gas atomized powders from different manufacturers were processed by SLM. The powders differ in particle size and its distribution, morphology and chemical composition. Cubic specimens (10 mm × 10 mm × 10 mm) were fabricated by SLM from the three different powder batches using optimized process parameters. The fabrication conditions were kept similar for the three powder batches. The influence of powder characteristics on porosity and microstructure of the obtained specimens were studied in detail. The SLM samples produced from the three different powder batches do not show any significant variations in their structural aspects. However, the microstructural aspects differ and the amount of porosity in these three specimens vary significantly. It shows that both the flowability of the powder and the apparent density have an influential role on the processability of AlSi12 SLM samples. PMID:29735932

Influence of Powder Characteristics on Processability of AlSi12 Alloy Fabricated by Selective Laser Melting.

PubMed

Baitimerov, Rustam; Lykov, Pavel; Zherebtsov, Dmitry; Radionova, Ludmila; Shultc, Alexey; Prashanth, Konda Gokuldoss

2018-05-07

Selective laser melting (SLM) is one of the additive manufacturing technologies that allows for the production of parts with complex shapes from either powder feedstock or from wires. Aluminum alloys have a great potential for use in SLM especially in automotive and aerospace fields. This paper studies the influence of starting powder characteristics on the processability of SLM fabricated AlSi12 alloy. Three different batches of gas atomized powders from different manufacturers were processed by SLM. The powders differ in particle size and its distribution, morphology and chemical composition. Cubic specimens (10 mm × 10 mm × 10 mm) were fabricated by SLM from the three different powder batches using optimized process parameters. The fabrication conditions were kept similar for the three powder batches. The influence of powder characteristics on porosity and microstructure of the obtained specimens were studied in detail. The SLM samples produced from the three different powder batches do not show any significant variations in their structural aspects. However, the microstructural aspects differ and the amount of porosity in these three specimens vary significantly. It shows that both the flowability of the powder and the apparent density have an influential role on the processability of AlSi12 SLM samples.

Spheroidization by Plasma Processing and Characterization of Stainless Steel Powder for 3D Printing

NASA Astrophysics Data System (ADS)

Ji, Lina; Wang, Changzhen; Wu, Wenjie; Tan, Chao; Wang, Guoyu; Duan, Xuan-Ming

2017-10-01

Stainless steel 316L (SS 316L) powder was spheroidized by plasma processing to improve its suitability for powder 3D printing. The obtained spheroidized (sphero) powder was characterized in terms of its crystalline phases, elemental composition, morphology, particle size and distribution, light absorption, and flow properties. The elemental composition of the sphero powder met the Chinese standard for SS 316L except for its Si content. The volume fraction of ferrite increased after plasma processing. Furthermore, plasma processing was shown to not only reduce the mean size of the particles in the size range of 10 to 100 μm but also generate particles in the size range of 0.1 to 10 μm. The smaller particles filled the voids among larger particles, increasing the powder density. The light absorption was also increased owing to enhanced internal reflection. Although the basic flow energy decreased after plasma processing, the flow function (FF) value was smaller for the sphero powder, indicating a lower flowability of the sphero powder. However, the density of SS 316L pieces printed with commercial and sphero powders was 98.76 pct and 98.16 pct of the SS 316L bulk density, respectively, indicating the suitability of the sphero powder for 3D printing despite an FF below 10.

Ultrathin ZnSe nanowires: one-pot synthesis via a heat-triggered precursor slow releasing route, controllable Mn doping and application in UV and near-visible light detection.

PubMed

Li, Dong; Xing, Guanjie; Tang, Shilin; Li, Xiaohong; Fan, Louzhen; Li, Yunchao

2017-10-12

We report herein a heat-triggered precursor slow releasing route for the one-pot synthesis of ultrathin ZnSe nanowires (NWs), which relies on the gradual dissolving of Se powder into oleylamine containing a soluble Zn precursor under heating. This route allows the reaction system to maintain a high monomer concentration throughout the entire reaction process, thus enabling the generation of ZnSe NWs with diameter down to 2.1 nm and length approaching 400 nm. The size-dependent optical properties and band-edge energy levels of the ZnSe NWs were then explored in depth by UV-visible spectroscopy and cyclic voltammetry, respectively. Considering their unique absorption properties, these NWs were specially utilized for fabricating photoelectrochemical-type photodetectors (PDs). Impressively, the PDs based on the ZnSe NWs with diameters of 2.1 and 4.5 nm exhibited excellent responses to UVA and near-visible light, respectively: both possessed ultrahigh on/off ratios (5150 for UVA and 4213 for near-visible light) and ultrawide linear response ranges (from 2.0 to 9000 μW cm -2 for UVA and 5.0 to 8000 μW cm -2 for near-visible light). Furthermore, these ZnSe NWs were selectively doped with various amounts of Mn 2+ to tune their emission properties. As a result, ZnSe NW film-based photochromic cards were creatively developed for visually detecting UVA and near-visible radiation.

Nonaqueous solution synthesis process for preparing oxide powders of lead zirconate titanate and related materials

DOEpatents

Voigt, J.A.; Sipola, D.L.; Tuttle, B.A.; Anderson, M.T.

1999-06-01

A process is disclosed for producing powders of perovskite-type compounds which comprises mixing a metal alkoxide solution with a lead acetate solution to form a homogeneous, clear metal solution, adding an oxalic acid/n-propanol solution to this metal solution to form an easily filterable, free-flowing precursor powder and then calcining this powder. This process provides fine perovskite-phase powders with ferroelectric properties which are particularly useful in a variety of electronic applications. 4 figs.

Nonaqueous solution synthesis process for preparing oxide powders of lead zirconate titanate and related materials

DOEpatents

Voigt, James A.; Sipola, Diana L.; Tuttle, Bruce A.; Anderson, Mark T.

1999-01-01

A process for producing powders of perovskite-type compounds which comprises mixing a metal alkoxide solution with a lead acetate solution to form a homogeneous, clear metal solution, adding an oxalic acid/n-propanol solution to this metal solution to form an easily filterable, free-flowing precursor powder and then calcining this powder. This process provides fine perovskite-phase powders with ferroelectric properties which are particularly useful in a variety of electronic applications.

Surpassing the Theoretical Limit of Porosity in Conventional Solid-State Foaming: Microstructure Characterization of Length Scales in a Copper Metal Foam

DTIC Science & Technology

2014-11-01

powder metallurgy processes (e.g., using a polymer foam as a fugitive template7) can exceed 85% porosity, it is more common for powder metallurgy ...for the 0.5 GPa compact is a remarkable result from a powder metallurgy process, especially because the pore structure is not dominated by necks...strengths in bulk engineering structures produced via powder metallurgy . Completely unique to this process is the ability to create foamed powder . This

Effect of reductant and PVP on morphology and magnetic property of ultrafine Ni powders prepared via hydrothermal route

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

Zhang, Jun, E-mail: j-zhang@126.com; Wang, Xiucai; Li, Lili

2013-10-15

Graphical abstract: The ultrafine Ni powders with the shapes including sphere, pearl-string, leaf, fish-bone, hexagonal sheet and silknet were prepared through one-step hydrothermal reduction using different reductants. Their saturation magnetization, remanent magnetization and coercivity sequentially increase, and the coercivity of hexagonal sheet-like Ni powders increases by 25% compared with the Ni bulk counterpart. - Highlights: • The ultrafine Ni powders with various shapes of sphere, fish-bone, hexagonal sheet, etc. • Facile and one-step hydrothermal reduction using three reductants and PVP additive was developed. • Magnetic properties of the ultrafine Ni powders with different shapes were measured. • Compared with bulkmore » Ni material, coercivity of hexagonal sheet Ni increases by 25%. • The formation mechanism of the shapes was suggested. - Abstract: The ultrafine nickel particles with different shapes including sphere, pearl-string, leaf, fish-bone, hexagonal sheet and silknet were prepared through one-step hydrothermal reduction using hydrazine hydrate, sodium hypophosphite and ethylene glycol as reductants, polyvinylpyrrolidone as structure-directing agent. It has been verified with the characterization of X-ray powder diffraction and transmission/scanning electronic microscopy that as-prepared products belong to face-centered cubic structure of nickel microcrystals with high purity and fine dispersity. The magnetic hysteresis loops measured at room temperature reveal that the values of saturation magnetization, remanent magnetization and coercivity rise sequentially from silknet, sphere to hexagonal sheet. In comparison with nickel bulk counterpart, the coercivity of the hexagonal sheet nickel powders increases by 25%.« less

Ceramic oxide powders and the formation thereof

DOEpatents

Katz, J.L.; Chenghung Hung.

1993-12-07

Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions. 14 figures.

Compact Process for the Preparation of Microfine Spherical High-Niobium-Containing TiAl Alloy Powders

NASA Astrophysics Data System (ADS)

Tong, J. B.; Lu, X.; Liu, C. C.; Wang, L. N.; Qu, X. H.

2015-03-01

High-Nb-containing TiAl alloys are a new generation of materials for high-temperature structural applications because of their superior high-temperature mechanical properties. The alloy powders can be widely used for additive manufacturing, thermal spraying, and powder metallurgy. Because of the difficulty of making microfine spherical alloy powders in quantity by conventional techniques, a compact method was proposed, which consisted of two-step ball milling of elemental powders and subsequent radio frequency (RF) argon plasma spheroidization. In comparison with conventional mechanical alloying techniques, the two-step milling process can be used to prepare alloy powders with uniform scale in a short milling time with no addition of process control agent. This makes the process effective and less contaminating. After RF argon plasma spheroidization, the powders produced exhibit good sphericity, and the number-average diameter is about 8.2 μm with a symmetric unimodal particle size distribution. The powders perform high composition homogeneity and contain predominately supersaturated α 2-Ti3Al phase. The oxygen and carbon contents of the spheroidized powder are 0.47% and 0.050%, respectively.

Improved silicon carbide for advanced heat engines

NASA Technical Reports Server (NTRS)

Whalen, T. J.; Winterbottom, W. L.

1986-01-01

Work performed to develop silicon carbide materials of high strength and to form components of complex shape and high reliability is described. A beta-SiC powder and binder system was adapted to the injection molding process and procedures and process parameters developed capable of providing a sintered silicon carbide material with improved properties. The initial effort has been to characterize the baseline precursor materials (beta silicon carbide powder and boron and carbon sintering aids), develop mixing and injection molding procedures for fabricating test bars, and characterize the properties of the sintered materials. Parallel studies of various mixing, dewaxing, and sintering procedures have been carried out in order to distinguish process routes for improving material properties. A total of 276 MOR bars of the baseline material have been molded, and 122 bars have been fully processed to a sinter density of approximately 95 percent. The material has a mean MOR room temperature strength of 43.31 ksi (299 MPa), a Weibull characteristic strength of 45.8 ksi (315 MPa), and a Weibull modulus of 8.0. Mean values of the MOR strengths at 1000, 1200, and 14000 C are 41.4, 43.2, and 47.2 ksi, respectively. Strength controlling flaws in this material were found to consist of regions of high porosity and were attributed to agglomerates originating in the initial mixing procedures. The mean stress rupture lift at 1400 C of five samples tested at 172 MPa (25 ksi) stress was 62 hours and at 207 MPa (30 ksi) stress was 14 hours. New fluid mixing techniques have been developed which significantly reduce flaw size and improve the strength of the material. Initial MOR tests indicate the strength of the fluid-mixed material exceeds the baseline property by more than 33 percent.

A novel low cost non-aqueous chemical route for giant dielectric constant CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Singh, Laxman; Kim, Ill Won; Woo, Won Seok; Sin, Byung Cheol; Lee, Hyung-il; Lee, Youngil

2015-05-01

This paper reports a simple, fast, low cost and environment-friendly route for preparing a highly crystalline giant dielectric material, CaCu3Ti4O12 (CCTO), through combustion of metal nitrates in non-aqueous precursor solution using inexpensive solid TiO2 powder. The route to producing pure phase CCTO ceramic using stable solid TiO2 is better than other several sol-gel routes reported earlier in which expensive alkoxides, oxynitrates, or chlorides of titanium are used as the titanium sources. X-ray diffraction revealed the formation of cubic perovskite CCTO. Scanning electron microscopy image showed the average grain sizes in the range of 1.5-5 μm. At 10 kHz and room temperature, the best CCTO ceramic exhibited a high dielectric constant, ε‧ ∼43325.24, with low dielectric loss, tan δ ∼0.088. The dielectric relaxation behavior was rationalized from impedance and modulus studies and the presence of a non-Debye type of relaxation was confirmed.

Electrostatic powder coating: Principles and pharmaceutical applications.

PubMed

Prasad, Leena Kumari; McGinity, James W; Williams, Robert O

2016-05-30

A majority of pharmaceutical powders are insulating materials that have a tendency to accumulate charge. This phenomenon has contributed to safety hazards and issues during powder handling and processing. However, increased understanding of this occurrence has led to greater understanding and control of processing and product performance. More recently, the charging of pharmaceutical powders has been employed to adopt electrostatic powder coating as a pharmaceutical process. Electrostatic powder coating is a mature technology used in the finishing industry and much of that knowledge applies to its use in pharmaceutical applications. This review will serve to summarize the principles of electrostatic powder coating and highlight some of the research conducted on its use for the preparation of pharmaceutical dosage forms. Copyright © 2016 Elsevier B.V. All rights reserved.

Effect of Powder Size and Shape on the SLS Processability and Mechanical Properties of a TPU Elastomer

NASA Astrophysics Data System (ADS)

Dadbakhsh, Sasan; Verbelen, Leander; Vandeputte, Tom; Strobbe, Dieter; Van Puyvelde, Peter; Kruth, Jean-Pierre

This work investigates the influence of powder size/shape on selective laser sintering (SLS) of a thermoplastic polyurethane (TPU) elastomer. It examines a TPU powder which had been cryogenically milled in two different sizes; coarse powder (D50∼200μm) with rough surfaces in comparison with a fine powder (D50∼63μm) with extremely fine flow additives. It is found that the coarse powder coalesces at lower temperatures and excessively smokes during the SLS processing. In comparison, the fine powder with flow additives is better processable at significantly higher powder bed temperatures, allowing a lower optimum laser energy input which minimizes smoking and degradation of the polymer. In terms of mechanical properties, good coalescence of both powders lead to parts with acceptable shear-punch strengths compared to injection molded parts. However, porosity and degradation from the optimum SLS parameters of the coarse powder drastically reduce the tensile properties to about one-third of the parts made from the fine powders as well as those made by injection molding (IM).

Quantitative analysis of packed and compacted granular systems by x-ray microtomography

NASA Astrophysics Data System (ADS)

Fu, Xiaowei; Milroy, Georgina E.; Dutt, Meenakshi; Bentham, A. Craig; Hancock, Bruno C.; Elliott, James A.

2005-04-01

The packing and compaction of powders are general processes in pharmaceutical, food, ceramic and powder metallurgy industries. Understanding how particles pack in a confined space and how powders behave during compaction is crucial for producing high quality products. This paper outlines a new technique, based on modern desktop X-ray tomography and image processing, to quantitatively investigate the packing of particles in the process of powder compaction and provide great insights on how powder densify during powder compaction, which relate in terms of materials properties and processing conditions to tablet manufacture by compaction. A variety of powder systems were considered, which include glass, sugar, NaCl, with a typical particle size of 200-300 mm and binary mixtures of NaCl-Glass Spheres. The results are new and have been validated by SEM observation and numerical simulations using discrete element methods (DEM). The research demonstrates that XMT technique has the potential in further investigating of pharmaceutical processing and even verifying other physical models on complex packing.

A novel route for the synthesis of nanotubes and fullerene-like nanostructures of molybdenum disulfide

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

Panigrahi, Pravas Kumar, E-mail: pravas.iit@gmail.com; Pathak, Amita, E-mail: ami@chem.iitkgp.ernet.in

Graphical abstract: Nanotubes and fullerene-like nanostructures of MoS{sub 2} were synthesized via a microwave-assisted route in solution phase. Highlights: Black-Right-Pointing-Pointer Microwave-assisted route for synthesis of nanotube and fullerene-like nanostructures of MoS{sub 2}. Black-Right-Pointing-Pointer Morphological analysis of the synthesized products. Black-Right-Pointing-Pointer Solvent plays important role in the modification of morphology of MoS{sub 2}. -- Abstract: The paper described the synthesis of nanotubes and fullerene-like nanostructures of MoS{sub 2} through a technically simple, rapid, and energy-efficient microwave-assisted synthesis technique, which involved the use of elemental sulfur dissolved in a mixture of monoethanolamine and hydrazine hydrate as the sulfide source. The microwave inducedmore » reaction between the molybdate with sulfide ions, in the presence of hydrazine hydrate in the reaction medium, resulted in the formation of gray colored powders of amorphous MoS{sub 2}. The as-obtained powders were calcined at 600 Degree-Sign C for 2 h and characterized by different techniques. HRTEM analysis of the calcined samples indicated the formation of fullerene-like MoS{sub 2} structures when the starting solution mixture was irradiated with microwave for a period of 200 s, while on 600 s of irradiation of the same revealed the formation of folded sheets like MoS{sub 2} nanotubes. BET surface areas of the calcined samples have been measured and a plausible reaction mechanism for the formation of nanotubes and fullerene-like nanostructures of MoS{sub 2} has been proposed.« less

Investigation of nanocrystalline zinc chromite obtained by two soft chemical routes

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

Gingasu, Dana; Mindru, Ioana, E-mail: imandru@yahoo.com; Culita, Daniela C.

2014-01-01

Graphical abstract: - Highlights: • Two soft chemical routes to synthesize zinc chromites are described. • Glycine is used as chelating agent (precursor method) and fuel (solution combustion method). • The synthesized chromites have crystallite size in the range of 18–27 nm. • An antiferromagnetic (AFM) transition is observed at about T{sub N} ∼ 18 K. - Abstract: Zinc chromite (ZnCr{sub 2}O{sub 4}) nanocrystalline powders were obtained by two different chemical routes: the precursor method and the solution combustion method involving glycine-nitrates. The complex compound precursors, [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COO){sub 8}]·9H{sub 2}O and [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COOH){sub 4.5}]·(NO{sub 3}){sub 8}·6H{submore » 2}O, were characterized by chemical analysis, infrared spectroscopy (IR), ultraviolet–visible spectroscopy (UV–vis) and thermal analysis. The structure, morphology, surface chemistry and magnetic properties of ZnCr{sub 2}O{sub 4} powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), infrared and Raman spectroscopy (RS), ultraviolet–visible spectroscopy (UV–vis) and magnetic measurements. X-ray diffraction patterns indicated the chromite spinel phase with good crystallinity and an average crystallite size of approximately 18–27 nm. The band gap values ranged between 3.31 and 3.33 eV. The magnetic measurements indicated an antiferromagnetic transition at T{sub N} ∼ 17.5/18 K.« less

Multi-photon excited coherent random laser emission in ZnO powders

NASA Astrophysics Data System (ADS)

Tolentino Dominguez, Christian; Gomes, Maria De A.; Macedo, Zélia S.; de Araújo, Cid B.; Gomes, Anderson S. L.

2014-11-01

We report the observation and analysis of anti-Stokes coherent random laser (RL) emission from zinc oxide (ZnO) powders excited by one-, two- or three-photon femtosecond laser radiation. The ZnO powders were produced via a novel proteic sol-gel, low-cost and environmentally friendly route using coconut water in the polymerization step of the metal precursor. One- and two-photon excitation at 354 nm and 710 nm, respectively, generated single-band emissions centred at about 387 nm. For three-photon excitation, the emission spectra showed a strong ultraviolet (UV) band (380-396 nm) attributed to direct three-photon absorption from the valence band to the conduction band. The presence of an intensity threshold and a bandwidth narrowing of the UV band from about 20 to 4 nm are clear evidence of RL action. The observation of multiple sub-nanometre narrow peaks in the emission spectra for excitation above the RL threshold is consistent with random lasing by coherent feedback.

Micrometric BN powders used as catalyst support: influence of the precursor on the properties of the BN ceramic

NASA Astrophysics Data System (ADS)

Perdigon-Melon, José Antonio; Auroux, Aline; Guimon, Claude; Bonnetot, Bernard

2004-02-01

Thin powders and foams of boron nitride have been prepared from molecular precursors for use as noble metal supports in the catalytic conversion of methane. Different precursors originating from borazines have been tested. The best results were obtained using a precursor derived from trichloroborazine (TCB) which, after reacting with ammonia at room temperature and then thermolyzing up to 1800°C, led to BN powders with a specific area of more than 300 m 2 g -1 and a micrometric spherical texture. Comparable results were obtained using polyborazylene under similar conditions. Aminoborazine-derived precursors did not yield such high specific area ceramics but the BN microstructure resembled a foam with a crystallized skin and amorphous internal part. These differences were related to the chemical mechanism of the conversion of the precursor into BN. Polyhaloborazines and polyborazines yielded BN through gas-solid reactions whereas aminoborazine polymers could be kept waxy up to high temperatures, which favored the glassy foam. Catalysts composed of BN support and platinum have been prepared using two routes: from a mixture of precursor or by impregnation of a BN powder leading to very different catalysts.

Innovative polymeric system (IPS) for solvent-free lipophilic drug transdermal delivery via dissolving microneedles.

PubMed

Dangol, Manita; Yang, Huisuk; Li, Cheng Guo; Lahiji, Shayan Fakhraei; Kim, Suyong; Ma, Yonghao; Jung, Hyungil

2016-02-10

Lipophilic drugs are potential drug candidates during drug development. However, due to the need for hazardous organic solvents for their solubilization, these drugs often fail to reach the pharmaceutical market, and in doing so highlight the importance of solvent free systems. Although transdermal drug delivery systems (TDDSs) are considered prospective safe drug delivery routes, a system involving lipophilic drugs in solvent free or powder form has not yet been described. Here, we report, for the first time, a novel approach for the delivery of every kind of lipophilic drug in powder form based on an innovative polymeric system (IPS). The phase transition of powder form of lipophilic drugs due to interior chemical bonds between drugs and biodegradable polymers and formation of nano-sized colloidal structures allowed the fabrication of dissolving microneedles (DMNs) to generate a powerful TDDS. We showed that IPS based DMN with powder capsaicin enhances the therapeutic effect for treatment of the rheumatic arthritis in a DBA/1 mouse model compared to a solvent-based system, indicating the promising potential of this new solvent-free platform for lipophilic drug delivery. Copyright © 2016 Elsevier B.V. All rights reserved.

Green biosynthesis of silver nanoparticles using Curcuma longa tuber powder

PubMed Central

Shameli, Kamyar; Ahmad, Mansor Bin; Zamanian, Ali; Sangpour, Parvanh; Shabanzadeh, Parvaneh; Abdollahi, Yadollah; Zargar, Mohsen

2012-01-01

Green synthesis of noble metal nanoparticles is a vastly developing area of research. Metallic nanoparticles have received great attention from chemists, physicists, biologists, and engineers who wish to use them for the development of a new-generation of nanodevices. In this study, silver nanoparticles were biosynthesized from aqueous silver nitrate through a simple and eco-friendly route using Curcuma longa tuber-powder extracts, which acted as a reductant and stabilizer simultaneously. Characterizations of nanoparticles were done using different methods, which included ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray fluorescence spectrometry, and Fourier-transform infrared spectroscopy. The ultraviolet-visible spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 415 nm. Transmission electron microscopy showed that mean diameter and standard deviation for the formation of silver nanoparticles was 6.30 ± 2.64 nm. Powder X-ray diffraction showed that the particles are crystalline in nature, with a face-centered cubic structure. The most needed outcome of this work will be the development of value-added products from C. longa for biomedical and nanotechnology-based industries. PMID:23341739

Uniform-droplet spray forming

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

Blue, C.A.; Sikka, V.K.; Chun, Jung-Hoon

1997-04-01

The uniform-droplet process is a new method of liquid-metal atomization that results in single droplets that can be used to produce mono-size powders or sprayed-on to substrates to produce near-net shapes with tailored microstructure. The mono-sized powder-production capability of the uniform-droplet process also has the potential of permitting engineered powder blends to produce components of controlled porosity. Metal and alloy powders are commercially produced by at least three different methods: gas atomization, water atomization, and rotating disk. All three methods produce powders of a broad range in size with a very small yield of fine powders with single-sized droplets thatmore » can be used to produce mono-size powders or sprayed-on substrates to produce near-net shapes with tailored microstructures. The economical analysis has shown the process to have the potential of reducing capital cost by 50% and operating cost by 37.5% when applied to powder making. For the spray-forming process, a 25% savings is expected in both the capital and operating costs. The project is jointly carried out at Massachusetts Institute of Technology (MIT), Tuffs University, and Oak Ridge National Laboratory (ORNL). Preliminary interactions with both finished parts and powder producers have shown a strong interest in the uniform-droplet process. Systematic studies are being conducted to optimize the process parameters, understand the solidification of droplets and spray deposits, and develop a uniform-droplet-system (UDS) apparatus appropriate for processing engineering alloys.« less

Comparison Study on Additive Manufacturing (AM) and Powder Metallurgy (PM) AlSi10Mg Alloys

NASA Astrophysics Data System (ADS)

Chen, B.; Moon, S. K.; Yao, X.; Bi, G.; Shen, J.; Umeda, J.; Kondoh, K.

2018-02-01

The microstructural and mechanical properties of AlSi10Mg alloys fabricated by additive manufacturing (AM) and powder metallurgy (PM) routes were investigated and compared. The microstructures were examined by scanning electron microscopy assisted with electron-dispersive spectroscopy. The crystalline features were studied by x-ray diffraction and electron backscatter diffraction. Room-temperature tensile tests and Vickers hardness measurements were performed to characterize the mechanical properties. It was found that the AM alloy had coarser Al grains but much finer Si precipitates compared with the PM alloy. Consequently, the AM alloy showed more than 100% increment in strength and hardness compared with the PM alloy due to the presence of ultrafine forms of Si, while exhibiting moderate ductility.

Plasma induced sp 2 to sp 3 transition in boron nitride

NASA Astrophysics Data System (ADS)

Zhang, J.; Cui, Q.; Li, X.; He, Z.; Li, W.; Ma, Y.; Guan, Q.; Gao, W.; Zou, G.

2004-12-01

The transition from sp 2 to sp 3 hybridization in boron nitride has been induced in plasma. Nano-crystals of cubic boron nitride (cBN) have been synthesized by direct current arc discharge method using hexagonal boron nitride (hBN) as the starting material. The characterization of the as-grown powders is carried out by X-ray diffraction, Fourier transform infrared spectroscopy and transmission electron microscopy. It has been shown that cBN and hBN grains with 20-60 nm in size co-exist in the powders. A reaction route of sublimation - re-hybridization - crystallization had been put forward to explain the mechanism of the hybridization transition and the growth of cBN by this method.

Gas atomization processing of tin and silicon modified LaNi 5 for nickel-metal hydride battery applications

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

Ting, Jason

1999-02-12

Numerous researchers have studied the relevant material properties of so-called AB 5 alloys for battery applications. These studies involved LaNi 5 substituted alloys which were prepared using conventional cast and crush alloying techniques. While valuable to the understanding of metal hydride effects, the previous work nearly ignored the potential for alternative direct powder production methods, like high pressure gas atomization (HPGA). Thus, there is a need to understand the relationship between gas atomization processes, powder particle solidification phases, and hydrogen absorption properties of ultra fine (< 25 μm) atomized powders with high surface area for enhanced battery performance. Concurrently, developmentmore » of a gas atomization nozzle that is more efficient than all current designs is needed to increase the yield of ultrafine AB 5 alloy powder for further processing advantage. Gas atomization processing of the AB 5 alloys was demonstrated to be effective in producing ultrafine spherical powders that were resilient to hydrogen cycling for the benefit of improving corrosion resistance in battery application. These ultrafine powders benefited from the rapid solidification process by having refined solute segregation in the microstructure of the gas atomized powders which enabled a rapid anneal treatment of the powders. The author has demonstrated the ability to produce high yields of ultrafine powder efficiently and cost effectively, using the new HPGA-III technology. Thus, the potential benefits of processing AB 5 alloys using the new HPGA technology could reduce manufacturing cost of nickel-metal hydride powder. In the near future, the manufacture of AB 5 alloy powders could become a continuous and rapid production process. The economic benefit of an improved AB 5 production process may thereby encourage the use of nickel-metal hydride rechargeable batteries in electrical vehicle applications in the foreseeable future.« less

Improved respirable fraction of budesonide powder for dry powder inhaler formulations produced by advanced supercritical CO2 processing and use of a novel additive.

PubMed

Miyazaki, Yuta; Aruga, Naoki; Kadota, Kazunori; Tozuka, Yuichi; Takeuchi, Hirofumi

2017-08-07

A budesonide (BDS) suspension was obtained via advanced supercritical carbon dioxide (scCO 2 ) processing. Thereafter, the suspension was freeze-dried (FD) to produce BDS particles for dry powder inhaler formulations (scCO 2 /FD processing). The scCO 2 /FD processed BDS powder showed low crystallinity by powder X-ray diffraction and a rough surface by scanning electron microscopy. The respirable fraction of BDS was assessed using a twin impinger and revealed that the amount of the scCO 2 /FD processed sample that reached stage 2 was 4-fold higher than that of the supplied powder. To extend the utility of scCO 2 processing, BDS particles for dry powder inhalers were fabricated by combining the scCO 2 system with various additives. When BDS was processed via scCO 2 /FD in the presence of the novel additive, namely, monoglyceride stearate (MGS), the residual BDS/MGS particles remaining in the capsule and devices decreased, followed by an increase in the respirable fraction of BDS 6-fold higher than with the supplied powder. The scCO 2 /FD processed BDS/MGS particles had a smooth surface, in contrast to the scCO 2 /FD processed BDS particles. A combination of BDS and an appropriate additive in scCO 2 treatment may induce changes in particle surface morphology, leading to an improvement in the inhalation properties of BDS. Copyright © 2017 Elsevier B.V. All rights reserved.

Oily wastewater treatment by adsorption-membrane filtration hybrid process using powdered activated carbon, natural zeolite powder and low cost ceramic membranes.

PubMed

Rasouli, Yaser; Abbasi, Mohsen; Hashemifard, Seyed Abdollatif

2017-08-01

In this research, four types of low cost and high performance ceramic microfiltration (MF) membranes have been employed in an in-line adsorption-MF process for oily wastewater treatment. Mullite, mullite-alumina, mullite-alumina-zeolite and mullite-zeolite membranes were fabricated as ceramic MF membranes by low cost kaolin clay, natural zeolite and α-alumina powder. Powdered activated carbon (PAC) and natural zeolite powder in concentrations of 100-800 mg L -1 were used as adsorbent agent in the in-line adsorption-MF process. Performance of the hybrid adsorption-MF process for each concentration of PAC and natural zeolite powder was investigated by comparing quantity of permeation flux (PF) and total organic carbon (TOC) rejection during oily wastewater treatment. Results showed that by application of 400 mg L -1 PAC in the adsorption-MF process with mullite and mullite-alumina membranes, TOC rejection was enhanced up to 99.5% in comparison to the MF only process. An increasing trend was observed in PF by application of 100-800 mg L -1 PAC. Also, results demonstrated that the adsorption-MF process with natural zeolite powder has higher performance in comparison to the MF process for all membranes except mullite-alumina membranes in terms of PF. In fact, significant enhancement of PF and TOC rejection up to 99.9% were achieved by employing natural zeolite powder in the in-line adsorption-MF hybrid process.

Preparation of superconductor precursor powders

DOEpatents

Bhattacharya, R.

1998-08-04

A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products. 7 figs.

Preparation of superconductor precursor powders

DOEpatents

Bhattacharya, Raghunath

1998-01-01

A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

Developments in the formulation and delivery of spray dried vaccines.

PubMed

Kanojia, Gaurav; Have, Rimko Ten; Soema, Peter C; Frijlink, Henderik; Amorij, Jean-Pierre; Kersten, Gideon

2017-10-03

Spray drying is a promising method for the stabilization of vaccines, which are usually formulated as liquids. Usually, vaccine stability is improved by spray drying in the presence of a range of excipients. Unlike freeze drying, there is no freezing step involved, thus the damage related to this step is avoided. The edge of spray drying resides in its ability for particles to be engineered to desired requirements, which can be used in various vaccine delivery methods and routes. Although several spray dried vaccines have shown encouraging preclinical results, the number of vaccines that have been tested in clinical trials is limited, indicating a relatively new area of vaccine stabilization and delivery. This article reviews the current status of spray dried vaccine formulations and delivery methods. In particular it discusses the impact of process stresses on vaccine integrity, the application of excipients in spray drying of vaccines, process and formulation optimization strategies based on Design of Experiment approaches as well as opportunities for future application of spray dried vaccine powders for vaccine delivery.

Hierarchical Na-doped cubic ZrO2 synthesis by a simple hydrothermal route and its application in biodiesel production

NASA Astrophysics Data System (ADS)

Lara-García, Hugo A.; Romero-Ibarra, Issis C.; Pfeiffer, Heriberto

2014-10-01

Hierarchical growth of cubic ZrO2 phase was successfully synthesized via a simple hydrothermal process in the presence of different surfactants (cationic, non-ionic and anionic) and sodium hydroxide. The structural and microstructural characterizations of different ZrO2 powders were performed using various techniques, such as X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption, scanning electron microscopy and infrared. Results indicated that sodium addition stabilized the cubic ZrO2 phase by a Na-doping process, independently of the surfactant used. In contrast, microstructural characteristics varied as a function of the surfactant and sodium presence. In addition, water vapor (H2O) and carbon dioxide (CO2) sorption properties were evaluated on ZrO2 samples. Results evidenced that sample surface reactivity changed as a function of the sodium content. Finally, this surface reactivity was evaluated on the biodiesel transesterification reaction using the different synthesized samples, obtaining yields of 93%.

Formation and mechanism of nanocrystalline AZ91 powders during HDDR processing

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

Liu, Yafen; Fan, Jianfeng, E-mail: fanjianfeng@tyu

2017-03-15

Grain sizes of AZ91 alloy powders were markedly refined to about 15 nm from 100 to 160 μm by an optimized hydrogenation-disproportionation-desorption-recombination (HDDR) process. The effect of temperature, hydrogen pressure and processing time on phase and microstructure evolution of AZ91 alloy powders during HDDR process was investigated systematically by X-ray diffraction, optical microscopy, scanning electron microscopy and transmission electron microscopy, respectively. The optimal HDDR process for preparing nanocrystalline Mg alloy powders is hydriding at temperature of 350 °C under 4 MPa hydrogen pressure for 12 h and dehydriding at 350 °C for 3 h in vacuum. A modified unreacted coremore » model was introduced to describe the mechanism of grain refinement of during HDDR process. - Highlights: • Grain size of the AZ91 alloy powders was significantly refined from 100 μm to 15 nm. • The optimal HDDR technology for nano Mg alloy powders is obtained. • A modified unreacted core model of grain refinement mechanism was proposed.« less

Monoclinic β-Li2TiO3 nanocrystalline particles employing novel urea assisted solid state route: Synthesis, characterization and sintering behavior

NASA Astrophysics Data System (ADS)

Tripathi, Biranchi M.; Mohanty, Trupti; Prakash, Deep; Tyagi, A. K.; Sinha, P. K.

2017-07-01

Pure phase monoclinic nano-crystalline Li2TiO3 powder was synthesized by a novel urea assisted solid state synthesis method using readily available and economical precursors. A single phase and well crystalline Li2TiO3 powder has been obtained at slightly lower temperature (600-700 °C) and shorter duration (2 h) as compared to the conventional solid state method. The proposed method has significant advantages in comparison to other viable methods mainly in terms of phase purity, powder properties and sinterability. Analysis of chemical composition using inductively coupled plasma atomic emission spectroscopy (ICP-AES) shows no loss of lithium from Li2TiO3 in the proposed method. The emergence of monoclinic Li2TiO3 phase was confirmed by X-ray diffraction (XRD) pattern of as-synthesized powder. The crystallite size of Li2TiO3 powder was calculated to be in the range of 15-80 nm, which varied as a function of urea composition and temperature. The morphology of as-prepared Li2TiO3 powders was examined by scanning electron microscope (SEM). The effect of urea composition on phase and morphology was investigated so as to delineate the role of urea. Upon sintering at < 1000 °C temperature, the Li2TiO3 powder compact attained about 98% of the theoretical density with fine grained (grain size: 2-3 μm) microstructure. It indicates excellent sinter-ability of Li2TiO3 powder synthesized by the proposed method. The fine grained structure is desirable for better tritium breeding performance of Li2TiO3. Electrochemical impedance spectroscopy at variable temperature showed good electrical properties of Li2TiO3. The proposed method is simple, anticipated to be cost effective and convenient to realise for large scale production of phase pure nanocrystalline and having significantly enhanced sinter-ability Li2TiO3 powder.

Preparation of glass-forming materials from granulated blast furnace slag

NASA Astrophysics Data System (ADS)

Alonso, M.; Sáinz, E.; Lopez, F. A.

1996-10-01

Glass precursor materials, to be used for the vitrification of hazardous wastes, have been prepared from blast furnace slag powder through a sol-gel route. The slag is initially reacted with a mixture of alcohol (ethanol or methanol) and mineral acid (HNO3 or H2SO4) to give a sol principally consisting of Si, Ca, Al, and Mg alkoxides. Gelation is carried out with variable amounts of either ammonia or water. The gelation rate can be made as fast as desired by adding excess hydrolizing agent or else by distilling the excess alcohol out of the alkoxide solution. The resulting gel is first dried at low temperature and ground. The powder thus obtained is then heat treated at several temperatures. The intermediate and final materials are characterized by thermal analysis, infrared (IR) spectroscopy, X-ray diffraction, scanning electron microscopy (SEM), and chemical analysis. From the results, the operating conditions yielding a variety of glass precursors differing in their composition are established. The method, in comparison with direct vitrification of slag, presents a number of advantages: (1) the glass precursor obtained devitrifies at higher temperatures; (2) it enables the adjustment, to a certain extent, of the chemical composition of the glass precursor; and (3) it permits recovering marketable materials at different stages of the process.

Fabrication of malachite with a hierarchical sphere-like architecture.

PubMed

Xu, Jiasheng; Xue, Dongfeng

2005-09-15

Malachite (Cu2(OH)2CO3) with a hierarchical sphere-like architecture has been successfully synthesized via a simple and mild hydrothermal route in the absence of any external inorganic additives or organic structure-directing templates. Powder X-ray diffraction, scanning electron microscopy, and Fourier transmission infrared spectrometry are used to characterize various properties of the obtained malachite samples. The hierarchical malachite particles are uniform spheres with a diameter of 10-20 microm, which are comprised of numerous two-dimensional microplatelets paralleling the sphere surface. The initial concentration of reagents, the hydrothermal reaction time, and temperature are important factors which dominantly affect the evolution of crystal morphologies. The growth of the hierarchical architecture is believed to be a layer-by-layer growth process. Further, copper oxide with the similar morphology can be easily obtained from the as-prepared malachite.

Fabrication of porous titanium scaffold materials by a fugitive filler method.

PubMed

Hong, T F; Guo, Z X; Yang, R

2008-12-01

A clean powder metallurgy route was developed here to produce Ti foams, using a fugitive polymeric filler, polypropylene carbonate (PPC), to create porosities in a metal-polymer compact at the pre-processing stage. The as-produced foams were studied by scanning electron microscopy (SEM), LECO combustion analyses and X-ray diffraction (XRD). Compression tests were performed to assess their mechanical properties. The results show that titanium foams with open pores can be successfully produced by the method. The compressive strength and modulus of the foams decrease with an increasing level of porosity and can be tailored to those of the human bones. After alkali treatment and soaking in a simulated body fluid (SBF) for 3 days, a thin apatite layer was formed along the Ti foam surfaces, which provides favourable bioactive conditions for bone bonding and growth.

New manufacturing method for Fe-Si magnetic powders using modified pack-cementation process

NASA Astrophysics Data System (ADS)

Byun, Ji Young; Kim, Jang Won; Han, Jeong Whan; Jang, Pyungwoo

2013-03-01

This paper describes a new method for making Fe-Si magnetic powders using a pack-cementation process. It was found that Fe-Si alloy powders were formed by a reaction of the pack mixture of Fe, Si, NaF, and Al2O3 powders at 900 °C for 24 h under a hydrogen atmosphere. Separation of the Fe-Si alloy powders was dependent on the particle size of the Fe powders in the pack. For small Fe powders, magnetic separation in a medium of strong alkali solution was recommended. But, for relatively larger Fe powders, the Fe-Si alloy powders were easily separated from Al2O3 powders using a magnet in air atmosphere. The Si content in the Fe-Si magnetic powders were easily controlled by changing the weight ratio of Si to (Si+Fe) in the pack.

Printability of calcium phosphate: calcium sulfate powders for the application of tissue engineered bone scaffolds using the 3D printing technique.

PubMed

Zhou, Zuoxin; Buchanan, Fraser; Mitchell, Christina; Dunne, Nicholas

2014-05-01

In this study, calcium phosphate (CaP) powders were blended with a three-dimensional printing (3DP) calcium sulfate (CaSO4)-based powder and the resulting composite powders were printed with a water-based binder using the 3DP technology. Application of a water-based binder ensured the manufacture of CaP:CaSO4 constructs on a reliable and repeatable basis, without long term damage of the printhead. Printability of CaP:CaSO4 powders was quantitatively assessed by investigating the key 3DP process parameters, i.e. in-process powder bed packing, drop penetration behavior and the quality of printed solid constructs. Effects of particle size, CaP:CaSO4 ratio and CaP powder type on the 3DP process were considered. The drop penetration technique was used to reliably identify powder formulations that could be potentially used for the application of tissue engineered bone scaffolds using the 3DP technique. Significant improvements (p<0.05) in the 3DP process parameters were found for CaP (30-110 μm):CaSO4 powders compared to CaP (<20 μm):CaSO4 powders. Higher compressive strength was obtained for the powders with the higher CaP:CaSO4 ratio. Hydroxyapatite (HA):CaSO4 powders showed better results than beta-tricalcium phosphate (β-TCP):CaSO4 powders. Solid and porous constructs were manufactured using the 3DP technique from the optimized CaP:CaSO4 powder formulations. High-quality printed constructs were manufactured, which exhibited appropriate green compressive strength and a high level of printing accuracy. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication, characterization, and irradiation of an austenitic oxide dispersion strengthened steel suited for next generation nuclear applications

NASA Astrophysics Data System (ADS)

Brooks, Adam J.

As nuclear energy systems become more advanced, the materials encompassing them need to perform at higher temperatures for longer periods of time. In this Master's thesis we experiment with an oxide dispersion strengthened (ODS) austenitic steel that has been recently developed. ODS materials have a small concentration of nano oxide particles dispersed in their matrix, and typically have higher strength and better extreme temperature creep resistance characteristics than ordinary steels. However, no ODS materials have ever been installed in a commercial power reactor to date. Being a newer research material, there are many unanswered phenomena that need to be addressed regarding the performance under irradiation. Furthermore, due to the ODS material traditionally needing to follow a powder metallurgy fabrication route, there are many processing parameters that need to be optimized before achieving a nuclear grade material specification. In this Master's thesis we explore the development of a novel ODS processing technology conducted in Beijing, China, to produce solutionized bulk ODS samples with 97% theoretical density. This is done using relatively low temperatures and ultra high pressure (UHP) equipment, to compact the mechanically alloyed (MA) steel powder into bulk samples without any thermal phase change influence or oxide precipitation. By having solutionized bulk ODS samples, transmission electron microscopy (TEM) observation of nano oxide precipitation within the steel material can be studied by applying post heat treatments. These types of samples will be very useful to the science and engineering community, to answer questions regarding material powder compacting, oxide synthesis, and performance. Subsequent analysis performed at Queen's University included X-ray diffraction (XRD) and inductively coupled plasma optical emission spectrometry (ICP-OES). Additional TEM in-situ 1MeV Kr2+ irradiation experiments coupled with energy dispersive X-ray (EDX) techniques, were also performed on large (200nm+) non-stoichiometric oxides embedded within the austenite steel grains, in an attempt to quantify the elemental compositional changes during high temperature (520°C) heavy ion irradiation.

Method of producing Pb-stabilized superconductor precursors and method of producing superconductor articles therefrom

DOEpatents

Kroeger, D.M.; Hsu, H.S.; Brynestad, J.

1995-03-07

Metal oxide superconductor powder precursors are prepared in an aerosol pyrolysis process. A solution of the metal cations is introduced into a furnace at 600--1,000 C for 0.1 to 60 seconds. The process produces micron to submicron size powders without the usual loss of the lead stabilizer. The resulting powders have a narrow particle size distribution, a small grain size, and are readily converted to a superconducting composition upon subsequent heat treatment. The precursors are placed in a metal body deformed to form a wire or tape and heated to form a superconducting article. The fine powders permit a substantial reduction in heat treatment time, thus enabling a continuous processing of the powders into superconducting wire, tape or multifilamentary articles by the powder-in-tube process. 3 figs.

Method of producing Pb-stabilized superconductor precursors and method of producing superconductor articles therefrom

DOEpatents

Kroeger, Donald M.; Hsu, Huey S.; Brynestad, Jorulf

1995-01-01

Metal oxide superconductor powder precursors are prepared in an aerosol pyrolysis process. A solution of the metal cations is introduced into a furnace at 600.degree.-1000.degree. C. for 0.1 to 60 seconds. The process produces micron to submicron size powders without the usual loss of the lead stabilizer. The resulting powders have a narrow particle size distribution, a small grain size, and are readily converted to a superconducting composition upon subsequent heat treatment. The precursors are placed in a metal body deformed to form a wire or tape and heated to form a superconducting article. The fine powders permit a substantial reduction in heat treatment time, thus enabling a continuous processing of the powders into superconducting wire, tape or multifilamentary articles by the powder-in-tube process.

Working with argan cake: a new etiology for hypersensitivity pneumonitis.

PubMed

Paris, Christophe; Herin, Fabrice; Reboux, Gabriel; Penven, Emmanuelle; Barrera, Coralie; Guidat, Cécile; Thaon, Isabelle

2015-03-06

Argan is now used worldwide in numerous cosmetic products. Nine workers from a cosmetic factory were examined in our occupational medicine department, following the diagnosis of a case of hypersensitivity pneumonitis (HP) related to handling of argan cakes. Operators were exposed to three forms of argan (crude granulates, powder or liquid) depending on the step of the process. All workers systematically completed standardized questionnaires on occupational and medical history, followed by medical investigations, comprising, in particular, physical examination and chest X-rays, total IgE and a systematic screening for specific serum antibodies directed against the usual microbial agents of domestic and farmer's HP and antigens derived from microbiological culture and extracts of various argan products. Subjects with episodes of flu-like syndrome several hours after handling argan cakes, were submitted to a one-hour challenge to argan cakes followed by physical examination, determination of Carbon Monoxide Diffusing Capacity (DLCO) and chest CT-scan on day 2, and, when necessary, bronchoalveolar lavage on day 4. Six of the nine workers experienced flu-like symptoms within 8 hours after argan handling. After challenge, two subjects presented a significant decrease of DLCO and alveolitis with mild lymphocytosis, and one presented ground glass opacities. These two patients and another patient presented significant arcs to both granulates and non-sterile powder. No reactivity was observed to sterile argan finished product, antigens derived from argan cultures (various species of Bacillus) and Streptomyces marokkonensis (reported in the literature to contaminate argan roots). We report the first evidence of hypersensitivity pneumonitis related to argan powder in two patients. This implies preventive measures to reduce their exposure and clinical survey to diagnose early symptoms. As exposure routes are different and antibodies were observed against argan powder and not the sterile form, consumers using argan-based cosmetics should not be concerned.

Counterflow diffusion flame synthesis of ceramic oxide powders

DOEpatents

Katz, J.L.; Miquel, P.F.

1997-07-22

Ceramic oxide powders and methods for their preparation are revealed. Ceramic oxide powders are obtained using a flame process whereby one or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein the precursors are converted into ceramic oxide powders. The nature of the ceramic oxide powder produced is determined by process conditions. The morphology, particle size, and crystalline form of the ceramic oxide powders may be varied by the temperature of the flame, the precursor concentration ratio, the gas stream and the gas velocity. 24 figs.

Counterflow diffusion flame synthesis of ceramic oxide powders

DOEpatents

Katz, Joseph L.; Miquel, Philippe F.

1997-01-01

Ceramic oxide powders and methods for their preparation are revealed. Ceramic oxide powders are obtained using a flame process whereby one or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein the precursors are converted into ceramic oxide powders. The nature of the ceramic oxide powder produced is determined by process conditions. The morphology, particle size, and crystalline form of the ceramic oxide powders may be varied by the temperature of the flame, the precursor concentration ratio, the gas stream and the gas velocity.

Optimizing Compliance and Thermal Conductivity of Plasma Sprayed Thermal Barrier Coatings via Controlled Powders and Processing Strategies

NASA Astrophysics Data System (ADS)

Tan, Yang; Srinivasan, Vasudevan; Nakamura, Toshio; Sampath, Sanjay; Bertrand, Pierre; Bertrand, Ghislaine

2012-09-01

The properties and performance of plasma-sprayed thermal barrier coatings (TBCs) are strongly dependent on the microstructural defects, which are affected by starting powder morphology and processing conditions. Of particular interest is the use of hollow powders which not only allow for efficient melting of zirconia ceramics but also produce lower conductivity and more compliant coatings. Typical industrial hollow spray powders have an assortment of densities resulting in masking potential advantages of the hollow morphology. In this study, we have conducted process mapping strategies using a novel uniform shell thickness hollow powder to control the defect microstructure and properties. Correlations among coating properties, microstructure, and processing reveal feasibility to produce highly compliant and low conductivity TBC through a combination of optimized feedstock and processing conditions. The results are presented through the framework of process maps establishing correlations among process, microstructure, and properties and providing opportunities for optimization of TBCs.

Powder Processing of Amorphous Tungsten-bearing Alloys and Composites

DTIC Science & Technology

2015-03-01

8725 John J. Kingman Road, MS-6201 Fort Belvoir, VA 22060-6201 T E C H N IC A L R E P O R T DTRA-TR-14-73 Powder Processing of Amorphous Tungsten...Technology, Boise State University, Army Research Laboratory Project Title: Powder Processing of Amorphous Tungsten-bearing Alloys and Composites...Our year 3 tasks, as laid out in the project proposal, were to 1) Consolidate amorphous or nanocrystalline powder blends 2) Mechanical testing

The Development of an Environmentally Compliant, Multi-Functional Aerospace Coating Using Molecular- and Nano-Engineering Methods

DTIC Science & Technology

2006-10-02

Al -TM-RE) alloy which could by spray applied using various deposition routes or deposited as a powder that is...corrosion properties of various spray deposited alloys from their properties as defective coatings on 2024-T3. "* HVOF spray deposited and cold spray ...layer. "* A method has been developed to distinguish the intrinsic corrosion properties of various spray deposited

30. BUILDING NO. 527, DEHYDRATING PRESSES, LOOKING SOUTH. ALUMINUM NARROWGUAGE ...

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

30. BUILDING NO. 527, DEHYDRATING PRESSES, LOOKING SOUTH. ALUMINUM NARROW-GUAGE GONDOLA CAR IN LEFT BACKGROUND BROUGHT MOISTENED GUN COTTON FROM REST HOUSE (BUILDING NO. 320-B) IN CANS. (ONE OF THESE CANS IS ON UNLOADING PLATFORM RUNNING BESIDE PRESSES). CONTENTS OF CANS WERE UNLOADED INTO PRESSES BY HAND. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

New chemistry of transition metal oxyhydrides

PubMed Central

Kobayashi, Yoji; Hernandez, Olivier; Tassel, Cédric; Kageyama, Hiroshi

2017-01-01

Abstract In this review we describe recent advances in transition metal oxyhydride chemistry obtained by topochemical routes, such as low temperature reduction with metal hydrides, or high-pressure solid-state reactions. Besides the crystal chemistry, magnetic and transport properties of the bulk powder and epitaxial thin film samples, the remarkable lability of the hydride anion is particularly highlighted as a new strategy to discover unprecedented mixed anion materials. PMID:29383042

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

Pązik, Robert, E-mail: R.Pazik@int.pan.wroc.pl; Zawisza, Katarzyna; Wroclaw University, Faculty of Chemistry, F. Joliot-Curie 14, 50-338 Wroclaw

Graphical abstract: Display Omitted Highlights: ► Convenient citric route was used for preparation of the Ca{sub 9}Al(PO{sub 4}){sub 7}:Eu{sup 3+} powders. ► We found that the thermal dependency of the Eu{sup 3+} emission shows two different temperature ranges. ► 80% of Eu{sup 3+} luminescence intensity is kept at 430 K. ► The possible quenching pathways were constructed using simplified one coordinate energy diagram. -- Abstract: The citric route was employed for synthesis of the pure phase Ca{sub 9}Al(PO{sub 4}){sub 7}:Eu{sup 3+} (CAlP:Eu{sup 3+}) powders as an attractive alternative to the solid state reaction (no need of multistep and long thermalmore » treatment). Structural properties of the final product were studied by means of X-ray diffraction as well as Rietveld refinement was conducted in order to calculate the cell parameters. The thermal behavior of the emission was studied using excitation line well matched with the {sup 7}F{sub 0} → {sup 5}D{sub 4} absorption band covering broad range of temperature. Activation energy was estimated to be equal to 10,550 cm{sup −1}. The thermal behavior of the Eu{sup 3+} luminescence in CAlP crystal lattice shown that the almost 80% of intensity is kept up to 430 K.« less

Synthesis of nanocrystalline zirconia by amorphous citrate route: structural and thermal (HTXRD) studies

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

Bhagwat, Mahesh; Ramaswamy, Veda

Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less

Synthesis of inorganic fullerene-like WS2 nanoparticles and their lubricating performance

NASA Astrophysics Data System (ADS)

Yang, Haibin; Liu, Shikai; Li, Jixue; Li, Minghui; Peng, Gang; Zou, Guangtian

2006-03-01

A facile, large-scale and low-cost route was used to synthesize inorganic fullerene-like (IF) WS2 nanoparticles by the reaction of sulfur powder (S) and as-prepared WO3 nanoparticles in a hydrogen atmosphere at a heating temperature of 500-650 °C. The as-synthesized IF-WS2 nanoparticles are of a closed hollow cage structure with an average size of about 50 nm. The composition, morphology and structure of the products were characterized by XRD, TEM, FE-SEM, and HRTEM. The influences of the main reaction conditions were investigated and the possible growth mechanism are proposed. It is worth noting that through changing the amount of as-prepared composite powder (WO3 and S) and the content of hydrogen, yields of IF-WS2 in larger scales can accordingly be easily obtained, and such a synthetic route may also be used in the synthesis of other transition IF metal dichalcogenides. Furthermore, tribological experiments emphasized the important role played by these as-synthesized IF-WS2 nanoparticles in providing excellent lubricating performance, which may bring a much brighter future for their applications in the lubricating field, or even arouse great interest of both scientists and industrialists for their many other important applications.

Corrosion Screening of EV31A Magnesium and Other Magnesium Alloys using Laboratory-Based Accelerated Corrosion and Electro-Chemical Methods

DTIC Science & Technology

2014-07-01

corrosion studies (16). A schematic of the SWAP process and example of the powder produced is included in figure 4. This alloy contains amounts of Al ...advanced powder -based alloy and ZAXE1711 (both from Japan) were produced using a Spinning Water Atomization Process (SWAP) to yield powder particles with...and ZAXE1711 Mg alloy powders and (b) morphology of coarse Mg alloy powder prepared by SWAP

Preparation of lead-zirconium-titanium film and powder by electrodeposition

DOEpatents

Bhattacharya, Raghu N.; Ginley, David S.

1995-01-01

A process for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications.

Preparation of lead-zirconium-titanium film and powder by electrodeposition

DOEpatents

Bhattacharya, R.N.; Ginley, D.S.

1995-10-31

A process is disclosed for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications. 4 figs.

Preparation of superconductor precursor powders

DOEpatents

Bhattacharya, Raghunath; Blaugher, Richard D.

1995-01-01

A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals, such as nitrate salts of thallium, barium, calcium, and copper, which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of thallium in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

Design of a uranium-dioxide powder spheroidization system by plasma processing

NASA Astrophysics Data System (ADS)

Cavender, Daniel

The plasma spheroidization system (PSS) is the first process in the development of a tungsten-uranium dioxide (W-UO2) ceramic-metallic (cermet) fuel for nuclear thermal rocket (NTR) propulsion. For the purposes of fissile fuel retention, UO2 spheroids ranging in size from 50 - 100 micrometers (μm) in diameter will be encapsulated in a tungsten shell. The PSS produces spherical particles by melting angular stock particles in an argon-hydrogen plasma jet where they become spherical due to surface tension. Surrogate CeO 2 powder was used in place of UO2 for system and process parameter development. Stock and spheroidized powders were micrographed using optical and scanning electron microscopy and evaluated by statistical methods to characterize and compare the spherocity of pre and post process powders. Particle spherocity was determined by irregularity parameter. Processed powders showed a statistically significant improvement in spherocity, with greater that 60% of the examined particles having an irregularity parameter of equal to or lower than 1.2, compared to stock powder.

Densification of powder metallurgy billets by a roll consolidation technique

NASA Technical Reports Server (NTRS)

Sellman, W. H.; Weinberger, W. R.

1973-01-01

Container design is used to convert partially densified powder metallurgy compacts into fully densified slabs in one processing step. Technique improves product yield, lowers costs and yields great flexibility in process scale-up. Technique is applicable to all types of fabricable metallic materials that are produced from powder metallurgy process.

Improved Properties of Pb Based BLZT Ferroelectric Ceramics

NASA Astrophysics Data System (ADS)

Kumar, Parveen; Singh, Sangeeta; Juneja, J. K.; Raina, K. K.; Prakash, Chandra

2011-11-01

Present report is concerning with investigation of effect of different sintering profiles on Pb based BLZT ceramics. The material powder of selected composition (Ba0.795La0.005Pb0.20Ti0.90Zr0.10O3) was prepared by solid state reaction route and then powder was compacted in the form of circular discs. The discs were then sintered at different temperatures (1325 °C for 4h, 1325 °C for 15min+1200 °C for 4h). Improved dielectric and ferroelectric properties were observed for samples sintered at 1200 °C. Shifting in Tc to higher temperature could be related to enhanced tetragonality, which was further confirmed by X-ray diffraction analysis. All these improvements evidences that there is less Pb loss in case of modified sintering profile.

A lucrative chemical processing of bamboo leaf biomass to synthesize biocompatible amorphous silica nanoparticles of biomedical importance

NASA Astrophysics Data System (ADS)

Rangaraj, Suriyaprabha; Venkatachalam, Rajendran

2017-06-01

Synthesis of silica nanoparticles from natural resources/waste via cost effective route is presently one of the anticipating strategies for extensive applications. This study reports the low-cost indigenous production of silica nanoparticles from the leftover of bamboo (leaf biomass) through thermal combustion and alkaline extraction, and examination of physico-chemical properties and yield percentage using comprehensive characterization tools. The outcome of primed silica powder exhibits amorphous particles (average size: 25 nm) with high surface area (428 m2 g-1) and spherical morphology. Despite the yield percentage of silica nanoparticles from bamboo leave ash is 50.2%, which is less than rice husk ask resources (62.1%), the bamboo waste is only an inexpensive resource yielding high purity (99%). Synthesis of silica nanoparticles from natural resources/waste with the help of lucrative route is at present times one of the anticipating strategies for extensive applications. In vitro study on animal cell lines (MG-63) shows non-toxic nature of silica nanoparticles up to 125 µg mL-1. Hence, this study highlights the feasibility for the mass production of silica nanoparticles from bamboo leave waste rather using chemical precursor of silica for drug delivery and other medical applications.

Emulsion Synthesis of Size-Tunable CH3NH3PbBr3 Quantum Dots: An Alternative Route toward Efficient Light-Emitting Diodes.

PubMed

Huang, Hailong; Zhao, Fangchao; Liu, Lige; Zhang, Feng; Wu, Xian-gang; Shi, Lijie; Zou, Bingsuo; Pei, Qibing; Zhong, Haizheng

2015-12-30

We report a facile nonaqueous emulsion synthesis of colloidal halide perovskite quantum dots by controlled addition of a demulsifier into an emulsion of precursors. The size of resulting CH3NH3PbBr3 quantum dots can be tuned from 2 to 8 nm by varying the amount of demulsifier. Moreover, this emulsion synthesis also allows the purification of these quantum dots by precipitation from the colloidal solution and obtains solid-state powder which can be redissolved for thin film coating and device fabrication. The photoluminescence quantum yields of the quantum dots is generally in the range of 80-92%, and can be well-preserved after purification (∼80%). Green light-emitting diodes fabricated comprising a spin-cast layer of the colloidal CH3NH3PbBr3 quantum dots exhibited maximum current efficiency of 4.5 cd/A, power efficiency of 3.5 lm/W, and external quantum efficiency of 1.1%. This provides an alternative route toward high efficient solution-processed perovskite-based light-emitting diodes. In addition, the emulsion synthesis is versatile and can be extended for the fabrication of inorganic halide perovskite colloidal CsPbBr3 nanocrystals.

Achieving high strength and high ductility in metal matrix composites reinforced with a discontinuous three-dimensional graphene-like network.

PubMed

Zhang, Xiang; Shi, Chunsheng; Liu, Enzuo; He, Fang; Ma, Liying; Li, Qunying; Li, Jiajun; Bacsa, Wolfgang; Zhao, Naiqin; He, Chunnian

2017-08-24

Graphene or graphene-like nanosheets have been emerging as an attractive reinforcement for composites due to their unique mechanical and electrical properties as well as their fascinating two-dimensional structure. It is a great challenge to efficiently and homogeneously disperse them within a metal matrix for achieving metal matrix composites with excellent mechanical and physical performance. In this work, we have developed an innovative in situ processing strategy for the fabrication of metal matrix composites reinforced with a discontinuous 3D graphene-like network (3D GN). The processing route involves the in situ synthesis of the encapsulation structure of 3D GN powders tightly anchored with Cu nanoparticles (NPs) (3D GN@Cu) to ensure mixing at the molecular level between graphene-like nanosheets and metal, coating of Cu on the 3D GN@Cu (3D GN@Cu@Cu), and consolidation of the 3D GN@Cu@Cu powders. This process can produce GN/Cu composites on a large scale, in which the in situ synthesized 3D GN not only maintains the perfect 3D network structure within the composites, but also has robust interfacial bonding with the metal matrix. As a consequence, the as-obtained 3D GN/Cu composites exhibit exceptionally high strength and superior ductility (the uniform and total elongation to failure of the composite are even much higher than the unreinforced Cu matrix). To the best of our knowledge, this work is the first report validating that a discontinuous 3D graphene-like network can simultaneously remarkably enhance the strength and ductility of the metal matrix.

Consolidation of Hierarchy-Structured Nanopowder Agglomerates and Its Application to Net-Shaping Nanopowder Materials

PubMed Central

Lee, Jai-Sung; Choi, Joon-Phil; Lee, Geon-Yong

2013-01-01

This paper provides an overview on our recent investigations on the consolidation of hierarchy-structured nanopowder agglomerates and related applications to net-shaping nanopowder materials. Understanding the nanopowder agglomerate sintering (NAS) process is essential to processing of net-shaped nanopowder materials and components with small and complex shape. The key concept of the NAS process is to enhance material transport through controlling the powder interface volume of nanopowder agglomerates. Based upon this concept, we have suggested a new idea of full density processing for fabricating micro-powder injection molded part using metal nanopowder agglomerates produced by hydrogen reduction of metal oxide powders. Studies on the full density sintering of die compacted- and powder injection molded iron base nano-agglomerate powders are introduced and discussed in terms of densification process and microstructure. PMID:28788317

Reducing metal alloy powder costs for use in powder bed fusion additive manufacturing: Improving the economics for production

NASA Astrophysics Data System (ADS)

Medina, Fransisco

Titanium and its associated alloys have been used in industry for over 50 years and have become more popular in the recent decades. Titanium has been most successful in areas where the high strength to weight ratio provides an advantage over aluminum and steels. Other advantages of titanium include biocompatibility and corrosion resistance. Electron Beam Melting (EBM) is an additive manufacturing (AM) technology that has been successfully applied in the manufacturing of titanium components for the aerospace and medical industry with equivalent or better mechanical properties as parts fabricated via more traditional casting and machining methods. As the demand for titanium powder continues to increase, the price also increases. Titanium spheroidized powder from different vendors has a price range from 260/kg-450/kg, other spheroidized alloys such as Niobium can cost as high as $1,200/kg. Alternative titanium powders produced from methods such as the Titanium Hydride-Dehydride (HDH) process and the Armstrong Commercially Pure Titanium (CPTi) process can be fabricated at a fraction of the cost of powders fabricated via gas atomization. The alternative powders can be spheroidized and blended. Current sectors in additive manufacturing such as the medical industry are concerned that there will not be enough spherical powder for production and are seeking other powder options. It is believed the EBM technology can use a blend of spherical and angular powder to build fully dense parts with equal mechanical properties to those produced using traditional powders. Some of the challenges with angular and irregular powders are overcoming the poor flow characteristics and the attainment of the same or better packing densities as spherical powders. The goal of this research is to demonstrate the feasibility of utilizing alternative and lower cost powders in the EBM process. As a result, reducing the cost of the raw material to reduce the overall cost of the product produced with AM. Alternative powders can be made by blending or re-spheroidizing HDH and CPTi powders. Machine modifications were performed to allow the testing and manufacturing with these low cost alternative powders. A comparison was made between alternative powders and gas atomized powders. Powders were compared in terms of morphology and at the microstructural level. Flowability of different powder blends was also measured. Finally, a comparison of parts fabricated from the multiple powder blends and gas atomized powder was made. It has been demonstrated that powder blending can produce fully dense parts in the Arcam system by utilizing the double melt technique or HIPing the built pars. The double melt technique increased the density of the sample part and modified the microstructure into finer martensitic grains. The HIP process can make a part fully dense regardless of what percentage of HDH powder blending is used. The HIP process yielded the same microstructure, regardless of the grain structure it started with. This research allows for the reduction of costs using titanium powders in the EBM system, but can also be implemented with more costly elements and alloys using other metal AM technologies. This includes niobium, tantalum, and nickel-based superalloys for use in various industries.

Argon-shielded hot pressing of titanium alloy (Ti6Al4V) powders.

PubMed

Gronostajski, Zbigniew; Bandoła, P; Skubiszewski, T

2010-01-01

The paper presents the method of the argon - shielded hot pressing of titanium alloy (Ti6A14V) powder (used in medical industry). The powders produced in the GA (gas atomization) process and in the HDH (hydride - dehydride) process were used in the experiments. A pressing process was conducted at a temperature of 800-850 degrees C for different lengths of time. An unoxidized sintered material, nearly as dense as a solid material and having a lamellar structure (alpha+beta), was obtained from the titanium alloy powder produced in the HDH process.

Cerebroprotective Actions of Triticum aestivum Linn Powder and Bauhinia purpurea Flower Powder in Surgically Induced Cerebral Infraction in Rats.

PubMed

Annapurna, Akula; Vishala, Thonangi C; Bitra, Veera R; Rapaka, Deepthi; Shaik, Asmath

2018-01-01

The prime objective of this study is to evaluate the cerebroprotective actions of Triticum aestivum (wheatgrass) powder and Bauhinia purpurea flower (dev kanchan) powder against the experimentally induced global ischemia reperfusion injury in rats. In the first phase of the studies, 1 h before the surgical procedure, the Wistar rats were orally served with varied doses of wheatgrass powder (5, 10, 30, and 100 μg/kg) and Bauhinia flower powder (30, 100, 200, and 300 μg/kg), respectively. The ischemia was induced by 30-min bilateral carotid artery occlusion in succession to reperfusion for 4 h. It was proved that the wheatgrass powder and Bauhinia flower powder yielded a significant, dose-dependent cerebroprotection in terms of reduction in cerebral infarct size when compared with the control group. Coming to the second phase of the studies, a certain potential dose of 10 μg/kg of wheatgrass and 200 μg/kg of Bauhinia flower powders was selected keeping the protective action in view, and the animals were treated for 15 days. The major findings of the study are that wheatgrass and Bauhinia flower powders significantly augmented the magnitude of the antioxidant enzymes, viz., super oxide dismutase and catalase, and further reduced the levels of lipid peroxidation. The present study clearly showed that the wheatgrass powder and Bauhinia flower powder possess significant antioxidant properties that may act as a key ingredient in various ayurvedic preparations for the treatment of various diseases like cerebral ischemic reperfusion injury. The wheat grass contains high amount of bioflavonoids, alkaloids, SOD etc which are responsible for anti oxidant activity.The Bauhinia purpurea contains glycosides, flavonoids and also plays a major role in DPPH activity which is responsible for anti oxidant activity.The wheat grass (10 mg/kg) and bauhinia (200 mg/kg) significantly(P < 0.0001) reduced the percentage of infract size when compared to Ischemia reperfusion control group.The wheat grass (10 mg/kg) and bauhinia (200 mg/kg) significantly (P <0.0001) reduced the lipid peroxidation (MDA) and increased SOD and Catalase. Abbreviations used: BCAO: Bilateral Carotid Artery Occlusion, MCA: middle cerebral artery, ROS: reactive oxygen species, SCMC: Sodium carboxy methyl cellulose, p.o: Per oral route, T.T.C: Triphenyl tetrazolium chloride, MDA: Malondialdehyde, SOD: Super oxide dismutase.

Cerebroprotective Actions of Triticum aestivum Linn Powder and Bauhinia purpurea Flower Powder in Surgically Induced Cerebral Infraction in Rats

PubMed Central

Annapurna, Akula; Vishala, Thonangi C.; Bitra, Veera R.; Rapaka, Deepthi; Shaik, Asmath

2017-01-01

Objective: The prime objective of this study is to evaluate the cerebroprotective actions of Triticum aestivum (wheatgrass) powder and Bauhinia purpurea flower (dev kanchan) powder against the experimentally induced global ischemia reperfusion injury in rats. Materials and Methods: In the first phase of the studies, 1 h before the surgical procedure, the Wistar rats were orally served with varied doses of wheatgrass powder (5, 10, 30, and 100 μg/kg) and Bauhinia flower powder (30, 100, 200, and 300 μg/kg), respectively. The ischemia was induced by 30-min bilateral carotid artery occlusion in succession to reperfusion for 4 h. It was proved that the wheatgrass powder and Bauhinia flower powder yielded a significant, dose-dependent cerebroprotection in terms of reduction in cerebral infarct size when compared with the control group. Coming to the second phase of the studies, a certain potential dose of 10 μg/kg of wheatgrass and 200 μg/kg of Bauhinia flower powders was selected keeping the protective action in view, and the animals were treated for 15 days. Results: The major findings of the study are that wheatgrass and Bauhinia flower powders significantly augmented the magnitude of the antioxidant enzymes, viz., super oxide dismutase and catalase, and further reduced the levels of lipid peroxidation. Conclusions: The present study clearly showed that the wheatgrass powder and Bauhinia flower powder possess significant antioxidant properties that may act as a key ingredient in various ayurvedic preparations for the treatment of various diseases like cerebral ischemic reperfusion injury. SUMMARY The wheat grass contains high amount of bioflavonoids, alkaloids, SOD etc which are responsible for anti oxidant activity.The Bauhinia purpurea contains glycosides, flavonoids and also plays a major role in DPPH activity which is responsible for anti oxidant activity.The wheat grass (10 mg/kg) and bauhinia (200 mg/kg) significantly(P < 0.0001) reduced the percentage of infract size when compared to Ischemia reperfusion control group.The wheat grass (10 mg/kg) and bauhinia (200 mg/kg) significantly (P <0.0001) reduced the lipid peroxidation (MDA) and increased SOD and Catalase. Abbreviations used: BCAO: Bilateral Carotid Artery Occlusion, MCA: middle cerebral artery, ROS: reactive oxygen species, SCMC: Sodium carboxy methyl cellulose, p.o: Per oral route, T.T.C: Triphenyl tetrazolium chloride, MDA: Malondialdehyde, SOD: Super oxide dismutase. PMID:29491626

Kinetic analysis of MgB2 layer formation in advanced internal magnesium infiltration (AIMI) processed MgB2 wires

PubMed Central

Li, G. Z.; Sumption, M. D.; Collings, E. W.

2015-01-01

Significantly enhanced critical current density (Jc) for MgB2 superconducting wires can be obtained following the advanced internal Mg infiltration (AIMI) route. But unless suitable precautions are taken, the AIMI-processed MgB2 wires will exhibit incomplete MgB2 layer formation, i.e. reduced superconductor core size and hence suppressed current-carrying capability. Microstructural characterization of AIMI MgB2 wires before and after the heat treatment reveals that the reaction mechanism changes from a “Mg infiltration-reaction” at the beginning of the heat treatment to a “Mg diffusion-reaction” once a dense MgB2 layer is formed. A drastic drop in the Mg transport rate from infiltration to diffusion causes the termination of the MgB2 core growth. To quantify this process, a two-stage kinetic model is built to describe the MgB2 layer formation and growth. The derived kinetic model and the associated experimental observations indicate that fully reacted AIMI-processed MgB2 wires can be achieved following the optimization of B particle size, B powder packing density, MgB2 reaction activation energy and its response to the additions of dopants. PMID:26973431

Mesoporous Titania Powders: The Role of Precursors, Ligand Addition and Calcination Rate on Their Morphology, Crystalline Structure and Photocatalytic Activity

PubMed Central

Masolo, Elisabetta; Meloni, Manuela; Garroni, Sebastiano; Mulas, Gabriele; Enzo, Stefano; Baró, Maria Dolors; Rossinyol, Emma; Rzeszutek, Agnieszka; Herrmann-Geppert, Iris; Pilo, Maria

2014-01-01

We evaluate the influence of the use of different titania precursors, calcination rate, and ligand addition on the morphology, texture and phase content of synthesized mesoporous titania samples, parameters which, in turn, can play a key role in titania photocatalytic performances. The powders, obtained through the evaporation-induced self-assembly method, are characterized by means of ex situ X-Ray Powder Diffraction (XRPD) measurements, N2 physisorption isotherms and transmission electron microscopy. The precursors are selected basing on two different approaches: the acid-base pair, using TiCl4 and Ti(OBu)4, and a more classic route with Ti(OiPr)4 and HCl. For both precursors, different specimens were prepared by resorting to different calcination rates and with and without the addition of acetylacetone, that creates coordinated species with lower hydrolysis rates, and with different calcination rates. Each sample was employed as photoanode and tested in the water splitting reaction by recording I-V curves and comparing the results with commercial P25 powders. The complex data framework suggests that a narrow pore size distribution, due to the use of acetylacetone, plays a major role in the photoactivity, leading to a current density value higher than that of P25. PMID:28344237

Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al₂O₃ Nanocomposite Synthesized by Ball Milling and Powder Metallurgy.

PubMed

Toozandehjani, Meysam; Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

2017-10-26

The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al₂O₃ (Al-5Al₂O₃) has been investigated. Al-5Al₂O₃ nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al₂O₃ nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness ( HV ), nano-hardness ( HN ), and Young's modulus ( E ) of Al-5Al₂O₃ nanocomposites. HV , HN , and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively.

Recycled tetrahedron-like CuCl from waste Cu scraps for lithium ion battery anode.

PubMed

Hou, Hongying; Yao, Yuan; Liu, Song; Duan, Jixiang; Liao, Qishu; Yu, Chengyi; Li, Dongdong; Dai, Zhipeng

2017-07-01

The wide applications of metal Cu inevitably resulted in a large quantity of waste Cu materials. In order to recover the useful Cu under the mild conditions and reduce the environmental emission, waste Cu scraps were recycled in the form of CuCl powders with high economic value added (EVA) via the facile hydrothermal route. The recycled CuCl powders were characterized in terms of scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The results suggested that the recycled CuCl powders consisted of many regular tetrahedron-like micro-particles. Furthermore, in order to reduce the cost of lithium ion battery (LIB) anode and build the connection of waste Cu scraps and LIB, the recycled CuCl powders were evaluated as the anode active material of LIB. As expected, the reversible discharge capacity was about 171.8mAh/g at 2.0C even after 50 cycles, implying the satisfactory cycle stability. Clearly, the satisfactory results may open a new avenue to develop the circular economy and the sustainable energy industry, which would be very important in terms of both the resource recovery and the environmental protection. Copyright © 2017. Published by Elsevier Ltd.

Strain Hardening Behaviour and Its Effect on Properties of ZrB2 Reinforced Al Composite Prepared by Powder Metallurgy Technique

NASA Astrophysics Data System (ADS)

Kaku, Sai Mahesh Yadav; Khanra, Asit Kumar; Davidson, M. J.

2018-04-01

Strain hardening behaviour has significant effect on altering the properties of materials. In the present study, Al-ZrB2 metal matrix composites are made through powder metallurgy route. Incremental weight percentage (wt%) of ZrB2 (0, 2, 4 and 6 wt%) are added to Aluminium matrix to produce different composites. The homogenous powder mixture is compacted and pressurelessly sintered. Sintering of composites is performed over a range of 450-575 °C. The optimized sintered condition is observed at 550 °C for 1 h in controlled atmosphere (argon gas flow). The sintered compacts are strained in incremental steps in different levels up to failure. A visible crack on the bulge of the powder preform is considered as the failure. Composites are strain hardened up to failure. To evaluate the effect of temperature on strain hardening, strain hardening is carried out at different temperatures. Composites are densified with the extent of straining and hardness increases with the increase of strain. Hardness increase with the increase in temperature is maintained during strain hardening. To evaluate the corrosion behaviour of Al-ZrB2 composite, potentiodynamic polarization study are performed on the strained composites. Corrosion rate decrease with the extent of straining.

Preparation of transparent conductors ferroelectric memory materials and ferrites

DOEpatents

Bhattacharya, Raghu Nath; Ginley, David S.

1998-01-01

A process for the preparation by electrodeposition of metal oxide film and powder compounds for ferroelectric memory materials and ferrites wherein the metal oxide includes a plurality of metals. The process comprises providing an electrodeposition bath, providing soluble salts of the metals to this bath, electrically energizing the bath to thereby cause formation of a recoverable film of metal on the electrode, recovering the resultant film as a film or a powder, and recovering powder formed on the floor of the bath. The films and powders so produced are subsequently annealed to thereby produce metal oxide for use in electronic applications. The process can be employed to produce metal-doped metal oxide film and powder compounds for transparent conductors. The process for preparation of these metal-doped metal oxides follows that described above.

Interactions and Supramolecular Organization of Sulfonated Indigo and Thioindigo Dyes in Layered Hydroxide Hosts.

PubMed

Costa, Ana L; Gomes, Ana C; Pereira, Ricardo C; Pillinger, Martyn; Gonçalves, Isabel S; Pineiro, Marta; Seixas de Melo, J Sérgio

2018-01-09

Supramolecularly organized host-guest systems have been synthesized by intercalating water-soluble forms of indigo (indigo carmine, IC) and thioindigo (thioindigo-5,5'-disulfonate, TIS) in zinc-aluminum-layered double hydroxides (LDHs) and zinc-layered hydroxide salts (LHSs) by coprecipitation routes. The colors of the isolated powders were dark blue for hybrids containing only IC, purplish blue or dark lilac for cointercalated samples containing both dyes, and ruby/wine for hybrids containing only TIS. The as-synthesized and thermally treated materials were characterized by Fourier transform infrared, Fourier transform Raman, and nuclear magnetic resonance spectroscopies, powder X-ray diffraction, scanning electron microscopy, and elemental and thermogravimetric analyses. The basal spacings found for IC-LDH, TIS-LDH, IC-LHS, and TIS-LHS materials were 21.9, 21.05, 18.95, and 21.00 Å, respectively, with intermediate spacings being observed for the cointercalated samples that either decreased (LDHs) or increased (LHSs) with increasing TIS content. UV-visible and fluorescence spectroscopies (steady-state and time-resolved) were used to probe the molecular distribution of the immobilized dyes. The presence of aggregates together with the monomer units is suggested for IC-LDH, whereas for TIS-LDH, IC-LHS, and TIS-LHS, the dyes are closer to the isolated situation. Accordingly, while emission from the powder H 2 TIS is strongly quenched, an increment in the emission of about 1 order of magnitude was observed for the TIS-LDH/LHS hybrids. Double-exponential fluorescence decays were obtained and associated with two monomer species interacting differently with cointercalated water molecules. The incorporation of both TIS and IC in the LDH and LHS hosts leads to an almost complete quenching of the fluorescence, pointing to a very efficient energy transfer process from (fluorescent) TIS to (nonfluorescent) IC.

Method to produce nanocrystalline powders of oxide-based phosphors for lighting applications

DOEpatents

Loureiro, Sergio Paulo Martins; Setlur, Anant Achyut; Williams, Darryl Stephen; Manoharan, Mohan; Srivastava, Alok Mani

2007-12-25

Some embodiments of the present invention are directed toward nanocrystalline oxide-based phosphor materials, and methods for making same. Typically, such methods comprise a steric entrapment route for converting precursors into such phosphor material. In some embodiments, the nanocrystalline oxide-based phosphor materials are quantum splitting phosphors. In some or other embodiments, such nanocrystalline oxide based phosphor materials provide reduced scattering, leading to greater efficiency, when used in lighting applications.

2. GENERAL VIEW LOOKING WEST AT BUILDINGS NO. 509, NO. ...

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

2. GENERAL VIEW LOOKING WEST AT BUILDINGS NO. 509, NO. 510, NO. 511 COTTON NITRATION LINE. COTTON STOREHOUSE (BUILDING NO. 509) IS IN BACKGROUND, COTTON PACKER AND DRY HOUSE IN MIDGROUND, NITRATING HOUSE (BUILDING NO. 511) IN FOREGROUND. CONVEYOR CARRIED COTTON FROM BUILDING NO. 510 to BUILDING NO. 511 IN 32 LB. LOTS. - Picatinny Arsenal, 500 Area, Powder Factory & Power House, State Route 15 near I-80, Dover, Morris County, NJ

Effects of process parameters on properties of porous foams formed by laser-assisted melting of steel powder (AISI P21)/foaming agent (ZrH2) mixture

NASA Astrophysics Data System (ADS)

Seo, Ja-Ye; Lee, Ki-Yong; Shim, Do-Sik

2018-01-01

This paper describes the fabrication of lightweight metal foams using the directed energy deposition (DED) method. DED is a highly flexible additive manufacturing process wherein a metal powder mixed with a foaming agent is sprayed while a high-power laser is used to simultaneously melt the powder mixture into layered metal foams. In this study, a mixture of a carbon steel material (P21 powder) and a widely used foaming agent, ZrH2, is used to fabricate metal foams. The effects of various process parameters, such as the laser power, powder feed rate, powder gas flow rate, and scanning speed, on the deposition characteristics (porosity, pore size, and pore distribution) are investigated. The synthesized metal foams exhibit porosities of 10% or lower, and a mean pore area of 7 × 105 μm2. It is observed that the degree of foaming increases in proportion to the laser power to a certain extent. The results also show that the powder feed rate has the most pronounced effect on the porosity of the metal foams, while the powder gas flow rate is the most suitable parameter for adjusting the size of the pores formed within the foams. Further, the scanning speed, which determines the amounts of energy and powder delivered, has a significant effect on the height of the deposits as well as on the properties of the foams. Thus, during the DED process for fabricating metal foams, the pore size and distribution and hence the foam porosity can be tailored by varying the individual process parameters. These findings should be useful as reference data for the design of processes for fabricating porous metallic materials that meet the specific requirements for specialized parts.

Influence of Powder Morphology and Microstructure on the Cold Spray and Mechanical Properties of Ti6Al4V Coatings

NASA Astrophysics Data System (ADS)

Munagala, Venkata Naga Vamsi; Akinyi, Valary; Vo, Phuong; Chromik, Richard R.

2018-06-01

The powder microstructure and morphology has significant influence on the cold sprayability of Ti6Al4V coatings. Here, we compare the cold sprayability and properties of coatings obtained from Ti6Al4V powders of spherical morphology (SM) manufactured using plasma gas atomization and irregular morphology (IM) manufactured using the Armstrong process. Coatings deposited using IM powders had negligible porosity and better properties compared to coatings deposited using SM powders due to higher particle impact velocities, porous surface morphology and more deformable microstructure. To evaluate the cohesive strength, multi-scale indentation was performed and hardness loss parameter was calculated. Coatings deposited using SM powders exhibited poor cohesive strength compared to coatings deposited using IM powders. Images of the residual indents showed de-bonding and sliding of adjacent splats in the coatings deposited using SM powders irrespective of the load. Coatings deposited using IM powders showed no evidence of de-bonding at low loads. At high loads, splat de-bonding was observed resulting in hardness loss despite negligible porosity. Thus, while the powders from Armstrong process lead to a significant improvement in sprayability and coating properties, further optimization of powder and cold spray process will be required as well as consideration of post-annealing treatments to obtain acceptable cohesive strength.

Mechanochemical processing for metals and metal alloys

DOEpatents

Froes, Francis H.; Eranezhuth, Baburaj G.; Prisbrey, Keith

2001-01-01

A set of processes for preparing metal powders, including metal alloy powders, by ambient temperature reduction of a reducible metal compound by a reactive metal or metal hydride through mechanochemical processing. The reduction process includes milling reactants to induce and complete the reduction reaction. The preferred reducing agents include magnesium and calcium hydride powders. A process of pre-milling magnesium as a reducing agent to increase the activity of the magnesium has been established as one part of the invention.

Computer Vision and Machine Learning for Autonomous Characterization of AM Powder Feedstocks

NASA Astrophysics Data System (ADS)

DeCost, Brian L.; Jain, Harshvardhan; Rollett, Anthony D.; Holm, Elizabeth A.

2017-03-01

By applying computer vision and machine learning methods, we develop a system to characterize powder feedstock materials for metal additive manufacturing (AM). Feature detection and description algorithms are applied to create a microstructural scale image representation that can be used to cluster, compare, and analyze powder micrographs. When applied to eight commercial feedstock powders, the system classifies powder images into the correct material systems with greater than 95% accuracy. The system also identifies both representative and atypical powder images. These results suggest the possibility of measuring variations in powders as a function of processing history, relating microstructural features of powders to properties relevant to their performance in AM processes, and defining objective material standards based on visual images. A significant advantage of the computer vision approach is that it is autonomous, objective, and repeatable.

Thermal aging of melt-spun NdFeB magnetic powder in hydrogen

NASA Astrophysics Data System (ADS)

Pinkerton, Frederick E.; Balogh, Michael P.; Ellison, Nicole; Foto, Aldo; Sechan, Martin; Tessema, Misle M.; Thompson, Margarita P.

2016-11-01

High energy product neodymium-iron-boron (NdFeB) magnets are the premier candidate for demanding electrified vehicle traction motor applications. Injection molded (IM) or compression molded (CM) magnets made using NdFeB powders are promising routes to improve motor efficiency, cost, and manufacturability. However, IM and CM NdFeB magnets are susceptible to substantial thermal aging losses at motor operating temperatures when exposed to the automatic transmission fluid (ATF) used as a lubricant and cooling medium. The intrinsic coercivity Hci of NdFeB IM and CM magnets degrades by as much as 18% when aged for 1000 h in ATF at 150 °C, compared to a 3% loss when aged in air. Here we report aging studies of rapidly quenched NdFeB powder in air, ATF, and H2 gas. Expansion of the NdFeB crystal lattice in both ATF and H2 identified hydrogen dissociated from the ATF during aging and diffused into the primary NdFeB phase as the probable cause of the coercivity loss of IM and CM magnets.

Mechanically activated synthesis of PZT and its electromechanical properties

NASA Astrophysics Data System (ADS)

Liu, X.; Akdogan, E. K.; Safari, A.; Riman, R. E.

2005-08-01

Mechanical activation was successfully used to synthesize nanostructured phase-pure Pb(Zr0.7Ti0.3)O3 (PZT) powders. Lead zirconium titanium (PbZrTi) hydrous oxide precursor, synthesized from chemical co-precipitation, was mechanically activated in a NaCl matrix. The synthesized PZT particles were characterized by using X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, laser-light diffraction, and nitrogen adsorption. Thermogravimetric analysis and differential thermal analysis were used to monitor dehydration and phase transformation of PbZrTi hydrous oxide precursor during mechanical activation. The best mechanical activation conditions corresponded to mechanically activating PbZrTi hydrous oxide precursor in a NaCl matrix with a NaCl/precursor weight ratio of 4:1 for 8 h. These conditions resulted in a dispersible phase-pure PZT powder with a median secondary-particle size of ˜110 nm. The properties of PZT 70/30 from mechanically activated powder, as measured on discs sintered at 1150 °C for 2 h, were found to be in close conformity to those obtained by a conventional mixed oxide solid state reaction route.

Synthesis of cerium oxide (CeO 2) by co-precipitation for application as a reference material for X-ray powder diffraction peak widths

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

de Lima Batista, Anderson Márcio; Miranda, Marcus Aurélio Ribeiro; Martins, Fátima Itana Chaves Custódio

Several methods can be used to obtain, from powder diffraction patterns, crystallite size and lattice strain of polycrystalline samples. Some examples are the Scherrer equation, Williamson–Hall plots, Warren/Averbach Fourier decomposition, Whole Powder Pattern Modeling, and Debye function analysis. To apply some of these methods, it is necessary to remove the contribution of the instrument to the widths of the diffraction peaks. Nowadays, one of the main samples used for this purpose is the LaB6 SRM660b commercialized by the National Institute of Standard Technology; the width of the diffraction peak of this sample is caused only by the instrumental apparatus. However,more » this sample can be expensive for researchers in developing countries. In this work, the authors present a simple route to obtain micron-sized polycrystalline CeO 2that have a full width at half maximum comparable with the SRM660b and therefore it can be used to remove instrumental broadening.« less

Ta2O5 nanowires: a novel synthetic method and their solar energy utilization.

PubMed

Lü, Xujie; Ding, Shangjun; Lin, Tianquan; Mou, Xinliang; Hong, Zhanglian; Huang, Fuqiang

2012-01-14

Single-crystalline uniform Ta(2)O(5) nanowires are prepared by a novel synthetic route. The formation of the nanowires involves an oriented attachment process caused by the reduction of surface energy. The nanowires are successfully applied to photocatalytic H(2) evolution, contaminant degradation, and dye-sensitized solar cells (DSCs). The Ta(2)O(5)-based DSCs reveal a significant photovoltaic response, which has not been reported. As a photocatalyst, the Ta(2)O(5) nanowires possess high H(2) evolution efficiency under Xe lamp irradiation, nearly 27-fold higher than the commercial powders. A better performance of photocatalytic contaminant degradation is also observed. Such improvements are ascribed to better charge transport ability for the single-crystalline wire and a higher potential energy of the conduction band. This new synthetic approach using a water-soluble precursor provides a versatile way to prepare nanostructured metal oxides.

IR-spectroscopical investigations on the glass structure of porous and sintered compacts of colloidal silica gels

NASA Astrophysics Data System (ADS)

Clasen, Rolf; Hornfeck, M.; Theiss, Wolfgang

1991-08-01

The forming and sintering of fumed silica powders is an interesting route for the preparation of large, very pure or doped silica glasses with a precise geometry. The processing from the shaping of a porous compact to the sintering of transparent silica glass can be successfully investigated with optical spectroscopy. As only the dielectric function DF (a dielectric function is the square root of the complex refractive index) characterizes the material, the vibrational bands were calculated from reflectance measurements. In compacts of fine particles, the topology cannot be neglected. Therefore, the models describing topological effects are briefly reviewed. With these model calculations it could be proven that new bands in the compacts and the significant shifts in the reflectance spectra during sintering are mainly caused by topological effects and that changes in the glass structure play only a secondary role.

Process for the synthesis of iron powder

DOEpatents

Not Available

1982-03-06

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder.

Process for the synthesis of iron powder

DOEpatents

Welbon, William W.

1983-01-01

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder.

The Application of Modern Powder Characterisation Methods in Product and Process Development of Solid Dosage Forms.

PubMed

Freeman, Tim; Brockbank, Katrina; Armstrong, Brian

2015-01-01

The pharmaceutical industry still produces the vast majority of their products, from powdered ingredients, in the form of solid doses. Despite their ubiquity, powders are difficult materials to characterise and understand, as evidenced by the frequent problems encountered during manufacture. The reason for this is their complex rheological behaviour coupled with numerous environmental variations, such as humidity. Equally, the range of processes used to manipulate powders subject them to extremes of stress from high compaction loads seen in compactors to the dispersed state seen in fluidised bed dryers. Thus, it is evident that ensuring that the powders characteristics are compatible with the way they are to be processed is a clear prerequisite for today's Quality by Design driven manufacturing. Modern, computer controlled instrumental techniques, including the dynamic, bulk and shear property measurements have enabled direct measurements of a powders response to aeration, consolidation and flow rate - all at low stresses - as well as quantifying shear and bulk properties (such as density, compressibility and permeability). In order to demonstrate how fully characterising a powder can be used in the design, operation and troubleshooting of processes, this paper will present examples of common pharmaceutical unit operations and the different powder characteristics that most influence the performance of each.

The Powdering Process with a Set of Ceramic Mills for Green Tea Promoted Catechin Extraction and the ROS Inhibition Effect.

PubMed

Fujioka, Kouki; Iwamoto, Takeo; Shima, Hidekazu; Tomaru, Keiko; Saito, Hideki; Ohtsuka, Masaki; Yoshidome, Akihiro; Kawamura, Yuri; Manome, Yoshinobu

2016-04-11

For serving green tea, there are two prominent methods: steeping the leaf or the powdered leaf (matcha style) in hot water. The purpose of the present study was to reveal chemical and functional differences before and after the powdering process of green tea leaf, since powdered green tea may contribute to expanding the functionality because of the different ingesting style. In this study, we revealed that the powdering process with a ceramic mill and stirring in hot water increased the average extracted concentration of epigallocatechin gallate (EGCG) by more than three times compared with that in leaf tea using high-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass Spectrometry (LC-MS/MS) analyses. Moreover, powdered green tea has a higher inhibition effect of reactive oxygen species (ROS) production in vitro compared with the same amount of leaf tea. Our data suggest that powdered green tea might have a different function from leaf tea due to the higher catechin contents and particles.

The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

Design of a Uranium Dioxide Spheroidization System

NASA Technical Reports Server (NTRS)

Cavender, Daniel P.; Mireles, Omar R.; Frendi, Abdelkader

2013-01-01

The plasma spheroidization system (PSS) is the first process in the development of tungsten-uranium dioxide (W-UO2) fuel cermets. The PSS process improves particle spherocity and surface morphology for coating by chemical vapor deposition (CVD) process. Angular fully dense particles melt in an argon-hydrogen plasma jet at between 32-36 kW, and become spherical due to surface tension. Surrogate CeO2 powder was used in place of UO2 for system and process parameter development. Particles range in size from 100 - 50 microns in diameter. Student s t-test and hypothesis testing of two proportions statistical methods were applied to characterize and compare the spherocity of pre and post process powders. Particle spherocity was determined by irregularity parameter. Processed powders show great than 800% increase in the number of spherical particles over the stock powder with the mean spherocity only mildly improved. It is recommended that powders be processed two-three times in order to reach the desired spherocity, and that process parameters be optimized for a more narrow particles size range. Keywords: spherocity, spheroidization, plasma, uranium-dioxide, cermet, nuclear, propulsion

Powder Processing of High Temperature Cermets and Carbides at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Salvail, Pat; Panda, Binayak; Hickman, Robert R.

2007-01-01

The Materials and Processing Laboratory at NASA Marshall Space Flight Center is developing Powder Metallurgy (PM) processing techniques for high temperature cermet and carbide material consolidation. These new group of materials would be utilized in the nuclear core for Nuclear Thermal Rockets (NTR). Cermet materials offer several advantages for NTR such as retention of fission products and fuels, better thermal shock resistance, hydrogen compatibility, high thermal conductivity, and high strength. Carbide materials offer the highest operating temperatures but are sensitive to thermal stresses and are difficult to process. To support the effort, a new facility has been setup to process refractory metal, ceramic, carbides and depleted uranium-based powders. The facility inciudes inert atmosphere glove boxes for the handling of reactive powders, a high temperature furnace, and powder processing equipment used for blending, milling, and sieving. The effort is focused on basic research to identify the most promising compositions and processing techniques. Several PM processing methods including Cold and Hot Isostatic Pressing are being evaluated to fabricate samples for characterization and hot hydrogen testing.

A new route for the synthesis of titanium silicalite-1

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

Vasile, Aurelia, E-mail: aurelia_vasile@yahoo.com; Busuioc-Tomoiaga, Alina Maria; Catalysis Research Department, ChemPerformance SRL, Iasi 700337

2012-01-15

Graphical abstract: Well-prepared TS-1 was synthesized by an innovative procedure using inexpensive reagents such as fumed silica and TPABr as structure-directing agent. This is the first time when highly crystalline TS-1 is obtained in basic medium, using sodium hydroxide as HO{sup -} ion source required for the crystallization process. Hydrolysis of titanium source has been prevented by titanium complexation with acetylacetone before structuring gel. Highlights: Black-Right-Pointing-Pointer TS-1 was obtained using cheap reagents as fumed silica and tetrapropylammonium bromide. Black-Right-Pointing-Pointer First time NaOH was used as source of OH{sup -} ions required for crystallization process. Black-Right-Pointing-Pointer The hydrolysis Ti alkoxides wasmore » controlled by Ti complexation with 2,4-pentanedione. -- Abstract: A new and efficient route using inexpensive reagents such as fumed silica and tetrapropylammonium bromide is proposed for the synthesis of titanium silicalite-1. High crystalline titanium silicalite-1 was obtained in alkaline medium, using sodium hydroxide as HO{sup -} ion source required for the crystallization process. Hydrolysis of titanium source with formation of insoluble oxide species was prevented by titanium complexation with before structuring gel. The final solids were fully characterized by powder X-ray diffraction, scanning electron microscopy, Fourier transform infrared, ultraviolet-visible diffuse reflectance, Raman and atomic absorption spectroscopies, as well as nitrogen sorption analysis. It was found that a molar ratio Ti:Si of about 0.04 in the initial reaction mixture is the upper limit to which well formed titanium silicalite-1 with channels free of crystalline or amorphous material can be obtained. Above this value, solids with MFI type structure containing both Ti isomorphously substituted in the network and extralattice anatase nanoparticles inside of channels is formed.« less

Recovery of yttrium from cathode ray tubes and lamps’ fluorescent powders: experimental results and economic simulation

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

Innocenzi, V., E-mail: valentina.innocenzi1@univaq.it; De Michelis, I.; Ferella, F.

2013-11-15

Highlights: • Fluorescent powder of lamps. • Fluorescent powder of cathode ray rubes. • Recovery of yttrium from fluorescent powders. • Economic simulation for the processes to recover yttrium from WEEE. - Abstract: In this paper, yttrium recovery from fluorescent powder of lamps and cathode ray tubes (CRTs) is described. The process for treating these materials includes the following: (a) acid leaching, (b) purification of the leach liquors using sodium hydroxide and sodium sulfide, (c) precipitation of yttrium using oxalic acid, and (d) calcinations of oxalates for production of yttrium oxides. Experimental results have shown that process conditions necessary tomore » purify the solutions and recover yttrium strongly depend on composition of the leach liquor, in other words, whether the powder comes from treatment of CRTs or lamp. In the optimal experimental conditions, the recoveries of yttrium oxide are about 95%, 55%, and 65% for CRT, lamps, and CRT/lamp mixture (called MIX) powders, respectively. The lower yields obtained during treatments of MIX and lamp powders are probably due to the co-precipitation of yttrium together with other metals contained in the lamps powder only. Yttrium loss can be reduced to minimum changing the experimental conditions with respect to the case of the CRT process. In any case, the purity of final products from CRT, lamps, and MIX is greater than 95%. Moreover, the possibility to treat simultaneously both CRT and lamp powders is very important and interesting from an industrial point of view since it could be possible to run a single plant treating fluorescent powder coming from two different electronic wastes.« less

Preparation of transparent conductors ferroelectric memory materials and ferrites

DOEpatents

Bhattacharya, R.N.; Ginley, D.S.

1998-07-28

A process is described for the preparation by electrodeposition of metal oxide film and powder compounds for ferroelectric memory materials and ferrites wherein the metal oxide includes a plurality of metals. The process comprises providing an electrodeposition bath, providing soluble salts of the metals to this bath, electrically energizing the bath to thereby cause formation of a recoverable film of metal on the electrode, recovering the resultant film as a film or a powder, and recovering powder formed on the floor of the bath. The films and powders so produced are subsequently annealed to thereby produce metal oxide for use in electronic applications. The process can be employed to produce metal-doped metal oxide film and powder compounds for transparent conductors. The process for preparation of these metal-doped metal oxides follows that described above.

Ultrasonic hot powder compaction of Ti-6Al-4V.

PubMed

Abedini, Rezvan; Abdullah, Amir; Alizadeh, Yunes

2017-07-01

Power ultrasonic has been recently employed in a wide variety of manufacturing processes among which ultrasonic assisted powder compaction is a promising powder materials processing technique with significant industrial applications. The products manufactured by the powder metallurgy commonly consist of residual porosities, material impurities, structural non-homogeneities and residual stress. In this paper, it is aimed to apply power ultrasonic to the hot consolidation process of Ti-6Al-4V titanium alloy powder in order to improve mechanical properties. To do this, the effects of ultrasonic power and process temperature and pressure were considered and then deeply studied through a series of experiments. It was shown that the addition of ultrasonic vibration leads to a significant improvement in the consolidation performance and the mechanical strength of the fabricated specimens. Copyright © 2017 Elsevier B.V. All rights reserved.

A Design of Experiment approach to predict product and process parameters for a spray dried influenza vaccine.

PubMed

Kanojia, Gaurav; Willems, Geert-Jan; Frijlink, Henderik W; Kersten, Gideon F A; Soema, Peter C; Amorij, Jean-Pierre

2016-09-25

Spray dried vaccine formulations might be an alternative to traditional lyophilized vaccines. Compared to lyophilization, spray drying is a fast and cheap process extensively used for drying biologicals. The current study provides an approach that utilizes Design of Experiments for spray drying process to stabilize whole inactivated influenza virus (WIV) vaccine. The approach included systematically screening and optimizing the spray drying process variables, determining the desired process parameters and predicting product quality parameters. The process parameters inlet air temperature, nozzle gas flow rate and feed flow rate and their effect on WIV vaccine powder characteristics such as particle size, residual moisture content (RMC) and powder yield were investigated. Vaccine powders with a broad range of physical characteristics (RMC 1.2-4.9%, particle size 2.4-8.5μm and powder yield 42-82%) were obtained. WIV showed no significant loss in antigenicity as revealed by hemagglutination test. Furthermore, descriptive models generated by DoE software could be used to determine and select (set) spray drying process parameter. This was used to generate a dried WIV powder with predefined (predicted) characteristics. Moreover, the spray dried vaccine powders retained their antigenic stability even after storage for 3 months at 60°C. The approach used here enabled the generation of a thermostable, antigenic WIV vaccine powder with desired physical characteristics that could be potentially used for pulmonary administration. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Resin-Powder Dispenser

NASA Technical Reports Server (NTRS)

Standfield, Clarence E.

1994-01-01

Resin-powder dispenser used at NASA's Langley Research Center for processing of composite-material prepregs. Dispenser evenly distributes powder (resin polymer and other matrix materials in powder form) onto wet uncured prepregs. Provides versatility in distribution of solid resin in prepreg operation. Used wherever there is requirement for even, continuous distribution of small amount of powder.

Initial Assessment of the Effects of Nonmetallic Inclusions on Fatigue Life of Powder-Metallurgy-Processed Udimet(TM) 720

NASA Technical Reports Server (NTRS)

Gabb, T. P.; Telesman, J.; Kantzos, P. T.; Bonacuse, P. J.; Barrie, R. L.

2002-01-01

The fatigue lives of modern powder metallurgy (PM) disk alloys are influenced by variabilities in alloy microstructure and mechanical properties. These properties can vary due to the different steps of materials/component processing and machining. One of these variables, the presence of nonmetallic inclusions, has been shown to significantly degrade low-cycle fatigue (LCF) life. Nonmetallic inclusions are inherent defects in powder alloys that are a by-product of powder-processing techniques. Contamination of the powder can occur in the melt, during powder atomization, or during any of the various handling processes through consolidation. In modern nickel disk powder processing facilities, the levels of inclusion contamination have been reduced to less than 1 part per million by weight. Despite the efforts of manufacturers to ensure the cleanliness of their powder production processes, the presence of inclusions remains a source of great concern for the designer. the objective of this study was to investigate the effects on fatigue life of these inclusions. Since natural inclusions occur so infrequently, elevated levels of inclusions were carefully introduced in a nickel-based disk superalloy, Udimet 720 (registered trademark of Special Metals Corporation), produced using PM processing. Multiple strain-controlled fatigue tests were then performed on this material at 650 C. Analyses were performed to compare the LCF lives and failure initiation sites as functions of inclusion content and fatigue conditions. A large majority of the failures in specimens with introduced inclusions occurred at cracks initiating from inclusions at the specimen surface. The inclusions could reduce fatigue life by up to 100 times. These effects were found to be dependent on strain range and strain ratio. Tests at lower strain ranges and higher strain ratios produced larger effects of inclusions on life.

Multiple feed powder splitter

DOEpatents

Lewis, Gary K.; Less, Richard M.

2001-01-01

A device for providing uniform powder flow to the nozzles when creating solid structures using a solid fabrication system such as the directed light fabrication (DLF) process. In the DLF process, gas entrained powders are passed through the focal point of a moving high-power laser light which fuses the particles in the powder to a surface being built up in layers. The invention is a device providing uniform flow of gas entrained powders to the nozzles of the DLF system. The device comprises a series of modular splitters which are slidably interconnected and contain an integral flow control mechanism. The device can take the gas entrained powder from between one to four hoppers and split the flow into eight tubular lines which feed the powder delivery nozzles of the DLF system.

Multiple feed powder splitter

DOEpatents

Lewis, Gary K.; Less, Richard M.

2002-01-01

A device for providing uniform powder flow to the nozzles when creating solid structures using a solid fabrication system such as the directed light fabrication (DLF) process. In the DLF process, gas entrained powders are passed through the focal point of a moving high-power laser light which fuses the particles in the powder to a surface being built up in layers. The invention is a device providing uniform flow of gas entrained powders to the nozzles of the DLF system. The device comprises a series of modular splitters which are slidably interconnected and contain an integral flow control mechanism. The device can take the gas entrained powder from between one to four hoppers and split the flow into eight tubular lines which feed the powder delivery nozzles of the DLF system.

Welding of Al6061and Al6082-Cu composite by friction stir processing

NASA Astrophysics Data System (ADS)

Iyer, R. B.; Dhabale, R. B.; Jatti, V. S.

2016-09-01

Present study aims at investigating the influence of process parameters on the microstructure and mechanical properties such as tensile strength and hardness of the dissimilar metal without and with copper powder. Before conducting the copper powder experiments, optimum process parameters were obtained by conducting experiments without copper powder. Taguchi's experimental L9 orthogonal design layout was used to carry out the experiments without copper powder. Threaded pin tool geometry was used for conducting the experiments. Based on the experimental results and Taguchi's analysis it was found that maximum tensile strength of 66.06 MPa was obtained at 1400 rpm spindle speed and weld speed of 20 mm/min. Maximum micro hardness (92 HV) was obtained at 1400 rpm spindle speed and weld speed of 16 mm/min. At these optimal setting of process parameters aluminium alloys were welded with the copper powder. Experimental results demonstrated that the tensile strength (96.54 MPa) and micro hardness (105 HV) of FSW was notably affected by the addition of copper powder when compared with FSW joint without copper powder. Tensile failure specimen was analysed using Scanning Electron Microscopy in order to study the failure mechanism.

The UO2 ex-ADU powder preparation and pellet sintering for optimum efficiency: experimental and modeling studies

NASA Astrophysics Data System (ADS)

Hung, Nguyen Trong; Thuan, Le Ba; Van Tung, Nguyen; Thuy, Nguyen Thanh; Lee, Jin-Young; Jyothi, Rajesh Kumar

2017-12-01

The UO2 nuclear fuel pellet process for light water reactors (LWR) includes the conversion of uranium hexafluoride (UF6) into UO2 powder and the fabrication of UO2 pellets from such UO2 powder. In the paper, studies on UO2 pellet process from ammonium diuranate-derived uranium dioxide powder (UO2 ex-ADU powder) were reported. The UO2 ex-ADU powders were converted from ADU at various temperatures of 973 K, 1023 K and 1073 K and then UO2 pellets prepared from the powders were sintered at temperatures of 1923 K, 1973 K and 2023 K for times of 4 h, 6 h and 8 h. Response surface methodology (RSM) based on quadratic central composite design (CCD) type of face centered (CCF) improved by Box and Hunter was used to model the UO2 pellet process, using MODDE 5.0 software as an assessing tool. On the base of the proposed model, the relationship between the technological parameters and density of the UO2 pellet product was suggested to control the UO2 ex-ADU pellet process as desired levels.

Process for the synthesis of iron powder

DOEpatents

Welbon, W.W.

1983-11-08

A process for preparing iron powder suitable for use in preparing the iron-potassium perchlorate heat-powder fuel mixture used in thermal batteries, comprises preparing a homogeneous, dense iron oxide hydroxide precipitate by homogeneous precipitation from an aqueous mixture of a ferric salt, formic or sulfuric acid, ammonium hydroxide and urea as precipitating agent; and then reducing the dense iron oxide hydroxide by treatment with hydrogen to prepare the iron powder. 2 figs.

Considerations on the construction of a Powder Bed Fusion platform for Additive Manufacturing

NASA Astrophysics Data System (ADS)

Andersen, Sebastian Aagaard; Nielsen, Karl-Emil; Pedersen, David Bue; Nielsen, Jakob Skov

As the demand for moulds and other tools becomes increasingly specific and complex, an additive manufacturing approach to production is making its way to the industry through laser based consolidation of metal powder particles by a method known as powder bed fusion. This paper concerns a variety of design choices facilitating the development of an experimental powder bed fusion machine tool, capable of manufacturing metal parts with strength matching that of conventional manufactured parts and a complexity surpassing that of subtractive processes. To understand the different mechanisms acting within such an experimental machine tool, a fully open and customizable rig is constructed. Emphasizing modularity in the rig, allows alternation of lasers, scanner systems, optical elements, powder deposition, layer height, temperature, atmosphere, and powder type. Through a custom-made software platform, control of the process is achieved, which extends into a graphical user interface, easing adjustment of process parameters and the job file generation.

Modeling of magnetic particle orientation in magnetic powder injection molding

NASA Astrophysics Data System (ADS)

Doo Jung, Im; Kang, Tae Gon; Seul Shin, Da; Park, Seong Jin

2018-03-01

The magnetic micro powder orientation under viscous shear flow has been analytically understood and characterized into a new analytical orientation model for a powder injection molding process. The effects of hydrodynamic force from the viscous flow, external magnetic force and internal dipole-dipole interaction were considered to predict the orientation under given process conditions. Comparative studies with a finite element method proved the calculation validity with a partial differential form of the model. The angular motion, agglomeration and magnetic chain formation have been simulated, which shows that the effect of dipole-dipole interaction among powders on the orientation state becomes negligible at a high Mason number condition and at a low λ condition (the ratio of external magnetic field strength and internal magnetic moment of powder). Our developed model can be very usefully employed in the process analysis and design of magnetic powder injection molding.

Powder Flux Regulation in the Laser Material Deposition Process

NASA Astrophysics Data System (ADS)

Arrizubieta, Jon Iñaki; Wegener, Maximiliam; Arntz, Kristian; Lamikiz, Aitzol; Ruiz, Jose Exequiel

In the present research work a powder flux regulation system has been designed, developed and validated with the aim of improving the Laser Material Deposition (LMD) process. In this process, the amount of deposited material per substrate surface unit area depends on the real feed rate of the nozzle. Therefore, a regulation system based on a solenoid valve has been installed at the nozzle entrance in order to control the powder flux. The powder flux control has been performed based on the machine real feed rate, which is compared with the programmed feed rate. An instantaneous velocity error is calculated and the powder flow is controlled as a function of this variation using Pulse Width Modulation (PWM) signals. Thereby, in zones where the Laser Material Deposition machine reduces the feed rate due to a trajectory change, powder accumulation can be avoided and the generated clads would present a homogeneous shape.

Experiment Analysis and Modelling of Compaction Behaviour of Ag60Cu30Sn10 Mixed Metal Powders

NASA Astrophysics Data System (ADS)

Zhou, Mengcheng; Huang, Shangyu; Liu, Wei; Lei, Yu; Yan, Shiwei

2018-03-01

A novel process method combines powder compaction and sintering was employed to fabricate thin sheets of cadmium-free silver based filler metals, the compaction densification behaviour of Ag60Cu30Sn10 mixed metal powders was investigated experimentally. Based on the equivalent density method, the density-dependent Drucker-Prager Cap (DPC) model was introduced to model the powder compaction behaviour. Various experiment procedures were completed to determine the model parameters. The friction coefficients in lubricated and unlubricated die were experimentally determined. The determined material parameters were validated by experiments and numerical simulation of powder compaction process using a user subroutine (USDFLD) in ABAQUS/Standard. The good agreement between the simulated and experimental results indicates that the determined model parameters are able to describe the compaction behaviour of the multicomponent mixed metal powders, which can be further used for process optimization simulations.

Bio-inspired piezoelectric artificial hair cell sensor fabricated by powder injection molding

NASA Astrophysics Data System (ADS)

Han, Jun Sae; Oh, Keun Ha; Moon, Won Kyu; Kim, Kyungseop; Joh, Cheeyoung; Seo, Hee Seon; Bollina, Ravi; Park, Seong Jin

2015-12-01

A piezoelectric artificial hair cell sensor was fabricated by the powder injection molding process in order to make an acoustic vector hydrophone. The entire process of powder injection molding was developed and optimized for PMN-PZT ceramic powder. The artificial hair cell sensor, which consists of high aspect ratio hair cell and three rectangular mechanoreceptors, was precisely fabricated through the developed powder injection molding process. The density and the dielectric property of the fabricated sensor shows 98% of the theoretical density and 85% of reference dielectric property of PMN-PZT ceramic powder. With regard to homogeneity, three rectangular mechanoreceptors have the same dimensions, with 3 μm of tolerance with 8% of deviation of dielectric property. Packaged vector hydrophones measure the underwater acoustic signals from 500 to 800 Hz with -212 dB of sensitivity. Directivity of vector hydrophone was acquired at 600 Hz as analyzing phase differences of electric signals.

Influence of Powder Characteristics on Formation of Porosity in Additive Manufacturing of Ti-6Al-4V Components

NASA Astrophysics Data System (ADS)

Iebba, Maurizio; Astarita, Antonello; Mistretta, Daniela; Colonna, Ivano; Liberini, Mariacira; Scherillo, Fabio; Pirozzi, Carmine; Borrelli, Rosario; Franchitti, Stefania; Squillace, Antonino

2017-08-01

This paper aims to study the genesis of defects in titanium components made through two different additive manufacturing technologies: selective laser melting and electron beam melting. In particular, we focussed on the influence of the powders used on the formation of porosities and cavities in the manufactured components. A detailed experimental campaign was carried out to characterize the components made through the two additive manufacturing techniques aforementioned and the powders used in the process. It was found that some defects of the final components can be attributed to internal porosities of the powders used in the manufacturing process. These internal porosities are a consequence of the gas atomization process used for the production of the powders themselves. Therefore, the importance of using tailored powders, free from porosities, in order to manufacture components with high mechanical properties is highlighted.

Influence of small particles inclusion on selective laser melting of Ti-6Al-4V powder

NASA Astrophysics Data System (ADS)

Gong, Haijun; Dilip, J. J. S.; Yang, Li; Teng, Chong; Stucker, Brent

2017-12-01

The particle size distribution and powder morphology of metallic powders have an important effect on powder bed fusion based additive manufacturing processes, such as selective laser melting (SLM). The process development and parameter optimization require a fundamental understanding of the influence of powder on SLM. This study introduces a pre-alloyed titanium alloy Ti-6Al-4V powder, which has a certain amount of small particles, for SLM. The influence of small particle inclusion is investigated through microscopy of surface topography, elemental and microstructural analysis, and mechanical testing, compared to the Ti-6Al-4V powder provided by SLM machine vendor. It is found that the small particles inclusion in Ti-6Al-4V powder has a noticeable effect on extra laser energy absorption, which may develop imperfections and deteriorate the SLM fatigue performance.

Crystallization stabilization mechanism of yttria-doped zirconia by hydrothermal treatment of mechanical mixtures of zirconia xerogel and crystalline yttria

NASA Astrophysics Data System (ADS)

Dell'Agli, G.; Mascolo, G.; Mascolo, M. C.; Pagliuca, C.

2005-06-01

Mechanical mixtures of zirconia xerogel and crystalline Y 2O 3 were hydrothermally treated by microwave and traditional route, respectively. Some mixtures were used either as powders form or as cylindrical compacts isostatically pressed at 150 MPa. The microwave-hydrothermal treatments were performed at 110, 150 and 200 °C for reaction times up to 2 h, whereas the traditional hydrothermal treatments were performed at 110 °C at increasing reaction times up to 7 days. All the treatments were performed in the presence of diluted (0.2 M) or concentrated (2.0 M) solution of (K 2CO 3+KOH) mineralizer. The crystallization-stabilization mechanism of synthesized Y-based zirconia powders and the reaction times for the full crystallization at the low temperature of hydrothermal treatments are discussed.

Relationship of Powder Feedstock Variability to Microstructure and Defects in Selective Laser Melted Alloy 718

NASA Technical Reports Server (NTRS)

Smith, T. M.; Kloesel, M. F.; Sudbrack, C. K.

2017-01-01

Powder-bed additive manufacturing processes use fine powders to build parts layer by layer. For selective laser melted (SLM) Alloy 718, the powders that are available off-the-shelf are in the 10-45 or 15-45 micron size range. A comprehensive investigation of sixteen powders from these typical ranges and two off-nominal-sized powders is underway to gain insight into the impact of feedstock on processing, durability and performance of 718 SLM space-flight hardware. This talk emphasizes an aspect of this work: the impact of powder variability on the microstructure and defects observed in the as-fabricated and full heated material, where lab-scale components were built using vendor recommended parameters. These typical powders exhibit variation in composition, percentage of fines, roughness, morphology and particle size distribution. How these differences relate to the melt-pool size, porosity, grain structure, precipitate distributions, and inclusion content will be presented and discussed in context of build quality and powder acceptance.

Potato powders prepared by successive cooking-process depending on resistant starch content affect the intestinal fermentation in rats.

PubMed

Kawakami, Sakura; Han, Kyu-Ho; Araki, Takahiro; Ohba, Kiyoshi; Wakabayashi, Tatsuya; Shimada, Kenichiro; Fukushima, Michihiro

2017-02-01

The effects of resistant starch (RS) in dry potato powders prepared by various processes on intestinal fermentation in rats were assessed. Rats were fed raw potato powder (RP), blanched potato powder (BP), steamed potato powder (SP), or drum-dried potato powder (DP) for 4 weeks. The cecal RS content was significantly higher in the RP group than in the control diet (CN) group and other dry potato powder groups. Cecum pH was significantly lower in the RP group compared to the CN group, and was also significantly lower than that in the SP, BP, and DP groups. Lactic acid bacteria levels in the RP group were significantly higher than those in the CN group, and levels in the SP group also increased relative to the control group. Lactobacillus levels in the RP group were higher than in the CN and other dry potato powder groups. Cecal short-chain fatty acid (SCFA) concentrations in the RP group followed by the SP group exhibited significantly higher levels relative to the control levels. Dry potato powders containing RS produced during the cooking process may represent a useful food material that increases intestinal concentrations of SCFA and enhances the growth of certain lactic acid bacteria.

Doping effects of Yb 3+ on the crystal structures, nanoparticle properties and electrical behaviors of ZrO 2 derived from a facile urea-based hydrothermal route

NASA Astrophysics Data System (ADS)

Zhang, Ya-Wen; Sun, Xiao; Xu, Gang; Yan, Chun-Hua

2004-06-01

Weakly-agglomerated nanocrystalline (ZrO 2) 1- x(Yb 2O 3) x ( x=0.02-0.2) powders with high surface area (109-151 m 2 g -1) were synthesized by a two-step hydrothermal process in the presence of urea: a stock solution of metal nitrates and urea was heated at 80 °C for 24 h and then at 180 °C for 48 h. For x=0.04-0.2, the as-derived powders were an assembly of uniform nanoparticles with well-defined edges in the size between 6.1-8.4 nm. Before and after calcination at 800 °C, the lattice parameters, microstrain and surface area of the (ZrO 2) 1- x(Yb 2O 3) x samples tended to increase with Yb 3+ concentration; while, the average crystallite size decreased correspondingly. In the Arrhenius plots over the measurement temperature range of 400-800 °C, the bulk ionic conductivity of the compacts sintered at 1400 °C for 24 h showed a maximum value at the composition of x=0.08 in cubic structure, with an activation energy of 0.89 eV. At 800 °C, σb=0.049 S cm -1 for x=0.08.

Monolithic Cu-Cr-Nb Alloys for High Temperature, High Heat Flux Applications

NASA Technical Reports Server (NTRS)

Ellis, David L.; Locci, Ivan E.; Michal, Gary M.; Humphrey, Derek M.

1999-01-01

Work during the prior four years of this grant has resulted in significant advances in the development of Cu-8 Cr4 Nb and related Cu-Cr-Nb alloys. The alloys are nearing commercial use in the Reusable Launch Vehicle (RLV) where they are candidate materials for the thrust cell liners of the aerospike engines being developed by Rocketdyne. During the fifth and final year of the grant, it is proposed to complete development of the design level database of mechanical and thermophysical properties and transfer it to NASA Glenn Research Center and Rocketdyne. The database development work will be divided into three main areas: Thermophysical Database Augmentation, Mechanical Testing and Metallography and Fractography. In addition to the database development, work will continue that is focussed on the production of alternatives to the powder metallurgy alloys currently used. Exploration of alternative alloys will be aimed at both the development of lower cost materials and higher performance materials. A key element of this effort will be the use of Thermo-Calc software to survey the solubility behavior of a wide range of alloying elements in a copper matrix. The ultimate goals would be to define suitable alloy compositions and processing routes to produce thin sheets of the material at either a lower cost, or, with improved mechanical and thermal properties compared to the current Cu-Cr-Nb powder metallurgy alloys.

Formation of quasi-single crystalline porous ZnO nanostructures with a single large cavity

NASA Astrophysics Data System (ADS)

Cho, Seungho; Kim, Semi; Jung, Dae-Won; Lee, Kun-Hong

2011-09-01

We report a method for synthesizing quasi-single crystalline porous ZnO nanostructures containing a single large cavity. The microwave-assisted route consists of a short (about 2 min) temperature ramping stage (from room temperature to 120 °C) and a stage in which the temperature is maintained at 120 °C for 2 h. The structures produced by this route were 200-480 nm in diameter. The morphological yields of this method were very high. The temperature- and time-dependent evolution of the synthesized powders and the effects of an additive, vitamin C, were studied. Spherical amorphous/polycrystalline structures (70-170 nm in diameter), which appeared transitorily, may play a key role in the formation of the single crystalline porous hollow ZnO nanostructures. Studies and characterization of the nanostructures suggested a possible mechanism for formation of the quasi-single crystalline porous ZnO nanostructures with an interior space.We report a method for synthesizing quasi-single crystalline porous ZnO nanostructures containing a single large cavity. The microwave-assisted route consists of a short (about 2 min) temperature ramping stage (from room temperature to 120 °C) and a stage in which the temperature is maintained at 120 °C for 2 h. The structures produced by this route were 200-480 nm in diameter. The morphological yields of this method were very high. The temperature- and time-dependent evolution of the synthesized powders and the effects of an additive, vitamin C, were studied. Spherical amorphous/polycrystalline structures (70-170 nm in diameter), which appeared transitorily, may play a key role in the formation of the single crystalline porous hollow ZnO nanostructures. Studies and characterization of the nanostructures suggested a possible mechanism for formation of the quasi-single crystalline porous ZnO nanostructures with an interior space. Electronic supplementary information (ESI) available: TEM images and the corresponding SAED image of a ZnO nanostructure synthesized from the reaction without l(+)-ascorbic acid at the 85 °C time point (Fig. S1). See DOI: 10.1039/c1nr10609k

Synthesis of the zeolitic imidazolate framework ZIF-4 from the ionic liquid 1-butyl-3-methylimidazolium imidazolate

NASA Astrophysics Data System (ADS)

Hovestadt, Maximilian; Schwegler, Johannes; Schulz, Peter S.; Hartmann, Martin

2018-05-01

A new synthesis route for the zeolitic imidazolate framework ZIF-4 using imidazolium imidazolate is reported. Additionally, the ionic liquid-derived material is compared to conventional ZIF-4 with respect to the powder X-ray diffraction pattern pattern, nitrogen uptake, particle size, and separation potential for olefin/paraffin gas mixtures. Higher synthesis yields were obtained, and the different particle size affected the performance in the separation of ethane and ethylene.

Effect of drying parameters on physiochemical and sensory properties of fruit powders processed by PGSS-, Vacuum- and Spray-drying.

PubMed

Feguš, Urban; Žigon, Uroš; Petermann, Marcus; Knez, Željko

2015-01-01

Aim of this experimental work was to investigate the possibility of producing fruit powders without employing drying aid and to investigate the effect of drying temperatures on the final powder characteristics. Raw fruit materials (banana puree, strawberry puree and blueberry concentrate) were processed using three different drying techniques each operating at a different temperature conditions: vacuum-drying (-27-17 °C), Spray-drying (130-160 °C) and PGSS-drying (112-152 °C). Moisture content, total colour difference, antioxidant activity and sensory characteristics of the processed fruit powders were analysed. The results obtained from the experimental work indicate that investigated fruit powders without or with minimal addition of maltodextrin can be produced. Additionally, it was observed that an increase in process temperature results in a higher loss of colour, antioxidant activity and intensity of the flavour profile.

Electrical properties of samarium cobaltite nanoparticles synthesized using Sol–Gel autocombustion route

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

Sathyamoorthy, B.; Md Gazzali, P.M.; Murugesan, C.

2014-05-01

Highlights: • The structural evolution and its electrical properties of samarium cobaltite nanograins are discussed. • Optimization of SmCoO{sub 3} nanograins is achieved by post sintering as-prepared gel at 800 °C. • The impedance spectra indicate the semiconducting behavior SmCoO{sub 3} nanograins. - Abstract: Nanograins of SmCoO{sub 3} are prepared by citric acid assisted Sol–Gel autocombustion route. The characterizations of crystal structure, surface morphology and electrical properties of SmCoO{sub 3} powder are done using XRD, HRSEM, FTIR and BDS. The structural evolution of SmCoO{sub 3} upon increasing the annealing temperature is followed using XRD and FTIR analyses. The powder samplemore » contains polycrystalline grains with average size equal to 35 nm and orthorhombic perovskite structure with Pbnm space group. The vibrational bands observed in FTIR spectrum at 545 cm{sup −1} and 439 cm{sup −1} correspond to Co-O stretching modes in cobaltite system. HRSEM images of the sample show the formation of hexagonal shaped grains of samarium cobaltite. The AC electrical conductivity of 4.914 × 10{sup −5} S cm{sup −1} at 295 K is measured for SmCoO{sub 3} nanoparticles. The impedance spectra bring out the semiconducting behavior of the material.« less

Structural, morphological and magnetic properties of Sr0.3La0.48Ca0.25n[Fe(2-0.4/n)O3]Co0.4 (n = 5.5, 5.6,5.7,5.8, 5.9, 6.0) hexaferrites prepared by facile ceramic route methodology

NASA Astrophysics Data System (ADS)

Rehman, Khalid Mehmood Ur; Liu, Xiansong; Yang, Yujie; Feng, Shuangjiu; Tang, Jin; Ali, Zulfiqar; Wazir, Z.; Khan, Muhammad Wasim; Shezad, Mudssir; Iqbal, Muhammad Shahid; Zhang, Cong; Liu, Chaocheng

2018-03-01

In present work, M-type strontium hexaferrite with chemical composition of Sr0.3La0.48Ca0.25n[Fe(2-0.4/n)O3]Co0.4 (n = 5.5, 5.6, 5.7, 5.8, 5.9, 6.0) magnetic powder were synthesized by using facile ceramic route methodology. The structural, morphological and magnetic properties of the products were investigated by using X-rays diffraction (XRD), Scanning Electron Microscopy (SEM) and Vibrating Sample Magnetometer (VSM) techniques, respectively. There is a single magnetoplumbite phase in the magnetic powders containing (5.5 ≤ n ≤5.8) and (n ≥ 5.9) magnetic some impurities begin to seem in the structure. The magnets have shaped hexagonal structures. Magnetic properties of the samples were metric by permanent magnetic measuring equipment Vibrating Sample Magnetometer, respectively. We report our investigation of n-aggregation iron content on crystalline size characterization and magnetic properties of the specimen. It is originate that the desirable quantity of n-aggregation iron content substitution may curiously increase saturation magnetization (Ms) and intrinsic coercivity (Hc). With the iron addition for the same sintering temperature at 1260 °C, (Ms) and (Hc) first increase and then decrease gradually.

Effects of Process Parameters and Cryotreated Electrode on the Radial Overcut of Aisi 304 IN SiC Powder Mixed Edm

NASA Astrophysics Data System (ADS)

Bhaumik, Munmun; Maity, Kalipada

Powder mixed electro discharge machining (PMEDM) is further advancement of conventional electro discharge machining (EDM) where the powder particles are suspended in the dielectric medium to enhance the machining rate as well as surface finish. Cryogenic treatment is introduced in this process for improving the tool life and cutting tool properties. In the present investigation, the characterization of the cryotreated tempered electrode was performed. An attempt has been made to study the effect of cryotreated double tempered electrode on the radial overcut (ROC) when SiC powder is mixed in the kerosene dielectric during electro discharge machining of AISI 304. The process performance has been evaluated by means of ROC when peak current, pulse on time, gap voltage, duty cycle and powder concentration are considered as process parameters and machining is performed by using tungsten carbide electrodes (untreated and double tempered electrodes). A regression analysis was performed to correlate the data between the response and the process parameters. Microstructural analysis was carried out on the machined surfaces. Least radial overcut was observed for conventional EDM as compared to powder mixed EDM. Cryotreated double tempered electrode significantly reduced the radial overcut than untreated electrode.

Novel Method for Making Biomedical Segregation-Free Ti-30Ta Alloy Spherical Powder for Additive Manufacturing

NASA Astrophysics Data System (ADS)

Xia, Yang; Fang, Zhigang Zak; Sun, Pei; Zhang, Ying; Zhu, Jun

2018-03-01

Ti-Ta alloys offer a good combination of high strength and low modulus among Ti-based alloys, and are ideal for biomedical applications. However, making Ti-Ta alloys has always been challenging because they tend to suffer from compositional segregation during melting due to the large difference between the melting points of Ti and Ta. This article describes a novel process for making spherical Ti-30Ta alloy powder through a unique powder metallurgy technique, namely the granulation-sintering-deoxygenation process. The results indicate that the compositional segregation problem can be overcome using this process technology. Combined with use of a deoxygenation process, the critical interstitial element, oxygen, can be controlled to < 400 ppm for powder with particle size < 75 µm. The destabilization effect of Ta on Ti-O solid solutions, and the resulting improved deoxygenation process for Ti-Ta, are discussed, as well as the phase composition and microstructure of the powders.

Magnesium Nanocomposites: Current Status and Prospects for Army Applications

DTIC Science & Technology

2011-09-01

and reinforcement that cannot be produced through melt-based processing . In mechanical alloying , the powder and milling media are placed into...mixing vessels that are agitated in a high-energy milling machine. During the mixing process , the powder particles undergo repeated cycles of cold ...welding and fracturing of interparticle bonds. At the end of the process , the powder has been alloyed to the desired composition. Although typically used

Microencapsulation of fish oil by spray granulation and fluid bed film coating.

PubMed

Anwar, Sri Haryani; Weissbrodt, Jenny; Kunz, Benno

2010-08-01

The stability of microencapsulated fish oil prepared with 2 production processes, spray granulation (SG) and SG followed by film coating (SG-FC) using a fluid bed equipment, was investigated. In the 1st process, 3 types of fish oil used were based on the ratios of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) (10/50, 33/22, and 18/12). Each type was emulsified with soluble soybean polysaccharide (SSPS) and maltodextrin to produce 25% oil powders. In the 2nd process, 15% film coating of hydroxypropyl betacyclodextrin (HPBCD) was applied to the granules from the 1st process. The powder stability against oxidation was examined by measurement of peroxide values (PV) and headspace propanal after storage at room temperature and at 3 to 4 degrees C for 6 wk. Uncoated powder containing the lowest concentration of PUFA (18/12) was found to be stable during storage at room temperature with maximum PV of 3.98 +/- 0.001 meq/kg oil. The PV increased sharply for uncoated powder with higher concentration of omega-3 (in 33/22 and 10/50 fish oils) after 3 wk storage. The PVs were in agreement with the concentration of propanal, and these 2 parameters remained constant for most of the uncoated powders stored at low temperature. Unexpectedly, the outcomes showed that the coated powders had lower stability than uncoated powders as indicated by higher initial PVs; more hydroperoxides were detected as well as increasing propanal concentration. The investigation suggests that the film-coating by HPBCD ineffectively protected fish oil as the coating process might have induced further oxidation; however, SG is a good method for producing fish oil powder and to protect it from oxidation because of the "onion skin" structure of granules produced in this process.

Developments in the formulation and delivery of spray dried vaccines

PubMed Central

Kanojia, Gaurav; Have, Rimko ten; Soema, Peter C.; Frijlink, Henderik; Amorij, Jean-Pierre; Kersten, Gideon

2017-01-01

ABSTRACT Spray drying is a promising method for the stabilization of vaccines, which are usually formulated as liquids. Usually, vaccine stability is improved by spray drying in the presence of a range of excipients. Unlike freeze drying, there is no freezing step involved, thus the damage related to this step is avoided. The edge of spray drying resides in its ability for particles to be engineered to desired requirements, which can be used in various vaccine delivery methods and routes. Although several spray dried vaccines have shown encouraging preclinical results, the number of vaccines that have been tested in clinical trials is limited, indicating a relatively new area of vaccine stabilization and delivery. This article reviews the current status of spray dried vaccine formulations and delivery methods. In particular it discusses the impact of process stresses on vaccine integrity, the application of excipients in spray drying of vaccines, process and formulation optimization strategies based on Design of Experiment approaches as well as opportunities for future application of spray dried vaccine powders for vaccine delivery. PMID:28925794

Nano-scaled top-down of bismuth chalcogenides based on electrochemical lithium intercalation

NASA Astrophysics Data System (ADS)

Chen, Jikun; Zhu, Yingjie; Chen, Nuofu; Liu, Xinling; Sun, Zhengliang; Huang, Zhenghong; Kang, Feiyu; Gao, Qiuming; Jiang, Jun; Chen, Lidong

2011-12-01

A two-step method has been used to fabricate nano-particles of layer-structured bismuth chalcogenide compounds, including Bi2Te3, Bi2Se3, and Bi2Se0.3Te2.7, through a nano-scaled top-down route. In the first step, lithium (Li) atoms are intercalated between the van der Waals bonded quintuple layers of bismuth chalcogenide compounds by controllable electrochemical process inside self-designed lithium ion batteries. And in the second step, the Li intercalated bismuth chalcogenides are subsequently exposed to ethanol, in which process the intercalated Li atoms would explode like atom-scaled bombs to exfoliate original microscaled powder into nano-scaled particles with size around 10 nm. The influence of lithium intercalation speed and amount to three types of bismuth chalcogenide compounds are compared and the optimized intercalation conditions are explored. As to maintain the phase purity of the final nano-particle product, the intercalation lithium amount should be well controlled in Se contained bismuth chalcogenide compounds. Besides, compared with binary bismuth chalcogenide compound, lower lithium intercalation speed should be applied in ternary bismuth chalcogenide compound.

An Investigation of Sintering Parameters on Titanium Powder for Electron Beam Melting Processing Optimization.

PubMed

Drescher, Philipp; Sarhan, Mohamed; Seitz, Hermann

2016-12-01

Selective electron beam melting (SEBM) is a relatively new additive manufacturing technology for metallic materials. Specific to this technology is the sintering of the metal powder prior to the melting process. The sintering process has disadvantages for post-processing. The post-processing of parts produced by SEBM typically involves the removal of semi-sintered powder through the use of a powder blasting system. Furthermore, the sintering of large areas before melting decreases productivity. Current investigations are aimed at improving the sintering process in order to achieve better productivity, geometric accuracy, and resolution. In this study, the focus lies on the modification of the sintering process. In order to investigate and improve the sintering process, highly porous titanium test specimens with various scan speeds were built. The aim of this study was to decrease build time with comparable mechanical properties of the components and to remove the residual powder more easily after a build. By only sintering the area in which the melt pool for the components is created, an average productivity improvement of approx. 20% was achieved. Tensile tests were carried out, and the measured mechanical properties show comparatively or slightly improved values compared with the reference.

Consolidation Process in Near Net Shape Manufacturing of Armstrong CP-Ti/Ti-6Al-4V Powders

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

Yamamoto, Yukinori; Kiggans, Jim; Clark, Michael B

2010-01-01

This paper summarizes our recent efforts to develop the manufacturing technologies of consolidated net-shape components by using new low-cost commercially pure titanium (CP-Ti) and Ti-6Al-4V alloy powders made by the Armstrong process. Fabrication processes of net shape/ near net shape components, such as uniaxial die-pressing, cold isostatic pressing (CIP), sintering, roll compaction and stamping, have been evaluated. The press-and-sinter processing of the powders were systematically investigated in terms of theoretical density and microstructure as a function of time, pressure, and temperature. Up to 96.4% theoretical density has been achieved with the press-and-sinter technology. Tensile properties of the consolidated samples exhibitmore » good ductility as well as equivalent yield/ultimate tensile strengths to those of fully consolidate materials, even with the presence of a certain amount of porosity. A consolidation model is also under development to interpret the powder deformation during processing. Net shape components made of the Armstrong powder can successfully be fabricated with clearer surface details by using press-and-sinter processing.« less

Using 3D Printing for Rapid Prototyping of Characterization Tools for Investigating Powder Blend Behavior.

PubMed

Hirschberg, Cosima; Boetker, Johan P; Rantanen, Jukka; Pein-Hackelbusch, Miriam

2018-02-01

There is an increasing need to provide more detailed insight into the behavior of particulate systems. The current powder characterization tools are developed empirically and in many cases, modification of existing equipment is difficult. More flexible tools are needed to provide understanding of complex powder behavior, such as mixing process and segregation phenomenon. An approach based on the fast prototyping of new powder handling geometries and interfacing solutions for process analytical tools is reported. This study utilized 3D printing for rapid prototyping of customized geometries; overall goal was to assess mixing process of powder blends at small-scale with a combination of spectroscopic and mechanical monitoring. As part of the segregation evaluation studies, the flowability of three different paracetamol/filler-blends at different ratios was investigated, inter alia to define the percolation thresholds. Blends with a paracetamol wt% above the percolation threshold were subsequently investigated in relation to their segregation behavior. Rapid prototyping using 3D printing allowed designing two funnels with tailored flow behavior (funnel flow) of model formulations, which could be monitored with an in-line near-infrared (NIR) spectrometer. Calculating the root mean square (RMS) of the scores of the two first principal components of the NIR spectra visualized spectral variation as a function of process time. In a same setup, mechanical properties (basic flow energy) of the powder blend were monitored during blending. Rapid prototyping allowed for fast modification of powder testing geometries and easy interfacing with process analytical tools, opening new possibilities for more detailed powder characterization.

Utilization of gas-atomized titanium and titanium-aluminide powder

NASA Astrophysics Data System (ADS)

Moll, John H.

2000-05-01

A gas-atomization process has been developed producing clean, high-quality, prealloyed spherical titanium and titanium-aluminide powder. The powder is being used to manufacture hot-isostatically pressed consolidated shapes for aerospace and nonaerospace allocations. These include gamma titanium-aluminide sheet and orthorhombic titanium-aluminide wire as well as niche markets, such as x-ray drift standards and sputtering targets. The powder is also being used in specialized processes, including metal-matrix composites, laser forming, and metal-injection molding.

Modern trends in increasing the quality of the steels intended for cutting and metal-working tools: I. Improvement of granule metallurgy processes

NASA Astrophysics Data System (ADS)

Belyanchikov, L. N.

2008-12-01

The following new technological processes for producing fine gas-atomized powders of tool and high-speed steels with a low content of nonmetallic inclusions are considered: the process designed by Böhler Uddeholm Powder Technology (Austria) and processes involving a heated gas. In the former process, a metal is poured from a ladle with electroslag heating, and the atomizing unit consists of three injectors. A new process of producing tools from fine powders by three-dimensional printing, i.e., so-called 3D-printing, is described.

Synthesis of Zeolites Using the ADOR (Assembly-Disassembly-Organization-Reassembly) Route

PubMed Central

Wheatley, Paul S.; Čejka, Jiří; Morris, Russell E.

2016-01-01

Zeolites are an important class of materials that have wide ranging applications such as heterogeneous catalysts and adsorbents which are dependent on their framework topology. For new applications or improvements to existing ones, new zeolites with novel pore systems are desirable. We demonstrate a method for the synthesis of novel zeolites using the ADOR route. ADOR is an acronym for Assembly, Disassembly, Organization and Reassembly. This synthetic route takes advantage of the assembly of a relatively poorly stable that which can be selectively disassembled into a layered material. The resulting layered intermediate can then be organized in different manners by careful chemical manipulation and then reassembled into zeolites with new topologies. By carefully controlling the organization step of the synthetic pathway, new zeolites with never before seen topologies are capable of being synthesized. The structures of these new zeolites are confirmed using powder X-ray diffraction and further characterized by nitrogen adsorption and scanning electron microscopy. This new synthetic pathway for zeolites demonstrates its capability to produce novel frameworks that have never been prepared by traditional zeolite synthesis techniques. PMID:27078165

Synthesis of Zeolites Using the ADOR (Assembly-Disassembly-Organization-Reassembly) Route.

PubMed

Wheatley, Paul S; Čejka, Jiří; Morris, Russell E

2016-04-03

Zeolites are an important class of materials that have wide ranging applications such as heterogeneous catalysts and adsorbents which are dependent on their framework topology. For new applications or improvements to existing ones, new zeolites with novel pore systems are desirable. We demonstrate a method for the synthesis of novel zeolites using the ADOR route. ADOR is an acronym for Assembly, Disassembly, Organization and Reassembly. This synthetic route takes advantage of the assembly of a relatively poorly stable that which can be selectively disassembled into a layered material. The resulting layered intermediate can then be organized in different manners by careful chemical manipulation and then reassembled into zeolites with new topologies. By carefully controlling the organization step of the synthetic pathway, new zeolites with never before seen topologies are capable of being synthesized. The structures of these new zeolites are confirmed using powder X-ray diffraction and further characterized by nitrogen adsorption and scanning electron microscopy. This new synthetic pathway for zeolites demonstrates its capability to produce novel frameworks that have never been prepared by traditional zeolite synthesis techniques.

Effect of organic fuels on surface area and photocatalytic activity of scheelite CaWO4 nanoparticles

NASA Astrophysics Data System (ADS)

Manjunath, Kusuma; Gujjarahalli Thimmanna, Chandrappa

2018-03-01

Discrete nanoscale calcium tungstate (CaWO4) nanoparticles with exquisite photocatalytic activities were synthesized through ultra-rapid solution combustion route. Here, we aim to study the effect of different fuels on the synthesis of CaWO4 nanoparticles which lead to improve the characteristic properties and morphological evolution of the powders. From BET surface area measurement, it is observed that CaWO4 nanoparticles synthesized by using citric acid as fuel exhibits relatively large surface area (31.78 m2 g‑1) as compared to other fuels. The powder x-ray diffraction (PXRD) studies reveal that CaWO4 nanoparticles belong to scheelite type tetragonal system. The morphology of CaWO4 nanoparticles investigated using scanning electron microscopy (SEM) reveals that the powders are highly porous and agglomerated. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) images of the CaWO4 nanoparticles show that a well-dispersed nearly oval-shaped nanoparticles with variable dimensions and lattice spacing that depends on the type of fuels used in the synthesis. The selected area electron diffraction (SAED) patterns of CaWO4 nanoparticles exhibit several concentric rings with bright spots indicating the polycrystalline nature of the powders. Investigation on photocatalytic activity of CaWO4 nanoparticles synthesized using citric acid shows highest (∼93%) degradation of methylene blue (MB).

Effect of Milling Time on the Microstructure, Physical and Mechanical Properties of Al-Al2O3 Nanocomposite Synthesized by Ball Milling and Powder Metallurgy

PubMed Central

Matori, Khamirul Amin; Ostovan, Farhad; Abdul Aziz, Sidek; Mamat, Md Shuhazlly

2017-01-01

The effect of milling time on the morphology, microstructure, physical and mechanical properties of pure Al-5 wt % Al2O3 (Al-5Al2O3) has been investigated. Al-5Al2O3 nanocomposites were fabricated using ball milling in a powder metallurgy route. The increase in the milling time resulted in the homogenous dispersion of 5 wt % Al2O3 nanoparticles, the reduction of particle clustering, and the reduction of distances between the composite particles. The significant grain refining during milling was revealed which showed as a reduction of particle size resulting from longer milling time. X-Ray diffraction (XRD) analysis of the nanocomposite powders also showed that designated ball milling contributes to the crystalline refining and accumulation of internal stress due to induced severe plastic deformation of the particles. It can be argued that these morphological and microstructural variations of nanocomposite powders induced by designated ball milling time was found to contribute to an improvement in the density, densification, micro-hardness (HV), nano-hardness (HN), and Young’s modulus (E) of Al-5Al2O3 nanocomposites. HV, HN, and E values of nanocomposites were increased by ~48%, 46%, and 40%, after 12 h of milling, respectively. PMID:29072632

The influence of the pressure and temperature on the light emission of the ZnO

NASA Astrophysics Data System (ADS)

Dantas, N. O.; Couto dos Santos, M. A.; Cunha, F.; Macêdo, M. A.

2007-09-01

A new route for the preparation of zinc oxide powder is described along with its characterization. A proteic sol was prepared dissolving zinc nitrate in filtered coconut water. After calcination at 1000 °C, the powder was compressed to 1.3×10 8 Pa and ZnO pellets were obtained. The emission spectra were recorded under UV excitation at 325 and 400 nm. The powder showed no spectroscopic response, whereas one peak around 396 nm was observed for the pressed powder (pellet with no heat treatment). The pellets were then annealed for 24 h at 500, 800 and 1000 °C. In the first case, bands at 396 and 440 nm and a structure of narrow peaks around 480 nm (oxygen vacancies) were observed. Increasing the annealing temperature led to a decrease in the intensity of the emissions at 440 and 480 nm. We propose that the high pressure induces a red-shift in the UV region of the ZnO nanopowder emission peaks to 396 nm. This is an indication that the ZnO nanopowder treated under pressure and sintering temperature exhibits the spectroscopic behavior characteristic of the ZnO single crystal. The disappearance of the 440 and 480 nm lines indicate the reduction of oxygen vacancies. The atomic force micrographs suggest a coalescence thermal point.

Toxicants in folk remedies: Implications of elevated blood lead in an American-born infant due to imported diaper powder

USGS Publications Warehouse

Karwowski, Mateusz P.; Morman, Suzette A.; Plumlee, Geoffrey S.; Law, Terence; Kellogg, Mark; Woolf, Alan D.

2016-01-01

Though most childhood lead exposure in the USA results from ingestion of lead-based paint dust, non-paint sources are increasingly implicated. We present interdisciplinary findings from and policy implications of a case of elevated blood lead (13–18 mcg/dL, reference level <5 mcg/dL) in a 9-month-old infant, linked to a non-commercial Malaysian folk diaper powder. Analyses showed the powder contains 62 % lead by weight (primarily lead oxide) and elevated antimony [1000 parts per million (ppm)], arsenic (55 ppm), bismuth (110 ppm), and thallium (31 ppm). These metals are highly bioaccessible in simulated gastric fluids, but only slightly bioaccessible in simulated lung fluids and simulated urine, suggesting that the primary lead exposure routes were ingestion via hand-mouth transmission and ingestion of inhaled dusts cleared from the respiratory tract. Four weeks after discontinuing use of the powder, the infant’s venous blood lead level was 8 mcg/dL. Unregulated, imported folk remedies can be a source of toxicant exposure. Additional research on import policy, product regulation, public health surveillance, and culturally sensitive risk communication is needed to develop efficacious risk reduction strategies in the USA. The more widespread use of contaminated folk remedies in the countries from which they originate is a substantial concern.

Toxicants in folk remedies: implications of elevated blood lead in an American-born infant due to imported diaper powder.

PubMed

Karwowski, Mateusz P; Morman, Suzette A; Plumlee, Geoffrey S; Law, Terence; Kellogg, Mark; Woolf, Alan D

2017-10-01

Though most childhood lead exposure in the USA results from ingestion of lead-based paint dust, non-paint sources are increasingly implicated. We present interdisciplinary findings from and policy implications of a case of elevated blood lead (13-18 mcg/dL, reference level <5 mcg/dL) in a 9-month-old infant, linked to a non-commercial Malaysian folk diaper powder. Analyses showed the powder contains 62 % lead by weight (primarily lead oxide) and elevated antimony [1000 parts per million (ppm)], arsenic (55 ppm), bismuth (110 ppm), and thallium (31 ppm). These metals are highly bioaccessible in simulated gastric fluids, but only slightly bioaccessible in simulated lung fluids and simulated urine, suggesting that the primary lead exposure routes were ingestion via hand-mouth transmission and ingestion of inhaled dusts cleared from the respiratory tract. Four weeks after discontinuing use of the powder, the infant's venous blood lead level was 8 mcg/dL. Unregulated, imported folk remedies can be a source of toxicant exposure. Additional research on import policy, product regulation, public health surveillance, and culturally sensitive risk communication is needed to develop efficacious risk reduction strategies in the USA. The more widespread use of contaminated folk remedies in the countries from which they originate is a substantial concern.

Enery Efficient Press and Sinter of Titanium Powder for Low-Cost Components in Vehicle Applications

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

Thomas Zwitter; Phillip Nash; Xiaoyan Xu

2011-03-31

This is the final technical report for the Department of Energy NETL project NT01931 Energy Efficient Press and Sinter of Titanium Powder for Low-Cost Components in Vehicle Applications. Titanium has been identified as one of the key materials with the required strength that can reduce the weight of automotive components and thereby reduce fuel consumption. Working with newly developed sources of titanium powder, Webster-Hoff will develop the processing technology to manufacture low cost vehicle components using the single press/single sinter techniques developed for iron based powder metallurgy today. Working with an automotive or truck manufacturer, Webster-Hoff will demonstrate the feasibilitymore » of manufacturing a press and sinter titanium component for a vehicle application. The project objective is two-fold, to develop the technology for manufacturing press and sinter titanium components, and to demonstrate the feasibility of producing a titanium component for a vehicle application. The lowest cost method for converting metal powder into a net shape part is the Powder Metallurgy Press and Sinter Process. The method involves compaction of the metal powder in a tool (usually a die and punches, upper and lower) at a high pressure (up to 60 TSI or 827 MPa) to form a green compact with the net shape of the final component. The powder in the green compact is held together by the compression bonds between the powder particles. The sinter process then converts the green compact to a metallurgically bonded net shape part through the process of solid state diffusion. The goal of this project is to expand the understanding and application of press and sinter technology to Titanium Powder applications, developing techniques to manufacture net shape Titanium components via the press and sinter process. In addition, working with a vehicle manufacturer, demonstrate the feasibility of producing a titanium component for a vehicle. This is not a research program, but rather a project to develop a process for press and sinter of net shape Titanium components. All of these project objectives have been successfully completed.« less

Synthesis of ITO Powder by Dry Process and Lifetime Characteristics of the ITO Target Fabricated with its Powder

NASA Astrophysics Data System (ADS)

Takahashi, Seiichiro; Itoh, Hironori; Komatsu, Ryuichi

Lifetime of an indium tin oxide (ITO) target is an important characteristic in the production of liquid crystal displays (LCDs). Increasing the sintering density of the ITO target is assumed to lead to an increased lifetime. So far, it has been clarified that the carbon concentration in In2O3 powder, the raw material of ITO targets, influences remarkably the target lifetime. In this study, with the aim of reducing the concentration of carbon in In2O3 powder, the synthesis of In2O3 powder containing dissolved Sn by a dry process was performed.

Metal powder production by gas atomization

NASA Technical Reports Server (NTRS)

Ting, E. Y.; Grant, N. J.

1986-01-01

The confined liquid, gas-atomization process was investigated. Results from a two-dimensional water model showed the importance of atomization pressure, as well as delivery tube and atomizer design. The atomization process at the tip of the delivery tube was photographed. Results from the atomization of a modified 7075 aluminum alloy yielded up to 60 wt pct. powders that were finer than 45 microns in diameter. Two different atomizer designs were evaluated. The amount of fine powders produced was correlated to a calculated gas-power term. An optimal gas-power value existed for maximized fine powder production. Atomization at gas-power greater than or less than this optimal value produced coarser powders.

Process of Making Boron-Fiber Reinforced Composite Tape

NASA Technical Reports Server (NTRS)

Belvin, Harry L. (Inventor); Cano, Roberto J. (Inventor); Johnston, Norman J. (Inventor); Marchello, Joseph M. (Inventor)

2002-01-01

The invention is an apparatus and method for producing a hybrid boron reinforced polymer matrix composition from powder pre-impregnated fiber tow bundles and a linear array of boron fibers. The boron fibers are applied onto the powder pre-impregnated fiber tow bundles and then are processed within a processing component having an impregnation bar assembly. After passing through variable-dimension forming nip-rollers, the powder pre-impregnated fiber tow bundles with the boron fibers become a hybrid boron reinforced polymer matrix composite tape. A driving mechanism pulls the powder pre-impregnated fiber tow bundles with boron fibers through the processing line of the apparatus and a take-up spool collects the formed hybrid boron-fiber reinforced polymer matrix composite tape.

Experimental study on the fabrication of advanced materials for energy applications using high energy mechanical milling

NASA Astrophysics Data System (ADS)

Narayana Swamy, Ashvin Kumar

The reaction of aluminum (Al) powder with water has the potential for on demand hydrogen generation. Conventional Al powders, however, react with water slowly due to a highly protective oxide layer on the particle surface. Current methods for Al activation involve harmful and expensive materials. The nano-scale Al powders also remain very expensive and have problems such as a large amount of oxide on the surface. The use of aluminum in an energy generation cycle is also hindered by the fact that, although Al is the most abundant metal in the Earth's crust, its recovery from ore consumes a lot of energy. Recycling aluminum hydroxide, formed as a result of Al reaction with water, would also require large amounts of energy. The energy consumption for production of Al powder and hence its cost could be significantly reduced by using recycled aluminum scrap and waste where aluminum is contained in metallic, non-oxidized form. The research work presented here investigates the preparation of an activated aluminum powder from aluminum foil that is widely available as scrap and waste. The obtained results demonstrate that a highly reactive, fine powder can be obtained from Al foil by high-energy ball milling with sodium chloride (NaCl). The obtained powder readily reacts with hot water, releasing hydrogen. Note that NaCl is an environment-friendly additive that can easily be removed after milling and recycled. After washing NaCl out, the powders retain a high reactivity with respect to hot water. As compared to previously studied activation of commercial Al powders, a major advantage of the investigated process is the feasibility of using secondary aluminum. Another area of research presented here is the synthesis of gallium oxide (Ga2O3) nanostructures for their use as high-temperature sensors. Quasi one-dimensional nanomaterials are of great interest due to increased focus on their importance in physics research and also their applications in the nanodevices industry. Since the mid 1950's, considerable research has been reported on the synthesis of filamentary crystals from alloys and metals. Since the discovery of carbon nanotubes (CNTs), there has been a tremendous surge in research activities for development and characterization of one-dimensional nanostructures. Most of the research is targeted towards the development of semiconductors such ZnO, Si, SnO2, and GaAs. Gallium oxide nanostructures have the ability to withstand high temperatures and also act as high-temperature sensors. In particular, they can be used as oxygen sensors at temperatures over 900 °C. These properties make gallium oxide nanostructures attractive for use in exhaust systems of the combustion chambers in power plants. beta-Ga2O3 nano-rods and nano-sheets were successfully synthesized by a simple method based on heating GaN in inert gas environment with traces of oxygen. Characterization of the obtained products showed nano-belts in the size range from 10 nm to 15 nm. Several other unique nano-structures were also synthesized. The results show a vapor-solid mechanism to be the prevailing growth route for the synthesis of nano-structures.

PLUTONIUM-HYDROGEN REACTION PRODUCT, METHOD OF PREPARING SAME AND PLUTONIUM POWDER THEREFROM

DOEpatents

Fried, S.; Baumbach, H.L.

1959-12-01

A process is described for forming plutonlum hydride powder by reacting hydrogen with massive plutonium metal at room temperature and the product obtained. The plutonium hydride powder can be converted to plutonium powder by heating to above 200 deg C.

Powder-Coated Towpreg: Avenues to Near Net Shape Fabrication of High Performance Composites

NASA Technical Reports Server (NTRS)

Johnston, N. J.; Cano, R. J.; Marchello, J. M.; Sandusky, D. A.

1995-01-01

Near net shape parts were fabricated from powder-coated preforms. Key issues including powder loss during weaving and tow/tow friction during braiding were addressed, respectively, by fusing the powder to the fiber prior to weaving and applying a water-based gel to the towpreg prior to braiding. A 4:1 debulking of a complex 3-D woven powder-coated preform was achieved in a single step utilizing expansion rubber molding. Also, a process was developed for using powder-coated towpreg to fabricate consolidated ribbon having good dimensional integrity and low voids. Such ribbon will be required for in situ fabrication of structural components via heated head advanced tow placement. To implement process control and ensure high quality ribbon, the ribbonizer heat transfer and pulling force were modeled from fundamental principles. Most of the new ribbons were fabricated from dry polyarylene ether and polymide powders.

The development of an alternative thermoplastic powder prepregging technique

NASA Technical Reports Server (NTRS)

Ogden, A. L.; Hyer, M. W.; Wilkes, G. L.; Loos, A. C.

1992-01-01

An alternative powder prepregging technique is discussed that is based on the deposition of powder onto carbon fibers that have been moistened using an ultrasonic humidifier. The dry fiber tow is initially spread to allow a greater amount of the fiber surface to be exposed to the powder, thus ensuring a significant amount of intimate contact between the fiber and the matrix. Moisture in the form of ultrafine water droplets is then deposited onto the spread fiber tow. The moisture promotes adhesion to the fiber until the powder can be tacked to the fibers by melting. Powdered resin is then sieved onto the fibers and then tacked onto the fibers by quick heating in a convective oven. This study focuses on the production of prepregs and laminates made with LaRC-TPI (thermoplastic polyimide) using this process. Although the process appears to be successful, early evaluation was hampered by poor interfacial adhesion. The adhesion problem, however, seems to be the result of a material system incompatibility, rather than being influenced by the process.

Environmental impacts of milk powder and butter manufactured in the Republic of Ireland.

PubMed

Finnegan, William; Goggins, Jamie; Clifford, Eoghan; Zhan, Xinmin

2017-02-01

The abolition of the milk quota system that was in place in Europe was abolished in 2015, which instigated an immediate increase in milk production in many European countries. This increase will aid in addressing the world's ever growing demand for food, but will incur increased stresses on the environmental impact and sustainability of the dairy industry. In this study, an environmental life cycle assessment was performed in order to estimate the environmental impacts associated with the manufacture of milk powder and butter in the Republic of Ireland. A farm gate to processing factory gate analysis, which includes raw milk transportation, processing into each product and packaging, is assessed in this study. Operational data was obtained from 5 dairy processing factories that produce milk powder (4 of which also produce butter). Results for each environmental impact category are presented per kilogram of product. Energy consumption (raw milk transportation and on-site electrical and thermal energy usage) contributes, on average, 89% and 78% of the total global warming potential, for milk powder and butter respectively, for the life cycle stages assessed. Similarly, energy consumption contributes, on average, 86% and 96% of the total terrestrial acidification potential for milk powder and butter respectively, for these life cycle stages. Emissions associated with wastewater treatment contribute approximately 10% and 40% to the total freshwater eutrophication potential and marine eutrophication potential, respectively, for both milk powder and butter production. In addition, packaging materials also has a significant contribution to these environmental impact categories for butter production. Results were also presented for three milk powder products being manufactured by the factories surveyed: skim milk powder, whole milk powder and full fat milk powder. The analysis presented in this paper helps to identify opportunities to reduce the environmental impacts associated with post-farm processing of milk powder and butter. Copyright © 2016 Elsevier B.V. All rights reserved.

Single-step laser deposition of functionally graded coating by dual ‘wire powder’ or ‘powder powder’ feeding—A comparative study

NASA Astrophysics Data System (ADS)

Syed, Waheed Ul Haq; Pinkerton, Andrew J.; Liu, Zhu; Li, Lin

2007-07-01

The creation of iron-copper (Fe-Cu) alloys has practical application in improving the surface heat conduction and corrosion resistance of, for example, conformal cooling channels in steel moulds, but is difficult to achieve because the elements have got low inter-solubility and are prone to solidification cracking. Previous work by these authors has reported a method to produce a graded iron-nickel-copper coating in a single-step by direct diode laser deposition (DLD) of nickel wire and copper powder as a combined feedstock. This work investigates whether dual powder feeds can be used in that process to afford greater geometric flexibility and compares attributes of the 'nickel wire and copper powder' and 'nickel powder and copper powder' processes for deposition on a H13 tool steel substrate. In wire-powder deposition, a higher temperature developed in the melt pool causing a clad with a smooth gradient structure. The nickel powder in powder-powder deposition did not impart much heat into the melt pool so the melt pool solidified with sharp composition boundaries due to single metal melting in some parts. In wire-powder experiments, a graded structure was obtained by varying the flow rates of wire and powder. However, a graded structure was not realised in powder-powder experiments by varying either the feed or the directions. Reasons for the differences and flow patterns in the melt pools and their effect on final part properties of parts produced are discussed.

Effect of Particle Morphology on Cold Spray Deposition of Chromium Carbide-Nickel Chromium Cermet Powders

NASA Astrophysics Data System (ADS)

Fernandez, Ruben; Jodoin, Bertrand

2017-08-01

Nickel chromium-chromium carbide coatings provide good corrosion and wear resistance at high temperatures, making them ideal for applications where a harsh environment and high temperatures are expected. Thermal spray processes are preferred as deposition technique of cermets, but the high process temperatures can lead to decarburization and reduction of the coatings properties. Cold spray uses lower temperatures preventing decarburization. Since the metallic phase remains solid, the feedstock powder morphology becomes crucial on the deposition behavior. Six commercially available powders were studied, varying in morphology and metal/ceramic ratios. The powders were categorized into 4 groups depending on their morphology. Spherical powders lead to substrate erosion due to their limited overall ductility. Porous agglomerated and sintered powders lead to severely cracked coatings. For dense agglomerated and sintered powders, the outcome depended on the initial metal/ceramic ratio: powders with 25 wt.% NiCr led to substrate erosion while 35 wt.% NiCr powders led to dense coatings. Finally, blended ceramic-metal mixtures also lead to dense coatings. All coatings obtained had lower ceramic content than the initial feedstock powders. Interrupted spray tests, combined with FEA, helped drawing conclusions on the deposition behavior to explain the obtained results.

Synthesis of TiCx Powder via the Underwater Explosion of an Explosive

NASA Astrophysics Data System (ADS)

Tanaka, Shigeru; Bataev, Ivan; Hamashima, Hideki; Tsurui, Akihiko; Hokamoto, Kazuyuki

2018-05-01

In this study, a novel approach to the explosive synthesis of titanium carbide (TiC) is discussed. Nonstoichiometric TiCx powder was produced via the underwater explosion of a Ti powder encapsulated within a spherical explosive charge. The explosion process, bubble formation, and synthesis process were visualized using high-speed camera imaging. It was concluded that synthesis occurred within the detonation gas during the first expansion/contraction cycle of the bubble, which was accompanied by a strong emission of light. The recovered powders were studied using scanning electron microscopy and X-ray diffraction. Submicron particles were generated during the explosion. An increase in the carbon content of the starting powder resulted in an increase in the carbon content of the final product. No oxide byproducts were observed within the recovered powders.

Nonword Reading: Comparing Dual-Route Cascaded and Connectionist Dual-Process Models with Human Data

ERIC Educational Resources Information Center

Pritchard, Stephen C.; Coltheart, Max; Palethorpe, Sallyanne; Castles, Anne

2012-01-01

Two prominent dual-route computational models of reading aloud are the dual-route cascaded (DRC) model, and the connectionist dual-process plus (CDP+) model. While sharing similarly designed lexical routes, the two models differ greatly in their respective nonlexical route architecture, such that they often differ on nonword pronunciation. Neither…

Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

NASA Astrophysics Data System (ADS)

Zhu, J.; Zhang, K.; Zhao, H. Y.

2018-01-01

Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

Silver Complexes of Dihalogen Molecules.

PubMed

Malinowski, Przemysław J; Himmel, Daniel; Krossing, Ingo

2016-08-01

The perfluorohexane-soluble and donor-free silver compound Ag(A) (A=Al(OR(F) )4 ; R(F) =C(CF3 )3 ) prepared using a facile novel route has unprecedented capabilities to form unusual and weakly bound complexes. Here, we report on the three dihalogen-silver complexes Ag(Cl2 )A, Ag(Br2 )A, and Ag(I2 )A derived from the soluble silver compound Ag(A) (characterized by single-crystal/powder XRD, Raman spectra, and quantum-mechanical calculations). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimal Design of Material and Process Parameters in Powder Injection Molding

NASA Astrophysics Data System (ADS)

Ayad, G.; Barriere, T.; Gelin, J. C.; Song, J.; Liu, B.

2007-04-01

The paper is concerned with optimization and parametric identification for the different stages in Powder Injection Molding process that consists first in injection of powder mixture with polymer binder and then to the sintering of the resulting powders part by solid state diffusion. In the first part, one describes an original methodology to optimize the process and geometry parameters in injection stage based on the combination of design of experiments and an adaptive Response Surface Modeling. Then the second part of the paper describes the identification strategy that one proposes for the sintering stage, using the identification of sintering parameters from dilatometeric curves followed by the optimization of the sintering process. The proposed approaches are applied to the optimization of material and process parameters for manufacturing a ceramic femoral implant. One demonstrates that the proposed approach give satisfactory results.

Experimental studies on a novel roll-to-roll powder hot embossing for large-area fabrication of micropyramid arrays on polymers

NASA Astrophysics Data System (ADS)

Yi, Peiyun; Deng, Yujun; Shu, Yunyi; Peng, Linfa

2018-08-01

Roll-to-roll (R2R) hot embossing is regarded as a cost-effective replication technology to fabricate microstructures on polymer films. However, the characteristics of continuous and fast forming for the R2R hot embossing process limits material flow during the filling stage and results in significant springback during the demolding stage. To resolve this issue, this study proposed a novel R2R powder hot embossing process, which combines the merits of the continuous fabrication of R2R hot embossing and near-net-shape forming of powder sintering and also decreases the whole cycle of the fabrication from films to microstructures. First, the relation between the molten layer thickness and processing parameters was discussed and an analytical model was established to predict the feed of the polymeric powder during R2R powder hot embossing. Then, with the use of a micro-pyramid array mold, the impact of the process parameters including mold temperature, feeding speed and applied force on the geometrical dimension of the patterned microstructures was discussed. Last, based on the response surface analysis, a process window, in terms of the mold temperature of 132 °C –145 °C, feeding speed of 0.1–1.4 m min‑1 and applied force of 15–50 kgf was determined for the continuous fabrication of completely-filled micropyramid arrays with the R2R powder hot embossing process. This research demonstrated the feasibility and superiority of the proposed R2R powder hot embossing process in continuously fabricating micropatterned structures on polymeric films.

Microstructural, optical and electrical transport properties of Cd-doped SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Mohsin Nizam Ansari, Mohd

2018-03-01

We have successfully investigated the structural, optical and dielectric properties of Cd assimilated SnO2 nanoparticles synthesized via very convenient precipitation route. The structural properties were studied by x-ray diffraction method (XRD) and Fourier Transform Infrared (FTIR) Spectroscopy. As-synthesized samples in the form of powder were examined for its morphology and average particle size by Transmission electron microscopy (TEM). The optical properties were studied by diffuse reflectance spectroscopy. Dielectric properties such that complex dielectric constant and ac conductivity were investigated by LCR meter. Average crystallite size calculated by XRD and average particle size obtained from TEM were found to be consistent and below 50 nm for all samples. The optical band gap of as-synthesized powder samples from absorption study was found in the range of 3.76 to 3.97 eV. The grain boundary parameters such that Rgb, Cgb and τ were evaluated using impedance spectroscopy.

Analysis of the co-deposition of Al2O3 particles with nickel by an electrolytic route: The influence of organic additives presence and Al2O3 concentration

NASA Astrophysics Data System (ADS)

Temam, H. B.; Temam, E. G.

2016-04-01

Alloy coatings were prepared by co-deposition of Al2O3 particles in Ni matrix on carbon steel substrate from nickel chloride bath in which metallic powders were held in suspension. The influence of metal powder amount in the bath on chemical composition, morphology, thickness, microhardness and corrosion behavior of obtained coatings, has been investigated. It was shown that the presence of Al2O3 particles in deposit greatly improves the hardness and the wear resistance of alloy coatings. Characterization by microanalysis (EDX) of the various deposits elaborated confirms that the rate of particles incorporated increases as the concentration of solid particles increasing. The results showed that the presence of organic additives in Ni-Al2O3 electrolyte deposition led to an increase in the hardness and corrosion resistance of the deposits.

New three-phase polymer-ceramic composite materials for miniaturized microwave antennas

NASA Astrophysics Data System (ADS)

Zhang, Li; Zhang, Jie; Yue, Zhenxing; Li, Longtu

2016-09-01

Unique polymer-ceramic composites for microwave antenna applications were prepared via melt extrusion using high-density polyethylene (HDPE) as the matrix and low-density polyethylene (LDPE) coated BaO-Nd2O3-TiO2 (BNT) ceramic-powders as the filler. By incorporating LDPE into the composites via a coating route, high ceramic-powder volume content (up to 50 vol%) could be achieved. The composites exhibited good microwave dielectric and thermomechanical behaviors. As BNT ceramic content increased from 10 vol% to 50 vol%, the permittivity of the composites increased from 3.45 (9 GHz) to 11.87 (7 GHz), while the dielectric loss remained lower than 0.0016. Microstrip antennas for applications in global positioning systems (GPS) were designed and fabricated from the composites containing 50 vol% BNT ceramics. The results indicate that the composites that have suitable permittivity and low dielectric loss are promising candidates for applications in miniaturized microwave devices, such as antennas.

Mechanical and Tribological Characteristics of the AMC, Prepared by P/M Route along with Thermo-Mechanical Treatment

NASA Astrophysics Data System (ADS)

Mohapatra, Sambit Kumar; Maity, Kalipada; Bhuyan, Subrat Kumar; Prasad Satpathy, Mantra

2018-03-01

Thermo mechanical treatments have the ameliorated impacts on the mechanical and tribological properties of powder metallurgy components. In this investigation an aluminium matrix composite (AMC) {Al (92) + Mg (5) + Gr (1) + Ti (2)} has been prepared by following powder metallurgy technique, with double axial compaction and ulterior sintering. Secondary thermo-mechanical treatment i.e. hot extrusion through mathematical contoured cosine profiled die was considered. The die causes minimum velocity relative differences across the extrusion exit cross-section, which provides smooth material flow. Comparative result analysis for the mechanical and tribological characteristics of the specimen before and after extrusion was concentrated. Extrusion engenders significant amount of improvements of the properties those are attributed to excellent bond strength and uniform density distribution due to high compressive stress. Oxidative and delaminated wear mechanisms were found predominating type. To furnish the suitable explanation scanning electron microscopies have been performed for the wear surfaces.

The preparation of Zr-deuteride and phase stability studies of the Zr-D system

NASA Astrophysics Data System (ADS)

Maimaitiyili, T.; Steuwer, A.; Bjerkén, C.; Blomqvist, J.; Hoelzel, M.; Ion, J. C.; Zanellato, O.

2017-03-01

Deuteride phases in the zirconium-deuterium system in the temperature range 25-286 °C have been studied in-situ by high resolution neutron diffraction. The study primarily focused on observations of δ→γ transformation at 180 °C, and the peritectoid reaction α + δ ↔ γ at 255 °C in commercial grade Zr powder that was deuterated to a deuterium/Zr ratio of one to one. A detailed description of the zirconium deuteride preparation route by high temperature gas loading is also described. The lattice parameters of α-Zr, δ-ZrDx and ε-ZrDx were determined by whole pattern crystal structure analysis, using Rietveld and Pawley refinements, and are in good agreement with values reported in the literature. The controversial γ-hydride phase was observed both in-situ and ex-situ in deuterated Zr powder after a heat treatment at 286 °C and slow cooling.

Synthesis of thoria nano-particles at low temperature through base electrogeneration on steel 316L surface: Effect of current density

NASA Astrophysics Data System (ADS)

Yousefi, Taher; Torab-Mostaedi, Meisam; Mobtaker, Hossein Ghasemi; Keshtkar, Ali Reza

2016-10-01

The strategy developed in this study, offers significant advantages (simplicity and cleanness of method and also a product purity and new morphology of the product) over the conventional routes for the synthesis of ThO2 nanostructure. The effect of current density on morphology was studied. The synthesized powder was characterized by means of Powder X-ray Diffraction (PXRD), Transmission Electron Microscopy (TEM, Phillips EM 2085) Brunauer-Emmett-Teller (BET) and Fourier Transform Infrared (FT-IR) spectroscopy. The results show that the current density has a great effect on the morphology of the samples. The average size of the particles decreases as the applied current density increases and the average size of the samples decreases from 50 to 15 nm when the current density increases from 2 to 5 mA cm-2.

Effects of Coating Materials and Processing Conditions on Flow Enhancement of Cohesive Acetaminophen Powders by High-Shear Processing With Pharmaceutical Lubricants.

PubMed

Wei, Guoguang; Mangal, Sharad; Denman, John; Gengenbach, Thomas; Lee Bonar, Kevin; Khan, Rubayat I; Qu, Li; Li, Tonglei; Zhou, Qi Tony

2017-10-01

This study has investigated the surface coating efficiency and powder flow improvement of a model cohesive acetaminophen powder by high-shear processing with pharmaceutical lubricants through 2 common equipment, conical comil and high-shear mixer. Effects of coating materials and processing parameters on powder flow and surface coating coverage were evaluated. Both Carr's index and shear cell data indicated that processing with the lubricants using comil or high-shear mixer substantially improved the flow of the cohesive acetaminophen powder. Flow improvement was most pronounced for those processed with 1% wt/wt magnesium stearate, from "cohesive" for the V-blended sample to "easy flowing" for the optimally coated sample. Qualitative and quantitative characterizations demonstrated a greater degree of surface coverage for high-shear mixing compared with comilling; nevertheless, flow properties of the samples at the corresponding optimized conditions were comparable between 2 techniques. Scanning electron microscopy images demonstrated different coating mechanisms with magnesium stearate or l-leucine (magnesium stearate forms a coating layer and leucine coating increases surface roughness). Furthermore, surface coating with hydrophobic magnesium stearate did not retard the dissolution kinetics of acetaminophen. Future studies are warranted to evaluate tableting behavior of such dry-coated pharmaceutical powders. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Self-sharpening-effect of nickel-diamond coatings sprayed by HVOF

NASA Astrophysics Data System (ADS)

Tillmann, W.; Brinkhoff, A.; Schaak, C.; Zajaczkowski, J.

2017-03-01

The durability of stone working and drilling tools is an increasingly significant requirement in industrial applications. These tools are mainly produced by brazing diamond metal matrix composites inserts to the tool body. These inserts are produced by sintering diamonds and metal powder (e.g. nickel). If the wear is too high, the diamonds will break out of the metal matrix and other diamonds will be uncovered. This effect is called self-sharpening. But diamonds are difficult to handle because of their thermal sensitivity. Due to their high thermal influence, manufacturing costs, and complicate route of manufacturing (first sintering, then brazing), there is a great need for alternative production methods for such tools. One alternative to produce wear-resistant and self-sharpening coatings are thermal spray processes as examined in this paper. An advantage of thermal spray processes is their smaller thermal influence on the diamond, due to the short dwelling time in the flame. To reduce the thermal influence during spraying, nickel coated diamonds were used in the HVOF-process (high velocity oxygen fuel process). The wear resistance was subsequently investigated by means of a standardized ball-on-disc test. Furthermore, a SEM (scanning electron microscope) was used to gain information about the wear-mechanism and the self-sharpening effect of the coating.

Slip casting nano-particle powders for making transparent ceramics

DOEpatents

Kuntz, Joshua D [Livermore, CA; Soules, Thomas F [Livermore, CA; Landingham, Richard Lee [Livermore, CA; Hollingsworth, Joel P [Oakland, CA

2011-04-12

A method of making a transparent ceramic including the steps of providing nano-ceramic powders in a processed or unprocessed form, mixing the powders with de-ionized water, the step of mixing the powders with de-ionized water producing a slurry, sonifing the slurry to completely wet the powder and suspend the powder in the de-ionized water, separating very fine particles from the slurry, molding the slurry, and curing the slurry to produce the transparent ceramic.

System Applies Polymer Powder To Filament Tow

NASA Technical Reports Server (NTRS)

Baucom, Robert M.; Snoha, John J.; Marchello, Joseph M.

1993-01-01

Polymer powder applied uniformly and in continuous manner. Powder-coating system applies dry polymer powder to continuous fiber tow. Unique filament-spreading technique, combined with precise control of tension on fibers in system, ensures uniform application of polymer powder to web of spread filaments. Fiber tows impregnated with dry polymer powders ("towpregs") produced for preform-weaving and composite-material-molding applications. System and process valuable to prepreg industry, for production of flexible filament-windable tows and high-temperature polymer prepregs.

Diversity and Antibiotic Susceptibility of Acinetobacter Strains From Milk Powder Produced in Germany

PubMed Central

Cho, Gyu-Sung; Li, Bo; Rostalsky, André; Fiedler, Gregor; Rösch, Niels; Igbinosa, Etinosa; Kabisch, Jan; Bockelmann, Wilhelm; Hammer, Philipp; Huys, Geert; Franz, Charles M. A. P.

2018-01-01

Forty-seven Acinetobacter spp. isolates from milk powder obtained from a powdered milk producer in Germany were investigated for their antibiotic resistance susceptibilities, in order to assess whether strains from food harbor multiple antibiotic resistances and whether the food route is important for dissemination of resistance genes. The strains were identified by 16S rRNA and rpoB gene sequencing, as well as by whole genome sequencing of selected isolates and their in silico DNA-DNA hybridization (DDH). Furthermore, they were genotyped by rep-PCR together with reference strains of pan-European groups I, II, and III strains of Acinetobacter baumannii. Of the 47 strains, 42 were identified as A. baumannii, 4 as Acinetobacter Pittii, and 1 as Acinetobacter calcoaceticus based on 16S rRNA gene sequencing. In silico DDH with the genome sequence data of selected strains and rpoB gene sequencing data suggested that the five non-A. baumannii strains all belonged to A. pittii, suggesting that the rpoB gene is more reliable than the 16S rRNA gene for species level identification in this genus. Rep-PCR genotyping of the A. baumannii strains showed that these could be grouped into four groups, and that some strains clustered together with reference strains of pan-European clinical group II and III strains. All strains in this study were intrinsically resistant toward chloramphenicol and oxacillin, but susceptible toward tetracycline, tobramycin, erythromycin, and ciprofloxacin. For cefotaxime, 43 strains (91.5%) were intermediate and 3 strains (6.4%) resistant, while 3 (6.4%) and 21 (44.7%) strains exhibited resistance to cefepime and streptomycin, respectively. Forty-six (97.9%) strains were susceptible to amikacin and ampicillin-sulbactam. Therefore, the strains in this study were generally not resistant to the clinically relevant antibiotics, especially tobramycin, ciprofloxacin, cefepime, and meropenem, suggesting that the food route probably poses only a low risk for multidrug resistant Acinetobacter strains or resistance genes. PMID:29636733

Process for microwave sintering boron carbide

DOEpatents

Holcombe, C.E.; Morrow, M.S.

1993-10-12

A method of microwave sintering boron carbide comprises leaching boron carbide powder with an aqueous solution of nitric acid to form a leached boron carbide powder. The leached boron carbide powder is coated with a glassy carbon precursor to form a coated boron carbide powder. The coated boron carbide powder is consolidated in an enclosure of boron nitride particles coated with a layer of glassy carbon within a container for microwave heating to form an enclosed coated boron carbide powder. The enclosed coated boron carbide powder is sintered within the container for microwave heating with microwave energy.

Process for microwave sintering boron carbide

DOEpatents

Holcombe, Cressie E.; Morrow, Marvin S.

1993-01-01

A method of microwave sintering boron carbide comprises leaching boron carbide powder with an aqueous solution of nitric acid to form a leached boron carbide powder. The leached boron carbide powder is coated with a glassy carbon precursor to form a coated boron carbide powder. The coated boron carbide powder is consolidated in an enclosure of boron nitride particles coated with a layer of glassy carbon within a container for microwave heating to form an enclosed coated boron carbide powder. The enclosed coated boron carbide powder is sintered within the container for microwave heating with microwave energy.

21 CFR 176.350 - Tamarind seed kernel powder.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 3 2014-04-01 2014-04-01 false Tamarind seed kernel powder. 176.350 Section 176... Paperboard § 176.350 Tamarind seed kernel powder. Tamarind seed kernel powder may be safely used as a component of articles intended for use in producing, manufacturing, packing, processing, preparing, treating...

Preparation and Wear Resistance of Aluminum Composites Reinforced with In Situ Formed TiO/Al2O3

NASA Astrophysics Data System (ADS)

Qin, Q. D.; Huang, B. W.; Li, W.; Zeng, Z. Y.

2016-05-01

An in situ TiO/Al2O3-reinforced Al composite is successfully prepared using a powder metallurgy route by the reaction of Ti2CO and Al powder. The Ti2CO powder is produced by carrying out a carbothermic reduction of titanium dioxide at 1000 °C. XRD results show that the final product is composed of Al, TiO, Al2O3, and Al3Ti. Morphology examination of the composite reveals the presence of bigger blocks of TiO and fine particles of Al2O3 and the volume fraction of reinforcement is found to range between 18 and 55%. As the volume fraction of the reinforced materials approaches 50%, the particles start to agglomerate. Dry sliding wear tests conducted using a conventional pin-on-disk testing machine show that the wear resistance of the composite is higher than that of the pure aluminum ingot. The wear rate of the composite increases almost linearly with the increase in the wear distance. The sliding wear test shows that as the volume fraction of the reinforced phase increases, the coefficient of friction decreases. The wear mechanism is also discussed.

EXAFS Study on LiFePO4 Powders Produced From Two Sol-Gel Routes

NASA Astrophysics Data System (ADS)

Negara, V. S. I.; Latif, C.; Wongtepa, W.; Pratapa, S.

2018-04-01

The local structure of LiFePO4 powders has been investigated using Fe K-edge Extended X-Ray Absorption Fine Structure (EXAFS) Spectroscopy data. The synthesis of LFP powders was carried out using two different sol-gel methods. The raw materials for Fe source were ironstone and commercial precursor of FeCl2·4H2O. Synthesis using natural materials produced two phases, namely LiFePO4 olivine and Li3Fe2(PO4)3 nasicon, whereas that using a commercial product produced a single phase of LiFePO4 olivine. The EXAFS data for both samples were collected at Synchrotron Light Research Institute (SLRI), Thailand. Fitting of the model on the experimental curve provided parameters that can be interpreted as the distance between Fe as the absorber and the nearest atoms on the LFP materials. The EXAFS data analysis has shown that synthesis of LFPs using different Fe sources gives slightly different nearest-neighbor distances, namely Fe-O of 0.21% -0.23%, Fe-P of 0.14% - 0.16%, Fe-Fe of 0.12% for both samples, respectively.

Investigation on structural properties of M-type strontium hexaferrite synthesized in presence of neem and aloe-vera plant leaves extract

NASA Astrophysics Data System (ADS)

Solanki, Neha; Jotania, Rajshree B.

2017-05-01

M-type strontium hexaferrite powder samples were synthesized using a green synthesis route with and without presence of Aloe vera and Neem leaves extract. The dry brownish precursors of strontium hexaferrite were recovered from a mixed solution of metal salts and leaves extract, heated at 100 °C. The obtained precursors were pre-heated at 500 °C for 4 hrs. followed by final heating at 950 °C for 4 hrs. in a muffle furnace to obtain SrFe12O19 hexaferrite powder. The obtained SrFe12O19 hexaferrite powder samples characterized at room temperature in order to check phase purity and structural properties. XRD analysis confirms that samples prepared without and with Aloe vera leaves extract (heated at 950 °C for 4 hrs.) show formation of α-Fe2O3 and M-phase; while the sample prepared in presence of Neem leaves extract (heated at 950 °C for 4 hrs.) show formation of mono phase of strontium hexaferrite. Lattice parameter (a) and cell volume (V) are found to increase in the samples prepared in presence of Aloe vera and Neem leaves extract.

Energy-Saving Sintering of Electrically Conductive Powders by Modified Pulsed Electric Current Heating Using an Electrically Nonconductive Die

NASA Astrophysics Data System (ADS)

Ito, Mikio; Kawahara, Kenta; Araki, Keita

2014-04-01

Sintering of Cu and thermoelectric Ca3Co4O9 was tried using a modified pulsed electric current sintering (PECS) process, where an electrically nonconductive die was used instead of a conventional graphite die. The pulsed electric current flowed through graphite punches and sample powder, which caused the Joule heating of the powder compact itself, resulting in sintering under smaller power consumption. Especially for the Ca3Co4O9 powder, densification during sintering was also accelerated by this modified PECS process.

A Dry Powder Process for Preparing Uni-Tape Prepreg from Polymer Powder Coated Filamentary Towpregs

NASA Technical Reports Server (NTRS)

Wilkinson, Steven P. (Inventor); Johnston, Norman J. (Inventor); Marchello, Joseph M. (Inventor)

1995-01-01

A process for preparing uni-tape prepreg from polymer powder coated filamentary towpregs is provided. A plurality of polymer powder coated filamentary towpregs are provided. The towpregs are collimated so that each towpreg is parallel. The sandwich is heated to a temperature wherein the polymer flows and intimately contacts the filaments and pressure is repeatedly applied perpendicularly to the sandwich with a longitudinal oscillating action wherein the filaments move apart and the polymer wets the filaments forming a uni-tape prepreg. The uni-tape prepreg is subsequently cooled.

Powder Metallurgy Reconditioning of Food and Processing Equipment Components

NASA Astrophysics Data System (ADS)

Nafikov, M. Z.; Aipov, R. S.; Konnov, A. Yu.

2017-12-01

A powder metallurgy method is developed to recondition the worn surfaces of food and processing equipment components. A combined additive is composed to minimize the powder losses in sintering. A technique is constructed to determine the powder consumption as a function of the required metallic coating thickness. A rapid method is developed to determine the porosity of the coating. The proposed technology is used to fabricate a wear-resistant defectless metallic coating with favorable residual stresses, and the adhesive strength of this coating is equal to the strength of the base metal.

Genotyping and Source Tracking of Cronobacter sakazakii and C. malonaticus Isolates from Powdered Infant Formula and an Infant Formula Production Factory in China

PubMed Central

Fei, Peng; Man, Chaoxin; Lou, Binbin; Forsythe, Stephen J.; Chai, Yunlei; Li, Ran; Niu, Jieting

2015-01-01

Cronobacter spp. (formerly defined as Enterobacter sakazakii) are opportunistic bacterial pathogens of both infants and adults. In this study, we analyzed 70 Cronobacter isolates from powdered infant formula (PIF) and an infant formula production facility in China to determine possible contamination routes. The strains were profiled by multilocus sequence typing (MLST), pulsed-field gel electrophoresis (PFGE), PCR-based O-antigen serotyping, and ompA and rpoB sequence analyses. The isolates were primarily Cronobacter sakazakii (66/70) or Cronobacter malonaticus (4/70). The strains were divided into 38 pulsotypes (PTs) using PFGE and 19 sequence types (STs) by MLST. In contrast, rpoB and ompA sequence analyses divided the strains into 10 overlapping clusters each. PCR serotyping of the 66 C. sakazakii and 4 C. malonaticus strains resulted in the identification of four C. sakazakii serotypes (O1, O2, O4, and O7) and a single C. malonaticus serotype, O2. The dominant C. sakazakii sequence types from PIF and an infant formula production factory in China were C. sakazakii clonal complex 4 (CC4) (n = 19), ST1 (n = 14), and ST64 (n = 11). C. sakazakii CC4 is a clonal lineage strongly associated with neonatal meningitis. In the process of manufacturing PIF, the spray-drying, fluidized-bed-drying, and packing areas were the main areas with Cronobacter contamination. C. sakazakii strains with the same pulsotypes (PT3 and PT2) and sequence types (ST1 and ST64) were isolated both from processing equipment and from the PIF finished product. PMID:26048942

Genotyping and Source Tracking of Cronobacter sakazakii and C. malonaticus Isolates from Powdered Infant Formula and an Infant Formula Production Factory in China.

PubMed

Fei, Peng; Man, Chaoxin; Lou, Binbin; Forsythe, Stephen J; Chai, Yunlei; Li, Ran; Niu, Jieting; Jiang, Yujun

2015-08-15

Cronobacter spp. (formerly defined as Enterobacter sakazakii) are opportunistic bacterial pathogens of both infants and adults. In this study, we analyzed 70 Cronobacter isolates from powdered infant formula (PIF) and an infant formula production facility in China to determine possible contamination routes. The strains were profiled by multilocus sequence typing (MLST), pulsed-field gel electrophoresis (PFGE), PCR-based O-antigen serotyping, and ompA and rpoB sequence analyses. The isolates were primarily Cronobacter sakazakii (66/70) or Cronobacter malonaticus (4/70). The strains were divided into 38 pulsotypes (PTs) using PFGE and 19 sequence types (STs) by MLST. In contrast, rpoB and ompA sequence analyses divided the strains into 10 overlapping clusters each. PCR serotyping of the 66 C. sakazakii and 4 C. malonaticus strains resulted in the identification of four C. sakazakii serotypes (O1, O2, O4, and O7) and a single C. malonaticus serotype, O2. The dominant C. sakazakii sequence types from PIF and an infant formula production factory in China were C. sakazakii clonal complex 4 (CC4) (n = 19), ST1 (n = 14), and ST64 (n = 11). C. sakazakii CC4 is a clonal lineage strongly associated with neonatal meningitis. In the process of manufacturing PIF, the spray-drying, fluidized-bed-drying, and packing areas were the main areas with Cronobacter contamination. C. sakazakii strains with the same pulsotypes (PT3 and PT2) and sequence types (ST1 and ST64) were isolated both from processing equipment and from the PIF finished product. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

Consumer acceptability and sensory profile of cooked broccoli with mustard seeds added to improve chemoprotective properties.

PubMed

Ghawi, Sameer Khalil; Shen, Yuchi; Niranjan, Keshavan; Methven, Lisa

2014-09-01

Broccoli, a rich source of glucosinolates, is a commonly consumed vegetable of the Brassica family. Hydrolysis products of glucosinolates, isothiocyanates, have been associated with health benefits and contribute to the flavor of Brassica. However, boiling broccoli causes the myrosinase enzyme needed for hydrolysis to denature. In order to ensure hydrolysis, broccoli must either be mildly cooked or active sources of myrosinase, such as mustard seed powder, can be added postcooking. In this study, samples of broccoli were prepared in 6 different ways; standard boiling, standard boiling followed by the addition of mustard seeds, sous vide cooking at low temperature (70 °C) and sous vide cooking at higher temperature (100 °C) and sous vide cooking at higher temperature followed by the addition of mustard seeds at 2 different concentrations. The majority of consumers disliked the mildly cooked broccoli samples (70 °C, 12 min, sous vide) which had a hard and stringy texture. The highest mean consumer liking was for standard boiled samples (100 °C, 7 min). Addition of 1% mustard seed powder developed sensory attributes, such as pungency, burning sensation, mustard odor, and flavor. One cluster of consumers (32%) found mustard seeds to be a good complement to cooked broccoli; however, the majority disliked the mustard-derived sensory attributes. Where the mustard seeds were partially processed, doubling the addition to 2% led to only the same level of mustard and pungent flavors as 1% unprocessed seeds, and mean consumer liking remained unaltered. This suggests that optimization of the addition level of partially processed mustard seeds may be a route to enhance bioactivity of cooked broccoli without compromising consumer acceptability. © 2014 Institute of Food Technologists®

NASA. Langley Research Center dry powder towpreg system

NASA Technical Reports Server (NTRS)

Baucom, Robert M.; Marchello, Joseph M.

1990-01-01

Dry powder polymer impregnated carbon fiber tows were produced for preform weaving and composite materials molding applications. In the process, fluidized powder is deposited on spread tow bundles and melted on the fibers by radiant heating to adhere the polymer to the fiber. Unit design theory and operating correlations were developed to provide the basis for scale up of the process to commercial operation. Special features of the operation are the pneumatic tow spreader, fluidized bed, resin feeder, and quality control system. Bench scale experiments, at tow speeds up to 50 cm/sec, demonstrated that process variables can be controlled to produce weavable LARC-TPI carbon fiber towpreg. The towpreg made by the dry powder process was formed into unidirectional fiber moldings and was woven and molded into preform material of good quality.

Process for synthesizing compounds from elemental powders and product

DOEpatents

Rabin, B.H.; Wright, R.N.

1993-12-14

A process for synthesizing intermetallic compounds from elemental powders is described. The elemental powders are initially combined in a ratio which approximates the stoichiometric composition of the intermetallic compound. The mixed powders are then formed into a compact which is heat treated at a controlled rate of heating such that an exothermic reaction between the elements is initiated. The heat treatment may be performed under controlled conditions ranging from a vacuum (pressureless sintering) to compression (hot pressing) to produce a desired densification of the intermetallic compound. In a preferred form of the invention, elemental powders of Fe and Al are combined to form aluminide compounds of Fe[sub 3] Al and FeAl. 25 figures.

Process for synthesizing compounds from elemental powders and product

DOEpatents

Rabin, Barry H.; Wright, Richard N.

1993-01-01

A process for synthesizing intermetallic compounds from elemental powders. The elemental powders are initially combined in a ratio which approximates the stoichiometric composition of the intermetallic compound. The mixed powders are then formed into a compact which is heat treated at a controlled rate of heating such that an exothermic reaction between the elements is initiated. The heat treatment may be performed under controlled conditions ranging from a vacuum (pressureless sintering) to compression (hot pressing) to produce a desired densification of the intermetallic compound. In a preferred form of the invention, elemental powders of Fe and Al are combined to form aluminide compounds of Fe.sub.3 Al and FeAl.

A Family of ACO Routing Protocols for Mobile Ad Hoc Networks.

PubMed

Rupérez Cañas, Delfín; Sandoval Orozco, Ana Lucila; García Villalba, Luis Javier; Kim, Tai-Hoon

2017-05-22

In this work, an ACO routing protocol for mobile ad hoc networks based on AntHocNet is specified. As its predecessor, this new protocol, called AntOR, is hybrid in the sense that it contains elements from both reactive and proactive routing. Specifically, it combines a reactive route setup process with a proactive route maintenance and improvement process. Key aspects of the AntOR protocol are the disjoint-link and disjoint-node routes, separation between the regular pheromone and the virtual pheromone in the diffusion process and the exploration of routes, taking into consideration the number of hops in the best routes. In this work, a family of ACO routing protocols based on AntOR is also specified. These protocols are based on protocol successive refinements. In this work, we also present a parallelized version of AntOR that we call PAntOR. Using programming multiprocessor architectures based on the shared memory protocol, PAntOR allows running tasks in parallel using threads. This parallelization is applicable in the route setup phase, route local repair process and link failure notification. In addition, a variant of PAntOR that consists of having more than one interface, which we call PAntOR-MI (PAntOR-Multiple Interface), is specified. This approach parallelizes the sending of broadcast messages by interface through threads.

Investigation of metal ions sorption of brown peat moss powder

NASA Astrophysics Data System (ADS)

Kelus, Nadezhda; Blokhina, Elena; Novikov, Dmitry; Novikova, Yaroslavna; Chuchalin, Vladimir

2017-11-01

For regularities research of sorptive extraction of heavy metal ions by cellulose and its derivates from aquatic solution of electrolytes it is necessary to find possible mechanism of sorption process and to choice a model describing this process. The present article investigates the regularities of aliovalent metals sorption on brown peat moss powder. The results show that sorption isotherm of Al3+ ions is described by Freundlich isotherm and sorption isotherms of Na+ i Ni2+ are described by Langmuir isotherm. To identify the mechanisms of brown peat moss powder sorption the IR-spectra of the initial brown peat moss powder samples and brown peat moss powder samples after Ni (II) sorption were studied. Metal ion binding mechanisms by brown peat moss powder points to ion exchange, physical adsorption, and complex formation with hydroxyl and carboxyl groups.

Effects of red pepper powder on microbial communities and metabolites during kimchi fermentation.

PubMed

Jeong, Sang Hyeon; Lee, Hyo Jung; Jung, Ji Young; Lee, Se Hee; Seo, Hye-Young; Park, Wan-Soo; Jeon, Che Ok

2013-01-01

To investigate the effects of red pepper powder on kimchi fermentation, Baechu (Chinese cabbage) and Mu (radish) kimchi, with and without red pepper powder, were prepared and their characteristics, including pH, colony-forming units (CFU), microbial communities, and metabolites, were periodically monitored for 40days. Measurements of pH and CFU showed that the lag phases of kimchi fermentation were clearly extended by the addition of red pepper powder. Microbial community analysis using a barcoded pyrosequencing analysis showed that the bacterial diversities in kimchi with red pepper powder decreased more slowly than kimchi without red pepper powder as kimchi fermentation progressed. The kimchi microbial communities were represented mainly by the genera Leuconostoc and Lactobacillus in all kimchi, and the abundance of Weissella was negligible in kimchi without red pepper powder. However, interestingly, kimchi with red pepper powder contained much higher proportions of Weissella than kimchi without red pepper powder, while the proportions of Leuconostoc and Lactobacillus were evidently lower in kimchi with red pepper powder compared to kimchi without red pepper powder. Metabolite analysis using a (1)H NMR technique also showed that the fermentation of kimchi with red pepper powder progressed a little more slowly than that of kimchi without red pepper powder. Principle component analysis using microbial communities and metabolites supported the finding that the addition of red pepper powder into kimchi resulted in the slowing of the kimchi fermentation process, especially during the early fermentation period and influenced the microbial succession and metabolite production during the kimchi fermentation processes. Copyright © 2012 Elsevier B.V. All rights reserved.

Facile synthesis of multi-shell structured binary metal oxide powders with a Ni/Co mole ratio of 1:2 for Li-Ion batteries

NASA Astrophysics Data System (ADS)

Choi, Seung Ho; Park, Sun Kyu; Lee, Jung-Kul; Kang, Yun Chan

2015-06-01

Multi-shell structured binary transition metal oxide powders with a Ni/Co mole ratio of 1:2 are prepared by a simple spray drying process. Precursor powder particles prepared by spray drying from a spray solution of citric acid and ethylene glycol have completely spherical shape, fine size, and a narrow size distribution. The precursor powders turn into multi-shell powders after a post heat-treatment at temperatures between 250 and 800 °C. The multi-shell structured powders are formed by repeated combustion and contraction processes. The multi-shell powders have mixed crystal structures of Ni1-xCo2O4-x and NiO phases regardless of the post-treatment temperature. The reversible capacities of the powders post-treated at 250, 400, 600, and 800 °C after 100 cycles are 584, 913, 808, and 481 mA h g-1, respectively. The low charge transfer resistance and high lithium ion diffusion rate of the multi-shell powders post-treated at 400 °C with optimum grain size result in superior electrochemical properties even at high current densities.

Improved Production Of Wrought Articles From Powders

NASA Technical Reports Server (NTRS)

Thomas, James R.; Singleton, Ogle R.

1994-01-01

Improved technique for consolidation of powders into dense articles developed. Peripheral bands used in consolidation, forging, and rolling operations. Facilitates consolidation of dispersion-hardened aluminous powders and composite mixtures for processing to such useful wrought articles as plates and sheets. Potential use in production of plates and sheets and perhaps other objects from "hard" powders, particularly from powders, objects made from which have propensity to crack when mechanically worked to other forms.

Experimental Equipment for Powder Processing

DTIC Science & Technology

2009-08-20

for a series of alumina and zirconia powder mixtures by TMDAR, CR-15 (alumina), as well as TZ3YS and CERAC-2003 (zirconia). The proportion of TMDAR...is known to cause abnormal grain growth. Fig.15 shows the seven representative curves obtained for our zirconia powder system. The 10% and 20...various zirconia powder mixtures. The maximum densification rate for each of our zirconia powder mixtures occurs within the relative density range of

Development of an Efficient Micro-Heat Exchanger: The Integration of Design Processing and Testing

DTIC Science & Technology

2005-11-01

together at high temperatures and cooled to room temperature. Additionally, alumina and zirconia powders have a major difference in densification...efficient heat exchanger. The main problem that needed to be resolved was the fact that the zirconia powders shrink much more than alumina powder...been measured. Our measurement in dimensions verifies that zirconia powders shrink substantially more than alumina powder except CR-15 after final

Effect of synthesis process on the microstructure and electrical conductivity of nickel/yttria-stabilized zirconia powders prepared by urea hydrolysis

NASA Astrophysics Data System (ADS)

Lin, Jyung-Dong; Wu, Zhao-Lun

In this study, NiO/YSZ composite powders were synthesized using hydrolysis on two solutions, one contains YSZ particles and Ni 2+ ion, and the other contains NiO particles, Zr 4+, and Y 3+ ions, with the aid of urea. The microstructure of the powders and sintered bulks was further characterized using X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The results indicated that various synthesis processes yielded NiO/YSZ powders with different morphologies. The NiO precursors would deposit onto the surface of YSZ particles, and NiO-deposited YSZ composite powders were obtained. Alternatively, it was not observed that YSZ precursors deposited onto the surface of NiO particles, thus, a uniform powder mixture of fine NiO and fine YSZ particles was produced. After sintering and subsequent reduction, these powders would lead to the variations of Ni distribution in the YSZ matrix and conductivity of cermets. Owing to the core-shell structure of the powders and the higher size ratio of YSZ and NiO particles, the conductivity of cermet with NiO-deposited YSZ powders containing 23 wt% NiO is comparable to those with a NiO/YSZ powder mixture containing 50 wt% NiO.

Nitride Fuel Development Using Cryo-process Technique

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

O'Brien, Brandi M; Windes, William E

A new cryo-process technique has been developed for the fabrication of advanced fuel for nuclear systems. The process uses a new cryo-processing technique whereby small, porous microspheres (<2000 µm) are formed from sub-micron oxide powder. A simple aqueous particle slurry of oxide powder is pumped through a microsphere generator consisting of a vibrating needle with controlled amplitude and frequency. As the water-based droplets are formed and pass through the microsphere generator they are frozen in a bath of liquid nitrogen and promptly vacuum freeze-dried to remove the water. The resulting porous microspheres consist of half micron sized oxide particles heldmore » together by electrostatic forces and mechanical interlocking of the particles. Oxide powder microspheres ranging from 750 µm to 2000 µm are then converted into a nitride form using a high temperature fluidized particle bed. Carbon black can be added to the oxide powder before microsphere formation to augment the carbothermic reaction during conversion to a nitride. Also, the addition of ethyl alcohol to the aqueous slurry reduces the surface tension energy of the droplets resulting in even smaller droplets forming in the microsphere generator. Initial results from this new process indicate a lower impurity contamination in the final nitrides due to the single feed stream of particles, material handling and conversion are greatly simplified, a minimum of waste and personnel exposure are anticipated, and finally the conversion kinetics may be greatly increased because of the small oxide powder size (sub-micron) forming the porous microsphere. Thus far the fabrication process has been successful in demonstrating all of these improvements with surrogate ZrO2 powder. Further tests will be conducted in the future using the technique on UO2 powders.« less

Evaluation of dairy powder products implicates thermophilic sporeformers as the primary organisms of interest.

PubMed

Watterson, M J; Kent, D J; Boor, K J; Wiedmann, M; Martin, N H

2014-01-01

Dairy powder products (e.g., sweet whey, nonfat dry milk, acid whey, and whey protein concentrate-80) are of economic interest to the dairy industry. According to the US Dairy Export Council, customers have set strict tolerances (<500 to <1,000/g) for thermophilic and mesophilic spores in dairy powders; therefore, understanding proliferation and survival of sporeforming organisms within dairy powder processing plants is necessary to control and reduce sporeformer counts. Raw, work-in-process, and finished product samples were collected from 4 dairy powder processing facilities in the northeastern United States over a 1-yr period. Two separate spore treatments: (1) 80°C for 12min (to detect sporeformers) and (2) 100°C for 30min (to detect highly heat resistant sporeformers) were applied to samples before microbiological analyses. Raw material, work-in-process, and finished product samples were analyzed for thermophilic, mesophilic, and psychrotolerant sporeformers, with 77.5, 71.0, and 4.6% of samples being positive for those organisms, respectively. Work-in-process and finished product samples were also analyzed for highly heat resistant thermophilic and mesophilic sporeformers, with 63.7 and 42.6% of samples being positive, respectively. Sporeformer prevalence and counts varied considerably by product and plant; sweet whey and nonfat dry milk showed a higher prevalence of thermophilic and mesophilic sporeformers compared with acid whey and whey protein concentrate-80. Unlike previous reports, we found limited evidence for increased spore counts toward the end of processing runs. Our data provide important insight into spore contamination patterns associated with production of different types of dairy powders and support that thermophilic sporeformers are the primary organism of concern in dairy powders. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Dry particle coating of polymer particles for tailor-made product properties

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

Blümel, C., E-mail: karl-ernst.wirth@fau.de; Schmidt, J., E-mail: karl-ernst.wirth@fau.de; Dielesen, A., E-mail: karl-ernst.wirth@fau.de

2014-05-15

Disperse polymer powders with tailor-made particle properties are of increasing interest in industrial applications such as Selective Laser Beam Melting processes (SLM). This study focuses on dry particle coating processes to improve the conductivity of the insulating polymer powder in order to assemble conductive devices. Therefore PP particles were coated with Carbon Black nanoparticles in a dry particle coating process. This process was investigated in dependence of process time and mass fraction of Carbon Black. The conductivity of the functionalized powders was measured by impedance spectroscopy. It was found that there is a dependence of process time, respectively coating ratiomore » and conductivity. The powder shows higher conductivities with increasing number of guest particles per host particle surface area, i.e. there is a correlation between surface functionalization density and conductivity. The assembled composite particles open new possibilities for processing distinct polymers such as PP in SLM process. The fundamentals of the dry particle coating process of PP host particles with Carbon Black guest particles as well as the influence on the electrical conductivity will be discussed.« less

The microstructure-processing-property relationships in an aluminum matrix composite system reinforced by aluminum-copper-iron alloy particles

NASA Astrophysics Data System (ADS)

Tang, Fei

Solid state vacuum sintering was studied in tap densified Al powder and in hot quasi-isostatically forged samples composed of commercial inert gas atomized or high purity Al powder, generated by a gas atomization reaction synthesis (GARS) technique. The GARS process results in spherical Al powder with a far thinner surface oxide. The overall results indicated the enhanced ability of GARS-processed Al and Al alloy powders for solid state sintering, which may lead to simplification of current Al powder consolidation processing methods. Elemental Al-based composites reinforced with spherical Al-Cu-Fe alloy powders were produced by quasi-isostatic forging and vacuum hot pressing (VHP) consolidation methods. It was proved that spherical Al-Cu-Fe alloy powders can serve as an effective reinforcement particulate for elemental Al-based composites, because of their high hardness and a preferred type of matrix/reinforcement interfacial bonding, with reduced strain concentration around the particles. Ultimate tensile strength and yield strength of the composites were increased over the corresponding Al matrix values, far beyond typical observations. This remarkable strengthening was achieved without precipitation hardening and without severe strain hardening during consolidation because of the matrix choice (elemental Al) and the "low shear" consolidation methods utilized. This reinforcement effectiveness is further evidenced by elastic modulus measurements of the composites that are very close to the upper bound predictions of the rule of mixtures. The load partitioning measurements by neutron diffraction showed that composite samples made from GARS powders present significantly higher load transfer efficiency than the composites made from commercially atomized powders. Further analysis of the load sharing measurements and the calculated values of the mismatch of coefficient of thermal expansion (CTE) and the geometrically necessary dislocation (GND) effects suggest that these strengthening mechanisms can be combined to predict accurately the strength of the composites. By neutron diffraction measurements, it also was found that the composites consolidated from Al and Al63Cu25Fe12 quasicrystal alloy reinforcement powders have compressive residual stress in the Al matrix, contrary to the tensile residual stress in typical Al/SiC composites. The composites made by the quasi-isostatic forging process exhibited higher tensile strengths and much higher compressive residual stresses than the composites made by the VHP process.

Ceramic components manufacturing by selective laser sintering

NASA Astrophysics Data System (ADS)

Bertrand, Ph.; Bayle, F.; Combe, C.; Goeuriot, P.; Smurov, I.

2007-12-01

In the present paper, technology of selective laser sintering/melting is applied to manufacture net shaped objects from pure yttria-zirconia powders. Experiments are carried out on Phenix Systems PM100 machine with 50 W fibre laser. Powder is spread by a roller over the surface of 100 mm diameter alumina cylinder. Design of experiments is applied to identify influent process parameters (powder characteristics, powder layering and laser manufacturing strategy) to obtain high-quality ceramic components (density and micro-structure). The influence of the yttria-zirconia particle size and morphology onto powder layering process is analysed. The influence of the powder layer thickness on laser sintering/melting is studied for different laser beam velocity V ( V = 1250-2000 mm/s), defocalisation (-6 to 12 mm), distance between two neighbour melted lines (so-called "vectors") (20-40 μm), vector length and temperature in the furnace. The powder bed density before laser sintering/melting also has significant influence on the manufactured samples density. Different manufacturing strategies are applied and compared: (a) different laser beam scanning paths to fill the sliced surfaces of the manufactured object, (b) variation of vector length (c) different strategies of powder layering, (d) temperature in the furnace and (e) post heat treatment in conventional furnace. Performance and limitations of different strategies are analysed applying the following criteria: geometrical accuracy of the manufactured samples, porosity. The process stability is proved by fabrication of 1 cm 3 volume cube.

Improved Small-Particle Powders for Plasma Spraying

NASA Technical Reports Server (NTRS)

Nguyen, QuynhGiao, N.; Miller, Robert A.; Leissler, George W.

2005-01-01

Improved small-particle powders and powder-processing conditions have been developed for use in plasma spray deposition of thermal-barrier and environmental barrier coatings. Heretofore, plasma-sprayed coatings have typically ranged in thickness from 125 to 1,800 micrometers. As explained below, the improved powders make it possible to ensure complete coverage of substrates at unprecedently small thicknesses of the order of 25 micrometers. Plasma spraying involves feeding a powder into a hot, high-velocity plasma jet. The individual powder particles melt in the plasma jet as they are propelled towards a substrate, upon which they splat to build up a coating. In some cases, multiple coating layers are required. The size range of the powder particles necessarily dictates the minimum thickness of a coating layer needed to obtain uniform or complete coverage. Heretofore, powder particle sizes have typically ranged from 40 to 70 micrometers; as a result, the minimum thickness of a coating layer for complete coverage has been about 75 micrometers. In some applications, thinner coatings or thinner coating layers are desirable. In principle, one can reduce the minimum complete-coverage thickness of a layer by using smaller powder particles. However, until now, when powder particle sizes have been reduced, the powders have exhibited a tendency to cake, clogging powder feeder mechanisms and feed lines. Hence, the main problem is one of synthesizing smaller-particle powders having desirable flow properties. The problem is solved by use of a process that begins with a spray-drying subprocess to produce spherical powder particles having diameters of less than 30 micrometers. (Spherical-particle powders have the best flow properties.) The powder is then passed several times through a commercial sifter with a mesh to separate particles having diameters less than 15 micrometers. The resulting fine, flowable powder is passed through a commercial fluidized bed powder feeder into a plasma spray jet.

A Novel Process for Joining Ti Alloy and Al Alloy using Two-Stage Sintering Powder Metallurgy

NASA Astrophysics Data System (ADS)

Long, Luping; Liu, Wensheng; Ma, Yunzhu; Wu, Lei; Liu, Chao

2018-04-01

The major challenges for conventional diffusion bonding of joining Ti alloy and Al alloy are the undesirable interfacial reaction, low matrixes and joint strength. To avoid the problem in diffusion bonding, a novel two-stage sintering powder metallurgy process is developed. In the present work, the interface characterization and joint performance of the bonds obtained by powder metallurgy bonding are investigated and are compared with the diffusion bonded Ti/Al joints obtained with the same and the optimized process parameters. The results show that no intermetallic compound is visible in the Ti/Al joint obtained by powder metallurgy bonding, while a new layer formed at the joint diffusion bonded with the same parameters. The maximum tensile strength of joint obtained by diffusion bonding is 58 MPa, while a higher tensile strength reaching 111 MPa for a bond made by powder metallurgy bonding. Brittle fractures occur at all the bonds. It is shown that the powder metallurgy bonding of Ti/Al is better than diffusion bonding. The results of this study should benefit the bonding quality.

Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

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

Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.

2014-01-01

Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrationalmore » and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.« less

Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

NASA Astrophysics Data System (ADS)

Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

2016-09-01

Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

A Hydrothermal Route to the Synthesis of CaTiO3 Nanocuboids Using P25 as the Titanium Source

NASA Astrophysics Data System (ADS)

Yan, Yuxiang; Yang, Hua; Zhao, Xinxin; Zhang, Haimin; Jiang, Jinlong

2018-03-01

CaTiO3 nanocuboids (width 0.3-0.5 μm, length 0.8-1.1 μm) have been synthesized by a hydrothermal route using commercial P25 as the titanium source. The as-prepared sample was systematically characterized by means of x-ray powder diffraction, field-emission scanning electron microscopy, field-emission transmission electron microscopy, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller, ultraviolet-visible diffuse reflectance spectroscopy and electrochemical impedance spectroscopy. The photocatalytic activity of the sample was evaluated by degrading rhodamine B under simulated sunlight irradiation. It is demonstrated that CaTiO3 nanocuboids exhibit superior photocatalytic activity when compared with CaTiO3 nanoparticles. By investigating the effect of scavengers on the dye degradation and the yield of hydroxyl (·OH) radicals, it is concluded that ·OH is the dominant reactive species.

Effects of Doping Ratio of Cobalt and Iron on the Structure and Optical Properties of Bi3.25La0.75Fe(x)Co(1-x)Ti2O12 (X = 0, 0.25, 0.5, 0.75, 1).

PubMed

Song, Myoung Geun; Han, Jun Young; Bark, Chung Wung

2015-10-01

The wide band gap of complex oxides is one of the major obstacles limiting their use in photovoltaic cells. To identify an effective route for tailoring the band gap of complex oxides, this study examined the effects of cobalt and iron doping on lanthanum-modified Bi4Ti3O2-based oxides synthesized using a solid reaction. The structural and optical properties were analyzed by X-ray diffraction and ultraviolet-visible absorption spectroscopy. As a result, the optimal iron to cobalt doping ratio in bismuth titanate powder resulted in an ~1.8 eV decrease in the optical band gap. This new route to reduce the optical bandgap can be adapted to the synthesis of other complex oxides.

Effect of composition on physical properties of food powders

NASA Astrophysics Data System (ADS)

Szulc, Karolina; Lenart, Andrzej

2016-04-01

The paper presents an influence of raw material composition and technological process applied on selected physical properties of food powders. Powdered multi-component nutrients were subjected to the process of mixing, agglomeration, coating, and drying. Wetting liquids ie water and a 15% water lactose solution, were used in agglomeration and coating. The analyzed food powders were characterized by differentiated physical properties, including especially: particle size, bulk density, wettability, and dispersibility. The raw material composition of the studied nutrients exerted a statistically significant influence on their physical properties. Agglomeration as well as coating of food powders caused a significant increase in particle size, decreased bulk density, increased apparent density and porosity, and deterioration in flowability in comparison with non-agglomerated nutrients.

Coercivity enhancement of anisotropic Dy-free Nd-Fe-B powders by conventional HDDR process

NASA Astrophysics Data System (ADS)

Morimoto, K.; Katayama, N.; Akamine, H.; Itakura, M.

2012-11-01

Coercivity enhancement of Dy-free Nd-Fe-Co-B-Ga-Zr powders was studied using the conventional hydrogenation-decomposition-desorption-recombination (HDDR) process. It was found that the addition of Al together with the proper Nd content and the slow hydrogen desorption of the HDDR treatment can induce high coercivity in the powder. For example, the 14.0 at% Nd-2.0 at% Al powder exhibits HcJ of 1560 kA/m, Br of 1.22 T, and (BH)max of 257 kJ/m3. The high coercivity inducement of the powder is thought to be attributed to the formation of Nd-rich phase, which continuously surrounds fine Nd2Fe14B grains.

Chemical precursors to non-oxide ceramics: Macro to nanoscale materials

NASA Astrophysics Data System (ADS)

Forsthoefel, Kersten M.

Non-oxide ceramics exhibit a number of important properties that make them ideal for technologically important applications (thermal and chemical stability, high strength and hardness, wear-resistance, light weight, and a range of electronic and optical properties). Unfortunately, traditional methodologies to these types of materials are limited to fairly simple shapes and complex processed forms cannot be attained through these methods. The establishment of the polymeric precursor approach has allowed for the generation of advanced materials, such as refractory non-oxide ceramics, with controlled compositions, under moderate conditions, and in processed forms. The goal of the work described in this dissertation was both to develop new processible precursors to technologically important ceramics and to achieve the formation of advanced materials in processed forms. One aspect of this research exploited previously developed preceramic precursors to boron carbide, boron nitride and silicon carbide for the generation of a wide variety of advanced materials: (1) ultra-high temperature ceramic (UHTC) structural materials composed of hafnium boride and related composite materials, (2) the quaternary borocarbide superconductors, and (3) on the nanoscale, non-oxide ceramic nanotubules. The generation of the UHTC and the quaternary borocarbide materials was achieved through a method that employs a processible polymer/metal(s) dispersion followed by subsequent pyrolyses. In the case of the UHTC, hafnium oxide, hafnium, or hafnium boride powders were dispersed in a suitable precursor to afford hafnium borides or related composite materials (HfB2/HfC, HfB2/HfN, HfB2/SiC) in high yields and purities. The quaternary borocarbide superconducting materials were produced from pyrolyses of dispersions containing appropriate stoichiometric amounts of transition metal, lanthanide metal, and the polyhexenyldecaborane polymer. Both chemical vapor deposition (CVD) based routes employing a molecular precursor and porous alumina templating routes paired with solution-based methodologies are shown to generate non-oxide ceramic nanotubules of boron carbide, boron nitride and silicon carbide compositions. In the final phase of this work, a new metal-catalyzed route to poly(1-alkenyl- o-carborane) homopolymers and related copolymers was developed. Both homopolymers of 1-alkenyl-o-carboranes (1-vinyl-, 1-butenyl-, 1-hexenyl-) and copolymers of 1-hexenyl-o-carborane and allyltrimethylsilane or 1-hexenyl-o-carborane and 6-hexenyldecaborane were synthesized via the Cp2ZrMe2/B(C6F5) 3 catalyst system. A copolymer containing 1-hexenyl-o-carborane and the cross-linking agent, 6-hexenyldecaborane, was synthetically designed which exhibits initial cross-linking at ˜250°C and then converts in 75% yields to boron carbide at 1250°C.

Temperature Field Simulation of Powder Sintering Process with ANSYS

NASA Astrophysics Data System (ADS)

He, Hongxiu; Wang, Jun; Li, Shuting; Chen, Zhilong; Sun, Jinfeng; You, Ying

2018-03-01

Aiming at the “spheroidization phenomenon” in the laser sintering of metal powder and other quality problems of the forming parts due to the thermal effect, the finite element model of the three-dimensional transient metal powder was established by using the atomized iron powder as the research object. The simulation of the mobile heat source was realized by means of parametric design. The distribution of the temperature field during the sintering process under different laser power and different spot sizes was simulated by ANSYS software under the condition of fully considering the influence of heat conduction, thermal convection, thermal radiation and thermophysical parameters. The influence of these factors on the actual sintering process was also analyzed, which provides an effective way for forming quality control.

In Situ 3D Monitoring of Geometric Signatures in the Powder-Bed-Fusion Additive Manufacturing Process via Vision Sensing Methods.

PubMed

Li, Zhongwei; Liu, Xingjian; Wen, Shifeng; He, Piyao; Zhong, Kai; Wei, Qingsong; Shi, Yusheng; Liu, Sheng

2018-04-12

Lack of monitoring of the in situ process signatures is one of the challenges that has been restricting the improvement of Powder-Bed-Fusion Additive Manufacturing (PBF AM). Among various process signatures.

A novel particle engineering technology to enhance dissolution of poorly water soluble drugs: spray-freezing into liquid.

PubMed

Rogers, True L; Nelsen, Andrew C; Hu, Jiahui; Brown, Judith N; Sarkari, Marazban; Young, Timothy J; Johnston, Keith P; Williams, Robert O

2002-11-01

A novel cryogenic spray-freezing into liquid (SFL) process was developed to produce microparticulate powders consisting of an active pharmaceutical ingredient (API) molecularly embedded within a pharmaceutical excipient matrix. In the SFL process, a feed solution containing the API was atomized beneath the surface of a cryogenic liquid such that the liquid-liquid impingement between the feed and cryogenic liquids resulted in intense atomization into microdroplets, which were frozen instantaneously into microparticles. The SFL micronized powder was obtained following lyophilization of the frozen microparticles. The objective of this study was to develop a particle engineering technology to produce micronized powders of the hydrophobic drug, danazol, complexed with hydroxypropyl-beta-cyclodextrin (HPbetaCD) and to compare these SFL micronized powders to inclusion complex powders produced from other techniques, such as co-grinding of dry powder mixtures and lyophilization of bulk solutions. Danazol and HPbetaCD were dissolved in a water/tetrahydrofuran cosolvent mixture prior to SFL processing or slow freezing. Identical quantities of the API and HPbetaCD used in the solutions were co-ground in a mortar and pestle and blended to produce a co-ground physical mixture for comparison. The powder samples were characterized by differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), scanning electron microscopy, surface area analysis, and dissolution testing. The results provided by DSC, XRD, and FTIR suggested the formation of inclusion complexes by both slow-freezing and SFL. However, the specific surface area was significantly higher for the latter. Dissolution results suggested that equilibration of the danazol/HPbetaCD solution prior to SFL processing was required to produce the most soluble conformation of the resulting inclusion complex following SFL. SFL micronized powders exhibited better dissolution profiles than the slowly frozen aggregate powder. Results indicated that micronized SFL inclusion complex powders dissolved faster in aqueous dissolution media than inclusion complexes formed by conventional techniques due to higher surface areas and stabilized inclusion complexes obtained by ultra-rapid freezing.

A Family of ACO Routing Protocols for Mobile Ad Hoc Networks

PubMed Central

Rupérez Cañas, Delfín; Sandoval Orozco, Ana Lucila; García Villalba, Luis Javier; Kim, Tai-hoon

2017-01-01

In this work, an ACO routing protocol for mobile ad hoc networks based on AntHocNet is specified. As its predecessor, this new protocol, called AntOR, is hybrid in the sense that it contains elements from both reactive and proactive routing. Specifically, it combines a reactive route setup process with a proactive route maintenance and improvement process. Key aspects of the AntOR protocol are the disjoint-link and disjoint-node routes, separation between the regular pheromone and the virtual pheromone in the diffusion process and the exploration of routes, taking into consideration the number of hops in the best routes. In this work, a family of ACO routing protocols based on AntOR is also specified. These protocols are based on protocol successive refinements. In this work, we also present a parallelized version of AntOR that we call PAntOR. Using programming multiprocessor architectures based on the shared memory protocol, PAntOR allows running tasks in parallel using threads. This parallelization is applicable in the route setup phase, route local repair process and link failure notification. In addition, a variant of PAntOR that consists of having more than one interface, which we call PAntOR-MI (PAntOR-Multiple Interface), is specified. This approach parallelizes the sending of broadcast messages by interface through threads. PMID:28531159

Powder bed charging during electron-beam additive manufacturing

DOE PAGES

Cordero, Zachary C.; Meyer, Harry M.; Nandwana, Peeyush; ...

2016-11-18

Electrons injected into the build envelope during powder-bed electron-beam additive manufacturing can accumulate on the irradiated particles and cause them to repel each other. Furthermore, these electrostatic forces can grow so large that they drive the particles out of the build envelope in a process known as smoking. Here, a model of powder bed charging is formulated and used to develop criteria that predict the conditions under which the powder bed will smoke. These criteria suggest dependences on particle size, pre-heat temperature, and process parameters that align closely with those observed in practice.

Spectroscopy investigation of nanostructured nickel–zinc ferrite obtained by mechanochemical synthesis

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

Lazarević, Zorica Ž., E-mail: lzorica@yahoo.com; Milutinović, Aleksandra N.; Jovalekić, Čedomir D.

2015-03-15

Highlights: • Nano powder of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} prepared by a soft mechanochemicaly after 10 h milling. • Phase formation controlled by XRD, Raman and IR spectroscopy. • Spectroscopy measurements indicate that the prepared samples have spinel structure. • The average particles size are found to be around 20 nm. • The degree of inversion is δ = 0.36 for NZF obtained from hydroxides for 10 h. - Abstract: Nano crystalline samples of nickel–zinc ferrite, Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} were prepared by mechanochemical route in a planetary ball mill starting from two mixtures of the appropriate quantitiesmore » of the powders: case (1) oxide powders: NiO, ZnO and α-Fe{sub 2}O{sub 3} in one case, and in the second case (2) hydroxide powders: Ni(OH){sub 2}, Zn(OH){sub 2} and Fe(OH){sub 3}. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman, IR and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.« less

In-situ characterization of laser-powder interaction and cooling rates through high-speed imaging of powder bed fusion additive manufacturing

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

Scipioni Bertoli, Umberto; Guss, Gabe; Wu, Sheldon

We report detailed understanding of the complex melt pool physics plays a vital role in predicting optimal processing regimes in laser powder bed fusion additive manufacturing. In this work, we use high framerate video recording of Selective Laser Melting (SLM) to provide useful insight on the laser-powder interaction and melt pool evolution of 316 L powder layers, while also serving as a novel instrument to quantify cooling rates of the melt pool. The experiment was performed using two powder types – one gas- and one water-atomized – to further clarify how morphological and chemical differences between these two feedstock materialsmore » influence the laser melting process. Finally, experimentally determined cooling rates are compared with values obtained through computer simulation, and the relationship between cooling rate and grain cell size is compared with data previously published in the literature.« less

Effects of annealing process on magnetic properties and structures of Nd-Pr-Ce-Fe-B melt-spun powders

NASA Astrophysics Data System (ADS)

Pei, Kun; Lin, Min; Yan, Aru; Zhang, Xing

2016-05-01

The effects of annealing process on magnetic properties and structures of Nd-Pr-Ce-Fe-B melt-spun powders have been investigated. The magnetic properties improve a lot when the annealing temperature is 590-650 °C and the annealing time exceeds 1 min. The magnetic properties is stable when the annealing time is 590-650 °C. The powders contains obvious grains when the annealing time is only 1 min, while the grains grow up obviously, leading to the decrease of Br and (BH)max, when the annealing time is more than 9 min. The Hcj changes little for different annealing time. The cooling rate also affects the magnetic properties of powders with different Ce-content. Faster cooling rate is favorable to improve magnetic properties with low Ce-content powders, while high Ce-content powders need slower cooling rate.

Advanced powder metallurgy aluminum alloys via rapid solidification technology

NASA Technical Reports Server (NTRS)

Ray, R.

1984-01-01

Aluminum alloys containing 10 to 11.5 wt. pct. of iron and 1.5 to 3 wt. pct. of chromium using the technique of rapid solidification powder metallurgy were studied. Alloys were prepared as thin ribbons (.002 inch thick) rapidly solidified at uniform rate of 10(6) C/second by the melt spinning process. The melt spun ribbons were pulverized into powders (-60 to 400 mesh) by a rotating hammer mill. The powders were consolidated by hot extrusion at a high reduction ratio of 50:1. The powder extrusion temperature was varied to determine the range of desirable processing conditions necessary to yield useful properties. Powders and consolidated alloys were characterized by SEM and optical metallography. The consolidated alloys were evaluated for (1) thermal stability, (2) tensile properties in the range, room temperature to 450 F, and (3) notch toughness in the range, room temperature to 450 F.

Treatment of refractory powders by a novel, high enthalpy dc plasma

NASA Astrophysics Data System (ADS)

Pershin, L.; Mitrasinovic, A.; Mostaghimi, J.

2013-06-01

Thermophysical properties of CO2-CH4 mixtures at high temperatures are very attractive for materials processing. In comparison with argon, at the same temperature, such a mixture possesses much higher enthalpy and higher thermal conductivity. At high temperatures, CO2-CH4 mixture has a complex composition with strong presence of CO which, in the case of powder treatment, could reduce oxidation. In this work, a dc plasma torch with graphite cathode was used to study the effect of plasma gas composition on spheroidization of tungsten carbide and alumina powders. Two different gas compositions were used to generate the plasma while the torch current was kept at 300 A. Various techniques were employed to assess the average concentration of carbides and oxides and the final shape of the treated powders. Process parameters such as input power and plasma gas composition allow controlling the degree of powder oxidation and spheroidization of high melting point ceramic powders.

Causal Factors of Weld Porosity in Gas Tungsten Arc Welding of Powder-Metallurgy-Produced Titanium Alloys

NASA Astrophysics Data System (ADS)

Muth, T. R.; Yamamoto, Y.; Frederick, D. A.; Contescu, C. I.; Chen, W.; Lim, Y. C.; Peter, W. H.; Feng, Z.

2013-05-01

An investigation was undertaken using gas tungsten arc (GTA) welding on consolidated powder metallurgy (PM) titanium (Ti) plate to identify the causal factors behind observed porosity in fusion welding. Tramp element compounds of sodium and magnesium, residual from the metallothermic reduction of titanium chloride used to produce the titanium, were remnant in the starting powder and were identified as gas-forming species. PM-titanium made from revert scrap, where sodium and magnesium were absent, showed fusion weld porosity, although to a lesser degree. We show that porosity was attributable to hydrogen from adsorbed water on the surface of the powders prior to consolidation. The removal and minimization of both adsorbed water on the surface of titanium powder and the residues from the reduction process prior to consolidation of titanium powders are critical for achieving equivalent fusion welding success similar to that seen in wrought titanium produced via the Kroll process.

In-situ characterization of laser-powder interaction and cooling rates through high-speed imaging of powder bed fusion additive manufacturing

DOE PAGES

Scipioni Bertoli, Umberto; Guss, Gabe; Wu, Sheldon; ...

2017-09-21

We report detailed understanding of the complex melt pool physics plays a vital role in predicting optimal processing regimes in laser powder bed fusion additive manufacturing. In this work, we use high framerate video recording of Selective Laser Melting (SLM) to provide useful insight on the laser-powder interaction and melt pool evolution of 316 L powder layers, while also serving as a novel instrument to quantify cooling rates of the melt pool. The experiment was performed using two powder types – one gas- and one water-atomized – to further clarify how morphological and chemical differences between these two feedstock materialsmore » influence the laser melting process. Finally, experimentally determined cooling rates are compared with values obtained through computer simulation, and the relationship between cooling rate and grain cell size is compared with data previously published in the literature.« less