Influence of grinding on service properties of VT-22 powder applied in additive technologies

NASA Astrophysics Data System (ADS)

Zakharov, M. N.; Rybalko, O. F.; Romanova, O. V.; Gelchinskiy, B. R.; Il'inykh, S. A.; Krashaninin, V. A.

2017-01-01

Powder of titanium alloy (VT-22) produced by plasma-spraying was subjected to grinding to obtain powder with size less 100 microns. These powders were sprayed by plasma unit using two types of gases, namely, air and air with methane (spraying in water and sputtering of coating on steel support). Influence of grinding time on yield of powder of required fraction was studied. Morphology and phase composition of the grinded powder and plasma sprayed one were under investigation. In the result of experiments, it appears that the grinding time genuinely influences the chemical and phase compositions, but there is no effect on physical-processing properties. For powders after plasma spraying some changes of non-metal elements content were detected by chemical analysis. Using gaseous mixture of air and methane in plasma spraying unit leads to formation of a new phase in the powder according X-ray diffraction data.

Determination of whey adulteration in milk powder by using laser induced breakdown spectroscopy.

PubMed

Bilge, Gonca; Sezer, Banu; Eseller, Kemal Efe; Berberoglu, Halil; Topcu, Ali; Boyaci, Ismail Hakki

2016-12-01

A rapid and in situ method has been developed to detect and quantify adulterated milk powder through adding whey powder by using laser induced breakdown spectroscopy (LIBS). The methodology is based on elemental composition differences between milk and whey products. Milk powder, sweet and acid whey powders were produced as standard samples, and milk powder was adulterated with whey powders. Based on LIBS spectra of standard samples and commercial products, species was identified using principle component analysis (PCA) method, and discrimination rate of milk and whey powders was found as 80.5%. Calibration curves were obtained with partial least squares regression (PLS). Correlation coefficient (R(2)) and limit of detection (LOD) values were 0.981 and 1.55% for adulteration with sweet whey powder, and 0.985 and 0.55% for adulteration with acid whey powder, respectively. The results were found to be consistent with the data from inductively coupled plasma - mass spectrometer (ICP-MS) method. Copyright © 2016 Elsevier Ltd. All rights reserved.

The effect of additive geometry on the integration of secondary elements during Friction Stir Processing

NASA Astrophysics Data System (ADS)

Zens, A.; Gnedel, M.; Zaeh, M. F.; Haider, F.

2018-06-01

Friction Stir Processing (FSP) can be used to locally modify properties in materials such as aluminium. This may be used, for example, to produce a fine microstructure or to integrate secondary elements into the base material. The purpose of this work is to examine the effect of the properties of the metal additives on the resulting material distribution in the processed region. For this, commercially pure iron and copper were integrated into an EN AW-1050 aluminium base material using FSP. Iron in the form of powder, wire and foil as well as copper in powder form were assessed. The various additive forms represent materials with differing surface-to-volume ratios as well as varying dispersion characteristics in the processing zone. The processing parameters for each additive form remained constant; however, two- and four-pass FSP processes were conducted. The results of CT analysis proved especially insightful regarding the spatial distribution of the various additive form within the workpiece. As expected, the powder additive was most widely distributed within the welding zone. Micro-hardness mappings showed that the powder additive contributed to the hardness within the weld nugget in comparison to the processed material without secondary elements.

SPHERICAL DIE

DOEpatents

Livingston, J.P.

1959-01-27

A die is presented for pressing powdered materials into a hemispherical shape of uniforin density and wall thickness comprising a fcmale and male die element held in a stationary spaced relation with the space being equivalent to the wall thickness and defining the hemispherical shape, a pressing ring linearly moveable along the male die element, an inlet to fill the space with powdered materials, a guiding system for moving the pressing ring along the male die element so as to press the powdered material and a heating system for heating the male element so that the powdered material is heated while being pressed.

Synthesis of Cu-W nanocomposite by high-energy ball milling.

PubMed

Venugopal, T; Rao, K Prasad; Murty, B S

2007-07-01

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.

Atomization methods for forming magnet powders

DOEpatents

Sellers, Charles H.; Branagan, Daniel J.; Hyde, Timothy A.

2000-01-01

The invention encompasses methods of utilizing atomization, methods for forming magnet powders, methods for forming magnets, and methods for forming bonded magnets. The invention further encompasses methods for simulating atomization conditions. In one aspect, the invention includes an atomization method for forming a magnet powder comprising: a) forming a melt comprising R.sub.2.1 Q.sub.13.9 B.sub.1, Z and X, wherein R is a rare earth element; X is an element selected from the group consisting of carbon, nitrogen, oxygen and mixtures thereof; Q is an element selected from the group consisting of Fe, Co and mixtures thereof; and Z is an element selected from the group consisting of Ti, Zr, Hf and mixtures thereof; b) atomizing the melt to form generally spherical alloy powder granules having an internal structure comprising at least one of a substantially amorphous phase or a substantially nanocrystalline phase; and c) heat treating the alloy powder to increase an energy product of the alloy powder; after the heat treatment, the alloy powder comprising an energy product of at least 10 MGOe. In another aspect, the invention includes a magnet comprising R, Q, B, Z and X, wherein R is a rare earth element; X is an element selected from the group consisting of carbon, nitrogen, oxygen and mixtures thereof; Q is an element selected from the group consisting of Fe, Co and mixtures thereof; and Z is an element selected from the group consisting of Ti, Zr, Hf and mixtures thereof; the magnet comprising an internal structure comprising R.sub.2.1 Q.sub.13.9 B.sub.1.

PATHFINDER ATOMIC POWER PLANT TECHNICAL PROGRESS REPORT FOR JULY 1, 1959- SEPTEMBER 30, 1959

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

None

1960-10-31

ABS>Fuel Element Research and Development. Dynamic and static corrosion tests on 8001 Al were completed. Annealmmmg of 1100 cladding on 5083 and M400 cladding on X2219 were tested at 500 deg C, and investigation continued on producing X8101 Al alloy cladding in tube plates by extrusion. Boiler fuel element capsule irradiation tests and subassembly tests are described Heat transfer loop studies and fuel fabrication for the critical facility are reported. Boiler fuel element mechanical design and testing progress is desc ribed. and the superheater fuel element temperature evaluating routine is discussed. Low- enrichment superheater fuel element development included design studiesmore » and stainless steel powder and UO/sub 2/ powder fabrication studies Reactor Mechanical Studies. Research is reported on vessel and structure design, fabrication, and testing, recirculation system design, steam separator tests, and control rod studies. Nuclear Analysis. Reactor physics studies are reported on nuclear constants, baffle plate analysis, comparison of core representations, delayed neutron fraction. and shielding analysis of the reactor building. Reactor and system dynamics and critical experiments were also studied. Chemistry. Progress is reported on recombiner. radioactive gas removal and storage, ion exchanger and radiochemical processing. (For preceding period see ACNP-5915.) (T.R.H.)« less

Comparison of the tribological properties of fluorinated cokes and graphites

NASA Technical Reports Server (NTRS)

Fusaro, Robert L.

1988-01-01

The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

Comparison of the tribological properties of fluorinated cokes and graphites

NASA Technical Reports Server (NTRS)

Fusaro, Robert L.

1987-01-01

The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

Practical soil analysis by laser induced breakdown spectroscopy employing subtarget supported micro mesh as a powder sample holder

NASA Astrophysics Data System (ADS)

Suyanto, Hery; Lie, Tjung Jie; Kurniawan, Koo Hendrik; Kagawa, Kiichiro; Tjia, May On

2017-11-01

A practical alternative of sample preparation technique is proposed for direct powder analysis using laser-induced breakdown spectroscopy (LIBS) instead of the commonly adopted treatment of pelletizing the powder. The resulted pellet is known to suffer from reduced sensitivity of emission. Besides, it may also give rise to interfering effect from the binder emission. We introduce in this report a more practical technique of using a subtarget supported micro mesh (SSMM) powder sample holder. The LIBS spectrum of standard soil powder measured with 13 mJ 1064 nm Nd:YAG laser in 0.65 kPa ambient air is shown to exhibit the sharp emission lines of all the major elements in the sample. A comparison with the emission spectra measured from the pelletized powder, the spectrum obtained using the SSMM sample holder shows distinctly superior spectral quality marked by the absence of matrix effect found in pelletized powder samples, and the much stronger intensity due to the more effective shock wave plasma induced thermal excitation process produced by the hard subtarget in the sample holder. Repeating the measurement on a number of the standard soil samples of various Pb contents is shown to yield a linear calibration line with practically zero intercept and a detection limit of less than 10 ppm. We have thus demonstrated the viability of the proposed powder sample holder for the development of practical and quantitative powder analysis in the field.

Nanostructuring of Aluminum Alloy Powders by Cryogenic Attrition with Hydrogen-Free Process Control Agent

DTIC Science & Technology

2015-02-01

Nanostructuring of Aluminum Alloy Powders by Cryogenic Attrition with Hydrogen-Free Process Control Agent by Frank Kellogg , Clara Hofmeister...Process Control Agent Frank Kellogg Bowhead Science and Technology Clara Hofmeister Advanced Materials Processing and Analysis Center...NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Frank Kellogg , Clara Hofmeister, Anit Giri, and Kyu Cho 5d. PROJECT NUMBER 5e

Coupling of in-situ X-ray Microtomography Observations with Discrete Element Simulations-Application to Powder Sintering

NASA Astrophysics Data System (ADS)

Olmos, L.; Bouvard, D.; Martin, C. L.; Bellet, D.; Di Michiel, M.

2009-06-01

The sintering of both a powder with a wide particle size distribution (0-63 μm) and of a powder with artificially created pores is investigated by coupling in situ X-ray microtomography observations with Discrete Element simulations. The micro structure evolution of the copper particles is observed by microtomography all along a typical sintering cycle at 1050° C at the European Synchrotron Research Facilities (ESRF, Grenoble, France). A quantitative analysis of the 3D images provides original data on interparticle indentation, coordination and particle displacements throughout sintering. In parallel, the sintering of similar powder systems has been simulated with a discrete element code which incorporates appropriate sintering contact laws from the literature. The initial numerical packing is generated directly from the 3D microtomography images or alternatively from a random set of particles with the same size distribution. The comparison between the information drawn from the simulations and the one obtained by tomography leads to the conclusion that the first method is not satisfactory because real particles are not perfectly spherical as the numerical ones. On the opposite the packings built with the second method show sintering behaviors close to the behaviors of real materials, although particle rearrangement is underestimated by DEM simulations.

Analysis of tablet compaction. I. Characterization of mechanical behavior of powder and powder/tooling friction.

PubMed

Cunningham, J C; Sinka, I C; Zavaliangos, A

2004-08-01

In this first of two articles on the modeling of tablet compaction, the experimental inputs related to the constitutive model of the powder and the powder/tooling friction are determined. The continuum-based analysis of tableting makes use of an elasto-plastic model, which incorporates the elements of yield, plastic flow potential, and hardening, to describe the mechanical behavior of microcrystalline cellulose over the range of densities experienced during tableting. Specifically, a modified Drucker-Prager/cap plasticity model, which includes material parameters such as cohesion, internal friction, and hydrostatic yield pressure that evolve with the internal state variable relative density, was applied. Linear elasticity is assumed with the elastic parameters, Young's modulus, and Poisson's ratio dependent on the relative density. The calibration techniques were developed based on a series of simple mechanical tests including diametrical compression, simple compression, and die compaction using an instrumented die. The friction behavior is measured using an instrumented die and the experimental data are analyzed using the method of differential slices. The constitutive model and frictional properties are essential experimental inputs to the finite element-based model described in the companion article. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 93:2022-2039, 2004

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.

Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

NASA Astrophysics Data System (ADS)

Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

2015-10-01

The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

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.

Analysis of Brazing Effect on Hot Corrosion Behavior of a Nickel-Based Aerospace Superalloy

NASA Astrophysics Data System (ADS)

Esmaeili, N.; Ojo, O. A.

2018-06-01

The effects of brazing and use of composite powder mixture as interlayer material on hot corrosion resistance of brazed IN738 superalloy were studied. Brazing was observed to result in significant reduction in the hot corrosion resistance of the superalloy. However, application of composite powder mixture, which consists of additive superalloy powder, enhanced the hot corrosion resistance of brazed samples. It is also found that although the use of composite powder mixture increased hot corrosion resistance of brazed alloy, if the additive powder completely melts, which is possible during brazing, it can significantly reduce the hot corrosion resistance of the brazed joint. Elemental micro-segregation during solidification of the joint with completely melted powder mixture produces chromium-depleted zones and consequently reduces hot corrosion resistance, since a uniform distribution and adequate chromium concentration are necessary to combat hot corrosion. This has not been previously reported in the literature and it is crucial to the use of composite powder mixture for enhancing the properties of brazed superalloys.

FABRICATION OF TUBE TYPE FUEL ELEMENT FOR NUCLEAR REACTORS

DOEpatents

Loeb, E.; Nicklas, J.H.

1959-02-01

A method of fabricating a nuclear reactor fuel element is given. It consists essentially of fixing two tubes in concentric relationship with respect to one another to provide an annulus therebetween, filling the annulus with a fissionablematerial-containing powder, compacting the powder material within the annulus and closing the ends thereof. The powder material is further compacted by swaging the inner surface of the inner tube to increase its diameter while maintaining the original size of the outer tube. This process results in reduced fabrication costs of powdered fissionable material type fuel elements and a substantial reduction in the peak core temperatures while materially enhancing the heat removal characteristics.

Comparative measurements of mineral elements in milk powders with laser-induced breakdown spectroscopy and inductively coupled plasma atomic emission spectroscopy.

PubMed

Lei, W Q; El Haddad, J; Motto-Ros, V; Gilon-Delepine, N; Stankova, A; Ma, Q L; Bai, X S; Zheng, L J; Zeng, H P; Yu, J

2011-07-01

Mineral elements contained in commercially available milk powders, including seven infant formulae and one adult milk, were analyzed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and laser-induced breakdown spectroscopy (LIBS). The purpose of this work was, through a direct comparison of the analytical results, to provide an assessment of the performance of LIBS, and especially of the procedure of calibration-free LIBS (CF-LIBS), to deal with organic compounds such as milk powders. In our experiments, the matrix effect was clearly observed affecting the analytical results each time laser ablation was employed for sampling. Such effect was in addition directly observed by determining the physical parameters of the plasmas induced on the different samples. The CF-LIBS procedure was implemented to deduce the concentrations of Mg and K with Ca as the internal reference element. Quantitative analytical results with CF-LIBS were validated with ICP-AES measurements and nominal concentrations specified for commercial milks. The obtained good results with the CF-LIBS procedure demonstrate its capacity to take into account the difference in physical parameters of the plasma in the calculation of the concentrations of mineral elements, which allows a significant reduction of the matrix effect related to laser ablation. We finally discuss the way to optimize the implementation of the CF-LIBS procedure for the analysis of mineral elements in organic materials.

Heat transfer model and finite element formulation for simulation of selective laser melting

NASA Astrophysics Data System (ADS)

Roy, Souvik; Juha, Mario; Shephard, Mark S.; Maniatty, Antoinette M.

2017-10-01

A novel approach and finite element formulation for modeling the melting, consolidation, and re-solidification process that occurs in selective laser melting additive manufacturing is presented. Two state variables are introduced to track the phase (melt/solid) and the degree of consolidation (powder/fully dense). The effect of the consolidation on the absorption of the laser energy into the material as it transforms from a porous powder to a dense melt is considered. A Lagrangian finite element formulation, which solves the governing equations on the unconsolidated reference configuration is derived, which naturally considers the effect of the changing geometry as the powder melts without needing to update the simulation domain. The finite element model is implemented into a general-purpose parallel finite element solver. Results are presented comparing to experimental results in the literature for a single laser track with good agreement. Predictions for a spiral laser pattern are also shown.

Chemical reactions of metal powders with organic and inorganic liquids during ball milling

NASA Technical Reports Server (NTRS)

Arias, A.

1975-01-01

Chromium and/or nickel powders were milled in metal chlorides and in organic liquids representative of various functional groups. The powders always reacted with the liquid and became contaminated with elements from them. The milled powders had specific surface areas ranging from 0.14 to 37 sq m/g, and the total contamination with elements from the milling liquid ranged from 0.01 to 56 weight percent. Compounds resulting from substitution, addition, or elimination reactions formed in or from the milling liquid.

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.

Characterization of ball-milled carbon nanotube dispersed aluminum mixed powders

NASA Astrophysics Data System (ADS)

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

2016-04-01

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

[Improvement of powder flowability and hygroscopicity of traditional Chinese medicine extract by surface coating modification technology].

PubMed

Zeng, Rong-Gui; Jiang, Qie-Ying; Liao, Zheng-Gen; Zhao, Guo-Wei; Luo, Yun; Luo, Juan; Lv, Dan

2016-06-01

To study the improvement of powder flowability and hygroscopicity of traditional Chinese medicine extract by surface coating modification technology. The 1% hydrophobic silica nanoparticles were used as surface modifier, and andrographis extract powder was taken as a model drug. Three different techniques were used for coating model drugs, with angle of repose, compressibility, flat angle and cohesion as the comprehensive evaluation indexes for the powder flowability. The powder particle size and the size distribution were measured by Mastersizer 2000. FEI scanning electron microscope was used to observe the surface morphology and structure of the powder. The percentage of Si element on the powder surface was measured by energy dispersive spectrometer. The hygroscopicity of powder was determined by Chinese pharmacopoeia method. All of the three techniques can improve the flowability of powder extract. In particular, hygroscopicity of extract powder can also be improved by dispersion and then high-speed mixing, which can produce a higher percentage of Si element on the powder surface. The improvement principle may be correlated with a modifier adhered to the powder surface. Copyright© by the Chinese Pharmaceutical Association.

Analysis of laser induced plasma of lithium iron phosphate/LiFePO4 using Nd:YAG laser at low pressure

NASA Astrophysics Data System (ADS)

Suliyanti, M. M.; Hidayah, A. N.; Isnaeni

2017-04-01

Preliminary analysis of lithium in Lithium Iron Phosphate (LiFePO4) powder using laser induced plasma spectroscopy at low pressure had been done. Recently, LiFePO4-based batteries are widely used in most electric cars and bikes due to less toxic. However, lithium (Li) element is very difficult to detect since it is a very light element. In this work, we used a Nd:YAG laser (1064 nm wavelength, 5 ns pulse width at 10 Hz repetition rate) that was focused on LiFePO4 sample at low pressure. The main Li peak emission in LiFePO4 powder and sheet can be easily detected using this technique. We report the results of experimental study on Li element emission lines at wavelength 460.18 nm, 610.37 nm and 670.83 nm using 2 mJ and 12 mJ laser irradiation at 5 Torr and 35 Torr air atmosphere. The results of this study showed promising application of laser-induced plasma spectroscopy to detect and analyse Li in various samples.

Sandia Corporation (Albuquerque, NM)

DOEpatents

Ewsuk, Kevin G [Albuquerque, NM; Arguello, Jr., Jose G.

2006-01-31

A method of designing a primary geometry, such as for a forming die, to be used in a powder pressing application by using a combination of axisymmetric geometric shapes, transition radii, and transition spaces to simulate the geometry where the shapes can be selected from a predetermined list or menu of axisymmetric shapes and then developing a finite element mesh to represent the geometry. This mesh, along with material properties of the component to be designed and powder, is input to a standard deformation finite element code to evaluate the deformation characteristics of the component being designed. The user can develop the geometry interactively with a computer interface in minutes and execute a complete analysis of the deformation characteristics of the simulated component geometry.

Heavy metal content and element analysis of infant formula and milk powder samples purchased on the Tanzanian market: International branded versus black market products.

PubMed

Sager, M; McCulloch, C R; Schoder, D

2018-07-30

Milk powder is a food for malnourished African children and for healthy infants of women with HIV/AIDS. High demand and low purchasing power has resulted in a huge informal, black market in Sub-Saharan Africa. Forty-three milk powder batches were analyzed for 43 chemical elements using ICP-MS One sample (2.3%) was contaminated at a lead concentration of 240 µg/kg dry weight exceeding the European threshold (130 µg/kg dry weight). Macroelement contents revealed a trend decreasing in concentration through skimmed, full cream products to infant formulae. Concentration ranges by dry weight differed in respect of uncertainty intervals of  ±10%. Median Ca, K and P concentrations declined from 11.14 g/kg to 3.21 g/kg, 14.11 g/kg to 4.95 g/kg and 9.12 g/kg to 2.75 g/kg dry mass, respectively. Milk powder samples obtained from the Tanzanian black market were comparable in respect of nutritional and chemical content to international branded full cream products. Copyright © 2018 Elsevier Ltd. All rights reserved.

Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS.

PubMed

Muller, Edson I; Souza, Juliana P; Muller, Cristiano C; Muller, Aline L H; Mello, Paola A; Bizzi, Cezar A

2016-08-15

In this work a green digestion method which only used H2O2 as an oxidant and high temperature and pressure in the single reaction chamber system (SRC-UltraWave™) was applied for subsequent elemental determination by inductively coupled plasma-based techniques. Milk powder was chosen to demonstrate the feasibility and advantages of the proposed method. Samples masses up to 500mg were efficiently digested, and the determination of Ca, Fe, K, Mg and Na was performed by inductively coupled plasma optical emission spectrometry (ICP-OES), while trace elements (B, Ba, Cd, Cu, Mn, Mo, Pb, Sr and Zn) were determined by inductively coupled plasma mass spectrometry (ICP-MS). Residual carbon (RC) lower than 918mgL(-1) of C was obtained for digests which contributed to minimizing interferences in determination by ICP-OES and ICP-MS. Accuracy was evaluated using certified reference materials NIST 1549 (non-fat milk powder certified reference material) and NIST 8435 (whole milk powder reference material). The results obtained by the proposed method were in agreement with the certified reference values (t-test, 95% confidence level). In addition, no significant difference was observed between results obtained by the proposed method and conventional wet digestion using concentrated HNO3. As digestion was performed without using any kind of acid, the characteristics of final digests were in agreement with green chemistry principles when compared to digests obtained using conventional wet digestion method with concentrated HNO3. Additionally, H2O2 digests were more suitable for subsequent analysis by ICP-based techniques due to of water being the main product of organic matrix oxidation. The proposed method was suitable for quality control of major components and trace elements present in milk powder in consonance with green sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.

The effect of thermal pre-treatment of titanium hydride (TiH2) powder in argon condition

NASA Astrophysics Data System (ADS)

Franciska P., L.; Erryani, Aprilia; Annur, Dhyah; Kartika, Ika

2018-04-01

Titanium hydride (TiH2) powders are used to enhance the foaming process in the formation of a highly porous metallic material with a cellular structure. But, the low temperature of hydrogen release is one of its problems. The present study, different thermal pre-treatment temperatures were employed to investigate the decomposition behavior of TiH2 to retard or delay a hydrogen gas release process during foaming. As a foaming agent, TiH2 was subjected to various heat treatments prior at 450 and 500°C during 2 hours in argon condition. To study the formation mechanism, the thermal behavior of titanium hydride and hydrogen release are investigated by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The morphology of pre-treated titanium hydride powders were examined using Scanning Electron Microscope (SEM) while unsure mapping and elemental composition of the pre-treated powders processed by Energy Dispersive Spectroscopy (EDS). To study the phase formation was characterized by X-ray diffraction analysis (XRD). In accordance with the results, an increase in pre-treatment temperature of TiH2 to higher degrees are changing the process of releasing hydrogen from titanium hydride powder. DTA/TGA results showed that thermal pre-treatment TiH2 at 450°C, released the hydrogen gas at 560°C in heat treatment when foaming process. Meanwhile, thermal pre-treatment in TiH2 at 500°C, released the hydrogen gas at 670°C when foaming process. There is plenty of direct evidence for the existence of oxide layers that showed by EDS analysis obtained in SEM. As oxygen is a light element and qualitative proof shows that the higher pre-treatment temperature produces more and thicker oxygen layers on the surface of the TiH2 powder particles. It might the thickness of oxide layer are different from different pre-treatment temperatures, which leading to the differences in the decomposition temperature. But from SEM result that oxidation of the powder does not change the powder morphology. The oxidation process also confirmed by XRD result, which showed higher thermal pre-treatment TiH2, more oxide higher peak is formed. The oxide layer of TiH2 particles is responsible for the observed shift in decomposition temperature and can prepare the stable foam that stabilizes forming of cell walls and avoid their collapse at higher temperatures.

Morphology and structural development of reduced anatase-TiO{sub 2} by pure Ti powder upon annealing and nitridation: Synthesis of TiO{sub x} and TiO{sub x}N{sub y} powders

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

Bolokang, A.S., E-mail: Sylvester.Bolokang@transnet.net; DST/CSIR National Centre for Nano-Structured Materials, Council for Scientific and Industrial Research, Pretoria 0001; Transnet Engineering, Product Development, Private Bag X 528, Kilnerpark 0127

2015-02-15

It is well known that nitriding of titanium is suitable for surface coating of biomaterials and in other applications such as anti-reflective coating, while oxygen-rich titanium oxynitride has been applied in thin film resistors and photocatalysis. Thus in this work anatase was reduced with pure titanium powder during annealing in argon. This was done to avoid any metallic contamination and unwanted residual metal doping. As a result, interesting and different types of particle morphology were synthesized when the pre-milled elemental anatase and titanium powders were mixed. The formation of metastable face centred cubic and monoclinic titanium monoxide was detected bymore » the X-ray diffraction technique. The phases were confirmed by energy dispersive X-ray spectroscopy analysis. Raman analysis revealed weak intensity peaks for samples annealed in argon as compared to those annealed under nitrogen. - Graphical abstract: Display Omitted - Highlights: • Reaction of TiO{sub 2} and Ti induced metastable FCC and monoclinic TiO{sub x}. • Compositions of mixed powder were prepared from the unmilled and pre-milled powders. • Nitridation of TiO{sub x} yielded TiO{sub x}N{sub y} phase. • Mixed morphology was observed on all three powder samples.« less

Bioavailability of elemental iron powders to rats is less than bakery-grade ferrous sulfate and predicted by iron solubility and particle surface area.

PubMed

Swain, James H; Newman, Samuel M; Hunt, Janet R

2003-11-01

Foods are fortified with elemental forms of iron to reduce iron deficiency. However, the nutritional efficacy of current, commercially produced elemental iron powders has not been verified. We determined the bioavailability of six commercial elemental iron powders and examined how physicochemistry influences bioavailability. Relative biological value (RBV) of the iron powders was determined using a hemoglobin repletion/slope ratio method, treating iron-deficient rats with repletion diets fortified with graded quantities of iron powders, bakery-grade ferrous sulfate or no added iron. Iron powders were assessed physicochemically by measuring iron solubility in hydrochloric acid at pH 1.0 and 1.7, surface area by nitrogen gas adsorption and surface microstructure by electron microscopy. Bioavailability from the iron powders, based on absolute iron intake, was significantly less than from FeSO4 (100%; P < 0.05) with the following rank order: Carbonyl (64%; Ferronyl, U.S.) > Electrolytic (54%; A-131, U.S.) > Electrolytic (46%; Electrolytic Iron, India) > H-Reduced (42%; AC-325, U.S.) > Reduced (24%; ATOMET 95SP, Canada) > CO-Reduced (21%; RSI-325, Sweden). Solubility testing of the iron powders resulted in different relative rankings and better RBV predictability with increasing time at pH 1.7 (R2 = 0.65 at 150 min). The prediction was improved with less time and lower pH (R2 = 0.82, pH 1.0 at 30 min). Surface area, ranging from 90 to 370 m2/kg, was also highly predictive of RBV (R2 = 0.80). Bioavailability of iron powders is less than bakery-grade ferrous sulfate and varies up to three times among different commercial forms. Solubility at pH 1.0 and surface area were predictive of iron bioavailability in rats.

Protective matching polymer powder coating of piezoelectric element

NASA Astrophysics Data System (ADS)

Gavrilova, V. A.; Fazlyyyakhmatov, M. G.; Kashapov, N. F.

2013-12-01

Objects of research are coatings and technology of their applying to the piezoelectric elements for ultrasound. Acoustic impedance and thicknesses of matching layers for medical ultrasound transducers have been defined. In this paper performance characteristics of coating systems with predetermined properties have been selected. The conditions for selection of polymer powder paint for quarter wave matching layer have been determined. Conditions of forming polymer powder coatings have been proposed.

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.

Method for measuring recovery of catalytic elements from fuel cells

DOEpatents

Shore, Lawrence [Edison, NJ; Matlin, Ramail [Berkeley, NJ

2011-03-08

A method is provided for measuring the concentration of a catalytic clement in a fuel cell powder. The method includes depositing on a porous substrate at least one layer of a powder mixture comprising the fuel cell powder and an internal standard material, ablating a sample of the powder mixture using a laser, and vaporizing the sample using an inductively coupled plasma. A normalized concentration of catalytic element in the sample is determined by quantifying the intensity of a first signal correlated to the amount of catalytic element in the sample, quantifying the intensity of a second signal correlated to the amount of internal standard material in the sample, and using a ratio of the first signal intensity to the second signal intensity to cancel out the effects of sample size.

Nuclear forensic analysis of uranium oxide powders interdicted in Victoria, Australia

DOE PAGES

Kristo, Michael Joseph; Keegan, Elizabeth; Colella, Michael; ...

2015-04-13

Nuclear forensic analysis was conducted on two uranium samples confiscated during a police investigation in Victoria, Australia. The first sample, designated NSR-F-270409-1, was a depleted uranium powder of moderate purity (~1000 μg/g total elemental impurities). The chemical form of the uranium was a compound similar to K 2(UO 2) 3O 4·4H 2O. While aliquoting NSR-F-270409-1 for analysis, the body and head of a Tineid moth was discovered in the sample. The second sample, designated NSR-F-270409-2, was also a depleted uranium powder. It was of reasonably high purity (~380 μg/g total elemental impurities). The chemical form of the uranium was primarilymore » UO 3·2H 2O, with minor phases of U 3O 8 and UO 2. While aliquoting NSR-F-270409-2 for analysis, a metal staple of unknown origin was discovered in the sample. The presence of 236U and 232U in both samples indicates that the uranium feed stocks for these samples experienced a neutron flux at some point in their history. The reactor burn-up calculated from the isotopic composition of the uranium is consistent with that of spent fuel from natural uranium (NU) fueled Pu production. These nuclear forensic conclusions allow us to categorically exclude Australia as the origin of the material and greatly reduce the number of candidate sources.« less

Induced wettability and surface-volume correlation of composition for bovine bone derived hydroxyapatite particles

NASA Astrophysics Data System (ADS)

Maidaniuc, Andreea; Miculescu, Florin; Voicu, Stefan Ioan; Andronescu, Corina; Miculescu, Marian; Matei, Ecaterina; Mocanu, Aura Catalina; Pencea, Ion; Csaki, Ioana; Machedon-Pisu, Teodor; Ciocan, Lucian Toma

2018-04-01

Hydroxyapatite powders characteristics need to be determined both for quality control purposes and for a proper control of microstructural features of bone reconstruction products. This study combines bulk morphological and compositional analysis methods (XRF, SEM-EDS, FT-IR) with surface-related methods (XPS, contact angle measurements) in order to correlate the characteristics of hydroxyapatite powders derived from bovine bone for its use in medical applications. An experimental approach for correlating the surface and volume composition was designed based on the analysis depth of each spectral method involved in the study. Next, the influences of powder particle size and forming method on the contact angle between water drops and ceramic surface were evaluated for identifying suitable strategies of tuning hydroxyapatite's wettability. The results revealed a preferential arrangement of chemical elements at the surface of hydroxyapatite particles which could induce a favourable material behaviour in terms of sinterability and biological performance.

URANIUM OXIDE-CONTAINING FUEL ELEMENT COMPOSITION AND METHOD OF MAKING SAME

DOEpatents

Handwerk, J.H.; Noland, R.A.; Walker, D.E.

1957-09-10

In the past, bodies formed of a mixture of uranium dioxide and aluminum powder have been used in fuel elements; however, these mixtures were found not to be suitable when exposed to temperatures of about 600 deg C, because at such high temperatures the fuel elements were distorted. If uranosic oxide, U/sub 3/O/sub 8/, is substituted for UO/sub 2/, the mechanical properties are not impaired when these materials are used at about 600 deg C and no distortion takes place. The uranosic oxide and aluminum, both in powder form, are first mixed, and after a homogeneous mixture has been obtained, are shaped into fuel elements by extrusion at elevated temperature. Magnesium powder may be used in place of the aluminum.

Synthesis of nano-forsterite powder by making use of natural silica sand

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

Nurbaiti, Upik, E-mail: upik-nurbaiti@mail.unnes.ac.id; Department of Physics, Faculty of Mathematics and Natural Sciences Semarang State University Jl. Raya Sekaran GunungPati, Semarang 50221; Suud, Fikriyatul Azizah

2016-02-08

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples weremore » characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.« less

Production and Characterization of WC-Reinforced Co-Based Superalloy Matrix Composites

NASA Astrophysics Data System (ADS)

Özgün, Özgür; Dinler, İlyas

2018-05-01

Cobalt-based superalloy matrix composite materials were produced through the powder metallurgy technique using element powders at high purity and nano-sized wolfram carbide (WC) reinforcement in this study. An alloy that had the same chemical composition as the Stellite 6 alloy but not containing carbon was selected as the matrix alloy. The powder mixtures obtained as a result of mixing WC reinforcing member and element powders at the determined ratio were shaped by applying 300 MPa of pressure. The green components were sintered under argon atmosphere at 1240 °C for 120 minutes. The densities of the sintered components were determined by the Archimedes' principle. Microstructural characterization was performed via X-ray diffraction analysis, scanning electron microscope examinations, and energy-dispersive spectrometry. Hardness measurements and tensile tests were performed for determining mechanical characteristics. The relative density values of the sintered components increased by increasing the WC reinforcement ratio and they could almost reach the theoretical density. It was determined from the microstructural examinations that the composite materials consisted of fine and equiaxed grains and coarse carbides demonstrating a homogeneous dispersion along the microstructure at the grain boundaries. As it was the case in the density values, the hardness and strength values of the composites increased by increasing the WC ratio.

Production and Characterization of WC-Reinforced Co-Based Superalloy Matrix Composites

NASA Astrophysics Data System (ADS)

Özgün, Özgür; Dinler, İlyas

2018-07-01

Cobalt-based superalloy matrix composite materials were produced through the powder metallurgy technique using element powders at high purity and nano-sized wolfram carbide (WC) reinforcement in this study. An alloy that had the same chemical composition as the Stellite 6 alloy but not containing carbon was selected as the matrix alloy. The powder mixtures obtained as a result of mixing WC reinforcing member and element powders at the determined ratio were shaped by applying 300 MPa of pressure. The green components were sintered under argon atmosphere at 1240 °C for 120 minutes. The densities of the sintered components were determined by the Archimedes' principle. Microstructural characterization was performed via X-ray diffraction analysis, scanning electron microscope examinations, and energy-dispersive spectrometry. Hardness measurements and tensile tests were performed for determining mechanical characteristics. The relative density values of the sintered components increased by increasing the WC reinforcement ratio and they could almost reach the theoretical density. It was determined from the microstructural examinations that the composite materials consisted of fine and equiaxed grains and coarse carbides demonstrating a homogeneous dispersion along the microstructure at the grain boundaries. As it was the case in the density values, the hardness and strength values of the composites increased by increasing the WC ratio.

Numerical simulation and parametric analysis of selective laser melting process of AlSi10Mg powder

NASA Astrophysics Data System (ADS)

Pei, Wei; Zhengying, Wei; Zhen, Chen; Junfeng, Li; Shuzhe, Zhang; Jun, Du

2017-08-01

A three-dimensional numerical model was developed to investigate effects of laser scanning speed, laser power, and hatch spacing on the thermodynamic behaviors of the molten pool during selective laser melting of AlSi10Mg powder. A randomly distributed packed powder bed was achieved using discrete element method (DEM). The powder bed can be treated as a porous media with interconnected voids in the simulation. A good agreement between numerical results and experimental results establish the validity of adopted method. The numerical results show that the Marangoni flow within the molten pool was significantly affected by the processing parameters. An intense Marangoni flow leads to a perturbation within the molten pool. In addition, a relatively high scanning speed tends to cause melt instability. The perturbation or the instability within the molten pool results in the formation of pores during SLM, which have a direct influence on the densification level.

Evaluation of mechanically alloyed Cu-based powders as filler alloy for brazing tungsten to a reduced activation ferritic-martensitic steel

NASA Astrophysics Data System (ADS)

de Prado, J.; Sánchez, M.; Ureña, A.

2017-07-01

80Cu-20Ti powders were evaluated for their use as filler alloy for high temperature brazing of tungsten to a reduced activation ferritic/martensitic steel (Eurofer), and its application for the first wall of the DEMO fusion reactor. The use of alloyed powders has not been widely considered for brazing purposes and could improve the operational brazeability of the studied system due to its narrower melting range, determined by DTA analysis, which enhances the spreading capabilities of the filler. Ti contained in the filler composition acts as an activator element, reacting and forming several interfacial layers at the Eurofer-braze, which enhances the wettability properties and chemical interaction at the brazing interface. Brazing thermal cycle also activated the diffusion phenomena, which mainly affected to the Eurofer alloying elements causing in it a softening band of approximately 400 μm of thickness. However, this softening effect did not degrade the shear strength of the brazed joints (94 ± 23 MPa), because failure during testing was always located at the tungsten-braze interface.

Mechanical behaviour of pressed and sintered titanium alloys obtained from master alloy addition powders.

PubMed

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

2012-11-01

The fabrication of the workhorse Ti-6Al-4V alloy and of the Ti-3Al-2.5V alloy was studied considering the master alloy addition variant of the blending elemental approach conventionally used for titanium powder metallurgy. The powders were characterised by means thermal analysis and X-ray diffraction and shaped by means of uniaxial pressing. The microstructural evolution with the sintering temperature (900-1400 °C) was evaluated by SEM and EDS was used to study the composition. XRD patterns as well as the density by Archimedes method were also obtained. The results indicate that master alloy addition is a suitable way to fabricate well developed titanium alloy but also to produce alloy with the desired composition, not available commercially. Density of 4.3 g/cm³ can be obtained where a temperature higher than 1200 °C is needed for the complete diffusion of the alloying elements. Flexural properties comparable to those specified for wrought Ti-6Al-4V medical devices are, generally, obtained. Copyright © 2012 Elsevier Ltd. All rights reserved.

Laser-ablation ICP-MS as a tool for whole rock trace element analyses on fused powders

NASA Astrophysics Data System (ADS)

Girard, G.; Rooney, T. O.

2013-12-01

Here we present an accurate and precise technique for routine trace element analysis of geologic materials by laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). We focus on rock powders previously prepared for X-ray fluorescence by fusion in a Li2B4O7 flux, and subsequently quenched in a Pt mold to form a glass disk. Our method allows for the analysis up to 30 trace elements by LA-ICP-MS using a Photon-Machines Analyte G2 193 nm excimer laser coupled to a Thermo-Fisher Scientific ICAP Q quadrupole ICP-MS. Analyses are run as scans on the surface of the disks. Laser ablation conditions for which trace element fractionation effects are minimal have been empirically determined to be ~ 4 J m-2 fluence, at 10 Hz , and 10 μm s-1 scan speed, using a 110 μm laser beam size. Ablated material is carried into the ICP-MS by a He carrier at a rate of 0.75 L min-1. Following pre-ablation to remove surface particles, samples are ablated for 200 s, of which 140 s are used for data acquisition. At the end of each scan, a gas blank is collected for 30 s. Dwell times for each element vary between 15 and 60 μs, depending on abundance and instrument sensitivity, allowing 120 readings of each element during the data acquisition time window. To correct for variations in the total volume of material extracted by the laser, three internal standards are used, Ca, Fe and Zr. These elements are routinely analyzed by X-ray fluorescence by the Geoanalytical laboratory at Michigan State University with precision and accuracy of <5%. The availability of several internal standards allows for better correction of possible persisting laser ablation fractionation effects; for a particular trace element, we correct using the internal standard that best reproduces its ablation behavior. Our calibration is based on a combination of fused powders of US Geological Survey and Geological Survey of Japan rock standards, NIST SRM 612 glass, and US Geological Survey natural and synthetic basalt glasses. Instrumental drift is monitored during each run using two fused standards analyzed multiple times as unknowns. We routinely achieve an external precision of <5% on multiple replicates of standards run as unknowns, which are also within <5% of certified values. Elements analyzed include most first row transition metals, large ion lithophile elements, high field strength elements, lanthanide and actinide rare earth elements.

NUCLEAR REACTOR FUEL ELEMENTS AND METHOD OF PREPARATION

DOEpatents

Kingston, W.E.; Kopelman, B.; Hausner, H.H.

1963-07-01

A fuel element consisting of uranium nitride and uranium carbide in the form of discrete particles in a solid coherent matrix of a metal such as steel, beryllium, uranium, or zirconium and clad with a metal such as steel, aluminum, zirconium, or beryllium is described. The element is made by mixing powdered uranium nitride and uranium carbide with powdered matrix metal, then compacting and sintering the mixture. (AEC)

Development of a Novel Ni-Fe-Cr-B-Si Interlayer Material for Transient Liquid Phase Bonding of Inconel 718

NASA Astrophysics Data System (ADS)

Tarai, U. K.; Robi, P. S.; Pal, Sukhomay

2018-04-01

A Ni-Cr-Fe-Si-B based interlayer material was developed by mechanical alloying (MA) process in a high-energy planetary ball mill. Equiaxed alloy powders of size 12 µm was obtained after milling for 50 hours. X-ray diffraction analysis of the milled powder revealed that milling of elemental powders initially resulted in microcrystalline alloy powder having face centered cubic structure, which on subsequent milling resulted in nano-crystallice alloy powder with a crystallite size of 3.2 nm. XRD analysis also reveals formation of metastable eutectic alloys resulting in lowering of the melting point of the interlayer material to 1025 °C. IN 718 superalloy samples were joined at 1050°C using the developed interlayer. A homogeneous joint was formed by the newly developed interlayer material. Three different zones were observed at the bond (i) isothermally solidified zone, (ii) diffusion affected zone and (iii) unaffected base metal. In the diffusion-affected zone, boron was present at the grain boundaries of Ni γ matrix in bulky metal borides form. The diffusion of boron from interlayer material into the base material was mechanism of isothermal solidification and bond formation in transient liquid phase bonding of IN 718.

Reproducing Kernel Particle Method in Plasticity of Pressure-Sensitive Material with Reference to Powder Forming Process

NASA Astrophysics Data System (ADS)

Khoei, A. R.; Samimi, M.; Azami, A. R.

2007-02-01

In this paper, an application of the reproducing kernel particle method (RKPM) is presented in plasticity behavior of pressure-sensitive material. The RKPM technique is implemented in large deformation analysis of powder compaction process. The RKPM shape function and its derivatives are constructed by imposing the consistency conditions. The essential boundary conditions are enforced by the use of the penalty approach. The support of the RKPM shape function covers the same set of particles during powder compaction, hence no instability is encountered in the large deformation computation. A double-surface plasticity model is developed in numerical simulation of pressure-sensitive material. The plasticity model includes a failure surface and an elliptical cap, which closes the open space between the failure surface and hydrostatic axis. The moving cap expands in the stress space according to a specified hardening rule. The cap model is presented within the framework of large deformation RKPM analysis in order to predict the non-uniform relative density distribution during powder die pressing. Numerical computations are performed to demonstrate the applicability of the algorithm in modeling of powder forming processes and the results are compared to those obtained from finite element simulation to demonstrate the accuracy of the proposed model.

[Ultra-Fine Pressed Powder Pellet Sample Preparation XRF Determination of Multi-Elements and Carbon Dioxide in Carbonate].

PubMed

Li, Xiao-li; An, Shu-qing; Xu, Tie-min; Liu, Yi-bo; Zhang, Li-juan; Zeng, Jiang-ping; Wang, Na

2015-06-01

The main analysis error of pressed powder pellet of carbonate comes from particle-size effect and mineral effect. So in the article in order to eliminate the particle-size effect, the ultrafine pressed powder pellet sample preparation is used to the determination of multi-elements and carbon-dioxide in carbonate. To prepare the ultrafine powder the FRITSCH planetary Micro Mill machine and tungsten carbide media is utilized. To conquer the conglomeration during the process of grinding, the wet grinding is preferred. The surface morphology of the pellet is more smooth and neat, the Compton scatter effect is reduced with the decrease in particle size. The intensity of the spectral line is varied with the change of the particle size, generally the intensity of the spectral line is increased with the decrease in the particle size. But when the particle size of more than one component of the material is decreased, the intensity of the spectral line may increase for S, Si, Mg, or decrease for Ca, Al, Ti, K, which depend on the respective mass absorption coefficient . The change of the composition of the phase with milling is also researched. The incident depth of respective element is given from theoretical calculation. When the sample is grounded to the particle size of less than the penetration depth of all the analyte, the effect of the particle size on the intensity of the spectral line is much reduced. In the experiment, when grounded the sample to less than 8 μm(d95), the particle-size effect is much eliminated, with the correction method of theoretical α coefficient and the empirical coefficient, 14 major, minor and trace element in the carbonate can be determined accurately. And the precision of the method is much improved with RSD < 2%, except Na2O. Carbon is ultra-light element, the fluorescence yield is low and the interference is serious. With the manual multi-layer crystal PX4, coarse collimator, empirical correction, X-ray spectrometer can be used to determine the carbon dioxide in the carbonate quantitatively. The intensity of the carbon is increase with the times of the measurement and the time delay even the pellet is stored in the dessicator. So employing the latest pressed powder pellet is suggested.

Gravity flow of powder in a lunar environment. Part 2: Analysis of flow initiation

NASA Technical Reports Server (NTRS)

Pariseau, W. G.

1971-01-01

A small displacement-small strain finite element technique utilizing the constant strain triangle and incremental constitutive equations for elasticplastic (media nonhardening and obeying a Coulomb yield condition) was applied to the analysis of gravity flow initiation. This was done in a V-shaped hopper containing a powder under lunar environmental conditions. Three methods of loading were examined. Of the three, the method of computing the initial state of stress in a filled hopper prior to drawdown, by adding material to the hopper layer by layer, was the best. Results of the analysis of a typical hopper problem show that the initial state of stress, the elastic moduli, and the strength parameters have an important influence on material response subsequent to the opening of the hopper outlet.

Non-linear optical properties of arylfuranylpropenones

NASA Astrophysics Data System (ADS)

Holla, B. Shivarama; Veerendra, B.; Indira, J.

2003-05-01

A series of arylfuranylpropenones 3a-i were synthesized by the reaction of 5-(2-nitro-4-methoxyphenyl)-2-furfural 1 with various acetophenones 2 by Claisen-Schmidt condensation. All the newly synthesized chalcones were characterized by elemental analysis and spectral studies. Most of them showed SHG conversion efficiency in powder form.

Processing of a porous titanium alloy from elemental powders using a solid state isothermal foaming technique.

PubMed

Nugroho, Aris W; Leadbeater, Garry; Davies, Ian J

2010-12-01

The authors have conducted a preliminary investigation with regard to the potential to manufacture porous titanium alloys for biomedical applications using toxic-free elemental powders, i.e., Ti, Nb, Ta, Zr, in combination with the pressurised gas bubble entrapment method and in contrast to standard processing routes that generally utilise prealloyed powder containing potentially toxic elements. Elemental powder compacts were either hot isostatic pressed (HIP-ed) at 1000°C and then foamed at 1150°C or else HIP-ed at 1100°C and foamed at 1350°C. Porous α + β alloys containing up to 45 vol% of porosity in the size range 20-200 μm were successfully produced, thus highlighting the potential of this manufacturing route. It was expected that further optimisation of the processing route would allow full development of the preferred β-Ti phase (from the point of view of elastic modulus compatibility between implant and bone) with this being the subject of future work by the authors.

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.

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.

Biosorption of praseodymium (III) using Terminalia arjuna bark powder in batch systems: isotherm and kinetic studies.

PubMed

Swain, Krishna Kumari; Mishra, Pravat Manjari; Devi, Aparna Prabha

2018-02-01

The high demand for rare earth elements (REEs) used in various advanced materials implies demand for increased production of REEs or the recycling of solutions to recover the REEs they contain. In this study, the biosorption of Pr(III) from aqueous solution by bark powder of Terminalia arjuna was examined in a batch system as a function of metal concentration, biosorbent dosage, pH and contact time. Results showed that T. arjuna bark powder has a high affinity for adsorbing Pr(III): more than 90% at pH 6.63. The adsorption of Pr(III) by T. arjuna bark powder was investigated by the Langmuir, Freundlich, Temkin and Dubinin-Radushkevich isotherm models. The kinetics of the biosorption process was tested with pseudo-first-order and pseudo-second-order models, and the results showed that the biosorption process was better fitted to the pseudo-second-order model. From Fourier transform infrared spectroscopy (FT-IR) analysis, it is confirmed that the biomolecules of T. arjuna bark powder are involved in the biosorption process of Pr(III) metal ions.

Multidisciplinary study of Wyoming test sites. [hydrology, biology, geology, lithology, geothermal, and land use

NASA Technical Reports Server (NTRS)

Houston, R. S. (Principal Investigator); Marrs, R. W.; Agard, S. S.; Downing, K. G.; Earle, J. L.; Froman, N. L.; Gordon, R.; Kolm, K. E.; Tomes, B.; Vietti, J.

1974-01-01

The author has identified the following significant results. Investigation of a variety of applications of EREP photographic data demonstrated that EREP S-190 data offer a unique combination of synoptic coverage and image detail. The broad coverage is ideal for regional geologic mapping and tectonic analysis while the detail is adequate for mapping of crops, mines, urban areas, and other relatively small features. The investigative team at the University of Wyoming has applied the EREP S-190 data to: (1) analysis of photolinear elements of the Powder River Basin, southern Montana, and the Wind River Mountains; (2) drainage analysis of the Powder River Basin and Beartooth Mountains; (3) lithologic and geologic mapping in the Powder River Basin, Black Hills, Green River Basin, Bighorn Basin and Southern Bighorn Mountains; (4) location of possible mineralization in the Absaroka Range; and (5) land use mapping near Riverton and Gillette. All of these applications were successful to some degree. Image enhancement procedures were useful in some efforts requiring distinction of small objects or subtle contrasts.

Some critical aspects of FT-IR, TGA, powder XRD, EDAX and SEM studies of calcium oxalate urinary calculi.

PubMed

Joshi, Vimal S; Vasant, Sonal R; Bhatt, J G; Joshi, Mihir J

2014-06-01

Urinary calculi constitute one of the oldest afflictions of humans as well as animals, which are occurring globally. The calculi vary in shape, size and composition, which influence their clinical course. They are usually of the mixed-type with varying percentages of the ingredients. In medical management of urinary calculi, either the nature of calculi is to be known or the exact composition of calculi is required. In the present study, two selected calculi were recovered after surgery from two different patients for detailed examination and investigated by using Fourier-Transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA), powder X-ray diffraction (XRD), scanning electron microscopy and energy dispersive analysis of X-rays (EDAX) techniques. The study demonstrated that the nature of urinary calculi and presence of major phase in mixed calculi could be identified by FT-IR, TGA and powder XRD, however, the exact content of various elements could be found by EDAX only.

The application of Westcott Formalism k0 NAA method to estimate short and medium lived elements in some Ghanaian herbal medicines complemented by AAS

NASA Astrophysics Data System (ADS)

Ayivor, J. E.; Okine, L. K. N.; Dampare, S. B.; Nyarko, B. J. B.; Debrah, S. K.

2012-04-01

The epithermal neutron shape factor, α of the inner and outer irradiation sites of the Ghana Research Reactor-1 (GHARR-1) was determined obtaining results of 0.105 for the inner (Channel 1) Irradiation site and 0.020 for the outer (channel 6) irradiation site. The neutron temperatures for the inner and outer irradiation sites were 27 °C and 20 °C, respectively. The α values used in Westcott Formalism k0 INAA was applied to determine multi elements in 13 Ghanaian herbal medicines used by the Centre for Scientific Research into Plant Medicine (CSRPM) for the management of various diseases complemented by Atomic Absorption Spectrometry. They are namely Mist. Antiaris, Mist. Enterica, Mist. Morazia, Mist. Nibima, Mist. Modium, Mist. Ninger, Mist Sodenia, Mist. Tonica, Chardicca Powder, Fefe Powder, Olax Powder, Sirrapac powder and Lippia Tea. Concentrations of Al, As, Br, K, Cl, Cu, Mg, Mn, Na and V were determined by short and medium irradiations at a thermal neutron flux of 5×1011 ncm-2 s-1. Fe, Cr, Pb, Co, Ni, Sn, Ca, Ba, Li and Sb were determined using Atomic Absorption Spectrometry (AAS). Ba, Cu, Li and V were present at trace levels whereas Al, Cl, Na, Ca were present at major levels. K, Br, Mg, Mn, Co, Ni, Fe and Sb were also present at minor levels. Arsenic was not detected in all samples. Standard Reference material, IAEA-V-10 Hay Powder was simultaneously analysed with samples. The precision and accuracy of the method using real samples and standard reference materials were evaluated and within ±10% of the reported value. Multivariate analytical techniques, such as cluster analysis (Q-mode and R-mode CA) and principal component analysis (PCA)/factor analysis (FA), have been applied to evaluate the chemical variations in the herbal medicine dataset. All the 13 samples may be grouped into 2 statistically significant clusters (liquid based and powdered herbal medicines), reflecting the different chemical compositions. R-mode CA and PCA suggest common sources for Co, Mg, Fe, Ca, Cr, Ni, Sn, Li and Sb and Na, V, Cl, Mn, Al, Br and K. The PCA/FA identified 3 dominant factors as responsible for the data structure, explaining 84.5% of the total variance in the dataset.

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

NASA Technical Reports Server (NTRS)

Ross, H. Richard

1993-01-01

A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

Advanced Mechanical Properties of a Powder Metallurgy Ti-Al-N Alloy Doped with Ultrahigh Nitrogen Concentration

NASA Astrophysics Data System (ADS)

Shen, J.; Chen, B.; Umeda, J.; Kondoh, K.

2018-03-01

Titanium and its alloys are recognized for their attractive properties. However, high-performance Ti alloys are often alloyed with rare or noble-metal elements. In the present study, Ti alloys doped with only ubiquitous elements were produced via powder metallurgy. The experimental results showed that pure Ti with 1.5 wt.% AlN incorporated exhibited excellent tensile properties, superior to similarly extruded Ti-6Al-4V. Further analysis revealed that its remarkably advanced strength could primarily be attributed to nitrogen solid-solution strengthening, accounting for nearly 80% of the strength increase of the material. In addition, despite the ultrahigh nitrogen concentration up to 0.809 wt.%, the Ti-1.5AlN sample showed elongation to failure of 10%. This result exceeds the well-known limitation for nitrogen (over 0.45 wt.%) that causes embrittlement of Ti alloys.

Elemental assessment of vegetation via portable X-ray fluorescence (PXRF) spectrometry.

PubMed

McGladdery, Candice; Weindorf, David C; Chakraborty, Somsubhra; Li, Bin; Paulette, Laura; Podar, Dorina; Pearson, Delaina; Kusi, Nana Yaw O; Duda, Bogdan

2018-03-15

Elemental concentrations in vegetation are of critical importance, whether establishing plant essential element concentrations (toxicity vs. deficiency) or investigating deleterious elements (e.g., heavy metals) differentially extracted from the soil by plants. Traditionally, elemental analysis of vegetation has been facilitated by acid digestion followed by quantification via inductively coupled plasma (ICP) or atomic absorption (AA) spectroscopy. Previous studies have utilized portable X-ray fluorescence (PXRF) spectroscopy to quantify elements in soils, but few have evaluated the vegetation. In this study, a PXRF spectrometer was employed to scan 228 organic material samples (thatch, deciduous leaves, grasses, tree bark, and herbaceous plants) from smelter-impacted areas of Romania, as well as National Institute of Standards and Technology (NIST) certified reference materials, to demonstrate the application of PXRF for elemental determination in vegetation. Samples were scanned in three conditions: as received from the field (moist), oven dry (70 °C), and dried and powdered to pass a 2 mm sieve. Performance metrics of PXRF models relative to ICP atomic emission spectroscopy were developed to asses optimal scanning conditions. Thatch and bark samples showed the highest mean PXRF and ICP concentrations (e.g., Zn, Pb, Cd, Fe), with the exceptions of K and Cl. Validation statistics indicate that the stable validation predictive capacity of PXRF increased in the following order: oven dry intact < field moist < oven dried and powdered. Even under field moist conditions, PXRF could reasonably be used for the determination of Zn (coefficient of determination, R 2 val 0.86; residual prediction deviation, RPD 2.72) and Cu (R 2 val 0.77; RPD 2.12), while dried and powdered samples allowed for stable validation prediction of Pb (R 2 val 0.90; RPD 3.29), Fe (R 2 val 0.80; RPD 2.29), Cd (R 2 val 0.75; RPD 2.07) and Cu (R 2 val 0.98; RPD of 8.53). Summarily, PXRF was shown to be a useful approach for quickly assessing the elemental concentration in vegetation. Future PXRF/vegetation research should explore additional elements and investigate its usefulness in evaluating phytoremediation effectiveness. Copyright © 2018 Elsevier Ltd. All rights reserved.

Charged particle induced delayed X-rays (DEX) for the analysis of intermediate and heavy elements

NASA Astrophysics Data System (ADS)

Pillay, A. E.; Erasmus, C. S.; Andeweg, A. H.; Sellschop, J. P. F.; Annegarn, H. J.; Dunn, J.

1988-12-01

The emission of K X-rays from proton-rich and metastable radionuclides, following proton activation of the stable isotopes of the elements of interest, has not been widely used as a means of analysis. The thrust of this paper proposes a nuclear technique using delayed X-rays for the analysis of low concentrations of intermediate and heavy elements. The method is similar to the delayed gamma-ray technique. Proton bombardment induces mainly (p, n) reactions whereas the delayed X-rays originate largely from e --capture and isomeric transition. Samples of rare earth and platinum group elements (PGE), in the form of compacted powders, were irradiated with an 11 MeV proton beam and delayed X-rays detected with a 100 mm 2 Ge detector. Single element spectra for a range of rare earths and PGEs are presented. Analytical conditions are demonstrated for Pd in the range 0.1-5%. Spectra from actual geological samples of a PGE ore, preconcentrated by fire-assay, and monazite are presented. All six platinum group elements are visible and interference-free in a single spectrum, a marked advance on other nuclear techniques for these elements, including PIXE and neutron activation analysis (NAA).

FUEL ELEMENTS FOR NUCLEAR REACTORS

DOEpatents

Blainey, A.; Lloyd, H.

1961-07-11

A method of sheathing a tubular fuel element for a nuclear reactor is described. A low melting metal core member is centered in a die, a layer of a powdered sheathing substance is placed on the bottom of the die, the tubular fuel element is inserted in the die, the space between the tubular fuel element and the die walls and core member is filled with the same powdered sheathing substance, a layer of the same substance is placed over the fissile material, and the charge within the die is subjected to pressure in the direction of the axis of the fuel element at the sintering temperature of the protective substance.

Nuclear forensic analysis of an unknown uranium ore concentrate sample seized in a criminal investigation in Australia

DOE PAGES

Keegan, Elizabeth; Kristo, Michael J.; Colella, Michael; ...

2014-04-13

In early 2009, a state policing agency raided a clandestine drug laboratory in a suburb of a major city in Australia. While searching the laboratory, they discovered a small glass jar labelled “Gamma Source” and containing a green powder. The powder was radioactive. This paper documents the detailed nuclear forensic analysis undertaken to characterize and identify the material and determine its provenance. Isotopic and impurity content, phase composition, microstructure and other characteristics were measured on the seized sample, and the results were compared with similar material obtained from the suspected source (ore and ore concentrate material). While an extensive rangemore » of parameters were measured, the key ‘nuclear forensic signatures’ used to identify the material were the U isotopic composition, Pb and Sr isotope ratios, and the rare earth element pattern. These measurements, in combination with statistical analysis of the elemental and isotopic content of the material against a database of uranium ore concentrates sourced from mines located worldwide, led to the conclusion that the seized material (a uranium ore concentrate of natural isotopic abundance) most likely originated from Mary Kathleen, a former Australian uranium mine.« less

Nuclear forensic analysis of an unknown uranium ore concentrate sample seized in a criminal investigation in Australia.

PubMed

Keegan, Elizabeth; Kristo, Michael J; Colella, Michael; Robel, Martin; Williams, Ross; Lindvall, Rachel; Eppich, Gary; Roberts, Sarah; Borg, Lars; Gaffney, Amy; Plaue, Jonathan; Wong, Henri; Davis, Joel; Loi, Elaine; Reinhard, Mark; Hutcheon, Ian

2014-07-01

Early in 2009, a state policing agency raided a clandestine drug laboratory in a suburb of a major city in Australia. During the search of the laboratory, a small glass jar labelled "Gamma Source" and containing a green powder was discovered. The powder was radioactive. This paper documents the detailed nuclear forensic analysis undertaken to characterise and identify the material and determine its provenance. Isotopic and impurity content, phase composition, microstructure and other characteristics were measured on the seized sample, and the results were compared with similar material obtained from the suspected source (ore and ore concentrate material). While an extensive range of parameters were measured, the key 'nuclear forensic signatures' used to identify the material were the U isotopic composition, Pb and Sr isotope ratios, and the rare earth element pattern. These measurements, in combination with statistical analysis of the elemental and isotopic content of the material against a database of uranium ore concentrates sourced from mines located worldwide, led to the conclusion that the seized material (a uranium ore concentrate of natural isotopic abundance) most likely originated from Mary Kathleen, a former Australian uranium mine. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Nuclear forensic analysis of an unknown uranium ore concentrate sample seized in a criminal investigation in Australia

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

Keegan, Elizabeth; Kristo, Michael J.; Colella, Michael

In early 2009, a state policing agency raided a clandestine drug laboratory in a suburb of a major city in Australia. While searching the laboratory, they discovered a small glass jar labelled “Gamma Source” and containing a green powder. The powder was radioactive. This paper documents the detailed nuclear forensic analysis undertaken to characterize and identify the material and determine its provenance. Isotopic and impurity content, phase composition, microstructure and other characteristics were measured on the seized sample, and the results were compared with similar material obtained from the suspected source (ore and ore concentrate material). While an extensive rangemore » of parameters were measured, the key ‘nuclear forensic signatures’ used to identify the material were the U isotopic composition, Pb and Sr isotope ratios, and the rare earth element pattern. These measurements, in combination with statistical analysis of the elemental and isotopic content of the material against a database of uranium ore concentrates sourced from mines located worldwide, led to the conclusion that the seized material (a uranium ore concentrate of natural isotopic abundance) most likely originated from Mary Kathleen, a former Australian uranium mine.« less

Effects of Process Parameters on Copper Powder Compaction Process Using Multi-Particle Finite Element Method

NASA Astrophysics Data System (ADS)

Güner, F.; Sofuoğlu, H.

2018-01-01

Powder metallurgy (PM) has been widely used in several industries; especially automotive and aerospace industries and powder metallurgy products grow up every year. The mechanical properties of the final product that is obtained by cold compaction and sintering in powder metallurgy are closely related to the final relative density of the process. The distribution of the relative density in the die is affected by parameters such as compaction velocity, friction coefficient and temperature. Moreover, most of the numerical studies utilizing finite element approaches treat the examined environment as a continuous media with uniformly homogeneous porosity whereas Multi-Particle Finite Element Method (MPFEM) treats every particles as an individual body. In MPFEM, each of the particles can be defined as an elastic- plastic deformable body, so the interactions of the particles with each other and the die wall can be investigated. In this study, each particle was modelled and analyzed as individual deformable body with 3D tetrahedral elements by using MPFEM approach. This study, therefore, was performed to investigate the effects of different temperatures and compaction velocities on stress distribution and deformations of copper powders of 200 µm-diameter in compaction process. Furthermore, 3-D MPFEM model utilized von Mises material model and constant coefficient of friction of μ=0.05. In addition to MPFEM approach, continuum modelling approach was also performed for comparison purposes.

In situ elaboration of a binary Ti-26Nb alloy by selective laser melting of elemental titanium and niobium mixed powders.

PubMed

Fischer, M; Joguet, D; Robin, G; Peltier, L; Laheurte, P

2016-05-01

Ti-Nb alloys are excellent candidates for biomedical applications such as implantology and joint replacement because of their very low elastic modulus, their excellent biocompatibility and their high strength. A low elastic modulus, close to that of the cortical bone minimizes the stress shielding effect that appears subsequent to the insertion of an implant. The objective of this study is to investigate the microstructural and mechanical properties of a Ti-Nb alloy elaborated by selective laser melting on powder bed of a mixture of Ti and Nb elemental powders (26 at.%). The influence of operating parameters on porosity of manufactured samples and on efficacy of dissolving Nb particles in Ti was studied. The results obtained by optical microscopy, SEM analysis and X-ray microtomography show that the laser energy has a significant effect on the compactness and homogeneity of the manufactured parts. Homogeneous and compact samples were obtained for high energy levels. Microstructure of these samples has been further characterized. Their mechanical properties were assessed by ultrasonic measures and the Young's modulus found is close to that of classically elaborated Ti-26 Nbingot. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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.

Metal vapor micro-jet controls material redistribution in laser powder bed fusion additive manufacturing.

PubMed

Ly, Sonny; Rubenchik, Alexander M; Khairallah, Saad A; Guss, Gabe; Matthews, Manyalibo J

2017-06-22

The results of detailed experiments and finite element modeling of metal micro-droplet motion associated with metal additive manufacturing (AM) processes are presented. Ultra high speed imaging of melt pool dynamics reveals that the dominant mechanism leading to micro-droplet ejection in a laser powder bed fusion AM is not from laser induced recoil pressure as is widely believed and found in laser welding processes, but rather from vapor driven entrainment of micro-particles by an ambient gas flow. The physics of droplet ejection under strong evaporative flow is described using simulations of the laser powder bed interactions to elucidate the experimental results. Hydrodynamic drag analysis is used to augment the single phase flow model and explain the entrainment phenomenon for 316 L stainless steel and Ti-6Al-4V powder layers. The relevance of vapor driven entrainment of metal micro-particles to similar fluid dynamic studies in other fields of science will be discussed.

SERS-active Au/SiO2 clouds in powder for rapid ex vivo breast adenocarcinoma diagnosis

PubMed Central

Cepeda-Pérez, Elisa; López-Luke, Tzarara; Salas, Pedro; Plascencia-Villa, Germán; Ponce, Arturo; Vivero-Escoto, Juan; José-Yacamán, Miguel; de la Rosa, Elder

2016-01-01

In the present work, we report a dry-based application technique of Au/SiO2 clouds in powder for rapid ex vivo adenocarcinoma diagnosis through surface-enhanced Raman scattering (SERS); using low laser power and an integration time of one second. Several characteristic Raman peaks frequently used for the diagnosis of breast adenocarcinoma in the range of the amide III are successfully enhanced by breading the tissue with Au/SiO2 powder. The SERS activity of these Au/SiO2 powders is attributed to their rapid rehydration upon contact with the wet tissues, which promotes the formation of gold nanoparticle aggregates. The propensity of the Au/SiO2 cloud structures to adsorb biomolecules in the vicinity of the gold nanoparticle clusters promotes the necessary conditions for SERS detection. In addition, electron microscopy, together with elemental analysis, have been used to confirm the structure of the new Au/SiO2 cloud material and to investigate its distribution in breast tissues. PMID:27375955

Metal vapor micro-jet controls material redistribution in laser powder bed fusion additive manufacturing

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

Ly, Sonny; Rubenchik, Alexander M.; Khairallah, Saad A.

The results of detailed experiments and finite element modeling of metal micro-droplet motion associated with metal additive manufacturing (AM) processes are presented. Ultra high speed imaging of melt pool dynamics reveals that the dominant mechanism leading to micro-droplet ejection in a laser powder bed fusion AM is not from laser induced recoil pressure as is widely believed and found in laser welding processes, but rather from vapor driven entrainment of micro-particles by an ambient gas flow. The physics of droplet ejection under strong evaporative flow is described using simulations of the laser powder bed interactions to elucidate the experimental results.more » Hydrodynamic drag analysis is used to augment the single phase flow model and explain the entrainment phenomenon for 316 L stainless steel and Ti-6Al-4V powder layers. The relevance of vapor driven entrainment of metal micro-particles to similar fluid dynamic studies in other fields of science will be discussed.« less

Metal vapor micro-jet controls material redistribution in laser powder bed fusion additive manufacturing

DOE PAGES

Ly, Sonny; Rubenchik, Alexander M.; Khairallah, Saad A.; ...

2017-06-22

The results of detailed experiments and finite element modeling of metal micro-droplet motion associated with metal additive manufacturing (AM) processes are presented. Ultra high speed imaging of melt pool dynamics reveals that the dominant mechanism leading to micro-droplet ejection in a laser powder bed fusion AM is not from laser induced recoil pressure as is widely believed and found in laser welding processes, but rather from vapor driven entrainment of micro-particles by an ambient gas flow. The physics of droplet ejection under strong evaporative flow is described using simulations of the laser powder bed interactions to elucidate the experimental results.more » Hydrodynamic drag analysis is used to augment the single phase flow model and explain the entrainment phenomenon for 316 L stainless steel and Ti-6Al-4V powder layers. The relevance of vapor driven entrainment of metal micro-particles to similar fluid dynamic studies in other fields of science will be discussed.« less

Formation of microporous NiTi by transient liquid phase sintering of elemental powders.

PubMed

Ismail, Muhammad Hussain; Goodall, Russell; Davies, Hywel A; Todd, Iain

2012-08-01

Porous metallic structures are attractive for biomedical implant applications as their open porosity simultaneously improves the degree of fixation and decreases the mismatch in stiffness between bone and implant, improving bonding and reducing stress-shielding effects respectively. NiTi alloys exhibit both the shape memory effect and pseudoelasticity, and are of particular interest, though they pose substantial problems in their processing. This is because the shape memory and pseudoelastic behaviours are exceptionally sensitive to the presence of oxygen, and other minor changes in alloy chemistry. Thus in processing careful control of composition and contamination is vital. In this communication, we investigate these issues in a novel technique for producing porous NiTi parts via transient liquid phase sintering following metal injection moulding (MIM) of elemental Ni and Ti powders, and report a new mechanism for pore formation in the powder processing of metallic materials from elemental powders. Copyright © 2012 Elsevier B.V. All rights reserved.

Thermal Modeling and Simulation of Electron Beam Melting for Rapid Prototyping on Ti6Al4V Alloys

NASA Astrophysics Data System (ADS)

Neira Arce, Alderson

To be a viable solution for contemporary engineering challenges, the use of titanium alloys in a wider range of applications requires the development of new techniques and processes that are able to decrease production cost and delivery times. As a result, the use of material consolidation in a near-net-shape fashion, using dynamic techniques like additive manufacturing by electron beam selective melting EBSM represents a promising method for part manufacturing. However, a new product material development can be cost prohibitive, requiring the use of computer modeling and simulation as a way to decrease turnaround time. To ensure a proper representation of the EBSM process, a thermophysical material characterization and comparison was first performed on two Ti6Al4V powder feedstock materials prepared by plasma (PREP) and gas atomized (GA) processes. This evaluation comprises an evaluation on particle size distribution, density and powder surface area, collectively with the temperature dependence on properties such as heat capacity, thermal diffusivity, thermal conductivity and surface emissivity. Multiple techniques were employed in this evaluation, including high temperature differential scanning calorimetry (HT-DSC), laser flash analysis (LFA), infrared remote temperature analysis (IR-Thermography), laser diffraction, liquid and gas pycnometry using mercury and krypton adsorption respectively. This study was followed by the review of complementary strategies to simulate the temperature evolution during the EBSM process, using a finite element analysis package called COMSOL Multiphysics. Two alternatives dedicated to representing a moving heat source (electron beam) and the powder bed were developed using a step-by-step approximation initiative. The first method consisted of the depiction of a powder bed discretized on an array of domains, each one representing a static melt pool, where the moving heat source was illustrated by a series of time dependant selective heating and cooling steps. The second method consisted of the solution of a prescribed domain, where each powder layer is discretized by an individual 3D element and the heat source is represented by a 1D element displaced by a temperature-coupling extrapolation routine. Two validation strategies were presented here; the first was used to confirm the accuracy of the proposed model strategy by setting up a controlled experiment; the second was used to validate the post-processing data obtained by the simulation by comparison with in-situ measured EBSM process temperature. Finally, a post-process part evaluation on surface finishing and part porosity was discussed including an assessment of the use of non-destructive inspection techniques such as 3D profilometry by axial chromatism for surface roughness, partial section analysis by serial block-face scanning electron microscopy (SBFSEM) and micro computed tomography (CT-Scan) for pore and inclusion detection.

Structural and Electrical Properties of Lithium-Ion Rechargeable Battery Using the LiFePO4/Carbon Cathode Material.

PubMed

Kim, Young-Sung; Jeoung, Tae-Hoon; Nam, Sung-Pill; Lee, Seung-Hwan; Kim, Jea-Chul; Lee, Sung-Gap

2015-03-01

LiFePO4/C composite powder as cathode material and graphite powder as anode material for Li-ion batteries were synthesized by using the sol-gel method. An electrochemical improvement of LiFePO4 materials has been achieved by adding polyvinyl alcohol as a carbon source into as-prepared materials. The samples were characterized by elemental analysis (EA), X-ray diffraction (XRD), and field emission scanning electron microscopy (FE-EM). The chemical composition of LiFePO4/C powders was in a good agreement with that of the starting solution. The capacity loss after 500 cycles of LiFePO4/C cell is 11.1% in room temperature. These superior electrochemical properties show that LiFePO4/C composite materials are promising candidates as cathode materials.

Epithermal Neutron Activation Analysis of the Asian Herbal Plants

NASA Astrophysics Data System (ADS)

Baljinnyam, N.; Jugder, B.; Norov, N.; Frontasyeva, M. V.; Ostrovnaya, T. M.; Pavlov, S. S.

2011-06-01

Asian medicinal herbs Chrysanthemum (Spiraea aquilegifolia Pall.) and Red Sandalwood (Pterocarpus Santalinus) are widely used in folk and Ayurvedic medicine for healing and preventing some diseases. The modern medical science has proved that the Chrysanthemum (Spiraea aquilegifolia Pall.) possesses the following functions: reducing blood press, dispelling cancer cell, coronary artery's expanding and bacteriostating and Red Sandalwood (Pterocarpus Santalinus) is recommended against headache, toothache, skin diseases, vomiting and sometimes it is taken for treatment of diabetes. Species of Chrysanthemums were collected in the north-eastern and central Mongolia, and the Red Sandalwood powder was imported from India. Samples of Chrysanthemums (branches, flowers and leaves) (0.5 g) and red sandalwood powder (0.5 g) were subjected to the multi-element instrumental neutron activation analysis using epithermal neutrons (ENAA) at the IBR-2 reactor, Frank Laboratory of Neutron Physics (FLNP) JINR, Dubna. A total of 41 elements (Na, Mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Zn, As, Se, Br, Rb, Sr, Zr, Mo, Cd, Cs, Ba, La, Hf, Ta, W, Sb, Au, Hg, Ce, Nd, Sm, Eu, Tb, Dy, Yb, Th, U, Lu) were determined. For the first time such a large group of elements was determined in the herbal plants used in Mongolia. The quality control of the analytical results was provided by using certified reference material Bowen Cabbage. The results obtained are compared to the "Reference plant» data (B. Markert, 1992) and interpreted in terms of excess of such elements as Se, Cr, Ca, Fe, Ni, Mo, and rare earth elements.

Fabrication of spherical high-nitrogen stainless steel powder alloys by mechanical alloying and thermal plasma spheroidization

NASA Astrophysics Data System (ADS)

Razumov, Nikolay G.; Wang, Qing Sheng; Popovich, Anatoly A.; Shamshurin, Aleksey I.

2018-04-01

This paper describes the results of experimental studies on the treatment of Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys, synthesized by the mechanical alloying (MA) of elemental powders in the flow of a radio frequency thermal plasma. The as-milled powder with irregular particles were successfully converted into spherical high-nitrogen stainless steel powder alloy. Measurement of the residual nitrogen content in the obtained powder, shown that during the plasma spheroidization process, part of the nitrogen escapes from the alloy.

Selective Laser Melting of Pure Copper

NASA Astrophysics Data System (ADS)

Ikeshoji, Toshi-Taka; Nakamura, Kazuya; Yonehara, Makiko; Imai, Ken; Kyogoku, Hideki

2017-12-01

Appropriate building parameters for selective laser melting of 99.9% pure copper powder were investigated at relatively high laser power of 800 W for hatch pitch in the range from 0.025 mm to 0.12 mm. The highest relative density of the built material was 99.6%, obtained at hatch pitch of 0.10 mm. Building conditions were also studied using transient heat analysis in finite element modeling of the liquidation and solidification of the powder layer. The estimated melt pool length and width were comparable to values obtained by observations using a thermoviewer. The trend for the melt pool width versus the hatch pitch agreed with experimental values.

Selective Laser Melting of Pure Copper

NASA Astrophysics Data System (ADS)

Ikeshoji, Toshi-Taka; Nakamura, Kazuya; Yonehara, Makiko; Imai, Ken; Kyogoku, Hideki

2018-03-01

Appropriate building parameters for selective laser melting of 99.9% pure copper powder were investigated at relatively high laser power of 800 W for hatch pitch in the range from 0.025 mm to 0.12 mm. The highest relative density of the built material was 99.6%, obtained at hatch pitch of 0.10 mm. Building conditions were also studied using transient heat analysis in finite element modeling of the liquidation and solidification of the powder layer. The estimated melt pool length and width were comparable to values obtained by observations using a thermoviewer. The trend for the melt pool width versus the hatch pitch agreed with experimental values.

Aluminum powder metallurgy processing

NASA Astrophysics Data System (ADS)

Flumerfelt, Joel Fredrick

In recent years, the aluminum powder industry has expanded into non-aerospace applications. However, the alumina and aluminum hydroxide in the surface oxide film on aluminum powder require high cost powder processing routes. A driving force for this research is to broaden the knowledge base about aluminum powder metallurgy to provide ideas for fabricating low cost aluminum powder components. The objective of this dissertation is to explore the hypothesis that there is a strong linkage between gas atomization processing conditions, as-atomized aluminum powder characteristics, and the consolidation methodology required to make components from aluminum powder. The hypothesis was tested with pure aluminum powders produced by commercial air atomization commercial inert gas atomization and gas atomization reaction synthesis (GARS). The commercial atomization methods are bench marks of current aluminum powder technology. The GARS process is a laboratory scale inert gas atomization facility. A benefit of using pure aluminum powders is an unambiguous interpretation of the results without considering the effects of alloy elements. A comparison of the GARS aluminum powders with the commercial aluminum powders showed the former to exhibit superior powder characteristics. The powders were compared in terms of size and shape, bulk chemistry, surface oxide chemistry and structure, and oxide film thickness. Minimum explosive concentration measurements assessed the dependence of explosibility hazard on surface area, oxide film thickness, and gas atomization processing conditions. The GARS aluminum powders were exposed to different relative humidity levels, demonstrating the effect of atmospheric conditions on post-atomization oxidation of aluminum powder. An Al-Ti-Y GARS alloy exposed in ambient air at different temperatures revealed the effect of reactive alloy elements on post-atomization powder oxidation. The pure aluminum powders were consolidated by two different routes, a conventional consolidation process for fabricating aerospace components with aluminum powder and a proposed alternative. The consolidation procedures were compared by evaluating the consolidated microstructures and the corresponding mechanical properties. A low temperature solid state sintering experiment demonstrated that tap densified GARS aluminum powders can form sintering necks between contacting powder particles, unlike the total resistance to sintering of commercial air atomization aluminum powder.

The precursors effects on biomimetic hydroxyapatite ceramic powders.

PubMed

Yoruç, Afife Binnaz Hazar; Aydınoğlu, Aysu

2017-06-01

In this study, effects of the starting material on chemical, physical, and biological properties of biomimetic hydroxyapatite ceramic powders (BHA) were investigated. Characterization and chemical analysis of BHA powders were performed by using XRD, FT-IR, and ICP-AES. Microstructural features such as size and morphology of the resulting BHA powders were characterized by using BET, nano particle sizer, pycnometer, and SEM. Additionally, biological properties of the BHA ceramic powders were also investigated by using water-soluble tetrazolium salts test (WST-1). According to the chemical analysis of BHA ceramic powders, chemical structures of ceramics which are prepared under different conditions and by using different starting materials show differences. Ceramic powders which are produced at 80°C are mainly composed of hydroxyapatite, dental hydroxyapatite (contain Na and Mg elements in addition to Ca), and calcium phosphate sulfide. However, these structures are altered at high temperatures such as 900°C depending on the features of starting materials and form various calcium phosphate ceramics and/or their mixtures such as Na-Mg-hydroxyapatite, hydroxyapatite, Mg-Whitlockit, and chloroapatite. In vitro cytotoxicity studies showed that amorphous ceramics produced at 80°C and ceramics containing chloroapatite structure as main or secondary phases were found to be extremely cytotoxic. Furthermore, cell culture studies showed that highly crystalline pure hydroxyapatite structures were extremely cytotoxic due to their high crystallinity values. Consequently, the current study indicates that the selection of starting materials which can be used in the production of calcium phosphate ceramics is very important. It is possible to produce calcium phosphate ceramics which have sufficient biocompatibility at physiological pH values and by using appropriate starting materials. Copyright © 2017 Elsevier B.V. All rights reserved.

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

X-ray chemical analyzer for field applications

DOEpatents

Gamba, Otto O. M.

1977-01-01

A self-supporting portable field multichannel X-ray chemical analyzer system comprising a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an X-ray energy dispersive spectrometry technique.

The effect of milling time on the synthesis of Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy

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

Kursun, C., E-mail: celalkursun@ksu.edu.tr; Gogebakan, M., E-mail: gogebakan@ksu.edu.tr

In the present work, nanocrystalline Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy was produced by mechanical alloying from mixtures of pure crystalline Cu, Mg, Ti and Ni powders using a Fritsch planetary ball mill with a ball to powder ratio of 10:1. Morphological changes, microstructural evolution and thermal behaviour of the Cu-Mg-Ti-Ni powders at different stages of milling were characterised by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray detection (SEM/EDX) and differential thermal analysis (DTA). This alloy resulted in formation of single phase solid solution with FCC structure α-Cu (Mg, Ti, Ni) after 80 h of milling. In the initialmore » stage of milling different sized and shaped elemental powders became uniform during mechanical alloying. The homogeneity of the Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy increased with increasing milling time. The EDX result also confirmed the compositional homogeneity of the powder alloy. The crystallite size of alloy was calculated below 10 nm from XRD data.« less

Qualitative Analysis of Dairy and Powder Milk Using Laser-Induced Breakdown Spectroscopy (LIBS).

PubMed

Alfarraj, Bader A; Sanghapi, Herve K; Bhatt, Chet R; Yueh, Fang Y; Singh, Jagdish P

2018-01-01

Laser-induced breakdown spectroscopy (LIBS) technique was used to compare various types of commercial milk products. Laser-induced breakdown spectroscopy spectra were investigated for the determination of the elemental composition of soy and rice milk powder, dairy milk, and lactose-free dairy milk. The analysis was performed using radiative transitions. Atomic emissions from Ca, K, Na, and Mg lines observed in LIBS spectra of dairy milk were compared. In addition, proteins and fat level in milks can be determined using molecular emissions such as CN bands. Ca concentrations were calculated to be 2.165 ± 0.203 g/L in 1% of dairy milk fat samples and 2.809 ± 0.172 g/L in 2% of dairy milk fat samples using the standard addition method (SAM) with LIBS spectra. Univariate and multivariate statistical analysis methods showed that the contents of major mineral elements were higher in lactose-free dairy milk than those in dairy milk. The principal component analysis (PCA) method was used to discriminate four milk samples depending on their mineral elements concentration. In addition, proteins and fat level in dairy milks were determined using molecular emissions such as CN band. We applied partial least squares regression (PLSR) and simple linear regression (SLR) models to predict levels of milk fat in dairy milk samples. The PLSR model was successfully used to predict levels of milk fat in dairy milk sample with the relative accuracy (RA%) less than 6.62% using CN (0,0) band.

Resistance heater for use in a glass melter

DOEpatents

Routt, K.R.; Porter, M.A.

1984-01-01

A resistance heating element that includes: a resistance heating medium of a mixture of electrically conductive and insulative particles in powdered form mixed together in predetermined proportions to achieve a given resistivity; a hollow outer electrode surrounding the resistance heating medium; and an inner electrode coaxially disposed within said outer electrode. In its preferred embodiments, the electrically conductive powder is selected from the group consisting essentially of graphite, Inconel alloy, molybdenum, nichrome alloy and stainless steel, while the insulator powder is silicon dioxide or alumina. The resistance heating element, being resistant to damage from mechanical shock and corrosion at elevated temperatures, is used in a glass melter.

Method of manufacturing iron aluminide by thermomechanical processing of elemental powders

DOEpatents

Deevi, Seetharama C.; Lilly, Jr., A. Clifton; Sikka, Vinod K.; Hajaligol, Mohammed R.

2000-01-01

A powder metallurgical process of preparing iron aluminide useful as electrical resistance heating elements having improved room temperature ductility, electrical resistivity, cyclic fatigue resistance, high temperature oxidation resistance, low and high temperature strength, and/or resistance to high temperature sagging. The iron aluminide has an entirely ferritic microstructure which is free of austenite and can include, in weight %, 20 to 32% Al, and optional additions such as .ltoreq.1% Cr, .gtoreq.05% Zr or ZrO.sub.2 stringers extending perpendicular to an exposed surface of the heating element, .ltoreq.2% Ti, .ltoreq.2% Mo, .ltoreq.1% Zr, .ltoreq.1% C, .ltoreq.0.1% B, .ltoreq.30% oxide dispersoid and/or electrically insulating or electrically conductive covalent ceramic particles, .ltoreq.1 % rare earth metal, .ltoreq.1% oxygen, and/or .ltoreq.3% Cu. The process includes forming a mixture of aluminum powder and iron powder, shaping the mixture into an article such as by cold rolling the mixture into a sheet, and sintering the article at a temperature sufficient to react the iron and aluminum powders and form iron aluminide. The sintering can be followed by hot or cold rolling to reduce porosity created during the sintering step and optional annealing steps in a vacuum or inert atmosphere.

Development of a mushroom powder Certified Reference Material for calcium, arsenic, cadmium and lead measurements.

PubMed

Chew, Gina; Sim, Lay Peng; Ng, Sin Yee; Ding, Yi; Shin, Richard Y C; Lee, Tong Kooi

2016-01-01

Isotope dilution mass spectrometry and standard addition techniques were developed for the analysis of four elements (Ca, As, Cd and Pb) in a mushroom powder material. Results from the validated methods were compared to those of other national metrology institutes in the CCQM-K89 intercomparisons and the results were in excellent agreement with the reference values. The same methods were then used for the assignment of reference values to a mushroom powder Certified Reference Material (CRM). The certified values obtained for Ca, As, Cd and Pb were 1.444 ± 0.099 mg/g, 5.61 ± 0.59 mg/kg, 1.191 ± 0.079 mg/kg and 5.23 ± 0.94 mg/kg, respectively. The expanded measurement uncertainties were obtained by combining the uncertainty contributions from characterization (uchar) and between-bottle homogeneity (ubb). Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

Effect of Heat Treatment Temperature on Chemical Compositions of Extracted Hydroxyapatite from Bovine Bone Ash

NASA Astrophysics Data System (ADS)

Younesi, M.; Javadpour, S.; Bahrololoom, M. E.

2011-11-01

This article presents the effect of heat treating temperature on chemical composition of hydroxyapatite (HA) that was produced by burning bovine bone, and then heat treating the obtained bone ash at different temperatures in range of 600-1100 °C in air. Bone ash and the resulting white powder from heat treating were characterized by Fourier transformed infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD). The FT-IR spectra confirmed that heat treating of bone ash at temperature of 800 °C removed the total of organic substances. x-ray diffraction analysis showed that the white powder was HA and HA was the only crystalline phase indicated in heat treating product. x-ray fluorescence analyses revealed that calcium and phosphorous were the main elements and magnesium and sodium were minor impurities of produced powder at 800 °C. The results of the energy dispersive x-ray analysis showed that Ca/P ratio in produced HA varies in range of 1.46-2.01. The resulting material was found to be thermally stable up to 1100 °C.

One-dimensional coordination polymers of whole row rare earth tris-pivalates

NASA Astrophysics Data System (ADS)

Tsymbarenko, Dmitry; Martynova, Irina; Grebenyuk, Dimitry; Shegolev, Vsevolod; Kuzmina, Natalia

2018-02-01

Fourteen 1D coordination polymers of rare earth pivalates [Ln(Piv)3]∞ (Ln = Y, La, Pr, Nd, Sm-Lu) were synthesized and characterized by powder X-ray diffraction, IR spectroscopy, TGA, and conventional elemental analysis. Crystal structures of [La(Piv)3]∞, [Yb(Piv)3]∞, [Lu(Piv)3]∞ were determined by means of single crystal X-ray analysis at 120 K, those of [Y(Piv)3]∞ and [Ho(Piv)3]∞ - from powder XRD data at 293 K. Transformation of [Ln(Piv)3]∞ structure and Piv- anions coordination mode along the whole row has been derived from powder XRD and IR spectroscopy results, and shown to crucially affect the relative location of 1D chains in the crystal structure, as well as the Ln···Ln distance within the single chain. Negative thermal expansion along 1D [Ln(Piv)3]∞ chain was revealed for Ln = Tm, Yb, Lu. Enforcement of 1D polymeric structure with the decrease of Ln ionic radius has been established from solid-state DFT calculations.

21 CFR 184.1375 - Iron, elemental.

Code of Federal Regulations, 2010 CFR

2010-04-01

... microscope, it appears as an amorphous powder free from particles having a crystalline structure. It is... pentacarbonyl. It occurs as a dark gray powder. When viewed under a microscope, it appears as spheres built up...

Phase transformation and magnetic properties of MnAl powders prepared by elemental-doping and salt-assisted ball milling

NASA Astrophysics Data System (ADS)

Qian, Hui-Dong; Si, Ping-Zhan; Choi, Chul-Jin; Park, Jihoon; Cho, Kyung Mox

2018-05-01

The effects of elemental doping of Si and Fe on the ɛ→τ phase transformation and the magnetic properties of MnAl were studied. The magnetic powders of Si- and Fe-doped MnAl were prepared by using induction melting followed by water-quenching, annealing, and salt-assisted ball-milling. The Fe-doped MnAl powders are mainly composed of the L10-structured τ-phase, while the Si-doped MnAl are composed of τ-phase and a small fraction of γ2- and β-phases. A unique thin leaves-like morphology with thickness of several tens of nanometers and diameter size up to 500 nm were observed in the Si-doped MnAl powders. The Fe-doped MnAl powders show irregular shape with much larger dimensions in the range from several to 10 μm. The morphology difference of the samples was ascribed to the variation of the mechanical properties affected by different doping elements. The phase transformation temperatures of the ɛ-phase of the samples were measured. The doping of Fe decreases the onset temperature of the massive phase transformation in MnAl, while the Si-doping increases the massive phase transformation temperature. Both Fe and Si increase the Curie temperature of MnAl. A substantially enhanced coercivity up to 0.45 T and 0.42 T were observed in the ball-milled MnAl powders doped with Si and Fe, respectively.

Synthesis of Amorphous Powders of Ni-Si and Co-Si Alloys by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Omuro, Keisuke; Miura, Harumatsu

1991-05-01

Amorphous powders of the Ni-Si and Co-Si alloys are synthesized by mechanical alloying (MA) from crystalline elemental powders using a high energy ball mill. The alloying and amorphization process is examined by X-ray diffraction, differential scanning calorimetry (DSC), and scanning electron microscopy. For the Ni-Si alloy, it is confirmed that the crystallization temperature of the MA powder, measured by DSC, is in good agreement with that of the powder sample prepared by mechanical grinding from the cast alloy ingot products of the same composition.

Elemental Composition of the Powder Particles Produced by Electric Discharge Dispersion of the Wastes of a VK8 Hard Alloy

NASA Astrophysics Data System (ADS)

Latypov, R. A.; Ageev, E. V.; Latypova, G. R.; Altukhov, A. Yu.; Ageeva, E. V.

2017-12-01

The powder fabricated by electric discharge dispersion of the wastes of a VK8 hard alloy is studied by electron-probe microanalysis. This powder formed by electric discharge dispersion in kerosene mainly contains tungsten and carbon and has low contents of oxygen, cobalt, and iron.

Finite Element Analysis of Interaction of Laser Beam with Material in Laser Metal Powder Bed Fusion Process.

PubMed

Fu, Guang; Zhang, David Z; He, Allen N; Mao, Zhongfa; Zhang, Kaifei

2018-05-10

A deep understanding of the laser-material interaction mechanism, characterized by laser absorption, is very important in simulating the laser metal powder bed fusion (PBF) process. This is because the laser absorption of material affects the temperature distribution, which influences the thermal stress development and the final quality of parts. In this paper, a three-dimensional finite element analysis model of heat transfer taking into account the effect of material state and phase changes on laser absorption is presented to gain insight into the absorption mechanism, and the evolution of instantaneous absorptance in the laser metal PBF process. The results showed that the instantaneous absorptance was significantly affected by the time of laser radiation, as well as process parameters, such as hatch space, scanning velocity, and laser power, which were consistent with the experiment-based findings. The applicability of this model to temperature simulation was demonstrated by a comparative study, wherein the peak temperature in fusion process was simulated in two scenarios, with and without considering the effect of material state and phase changes on laser absorption, and the simulated results in the two scenarios were then compared with experimental data respectively.

Temperature evolution during compaction of pharmaceutical powders.

PubMed

Zavaliangos, Antonios; Galen, Steve; Cunningham, John; Winstead, Denita

2008-08-01

A numerical approach to the prediction of temperature evolution in tablet compaction is presented here. It is based on a coupled thermomechanical finite element analysis and a calibrated Drucker-Prager Cap model. This approach is capable of predicting transient temperatures during compaction, which cannot be assessed by experimental techniques due to inherent test limitations. Model predictions are validated with infrared (IR) temperature measurements of the top tablet surface after ejection and match well with experiments. The dependence of temperature fields on speed and degree of compaction are naturally captured. The estimated transient temperatures are maximum at the end of compaction at the center of the tablet and close to the die wall next to the powder/die interface.

On the Influence of Material Parameters in a Complex Material Model for Powder Compaction

NASA Astrophysics Data System (ADS)

Staf, Hjalmar; Lindskog, Per; Andersson, Daniel C.; Larsson, Per-Lennart

2016-10-01

Parameters in a complex material model for powder compaction, based on a continuum mechanics approach, are evaluated using real insert geometries. The parameter sensitivity with respect to density and stress after compaction, pertinent to a wide range of geometries, is studied in order to investigate completeness and limitations of the material model. Finite element simulations with varied material parameters are used to build surrogate models for the sensitivity study. The conclusion from this analysis is that a simplification of the material model is relevant, especially for simple insert geometries. Parameters linked to anisotropy and the plastic strain evolution angle have a small impact on the final result.

FUEL ELEMENTS FOR NUCLEAR REACTORS AND PROCESS OF MAKING

DOEpatents

Roake, W.E.

1958-08-19

A process is described for producing uranium metal granules for use in reactor fuel elements. The granules are made by suspending powdered uramiunn metal or uranium hydride in a viscous, non-reactive liquid, such as paraffin oil, aad pouring the resulting suspension in droplet, on to a bed of powdered absorbent. In this manner the liquid vehicle is taken up by the sorbent and spherical pellets of uranium metal are obtained. The

Cytotoxicity of titanium and titanium alloying elements.

PubMed

Li, Y; Wong, C; Xiong, J; Hodgson, P; Wen, C

2010-05-01

It is commonly accepted that titanium and the titanium alloying elements of tantalum, niobium, zirconium, molybdenum, tin, and silicon are biocompatible. However, our research in the development of new titanium alloys for biomedical applications indicated that some titanium alloys containing molybdenum, niobium, and silicon produced by powder metallurgy show a certain degree of cytotoxicity. We hypothesized that the cytotoxicity is linked to the ion release from the metals. To prove this hypothesis, we assessed the cytotoxicity of titanium and titanium alloying elements in both forms of powder and bulk, using osteoblast-like SaOS(2) cells. Results indicated that the metal powders of titanium, niobium, molybdenum, and silicon are cytotoxic, and the bulk metals of silicon and molybdenum also showed cytotoxicity. Meanwhile, we established that the safe ion concentrations (below which the ion concentration is non-toxic) are 8.5, 15.5, 172.0, and 37,000.0 microg/L for molybdenum, titanium, niobium, and silicon, respectively.

Reverse micelle synthesis of nanoscale metal containing catalysts

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

Darab, J.G.; Fulton, J.L.; Linehan, J.C.

1993-03-01

The need for morphological control during the synthesis of catalyst precursor powders is generally accepted to be important. In the liquefaction of coal, for example, iron-bearing catalyst precursor particles containing individual crystallites with diameters in the 1-100 nanometer range are believed to achieve good dispersion through out the coal-solvent slurry during liquefaction 2 runs and to undergo chemical transformations to catalytically active iron sulfide phases. The production of the nanoscale powders described here employs the confining spherical microdomains comprising the aqueous phase of a modified reverse micelle (MRM) microemulsion system as nanoscale reaction vessels in which polymerization, electrochemical reduction andmore » precipitation of solvated salts can occur. The goal is to take advantage of the confining nature of micelles to kinetically hinder transformation processes which readily occur in bulk aqueous solution in order to control the morphology and phase of the resulting powder. We have prepared a variety of metal, alloy, and metal- and mixed metal-oxide nanoscale powders from appropriate MRM systems. Examples of nanoscale powders produced include Co, Mo-Co, Ni{sub 3}Fe, Ni, and various oxides and oxyhydroxides of iron. Here, we discuss the preparation and characterization of nickel metal (with a nickel oxide surface layer) and iron oxyhydroxide MRM nanoscale powders. We have used extended x-ray absorption fine structure (EXAFS) spectroscopy to study the chemical polymerization process in situ, x-ray diffraction (XRD), scanning and transmission electron microcroscopies (SEM and TEM), elemental analysis and structural modelling to characterize the nanoscale powders produced. The catalytic activity of these powders is currently being studied.« less

Reutilization of granite powder as an amendment and fertilizer for acid soils.

PubMed

Barral Silva, M T; Silva Hermo, B; García-Rodeja, E; Vázquez Freire, N

2005-11-01

The properties of granite powders--a granite manufacturing waste product-were analyzed to assess their potential use as amendments and fertilizers on acid soils. Two types of powders were characterized: one produced during cutting of granite with a diamond-edged disc saw, comprising only rock powder, the other produced during cutting with a multi-blade bandsaw, containing calcium hydroxide and metal filings added during the cutting procedure. The acid neutralizing capacity of the granite powders was assessed in short- (2-3 h) and medium-term (1-30 d) experiments. The powders showed a buffering capacity at around pH 8, which corresponded to the rapid dissolution of basic cations, and another buffering effect at pH<4.5, attributable to the dissolution of Fe and Al. The acid neutralizing capacity (ANC) determined in the short-term experiments, to a final pH of 4.5, varied between 5 and 61 cmol H+kg(-1) powder. The ANC to pH 4.5 obtained in the medium-term experiments was much higher than that obtained in the short-term experiments, reaching a maximum ANC value of 200 cmol H+kg(-1) powder. There was no great difference in the neutralizing capacity determined at between 1 and 30 d. The most abundant elements in acid solutions obtained at the end of medium-term experiments were Mg and Ca for disc saw powders, whereas Ca and Fe (at pH<5) were the most soluble elements in the bandsaw powders. The rapid release of these cations suggests the possible effective use of the granite powders as a source of nutrients on being added to acid soils.

Effects of Alloying Elements on the Formation of Core-Shell-Structured Reinforcing Particles during Heating of Al–Ti Powder Compacts

PubMed Central

Chen, Tijun; Gao, Min; Tong, Yunqi

2018-01-01

To prepare core-shell-structured Ti@compound particle (Ti@compoundp) reinforced Al matrix composite via powder thixoforming, the effects of alloying elements, such as Si, Cu, Mg, and Zn, on the reaction between Ti powders and Al melt, and the microstructure of the resulting reinforcements were investigated during heating of powder compacts at 993 K (720 °C). Simultaneously, the situations of the reinforcing particles in the corresponding semisolid compacts were also studied. Both thermodynamic analysis and experiment results all indicate that Si participated in the reaction and promoted the formation of Al–Ti–Si ternary compounds, while Cu, Mg, and Zn did not take part in the reaction and facilitated Al3Ti phase to form to different degrees. The first-formed Al–Ti–Si ternary compound was τ1 phase, and then it gradually transformed into (Al,Si)3Ti phase. The proportion and existing time of τ1 phase all increased as the Si content increased. In contrast, Mg had the largest, Cu had the least, and Si and Zn had an equivalent middle effect on accelerating the reaction. The thicker the reaction shell was, the larger the stress generated in the shell was, and thus the looser the shell microstructure was. The stress generated in (Al,Si)3Ti phase was larger than that in τ1 phase, but smaller than that in Al3Ti phase. So, the shells in the Al–Ti–Si system were more compact than those in the other systems, and Si element was beneficial to obtain thick and compact compound shells. Most of the above results were consistent to those in the semisolid state ones except the product phase constituents in the Al–Ti–Mg system and the reaction rate in the Al–Ti–Zn system. More importantly, the desirable core-shell structured Ti@compoundp was only achieved in the semisolid Al–Ti–Si system. PMID:29342946

Effects of Alloying Elements on the Formation of Core-Shell-Structured Reinforcing Particles during Heating of Al-Ti Powder Compacts.

PubMed

Chen, Tijun; Gao, Min; Tong, Yunqi

2018-01-15

To prepare core-shell-structured Ti@compound particle (Ti@compound p ) reinforced Al matrix composite via powder thixoforming, the effects of alloying elements, such as Si, Cu, Mg, and Zn, on the reaction between Ti powders and Al melt, and the microstructure of the resulting reinforcements were investigated during heating of powder compacts at 993 K (720 °C). Simultaneously, the situations of the reinforcing particles in the corresponding semisolid compacts were also studied. Both thermodynamic analysis and experiment results all indicate that Si participated in the reaction and promoted the formation of Al-Ti-Si ternary compounds, while Cu, Mg, and Zn did not take part in the reaction and facilitated Al₃Ti phase to form to different degrees. The first-formed Al-Ti-Si ternary compound was τ1 phase, and then it gradually transformed into (Al,Si)₃Ti phase. The proportion and existing time of τ1 phase all increased as the Si content increased. In contrast, Mg had the largest, Cu had the least, and Si and Zn had an equivalent middle effect on accelerating the reaction. The thicker the reaction shell was, the larger the stress generated in the shell was, and thus the looser the shell microstructure was. The stress generated in (Al,Si)₃Ti phase was larger than that in τ1 phase, but smaller than that in Al₃Ti phase. So, the shells in the Al-Ti-Si system were more compact than those in the other systems, and Si element was beneficial to obtain thick and compact compound shells. Most of the above results were consistent to those in the semisolid state ones except the product phase constituents in the Al-Ti-Mg system and the reaction rate in the Al-Ti-Zn system. More importantly, the desirable core-shell structured Ti@compound p was only achieved in the semisolid Al-Ti-Si system.

Reverse micelle synthesis of nanoscale metal containing catalysts. [Nickel metal (with a nickel oxide surface layer) and iron oxyhydroxide nanoscale powders

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

Darab, J.G.; Fulton, J.L.; Linehan, J.C.

1993-03-01

The need for morphological control during the synthesis of catalyst precursor powders is generally accepted to be important. In the liquefaction of coal, for example, iron-bearing catalyst precursor particles containing individual crystallites with diameters in the 1-100 nanometer range are believed to achieve good dispersion through out the coal-solvent slurry during liquefaction 2 runs and to undergo chemical transformations to catalytically active iron sulfide phases. The production of the nanoscale powders described here employs the confining spherical microdomains comprising the aqueous phase of a modified reverse micelle (MRM) microemulsion system as nanoscale reaction vessels in which polymerization, electrochemical reduction andmore » precipitation of solvated salts can occur. The goal is to take advantage of the confining nature of micelles to kinetically hinder transformation processes which readily occur in bulk aqueous solution in order to control the morphology and phase of the resulting powder. We have prepared a variety of metal, alloy, and metal- and mixed metal-oxide nanoscale powders from appropriate MRM systems. Examples of nanoscale powders produced include Co, Mo-Co, Ni[sub 3]Fe, Ni, and various oxides and oxyhydroxides of iron. Here, we discuss the preparation and characterization of nickel metal (with a nickel oxide surface layer) and iron oxyhydroxide MRM nanoscale powders. We have used extended x-ray absorption fine structure (EXAFS) spectroscopy to study the chemical polymerization process in situ, x-ray diffraction (XRD), scanning and transmission electron microcroscopies (SEM and TEM), elemental analysis and structural modelling to characterize the nanoscale powders produced. The catalytic activity of these powders is currently being studied.« less

Sol-gel synthesis and characterisation of nano-scale hydroxyapatite

NASA Astrophysics Data System (ADS)

Bilton, M.; Brown, A. P.; Milne, S. J.

2010-07-01

Hydroxyapatite (HAp) forms the main mineral component of bone and teeth. This naturally occurring HAp is in the form of nano-metre sized crystallites of Ca10(PO4)6(OH)2 that contain a number of cation and anion impurities, for example CO32-, F-, Na+, Mg2+ and Sr2+. Synthetic nano-sized HAp particles exhibit favourable biocompatibility and bioactivity and in order to better match the composition to natural HAp there is great interest in producing a range of chemically modified powders. In this study, two HAp powders have been synthesised via a water-based low-temperature sol-gel method and a third, commercial powder from Sigma-Aldrich have been analysed. Subsequent powder calcination has been carried out within the temperature range of 500-700 °C and the products characterised by bulk chemical analysis, X-ray diffraction and electron microscopy. Energy dispersive X-ray spectroscopy (EDX) in the TEM has been used to assess the composition of individual HAp particles. In order to do this accurately it is first necessary to account for the sensitivity of the HAp structure and composition to irradiation by the high energy electron beam of the TEM. This was done by monitoring the estimated Ca/P ratio derived from TEM-EDX of stoichiometric HAp under increasing levels of electron fluence. A fluence threshold (at a given beam energy) was established below which the measured Ca/P ratio can be considered to be stable. Subsequent elemental analysis at or below this threshold has enabled the variation in composition between particles both within and between synthesis batches to be accurately assessed. Compositional variability between particles is also evident, even in the commercial powder, but is far greater in the powders prepared by the sol-gel method.

Direct Metal Deposition of Refractory High Entropy Alloy MoNbTaW

NASA Astrophysics Data System (ADS)

Dobbelstein, Henrik; Thiele, Magnus; Gurevich, Evgeny L.; George, Easo P.; Ostendorf, Andreas

Alloying of refractory high entropy alloys (HEAs) such as MoNbTaW is usually done by vacuum arc melting (VAM) or powder metallurgy (PM) due to the high melting points of the elements. Machining to produce the final shape of parts is often needed after the PM process. Casting processes, which are often used for aerospace components (turbine blades, vanes), are not possible. Direct metal deposition (DMD) is an additive manufacturing technique used for the refurbishment of superalloy components, but generating these components from the bottom up is also of current research interest. MoNbTaW possesses high yield strength at high temperatures and could be an alternative to state-of-the-art materials. In this study, DMD of an equimolar mixture of elemental powders was performed with a pulsed Nd:YAG laser. Single wall structures were built, deposition strategies developed and the microstructure of MoNbTaW was analyzed by back scattered electrons (BSE) and energy dispersive X-ray (EDX) spectroscopy in a scanning electron microscope. DMD enables the generation of composition gradients by using dynamic powder mixing instead of pre-alloyed powders. However, the simultaneous handling of several elemental or pre-alloyed powders brings new challenges to the deposition process. The influence of thermal properties, melting point and vapor pressure on the deposition process and chemical composition will be discussed.

Immobilization of Chlorosulfonyl-Calix[4]arene onto the surface of silica gel through the directly estrification

NASA Astrophysics Data System (ADS)

Taghvaei-Ganjali, Saeed; Zadmard, Reza; Saber-Tehrani, Mandana

2012-06-01

For the first time Chlorosulfonyl-Calix[4]arene has been chemically bonded to silica gel through the directly estrification without silane coupling agent to prepare Chlorosulfonyl-Calix[4]arene-bonded silica gel. Sample characterization was performed by various techniques such as elemental analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), powder X-ray diffraction (XRD), N2 adsorption-desorption, thermal gravimetric analysis (TGA), 29Si CP/MAS spectroscopy and acid-base titration. All data approve the successful incorporation of organic group via covalent bond. From the comparison between sulfur content determined by elemental analysis and the number of H+ determined by acid-base titration, it was shown that two ester units took place onto the new synthesized sample and two acidic sites exist on the surface.

Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.

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

Baljinnyam, N.; Frontasyeva, M. V.; Ostrovnaya, T. M.

Asian medicinal herbs Chrysanthemum (Spiraea aquilegifolia Pall.) and Red Sandalwood (Pterocarpus Santalinus) are widely used in folk and Ayurvedic medicine for healing and preventing some diseases. The modern medical science has proved that the Chrysanthemum (Spiraea aquilegifolia Pall.) possesses the following functions: reducing blood press, dispelling cancer cell, coronary artery's expanding and bacteriostating and Red Sandalwood (Pterocarpus Santalinus) is recommended against headache, toothache, skin diseases, vomiting and sometimes it is taken for treatment of diabetes. Species of Chrysanthemums were collected in the north-eastern and central Mongolia, and the Red Sandalwood powder was imported from India. Samples of Chrysanthemums (branches, flowersmore » and leaves)(0.5 g) and red sandalwood powder (0.5 g) were subjected to the multi-element instrumental neutron activation analysis using epithermal neutrons (ENAA) at the IBR-2 reactor, Frank Laboratory of Neutron Physics (FLNP) JINR, Dubna. A total of 41 elements (Na, Mg, Al, Cl, K, Ca, Sc, V, Cr, Mn, Fe, Co, Ni, Zn, As, Se, Br, Rb, Sr, Zr, Mo, Cd, Cs, Ba, La, Hf, Ta, W, Sb, Au, Hg, Ce, Nd, Sm, Eu, Tb, Dy, Yb, Th, U, Lu) were determined. For the first time such a large group of elements was determined in the herbal plants used in Mongolia. The quality control of the analytical results was provided by using certified reference material Bowen Cabbage. The results obtained are compared to the ''Reference plant? data (B. Markert, 1992) and interpreted in terms of excess of such elements as Se, Cr, Ca, Fe, Ni, Mo, and rare earth elements.« less

Effect of Zr, Nb and Ti addition on injection molded 316L stainless steel for bio-applications: Mechanical, electrochemical and biocompatibility properties.

PubMed

Gulsoy, H Ozkan; Pazarlioglu, Serdar; Gulsoy, Nagihan; Gundede, Busra; Mutlu, Ozal

2015-11-01

The research investigated the effect of Zr, Nb and Ti additions on mechanical, electrochemical properties and biocompatibility of injection molded 316L stainless steel. Addition of elemental powder is promoted to get high performance of sintered 316L stainless steels. The amount of additive powder plays a role in determining the sintered microstructure and all properties. In this study, 316L stainless steel powders used with the elemental Zr, Nb and Ti powders. A feedstock containing 62.5 wt% powders loading was molded at different injection molded temperature. The binders were completely removed from molded components by solvent and thermal debinding at different temperatures. The debinded samples were sintered at 1350°C for 60 min. Mechanical, electrochemical property and biocompatibility of the sintered samples were performed mechanical, electrochemical, SBF immersion tests and cell culture experiments. Results of study showed that sintered 316L and 316L with additives samples exhibited high corrosion properties and biocompatibility in a physiological environment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Phase and crystallite size analysis of (Ti1-xMox)C-(Ni,Cr) cermet obtained by mechanical alloying

NASA Astrophysics Data System (ADS)

Suryana, Anis, Muhammad; Manaf, Azwar

2018-04-01

In this paper, we report the phase and crystallite size analysis of (Ti1-xMox)C-(Ni,Cr) with x = 0-0.5 cermet obtained by mechanical alloying of Ti, Mo, Ni, Cr and C elemental powders using a high-energy shaker ball mill under wet condition for 10 hours. The process used toluene as process control agent and the ball to mass ratio was 10:1. The mechanically milled powder was then consolidated and subsequently heated at a temperature 850°C for 2 hours under an argon flow to prevent oxidation. The product was characterized by X-ray diffraction (XRD) and scanning electron microscope equipped with energy dispersive analyzer. Results shown that, by the selection of appropriate condition during the mechanical alloying process, a metastable Ti-Ni-Cr-C powders could be obtained. The powder then allowed the in situ synthesis of TiC-(Ni,Cr) cermet which took place during exposure time at a high temperature that applied in reactive sintering step. Addition to molybdenum has caused shifting the TiC XRD peaks to a slightly higher angle which indicated that molybdenum dissolved in TiC phase. The crystallite size distribution of TiC is discussed in the report, which showing that the mean size decreased with the addition of molybdenum.

Adsorption of polyethylene glycol (PEG) onto cellulose nano-crystals to improve its dispersity.

PubMed

Cheng, Dong; Wen, Yangbing; Wang, Lijuan; An, Xingye; Zhu, Xuhai; Ni, Yonghao

2015-06-05

In this work, the adsorption of polyethylene glycol (PEG) onto cellulose nano-crystals (CNC) was investigated for preparing re-dispersible dried CNC. Results showed that the re-dispersity of CNC in water can be significantly enhanced using a PEG1000 dosage of 5wt% (based on the dry weight of CNC). The elemental analysis confirmed the adsorption of PEG onto the CNC surface. Transmission electron microscopy (TEM) was used to characterize the dry powder and indicated that the irreversible agglomeration of CNC after drying was essentially eliminated based on the PEG adsorption concept. Thermo-gravimetric analysis (TGA) and X-ray diffraction (XRD) suggested that CNC crystallinity and thermal stability were not affected by the adsorption of PEG. Thus, the adsorption of PEG has great potential for producing re-dispersible powder CNC. Copyright © 2015 Elsevier Ltd. All rights reserved.

Experimental and Numerical Analysis of Injection Molding of Ti-6Al-4V Powders for High-Performance Titanium Parts

NASA Astrophysics Data System (ADS)

Lin, Dongguo; Kang, Tae Gon; Han, Jun Sae; Park, Seong Jin; Chung, Seong Taek; Kwon, Young-Sam

2018-02-01

Both experimental and numerical analysis of powder injection molding (PIM) of Ti-6Al-4V alloy were performed to prepare a defect-free high-performance Ti-6Al-4V part with low carbon/oxygen contents. The prepared feedstock was characterized with specific experiments to identify its viscosity, pressure-volume-temperature and thermal properties to simulate its injection molding process. A finite-element-based numerical scheme was employed to simulate the thermomechanical process during the injection molding. In addition, the injection molding, debinding, sintering and hot isostatic pressing processes were performed in sequence to prepare the PIMed parts. With optimized processing conditions, the PIMed Ti-6Al-4V part exhibits excellent physical and mechanical properties, showing a final density of 99.8%, tensile strength of 973 MPa and elongation of 16%.

Finite element analysis of acoustic streaming in a Kundt tube with bended wall

NASA Astrophysics Data System (ADS)

Wada, Yuji; Yuge, Kohei

2018-07-01

Acoustic streaming near artificially prescribed ridges is simulated and discussed to understand the mechanism of Kundt tube powder-ridge generation. A viscoacoustic harmonic finite element analysis (FEA) and a static-fluid FEA are coupled using an acoustic streaming driving force to derive acoustic streaming. The half-wavelength mode is excited in an acoustic tube where the calculation mesh is distorted to form a sinusoidal bottom stick wall. Consequently, intense Schlichting streaming is obtained when the height and interval of the ridge agree with those in the literature. The mechanism underlying the regular ridge interval is related to the conversion of mainstream particle velocity into ridge-localized velocity, which produces an inlet or outlet vertical streaming in ridge valleys.

Synthesis, crystal growth and characterization of a phase matchable nonlinear optical single crystal: p-chloro dibenzylideneacetone

NASA Astrophysics Data System (ADS)

Ravindra, H. J.; John Kiran, A.; Nooji, Satheesha Rai; Dharmaprakash, S. M.; Chandrasekharan, K.; Kalluraya, Balakrishna; Rotermund, Fabian

2008-05-01

Good quality single crystals of p-chloro dibenzylideneacetone (CDBA) of size 13 mm×8 mm×2 mm were grown by slow evaporation solution growth technique. The grown crystals were confirmed by elemental analysis, Fourier transform infrared (FTIR) analysis and single crystal X-ray diffraction techniques. From the thermo gravimetric/differential thermal (TG/DT) analysis, the CDBA was found to be thermally stable up to 250 °C. The mechanical stability of the crystal is comparable with that of the other reported chalcones. The lower optical cut-off wavelength for this crystal was observed at 440 nm. The laser damage threshold of the crystal was 0.6 GW/cm 2 at 532 nm. The second harmonic generation conversion efficiency of the powder sample of CDBA was found to be 4.5 times greater than that of urea. We also demonstrate the existence of the phase matching property in this crystal using Kurtz powder technique.

On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

PubMed

Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

2014-12-03

We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

[The study of ultra-fine diamond powder used in magnetic head polishing slurry].

PubMed

Jin, Hong-Yun; Hou, Shu-En; Pan, Yong; Xiao, Hong-Yan

2008-05-01

In the present paper, atomic absorption spectrometry(AAS), inductively-coupled plasma mass spectrometry (ICP-MS), transmission electron microscopy (TEM), X-ray diffraction (XRD) and laser Raman spectroscopy (RM) were employed to study the commercial ultra-fine diamond powders prepared by the static pressure-catalyst method and used in magnetic head polishing slurry. The results of AAS and ICP-MS indicated that there were silicon oxide, Fe, Ni, Al and some other metal elements in the ultra-fine powders. XRD patterns showed the peaks of SiO2 at 2theta = 35.6 degrees, 39.4 degrees and 59.7 degrees and diamond sharp peaks in agreement with the results above. Diamond sharp peaks implied perfect crystal and high-hardness beneficial to high-efficiency in polishing. The broader Raman band of graphite at 1 592 cm(-1) observed by Raman analysis proved graphite existing in the diamond powders. In the TEM images, the size of ultra-fine powders was estimated between 0.1 and 0.5 microm distributed in a wide scope, however, sharp edges of the powder particles was useful to polish. The ultra-fine diamond powders have many advantages, for example, high-hardness, well abrasion performance, high-polishing efficiency and being useful in magnetic head polishing slurry. But, the impurities influence the polishing efficiency, shortening its service life and the wide distribution reduces the polishing precision. Consequently, before use the powders must be purified and classified. The purity demands is 99.9% and trace silicon oxide under 0.01% should be reached. The classification demands that the particle distribution should be in a narrower scope, with the mean size of 100 nm and the percentage of particles lager than 200 nm not over 2%.

Fatigue Performance of Powder Metallurgy (PM) Ti-6Al-4V Alloy: A Critical Analysis of Current Fatigue Data and Metallurgical Approaches for Improving Fatigue Strength

NASA Astrophysics Data System (ADS)

Cao, Fei; Ravi Chandran, K. S.

2016-03-01

A comprehensive assessment of fatigue performance of powder metallurgy (PM) Ti-6Al-4V alloy, manufactured using various powder-based processing approaches to-date, is performed in this work. The focus is on PM processes that use either blended element (BE) or pre-alloyed (PA) powder as feedstock. Porosity and the microstructure condition have been found to be the two most dominant material variables that control the fatigue strength. The evaluation reveals that the fatigue performance of PM Ti-6Al-4V, in the as-sintered state, is far lower than that in the wrought condition. This is largely caused by residual porosity, even if it is present in small amounts, or, by the coarse lamellar colony microstructure. The fatigue strength is significantly improved by the closure of pores, and it approaches the levels of wrought Ti-6Al-4V alloys, after hot-isostatic-pressing (HIPing). Further thermo-mechanical and heat treatments lead to additional increases in fatigue strength-in one case, a high fatigue strength level, exceeding that of the mill-annealed condition, was achieved. The work identifies the powder, process and microstructure improvements that are necessary for achieving high fatigue strength in powder metallurgical Ti-6Al-4V alloys in order for them to effectively compete with wrought forms. The present findings, gathered from the traditional titanium powder metallurgy, are also directly applicable to additively manufactured titanium, because of the similarities in pores, defects, and microstructures between the two manufacturing processes.

Effect of powder reactivity on fabrication and properties of NiAl/Al2O3 composite coated on cast iron using spark plasma sintering

NASA Astrophysics Data System (ADS)

Beyhaghi, Maryam; Kiani-Rashid, Ali-Reza; Kashefi, Mehrdad; Khaki, Jalil Vahdati; Jonsson, Stefan

2015-07-01

Powder mixtures of Ni, NiO and Al are ball milled for 1 and 10 h. X-ray diffractometry and differential thermal analysis show that while ball milling for 1 h produced mechanically activated powder; 10 h ball milling produced NiAl and Al2O3 phases. Dense NiAl/Al2O3 composite coatings are formed on gray cast iron substrate by spark plasma sintering (SPS) technique. The effect of powder reactivity on microstructure, hardness and scratch hardness of NiAl/Al2O3 coatings after SPS is discussed. Results show that in the coating sample made of mechanically activated powder in situ synthesis of NiAl/Al2O3 composite coating is fulfilled and a thicker well-formed diffusion bond layer at the interface between coating and substrate is observed. The diffusion of elements across the bond layers and phase evolution in the bond layers were investigated. No pores or cracks were observed at the interface between coating layer and substrate in any of samples. Higher Vickers hardness and scratch hardness values in coating made of 10 h ball milled powder than in coating fabricated from 1 h ball milled powder are attributed to better dispersion of Al2O3 reinforcement particles in NiAl matrix and nano-crystalline structure of NiAl matrix. Scratched surface of coatings did not reveal any cracking or spallation at coating-substrate interface indicating their good adherence at test conditions.

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

Kristo, Michael Joseph; Keegan, Elizabeth; Colella, Michael

Nuclear forensic analysis was conducted on two uranium samples confiscated during a police investigation in Victoria, Australia. The first sample, designated NSR-F-270409-1, was a depleted uranium powder of moderate purity (~1000 μg/g total elemental impurities). The chemical form of the uranium was a compound similar to K 2(UO 2) 3O 4·4H 2O. While aliquoting NSR-F-270409-1 for analysis, the body and head of a Tineid moth was discovered in the sample. The second sample, designated NSR-F-270409-2, was also a depleted uranium powder. It was of reasonably high purity (~380 μg/g total elemental impurities). The chemical form of the uranium was primarilymore » UO 3·2H 2O, with minor phases of U 3O 8 and UO 2. While aliquoting NSR-F-270409-2 for analysis, a metal staple of unknown origin was discovered in the sample. The presence of 236U and 232U in both samples indicates that the uranium feed stocks for these samples experienced a neutron flux at some point in their history. The reactor burn-up calculated from the isotopic composition of the uranium is consistent with that of spent fuel from natural uranium (NU) fueled Pu production. These nuclear forensic conclusions allow us to categorically exclude Australia as the origin of the material and greatly reduce the number of candidate sources.« less

Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

PubMed

Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B

2014-10-15

Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. Copyright © 2014 Elsevier B.V. All rights reserved.

Data on Molluscan Shells in parts of Nellore Coast, southeast coast of India.

PubMed

Lakshmanna, B; Jayaraju, N; Prasad, T Lakshmi; Sreenivasulu, G; Nagalakshmi, K; Kumar, M Pramod; Madakka, M

2018-02-01

X-ray diffraction (XRD), Scanning Electron Microscope-Energy Dispersive Spectroscopy (SEM-EDS), and Fourier Transform Infrared Spectroscopy (FT-IR), were applied to analyze the organic matrix of two Molluscan shells . The Mollusca shells are mineral structure and calcium carbonate crystallized as aragonite. The FT-IR spectra showed Alkyl Halide, Alkanes, Alcohols, Amides, Aromatic, and Hydroxyl groups in the organic matrix of the whole (organic and mineral) Molluscan shells. SEM images of particles of the two Molluscan shells at different magnifications were taken. The morphologies of the samples show a flake like structures with irregular grains, their sizes are at micrometric scale and the chemical analysis of EDS indicated that the major elements of Cardita and Gastropoda were C, O, and Ca, consistent with the results of XRD analysis. The results of the analysis of the EDS spectra of the shells showed that the content of most of the powder composition of shells is the element carbon, calcium oxygen, aluminium, and lead peaks that appear on the Cardita and Gastropoda and shells powders tap EDS spectra. The present work examined organic matrix of the selected shells of the heavily polluted and light polluted sites, along Nellore Coast, South East Coast of India. The heavily polluted sites have significantly thickened shells. The data demonstrated the sensitivity of this abundant and widely distributed intertidal fragile environment.

Heat removal from bipolar transistor by loop heat pipe with nickel and copper porous structures.

PubMed

Nemec, Patrik; Smitka, Martin; Malcho, Milan

2014-01-01

Loop heat pipes (LHPs) are used in many branches of industry, mainly for cooling of electrical elements and systems. The loop heat pipe is a vapour-liquid phase-change device that transfers heat from evaporator to condenser. One of the most important parts of the LHP is the porous wick structure. The wick structure provides capillary force to circulate the working fluid. To achieve good thermal performance of LHP, capillary wicks with high permeability and porosity and fine pore radius are expected. The aim of this work was to develop porous structures from copper and nickel powder with different grain sizes. For experiment copper powder with grain size of 50 and 100 μm and nickel powder with grain size of 10 and 25 μm were used. Analysis of these porous structures and LHP design are described in the paper. And the measurements' influences of porous structures in LHP on heat removal from the insulated gate bipolar transistor (IGBT) have been made.

Effects of Some Light Alloying Elements on the Oxidation Behavior of Fe and Ni-Cr Based Alloys During Air Plasma Spraying

NASA Astrophysics Data System (ADS)

Zeng, Zhensu; Kuroda, Seiji; Kawakita, Jin; Komatsu, Masayuki; Era, Hidenori

2010-01-01

The oxidation behavior of iron binary powders with addition of Si (1, 4 wt.%) and B (1, 3 wt.%) and that of a Ni-Cr based alloy powder with Si (4.3 wt.%), B (3.0 wt.%), and C (0.8 wt.%) additions during atmosphere plasma spray (APS) have been investigated. Analysis of the chemical composition and phases of oxides in the captured in-flight particles and deposited coatings was carried out. The results show that the addition of Si and B to iron effectively reduced the oxygen contents in the coatings, especially during the in-flight period at higher particles temperature. Ni-Cr based alloy powder with Si, B, and C additions reduced the oxidation of the base alloys significantly. Preferential oxidation and subsequent vaporization of Si, B, and C from the surface of the sprayed particles are believed to play a major role in controlling oxidation in the APS process.

Heat Removal from Bipolar Transistor by Loop Heat Pipe with Nickel and Copper Porous Structures

PubMed Central

Smitka, Martin; Malcho, Milan

2014-01-01

Loop heat pipes (LHPs) are used in many branches of industry, mainly for cooling of electrical elements and systems. The loop heat pipe is a vapour-liquid phase-change device that transfers heat from evaporator to condenser. One of the most important parts of the LHP is the porous wick structure. The wick structure provides capillary force to circulate the working fluid. To achieve good thermal performance of LHP, capillary wicks with high permeability and porosity and fine pore radius are expected. The aim of this work was to develop porous structures from copper and nickel powder with different grain sizes. For experiment copper powder with grain size of 50 and 100 μm and nickel powder with grain size of 10 and 25 μm were used. Analysis of these porous structures and LHP design are described in the paper. And the measurements' influences of porous structures in LHP on heat removal from the insulated gate bipolar transistor (IGBT) have been made. PMID:24959622

Modeling of the thermal physical process and study on the reliability of linear energy density for selective laser melting

NASA Astrophysics Data System (ADS)

Xiang, Zhaowei; Yin, Ming; Dong, Guanhua; Mei, Xiaoqin; Yin, Guofu

2018-06-01

A finite element model considering volume shrinkage with powder-to-dense process of powder layer in selective laser melting (SLM) is established. Comparison between models that consider and do not consider volume shrinkage or powder-to-dense process is carried out. Further, parametric analysis of laser power and scan speed is conducted and the reliability of linear energy density as a design parameter is investigated. The results show that the established model is an effective method and has better accuracy allowing for the temperature distribution, and the length and depth of molten pool. The maximum temperature is more sensitive to laser power than scan speed. The maximum heating rate and cooling rate increase with increasing scan speed at constant laser power and increase with increasing laser power at constant scan speed as well. The simulation results and experimental result reveal that linear energy density is not always reliable using as a design parameter in the SLM.

Synthesis and characterization of thermally evaporated Cu2SnSe3 ternary semiconductor

NASA Astrophysics Data System (ADS)

Hamdani, K.; Chaouche, M.; Benabdeslem, M.; Bechiri, L.; Benslim, N.; Amara, A.; Portier, X.; Bououdina, M.; Otmani, A.; Marie, P.

2014-11-01

Copper Tin Selenide (CuSnSe) powder was mechanically alloyed by high energy planetary ball milling, starting from elemental powders. Synthesis time and velocity have been optimized to produce Cu2SnSe3 materials. Thin films were prepared by thermal evaporation on Corning glass substrate at Ts = 300 °C. The structural, compositional, morphological and optical properties of the synthesized semiconductor have been analyzed by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM) and transmission electron microscopy. The analyzed powder exhibited a cubic crystal structure, with the presence of Cu2Se as a secondary phase. On the other hand, the deposited films showed a cubic Cu2SnSe3 ternary phase and extra peaks belonging to some binary compounds. Furthermore, optical measurements showed that the deposited layers have a relatively high absorption coefficient of 105 cm-1 and present a band gap of 0.94 eV.

[Study on hydrothermal stability of the collagen].

PubMed

Wang, Yajuan; Chen, Hui; Shan, Zhihua

2009-02-01

The low hydrothermal stability of the raw collagen restricts its usage. To improve the hydrothermal stability of collagen, two kinds of materials with weak astringency were used by experts. The research proved that the synergistic effect was formed during the process. In this study, by using UV, FT-IR, 13CNMR spectra and elemental analysis on the salicylic acid and metal-salicylic complexes, we could get the structural formula of every compound. And then, the hide powder was treated with the compounds. At last, the treated hide powder was tested by DSC. It could be presumed that the Rigid Matrix formed between the collagen doses can increase the hydrothermal stability of raw collagen, The result indicated that salicylic-chrome with large stable constant was better than others in improving the heat resistance of raw collagen, and the denaturalization temperature of hide powder treated with salicylic-chrome was 146.7 degrees C. Salicylic-aluminum was in the second place, the relevant temperature being 145.7 degrees C.

Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil.

PubMed

Kappen, P; Arhatari, B D; Luu, M B; Balaur, E; Caradoc-Davies, T

2013-06-01

This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography∕diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

Simulation of Powder Layer Deposition in Additive Manufacturing Processes Using the Discrete Element Method

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

Herbold, E. B.; Walton, O.; Homel, M. A.

2015-10-26

This document serves as a final report to a small effort where several improvements were added to a LLNL code GEODYN-­L to develop Discrete Element Method (DEM) algorithms coupled to Lagrangian Finite Element (FE) solvers to investigate powder-­bed formation problems for additive manufacturing. The results from these simulations will be assessed for inclusion as the initial conditions for Direct Metal Laser Sintering (DMLS) simulations performed with ALE3D. The algorithms were written and performed on parallel computing platforms at LLNL. The total funding level was 3-­4 weeks of an FTE split amongst two staff scientists and one post-­doc. The DEM simulationsmore » emulated, as much as was feasible, the physical process of depositing a new layer of powder over a bed of existing powder. The DEM simulations utilized truncated size distributions spanning realistic size ranges with a size distribution profile consistent with realistic sample set. A minimum simulation sample size on the order of 40-­particles square by 10-­particles deep was utilized in these scoping studies in order to evaluate the potential effects of size segregation variation with distance displaced in front of a screed blade. A reasonable method for evaluating the problem was developed and validated. Several simulations were performed to show the viability of the approach. Future investigations will focus on running various simulations investigating powder particle sizing and screen geometries.« less

Analysis of Rare Earth Elements in Uranium Using Handheld Laser-Induced Breakdown Spectroscopy (HH LIBS)

DOE PAGES

Manard, Benjamin T.; Wylie, E. Miller; Willson, Stephen P.

2018-05-22

In this paper, a portable handheld laser-induced breakdown spectroscopy (HH LIBS) instrument was evaluated as a rapid method to qualitatively analyze rare earth elements in a uranium oxide matrix. This research is motivated by the need for development of a method to perform rapid, at-line chemical analysis in a nuclear facility, particularly to provide a rapid first pass analysis to determine if additional actions or measurements are warranted. This will result in the minimization of handling and transport of radiological and nuclear material and subsequent exposure to their associated hazards. In this work, rare earth elements (Eu, Nd, and Yb)more » were quantitatively spiked into a uranium oxide powder and analyzed by the HH LIBS instrumentation. This method demonstrates the ability to rapidly identify elemental constituents in sub-percent levels in a uranium matrix. Preliminary limits of detection (LODs) were determined with values on the order of hundredths of a percent. Validity of this methodology was explored by employing a National Institute of Standards and Technology (NIST) standard reference materials (SRM) 610 and 612 (Trace Elements in Glass). Finally, it was determined that the HH LIBS method was able to clearly discern the rare earths elements of interest in the glass or uranium matrices.« less

Analysis of Rare Earth Elements in Uranium Using Handheld Laser-Induced Breakdown Spectroscopy (HH LIBS)

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

Manard, Benjamin T.; Wylie, E. Miller; Willson, Stephen P.

In this paper, a portable handheld laser-induced breakdown spectroscopy (HH LIBS) instrument was evaluated as a rapid method to qualitatively analyze rare earth elements in a uranium oxide matrix. This research is motivated by the need for development of a method to perform rapid, at-line chemical analysis in a nuclear facility, particularly to provide a rapid first pass analysis to determine if additional actions or measurements are warranted. This will result in the minimization of handling and transport of radiological and nuclear material and subsequent exposure to their associated hazards. In this work, rare earth elements (Eu, Nd, and Yb)more » were quantitatively spiked into a uranium oxide powder and analyzed by the HH LIBS instrumentation. This method demonstrates the ability to rapidly identify elemental constituents in sub-percent levels in a uranium matrix. Preliminary limits of detection (LODs) were determined with values on the order of hundredths of a percent. Validity of this methodology was explored by employing a National Institute of Standards and Technology (NIST) standard reference materials (SRM) 610 and 612 (Trace Elements in Glass). Finally, it was determined that the HH LIBS method was able to clearly discern the rare earths elements of interest in the glass or uranium matrices.« less

Analysis of Rare Earth Elements in Uranium Using Handheld Laser-Induced Breakdown Spectroscopy (HH LIBS).

PubMed

Manard, Benjamin T; Wylie, E Miller; Willson, Stephen P

2018-01-01

A portable handheld laser-induced breakdown spectroscopy (HH LIBS) instrument was evaluated as a rapid method to qualitatively analyze rare earth elements in a uranium oxide matrix. This research is motivated by the need for development of a method to perform rapid, at-line chemical analysis in a nuclear facility, particularly to provide a rapid first pass analysis to determine if additional actions or measurements are warranted. This will result in the minimization of handling and transport of radiological and nuclear material and subsequent exposure to their associated hazards. In this work, rare earth elements (Eu, Nd, and Yb) were quantitatively spiked into a uranium oxide powder and analyzed by the HH LIBS instrumentation. This method demonstrates the ability to rapidly identify elemental constituents in sub-percent levels in a uranium matrix. Preliminary limits of detection (LODs) were determined with values on the order of hundredths of a percent. Validity of this methodology was explored by employing a National Institute of Standards and Technology (NIST) standard reference materials (SRM) 610 and 612 (Trace Elements in Glass). It was determined that the HH LIBS method was able to clearly discern the rare earths elements of interest in the glass or uranium matrices.

Plasma Methods of Obtainment of Multifunctional Composite Materials, Dispersion-Hardened by Nanoparticles

NASA Astrophysics Data System (ADS)

Sizonenko, O. N.; Grigoryev, E. G.; Pristash, N. S.; Zaichenko, A. D.; Torpakov, A. S.; Lypian, Ye. V.; Tregub, V. A.; Zholnin, A. G.; Yudin, A. V.; Kovalenko, A. A.

2017-09-01

High voltage electric discharge (HVED) in disperse system "hydrocarbon liquid - powder" due to impact of plasma discharge channel, electromagnetic fields, shock waves mechanical impact, hydro flows and volume microcavitation leads to synthesis of nanocarbon, metal powders dispersion and synthesis of micro- (from 10-6 to 10-7 m) and nanosized (from 10-7 to 10-9 m) composite powders of hardening phases. Spark plasma sintering (SPS) of powder mixtures allows targeted control of grain growth rate and thus allows obtainment of multifunctional composite materials dispersion hardened by nanoparticles. Processes of HVED synthesis of micro- and nanosized powders of new compositions from elemental metal powders and their mixtures with the subsequent application of high-speed SPS of obtained powders create conditions for increase of strength (by 10-20 %), hardness and wear-resistance (by 30-60 %) of obtained materials.

Investigation of the effect of alumina and compaction pressure on physical, electrical and tribological properties of Al-Fe-Cr-Al2O3 powder composites

NASA Astrophysics Data System (ADS)

Mohsin, Mohammad; Mohd, Aas; Suhaib, M.; Arif, Sajjad; Arif Siddiqui, M.

2017-10-01

In this experimental work, aluminium Al-20Fe-5Cr (in wt.%) matrix reinforced with varying wt.% Al2O3 (0, 10, 20 and 30) and compaction pressure (470, 550 and 600 MPa) were prepared by powder metallurgy technique. The characterization of composites were performed by scanning electron microscopy (SEM), x-ray diffraction (XRD), energy dispersive spectrum (EDS) and elemental mapping. Uniform distribution of Al2O3 in aluminium matrix were observed by elemental mapping. The composites showed an increase in density and hardness by increasing both alumina and compaction pressure. While, electrical conductivity decreased by the addition of alumina. The tribological study of the composites were performed on pin-on-disc apparatus at sliding conditions (applied load 40 N, sliding speed 1.5 m s-1, sliding distance 300 m). The tribological properties of the composites were improved by increasing alumina and compaction pressure. SEM analysis were also carried out to understand wear mechanism of the worn surfaces of various fabricated composites and aluminium matrix.

Powder metallurgy of Ge, Si, and Ge-Si

NASA Astrophysics Data System (ADS)

Schilz, Jürgen; Langenbach, Marion

1993-03-01

id="ab1"Planetary ball-milling and pressing behaviour of Ge, Si and Ge-Si powder mixtures are investigated. Scanning and transmission electron microscopy observations revealed the different microstructure of the two elements after milling: Ge remains in a microcrystalline state, whereas Si can be comminuted into grains consisting of nanocrystalline regions. Planetary milling of the two elements together, using agate balls and vial, did not reveal any compound formation. By hot-isostatic pressing, pure Ge and Ge-Si mixtures were densified to a higher value than pure Si. This denotes a plastic flow of the Ge component at a process temperature of 800°C. The microhardness of hot-pressed Ge reaches the bulk value; hot-pressed Si is very soft. Energy dispersive X-ray analysis and X-ray diffraction did not detect any impurity contamination from vial and milling media wear. Moreover, by electrical transport measurements it turned out that the net carrier concentration density resulting from electrical active impurities introduced by the milling and pressing process is below 2 x 1016 cm 3 at room temperature.

Production of High-Purity Anhydrous Nickel(II) Perrhenate for Tungsten-Based Sintered Heavy Alloys

PubMed Central

Leszczyńska-Sejda, Katarzyna; Benke, Grzegorz; Kopyto, Dorota; Majewski, Tomasz; Drzazga, Michał

2017-01-01

This paper presents a method for the production of high-purity anhydrous nickel(II) perrhenate. The method comprises sorption of nickel(II) ions from aqueous nickel(II) nitrate solutions, using strongly acidic C160 cation exchange resin, and subsequent elution of sorbed nickel(II) ions using concentrated perrhenic acid solutions. After the neutralization of the resulting rhenium-nickel solutions, hydrated nickel(II) perrhenate is then separated and then dried at 160 °C to obtain the anhydrous form. The resulting compound is reduced in an atmosphere of dissociated ammonia in order to produce a Re-Ni alloy powder. This study provides information on the selected properties of the resulting Re-Ni powder. This powder was used as a starting material for the production of 77W-20Re-3Ni heavy alloys. Microstructure examination results and selected properties of the produced sintered heavy alloys were compared to sintered alloys produced using elemental W, Re, and Ni powders. This study showed that the application of anhydrous nickel(II) perrhenate in the production of 77W-20Re-3Ni results in better properties of the sintered alloys compared to those made from elemental powders. PMID:28772808

Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples.

PubMed

Boulyga, Sergei F; Heilmann, Jens; Prohaska, Thomas; Heumann, Klaus G

2007-10-01

A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for (35)Cl+ to more than 6 x 10(5) cps for (238)U+ for 1 microg of trace element per gram of coal sample. Detection limits vary from 450 ng g(-1) for chlorine and 18 ng g(-1) for sulfur to 9.5 pg g(-1) for mercury and 0.3 pg g(-1) for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis.

End-of-life nickel-cadmium accumulators: characterization of electrode materials and industrial Black Mass.

PubMed

Hazotte, Claire; Leclerc, Nathalie; Diliberto, Sébastien; Meux, Eric; Lapicque, Francois

2015-01-01

The aim of this paper is the characterization of spent NiCd batteries and the characterization of an industrial Black Mass obtained after crushing spent NiCd batteries and physical separation in a treatment plant. The characterization was first performed with five cylindrical NiCd batteries which were manually dismantled. Their characterization includes mass balance of the components, active powders elemental analysis and phase identification by X-ray powder diffraction. Chemical speciation of the two metals was also investigated. For cadmium, speciation was previously developed on solid synthetic samples. In a spent battery, the active powders correspond to about 43% of the battery weight. The other components are the separator and polymeric pieces (5%), the support plates (25%) and the carbon steel external case (27%). The sequential procedure shows that the nickel in the positive powders from the dismantled Ni-Cd batteries is distributed between Ni0 (39.7%), Ni(OH)2 (58.5%) and NiOOH (1.8%). Cadmium in the negative powder is about 99.9% as the Cd(OH)2 form with 0.1% of metal cadmium. In the industrial Black Mass, the distribution of cadmium is the same, whereas the distribution of nickel is Ni0 (46.9%), Ni(OH)2 (43.2%) and NiOOH (9.9%). This material contains also 1.8% cobalt and approx. 1% iron.

Performance of planar single cell lanthanum gallate based solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Maffei, N.; Kuriakose, A. K.

A novel synthesis of high purity, single phase strontium-magnesium doped lanthanum gallate through a nitrate route is described. The prepared powder is formed into planar monolithic elements by uniaxial pressing followed by isostatic pressing and sintering. XRD analysis of the sintered elements reveal no detectable secondary phases. The performance of the electrolyte in solid oxide fuel cells (SOFC) with three different anode/cathode combinations tested at 700°C with respect to the J- V and power density is reported. The data show that the characteristics of this SOFC are strongly dependent on the particular anode/cathode system chosen.

A Morphological Approach to the Modeling of the Cold Spray Process

NASA Astrophysics Data System (ADS)

Delloro, F.; Jeandin, M.; Jeulin, D.; Proudhon, H.; Faessel, M.; Bianchi, L.; Meillot, E.; Helfen, L.

2017-12-01

A coating buildup model was developed, the aim of which was simulating the microstructure of a tantalum coating cold sprayed onto a copper substrate. To do so, first was operated a fine characterization of the irregular tantalum powder in 3D, using x-ray microtomography and developing specific image analysis algorithms. Particles were grouped by shape in seven classes. Afterward, 3D finite element simulations of the impact of the previously observed particles were realized. To finish, a coating buildup model was developed, based on the results of finite element simulations of particle impact. In its first version, this model is limited to 2D.

Electroerosion micro- and nanopowders for the production of hard alloys

NASA Astrophysics Data System (ADS)

Latypov, R. A.; Ageeva, E. V.; Kruglyakov, O. V.; Latypova, G. R.

2016-06-01

The shape and the surface morphology of the powder particles fabricated by the electroerosion dispersion of tungsten-containing wastes in illuminating oil are studied. The hard alloy fabricated from these powder particles is analyzed by electron-probe microanalysis. The powder synthesized by the electroerosion dispersion of the wastes of sintered hard alloys is found to consist of particles of a spherical or elliptical shape, an irregular shape (conglomerates), and a fragment shape. It is shown that W, Ti, and Co are the main elements in the hard alloy fabricated from the powder synthesized by electroerosion dispersion in illuminating oil.

Elemental source attribution signatures for calcium ammonium nitrate (CAN) fertilizers used in homemade explosives

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

Fraga, Carlos G.; Mitroshkov, Alexander V.; Mirjankar, Nikhil S.

Calcium ammonium nitrate (CAN) is a widely available fertilizer composed of ammonium nitrate mixed with some form of calcium carbonate such as limestone or dolomite. CAN is also frequently used to make homemade explosives. The potential of using elemental profiling and chemometrics to match both pristine and reprocessed CAN fertilizers to their factories for use in future forensic investigations was examined. Inductively coupled plasma-mass spectrometry (ICP-MS) analysis was performed on 64 elements in 125 samples from 11 CAN stocks from 6 different CAN factories. Fisher ratio, degree-of-class-separation, and partial least squares discriminant analysis (PLSDA) were used to develop a modelmore » using the concentrations of Na, V, Mn, Cu, Ga, Sr, Ba and U to classify a validation set of CAN samples into 5 factory groups; one group was two factories from the same fertilizer company. In terms of the pristine CAN samples, i.e., unadulterated prills, 64% of the test samples were matched to their correct factory group with zero false positives. The same PLSDA model was used to correctly match 100% of the CAN samples that were reprocessed by crushing and mixing the CAN with powdered sugar. In the case of crushed CAN samples mixed with aluminum powder, correct matches were made for zero to 100% of the samples depending on the factory the CAN originated. Remarkably, for one factory, 100% of the ammonium nitrate samples that were extracted from CAN using tap or bottled water were matched to the correct CAN factory group. Lastly, the water-insoluble (calcium carbonate) portions of CAN provided a greater degree of discrimination between factories than the water-soluble portions of CAN. In summary, this work illustrates that sourcing unadulterated CAN fertilizer can potentially be done with high frequency and high confidence using elemental profiling and chemometrics while the sourcing of reprocessed CAN is dependent on how much an adulterant alters the recovered elemental profile of CAN.« less

Neutron- and photon-activation detection limits in breast milk analysis for prospective dose evaluation of the suckling infant.

PubMed

Tsipenyuk, Yu M; Firsov, V I; Cantone, M C

2009-01-01

Complex situations related to the environment, as in the regions affected by the Chernobyl accident and regions in which nuclear weapons testing were undertaken, as in Semipalatinsk, could be reflected in the trace element content in mothers' milk. The evaluation of fractional transfer to milk of ingested or inhaled activity and of the corresponding dose coefficients for the infant, following a mothers' radioactive intake, can take advantage from wide-ranging studies of elemental and radionuclide contents in mothers' milk. In this work the possibility to determine elements, such as Ru, Zr, Nb, Te, Ce, Th, U, in milk powder has been investigated. Although results from elemental analyses of breast milk are to be found in the literature, the determination of the identified elements has attracted poor attention since they are not considered essential elements from a biological point of view. Nevertheless, in the case of radioactive releases to the environment, such data could be of interest in evaluation of dose to the breast-fed infant.

Direct-current arc and alternating-current spark emission spectrographic field methods for the semiquantitative analysis of geologic materials

USGS Publications Warehouse

Grimes, D.J.; Marranzino, A.P.

1968-01-01

Two spectrographic methods are used in mobile field laboratories of the U. S. Geological Survey. In the direct-current arc method, the ground sample is mixed with graphite powder, packed into an electrode crater, and burned to completion. Thirty elements are determined. In the spark method, the sample, ground to pass a 150-mesh screen, is digested in hydrofluoric acid followed by evaporation to dryness and dissolution in aqua regia. The solution is fed into the spark gap by means of a rotating-disk electrode arrangement and is excited with an alternating-current spark discharge. Fourteen elements are determined. In both techniques, light is recorded on Spectrum Analysis No. 1, 35-millimeter film, and the spectra are compared visually with those of standard films.

A Study of Compaction and Deformation of a Powder Composite Material of the `Aluminum - Rare Earth Elements' System

NASA Astrophysics Data System (ADS)

Rudskoy, A. I.; Tsemenko, V. N.; Ganin, S. V.

2015-01-01

The possibility of fabrication of preforms of a composite material with special radiation-protective properties on the base of mechanically alloyed powders of the Al - REM system with the use of methods of severe plastic deformation is shown.

[Rapid determination of major and trace elements in the salt lake clay minerals by X-ray fluorescence spectrometry].

PubMed

Wang, Xiao-Huan; Meng, Qing-Fen; Dong, Ya-Ping; Chen, Mei-Da; Li, Wu

2010-03-01

A rapid multi-element analysis method for clay mineral samples was described. This method utilized a polarized wave-length dispersive X-ray fluorescence spectrometer--Axios PW4400, which had a maximum tube power of 4 000 watts. The method was developed for the determination of As, Mn, Co, Cu, Cr, Dy, Ga, Mo, P, Pb, Rb, S, Sr, Ni, ,Cs, Ta, Th, Ti, U, V, Y, Zn, Zr, MgO, K2O, Na2O, CaO, Fe2O3, Al2O3, SiO2 and so on. Thirty elements in clay mineral species were measured by X-ray fluorescence spectrometry with pressed powder pellets. Spectral interferences, in particular the indirect interferences of each element, were studied. A method to distinguish the interference between each other periodic elements in element periodic table was put forward. The measuring conditions and existence were mainly investigated, and the selected background position as well as corrected spectral overlap for the trace elements were also discussed. It was found that the indirect spectral overlap line was the same important as direct spectral overlap line. Due to inducing the effect of indirect spectral overlap, some elements jlike Bi, Sn, W which do not need analysis were also added to the elements channel. The relative standard deviation (RSD) was in the range of 0.01% to 5.45% except three elements Mo, Cs and Ta. The detection limits, precisions and accuracies for most elements using this method can meet the requirements of sample analysis in clay mineral species.

Growth and characterization of barium complex of 1,3,5-triazinane-2,4,6-trione in gel: a corrosion inhibiting material

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Babu, K. Rajendra

2018-05-01

Good quality prismatic crystals of industrially applicable corrosion inhibiting barium complex of 1,3,5-triazinane-2,4,6-trione have been grown by conventional gel method. The crystal structure, packing, and nature of bonds are revealed in the single crystal X-ray diffraction analysis. The crystal has a three-dimensional polymeric structure having a triclinic crystal system with the space group P-1. The powder X-ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal are identified by Fourier transform infrared spectroscopy. Elemental analysis confirms the stoichiometry of the elements present in the complex. Thermogravimetric analysis and differential thermal analysis reveal its good thermal stability. The optical properties like band gap, refractive index and extinction coefficient are evaluated from the UV-visible spectral analysis. The singular property of the material, corrosion inhibition efficiency achieved by the adsorption of the sample molecules is determined by the weight loss method.

Characterization, Processing, and Consolidation of Nanoscale Tungsten Powder

DTIC Science & Technology

2009-12-01

gas fusion, and all other elements were measured by direct current plasma emission spectroscopy. The analysis showed a relatively high amount of...measured by direct current plasma emission spectroscopy, and oxygen was detected by inert gas fusion. The results show that carbon and cobalt levels...of law, no person shall be subject to any penalty for failing to comply with a collection of information if it does not display a currently valid OMB

Acetone sensor based on zinc oxide hexagonal tubes

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

Hastir, Anita, E-mail: anitahastir@gmail.com; Singh, Onkar, E-mail: anitahastir@gmail.com; Anand, Kanika, E-mail: anitahastir@gmail.com

2014-04-24

In this work hexagonal tubes of zinc oxide have been synthesized by co-precipitation method. For structural, morphological, elemental and optical analysis synthesized powders were characterized by using x-ray diffraction, field emission scanning microscope, EDX, UV-visible and FTIR techniques. For acetone sensing thick films of zinc oxide have been deposited on alumina substrate. The fabricated sensors exhibited maximum sensing response towards acetone vapour at an optimum operating temperature of 400°C.

Structure of Al-Fe alloys prepared by different methods after severe plastic deformation under pressure

NASA Astrophysics Data System (ADS)

Dobromyslov, A. V.; Taluts, N. I.

2017-06-01

Al-Fe alloys prepared by casting, rapid quenching from the melt, and mechanical alloying from elemental powders have been studied using X-ray diffraction analysis, optical metallography, transmission electron microscopy, and microhardness measurements in the initial state and after severe plastic deformation by high-pressure torsion using Bridgman anvils. The relationship between the phase composition, microstructure, and the microhardness of the investigated alloys has been established.

Roles of Cationic and Elemental Calcium in the Electro-Reduction of Solid Metal Oxides in Molten Calcium Chloride

NASA Astrophysics Data System (ADS)

Qiu, Guohong; Jiang, Kai; Ma, Meng; Wang, Dihua; Jin, Xianbo; Chen, George Z.

2007-06-01

Previous work, mainly from this research group, is re-visited on electrochemical reduction of solid metal oxides, in the form of compacted powder, in molten CaCl2, aiming at further understanding of the roles of cationic and elemental calcium. The discussion focuses on six aspects: 1.) debate on two mechanisms proposed in the literature, i. e. electro-metallothermic reduction and electro-reduction (or electro-deoxidation), for the electrolytic removal of oxygen from solid metals or metal oxides in molten CaCl2; 2.) novel metallic cavity working electrodes for electrochemical investigations of compacted metal oxide powders in high temperature molten salts assisted by a quartz sealed Ag/AgCl reference electrode (650 ºC- 950 ºC); 3.) influence of elemental calcium on the background current observed during electrolysis of solid metal oxides in molten CaCl2; 4.) electrochemical insertion/ inclusion of cationic calcium into solid metal oxides; 5.) typical features of cyclic voltammetry and chronoamperometry (potentiostatic electrolysis) of metal oxide powders in molten CaCl2; and 6.) some kinetic considerations on the electrolytic removal of oxygen.

Metal alloy coatings and methods for applying

DOEpatents

Merz, Martin D.; Knoll, Robert W.

1991-01-01

A method of coating a substrate comprises plasma spraying a prealloyed feed powder onto a substrate, where the prealloyed feed powder comprises a significant amount of an alloy of stainless steel and at least one refractory element selected from the group consisting of titanium, zirconium, hafnium, niobium, tantalum, molybdenum, and tungsten. The plasma spraying of such a feed powder is conducted in an oxygen containing atmosphere and forms an adherent, corrosion resistant, and substantially homogenous metallic refractory alloy coating on the substrate.

Oxide-dispersion strengthening of porous powder metalurgy parts

DOEpatents

Judkins, Roddie R.

2002-01-01

Oxide dispersion strengthening of porous metal articles includes the incorporation of dispersoids of metallic oxides in elemental metal powder particles. Porous metal articles, such as filters, are fabricated using conventional techniques (extrusion, casting, isostatic pressing, etc.) of forming followed by sintering and heat treatments that induce recrystallization and grain growth within powder grains and across the sintered grain contact points. The result is so-called "oxide dispersion strengthening" which imparts, especially, large increases in creep (deformation under constant load) strength to the metal articles.

Structure and electrical properties of intergrowth bismuth layer-structured Bi4Ti3O12-CaBi4Ti4O15 ferroelectric ceramics

NASA Astrophysics Data System (ADS)

Choi, Gi Ppeum; Cho, Sam Yeon; Bu, Sang Don

2016-09-01

Pb-free ferroelectric Bi4Ti3O12-CaBi4Ti4O15 (BIT-CBT) ceramics were manufactured using a solid-state reaction method. Structural analysis by using X-ray diffraction confirmed the presence of a second phase of Bi2Ti2O7, and the surface depth X-ray diffraction analysis revealed that this phase existed only on the surface. This second phase appears to have been caused by the volatilization of Bi ions at high sintering temperatures. For resolution of the issue of volatilization of Bi ions and manufacture of BIT-CBT ceramics with a single phase, Bi2O3 powder was added to the BIT-CBT mixture, and a powder-bed method, in which pellets were covered with BIT-CBT powder, was used to manufacture the ceramic. The piezoelectric coefficient of the single-phase BIT-CBT ceramics was 12.4 pC/N while the residual polarization and the coercive electric field were 11.3 μC/cm2, and 125 kV/cm, respectively. The results suggest that single-phase BIT-CBT ceramics are suitable for the manufacture of elements incorporating these electrical characteristics.

Modelling and Characterization of Effective Thermal Conductivity of Single Hollow Glass Microsphere and Its Powder.

PubMed

Liu, Bing; Wang, Hui; Qin, Qing-Hua

2018-01-14

Tiny hollow glass microsphere (HGM) can be applied for designing new light-weighted and thermal-insulated composites as high strength core, owing to its hollow structure. However, little work has been found for studying its own overall thermal conductivity independent of any matrix, which generally cannot be measured or evaluated directly. In this study, the overall thermal conductivity of HGM is investigated experimentally and numerically. The experimental investigation of thermal conductivity of HGM powder is performed by the transient plane source (TPS) technique to provide a reference to numerical results, which are obtained by a developed three-dimensional two-step hierarchical computational method. In the present method, three heterogeneous HGM stacking elements representing different distributions of HGMs in the powder are assumed. Each stacking element and its equivalent homogeneous solid counterpart are, respectively, embedded into a fictitious matrix material as fillers to form two equivalent composite systems at different levels, and then the overall thermal conductivity of each stacking element can be numerically determined through the equivalence of the two systems. The comparison of experimental and computational results indicates the present computational modeling can be used for effectively predicting the overall thermal conductivity of single HGM and its powder in a flexible way. Besides, it is necessary to note that the influence of thermal interfacial resistance cannot be removed from the experimental results in the TPS measurement.

Value assignment of nutrient concentrations in five standard reference materials and six reference materials.

PubMed

Sharpless, K E; Gill, L M

2000-01-01

A number of food-matrix reference materials (RMs) are available from the National Institute of Standards and Technology (NIST) and from Agriculture Canada through NIST. Most of these materials were originally value-assigned for their elemental composition (major, minor, and trace elements), but no additional nutritional information was provided. Two of the materials were certified for selected organic constituents. Ten of these materials (Standard Reference Material [SRM] 1,563 Cholesterol and Fat-Soluble Vitamins in Coconut Oil [Natural and Fortified], SRM 1,566b Oyster Tissue, SRM 1,570a Spinach Leaves, SRM 1,974a Organics in Mussel Tissue (Mytilus edulis), RM 8,415 Whole Egg Powder, RM 8,418 Wheat Gluten, RM 8,432 Corn Starch, RM 8,433 Corn Bran, RM 8,435 Whole Milk Powder, and RM 8,436 Durum Wheat Flour) were recently distributed by NIST to 4 laboratories with expertise in food analysis for the measurement of proximates (solids, fat, protein, etc.), calories, and total dietary fiber, as appropriate. SRM 1846 Infant Formula was distributed as a quality control sample for the proximates and for analysis for individual fatty acids. Two of the materials (Whole Egg Powder and Whole Milk Powder) were distributed in an earlier interlaboratory comparison exercise in which they were analyzed for several vitamins. Value assignment of analyte concentrations in these 11 SRMs and RMs, based on analyses by the collaborating laboratories, is described in this paper. These materials are intended primarily for validation of analytical methods for the measurement of nutrients in foods of similar composition (based on AOAC INTERNATIONAL's fat-protein-carbohydrate triangle). They may also be used as "primary control materials" in the value assignment of in-house control materials of similar composition. The addition of proximate information for 10 existing reference materials means that RMs are now available from NIST with assigned values for proximates in 6 of the 9 sectors of the AOAC triangle. Five of these materials have values assigned for total dietary fiber-the first such information provided for materials available from NIST.

Fractionation of elements by particle size of ashes ejected from Copahue Volcano, Argentina.

PubMed

Gómez, Dario; Smichowski, Patricia; Polla, Griselda; Ledesma, Ariel; Resnizky, Sara; Rosa, Susana

2002-12-01

The volcano Copahue, Neuquén province, Argentina has shown infrequent explosive eruptions since the 18th century. Recently, eruptive activity and seismicity were registered in the period July-October, 2000. As a consequence, ash clouds were dispersed by winds and affected Caviahue village located at about 9 km east of the volcano. Samples of deposited particles from this area were collected during this episode for their chemical analysis to determine elements of concern with respect to the health of the local population and its environment. Different techniques were used to evaluate the distribution of elements in four particle size ranges from 36 to 300 microm. X-ray powder diffraction (XRD) was selected to detect major components namely, minerals, silicate glass, fragments of rocks and sulfurs. Major and minor elements (Al, Ca, Cl, Fe, K, Mg, Mn, Na, S, Si and Ti), were detected by energy dispersive X ray analysis (EDAX). Trace element (As, Cd, Cr, Cu, Hg, Ni, Pb, Sb, U, V and Zn) content was quantified by inductively coupled plasma-mass spectrometry (ICP-MS). Nuclear activation analysis (NAA) was employed for the determination of Ce, Co, Cs, Eu, Hf, La, Lu, Rb, Sc, Sm, Ta and Yb. An enrichment was observed in the smallest size fraction of volcanic ashes for four elements (As, Cd, Cu and Sb) of particular interest from the environmental and human health point of view.

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.

Microstructure transformation of Cr-Al coating on carbon steel prepared by ball milling method as a function of tungsten doping

NASA Astrophysics Data System (ADS)

Wismogroho, A. S.; Sudiro, T.; Didik, A.; Ciswandi

2018-03-01

In present work, Cr-Al coatings containing 0, 1, 2, 3, and 5% W have been prepared on the surface of low carbon steel by mechanical alloying technique. The composition of each powder was milled for 2 hour in a stainless steel crucible with a ball to powder ratio of 10:1. Afterward, the Cr-Al-W powder and substrate were mechanically alloyed in air for 1 hour. The heat treatment of coated samples was carried out at 800 °C in a vacuum furnace for 2 hour. In order to characterize the phase composition and microstructure of the coating before and after heat treatment, XRD and SEM-EDX were used. The analysis results reveal that the ball milling process induces the formation of homogeneous Cr-Al-W coating structure with a thickness of about 80 μm. The phase observation shows individual peaks of each starting elements, along with the occurrence of powder refinement and solid solution formation. After heat treatment, AlCr2 and Al8Cr5 phases were formed. The addition of W accelerates the formation of AlCr2, but inhibits the formation of Al8Cr5. The detail of the results was presented in this paper.

Design of Natural Hydroxyapatite as bio-composite ceramics (HAP): Experimental and Numerical Study

NASA Astrophysics Data System (ADS)

Belghazi, Z.; Katundi, D.; Ayari, F.; Bayraktar, E.

2011-01-01

Hydroxyapatite (HAP—Ca10(PO4)6 (OH)2), which exhibits excellent biocompatibility in the body, is one of the most widely used bioactive ceramics for biomedical applications. Along with the ability to carry the load, one of the most important properties of materials used for bone replacement is biocompatibility. In fact, HAP is a bioactive material and it can incorporate into bone structures, supporting bone in-growth without breaking down or dissolving, and it interacts with the living tissue due to the presence of free calcium and phosphate compounds. Generally, Al2O3 powder is added to HAP powder in order to obtain high fracture toughness. Al2O3 has good mechanical properties as compared with HAP, and exhibits extremely high stability with human tissues [1-6]. In this paper, the effect of microwave sintering temperature on the relative density, hardness, and phase purity of compacted bovine Hydroxyapatite (BHA) powder was reported. This research is a comprehensive attempt to develop Hydroxyapatite bio composite ceramics reinforced with alumina—Al2O3, pure titanium and pure pulverised boron powder. A Finite Element (FEM) analysis is also used for modelling to simulate the macroscopic behaviour of this material, taking into account the relevant microscopic scales.

Film analysis employing subtarget effect using 355 nm Nd-YAG laser-induced plasma at low pressure

NASA Astrophysics Data System (ADS)

Hedwig, Rinda; Budi, Wahyu Setia; Abdulmadjid, Syahrun Nur; Pardede, Marincan; Suliyanti, Maria Margaretha; Lie, Tjung Jie; Kurniawan, Davy Putra; Kurniawan, Koo Hendrik; Kagawa, Kiichiro; Tjia, May On

2006-12-01

The applicability of spectrochemical analysis for liquid and powder samples of minute amount in the form of thin film was investigated using ultraviolet Nd-YAG laser (355 nm) and low-pressure ambient air. A variety of organic samples such as commercial black ink usually used for stamp pad, ginseng extract, human blood, liquid milk and ginseng powder was prepared as film deposited on the surface of an appropriate hard substrate such as copper plate or glass slide. It was demonstrated that in all cases studied, good quality spectra were obtained with very low background and free from undesirable contamination by the substrate elements, featuring ppm or even sub-ppm sensitivity and worthy of application for quantitative analysis of organic samples. The proper preparation of the films was found to be crucial in achieving the high quality spectra. It was further shown that much inferior results were obtained when the atmospheric-pressure (101 kPa) operating condition of laser-induced breakdown spectroscopy or the fundamental wavelength of the Nd-YAG laser was employed due to the excessive or improper laser ablation process.

Mercury

MedlinePlus

Mercury is an element that is found in air, water and soil. It has several forms. Metallic mercury is a shiny, silver-white, odorless liquid. If ... with other elements to form powders or crystals. Mercury is in many products. Metallic mercury is used ...

Residual stress prediction in a powder bed fusion manufactured Ti6Al4V hip stem

NASA Astrophysics Data System (ADS)

Barrett, Richard A.; Etienne, Titouan; Duddy, Cormac; Harrison, Noel M.

2017-10-01

Powder bed fusion (PBF) is a category of additive manufacturing (AM) that is particularly suitable for the production of 3D metallic components. In PBF, only material in the current build layer is at the required melt temperature, with the previously melted and solidified layers reducing in temperature, thus generating a significant thermal gradient within the metallic component, particularly for laser based PBF components. The internal thermal stresses are subsequently relieved in a post-processing heat-treatment step. Failure to adequately remove these stresses can result in cracking and component failure. A prototype hip stem was manufactured from Ti6Al4V via laser PBF but was found to have fractured during over-seas shipping. This study examines the evolution of thermal stresses during the laser PBF manufacturing and heat treatment processes of the hip stem in a 2D finite element analysis (FEA) and compares it to an electron beam PBF process. A custom written script for the automatic conversion of a gross geometry finite element model into a thin layer- by-layer finite element model was developed. The build process, heat treatment (for laser PBF) and the subsequent cooling were simulated at the component level. The results demonstrate the effectiveness of the heat treatment in reducing PBF induced thermal stresses, and the concentration of stresses in the region that fractured.

Determination of sixteen elements and arsenic species in brown, polished and milled rice.

PubMed

Narukawa, Tomohiro; Matsumoto, Eri; Nishimura, Tsutomu; Hioki, Akiharu

2014-01-01

The concentrations of 16 elements in 10 rice flour samples and the distribution of the elements in the rice grains from which the flour were made were determined by ICP-MS and ICP-OES after microwave-assisted digestion of the samples. Arsenic speciation analysis was carried out by HPLC-ICP-MS following heat-assisted extraction of the sample. The concentrations of inorganic As (As(III) and As(V)), monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA) and their distribution in the rice grains were determined. Portions of the brown rice were polished/milled to different degrees to yield milled off samples and polished rice samples. All samples were powdered and analyzed for 16 elements and for As species. The recoveries and mass balances for all elements in all samples showed good agreements with the starting materials. As(III), As(V), MMAA and DMAA were detected, and the sums of the concentrations of all species in the extract were 86-105% of the total As concentration in each case.

Micro-feeding and dosing of powders via a small-scale powder pump.

PubMed

Besenhard, M O; Fathollahi, S; Siegmann, E; Slama, E; Faulhammer, E; Khinast, J G

2017-03-15

Robust and accurate powder micro-feeding (<100mg/s) and micro-dosing (<5 mg) are major challenges, especially with regard to regulatory limitations applicable to pharmaceutical development and production. Since known micro-feeders that yield feed rates below 5mg/s use gravimetric feeding principles, feed rates depend primarily on powder properties. In contrast, volumetric powder feeders do not require regular calibration because their feed rates are primarily determined by the feeder's characteristic volume replacement. In this paper, we present a volumetric micro-feeder based on a cylinder piston system (i.e., a powder pump), which allows accurate micro-feeding and feed rates of a few grams per hours even for very fine powders. Our experimental studies addressed the influence of cylinder geometries, the initial conditions of bulk powder, and the piston speeds. Additional computational studies via Discrete Element Method simulations offered a better understanding of the feeding process, its possible limitations and ways to overcome them. The powder pump is a simple yet valuable tool for accurate powder feeding at feed rates of several orders of magnitude. Copyright © 2016 Elsevier B.V. All rights reserved.

Dysprosium-free melt-spun permanent magnets.

PubMed

Brown, D N; Wu, Z; He, F; Miller, D J; Herchenroeder, J W

2014-02-12

Melt-spun NdFeB powders can be formed into a number of different types of permanent magnet for a variety of applications in electronics, automotive and clean technology industries. The melt-spinning process produces flake powder with a fine uniform array of nanoscale Nd2Fe14B grains. These powders can be net-shape formed into isotropic polymer-bonded magnets or hot formed into fully dense magnets. This paper discusses the influence of heavy rare earth elements and microstructure on the magnetic performance, thermal stability and material cost of NdFeB magnets. Evidence indicates that melt-spun nanocrystalline NdFeB magnets are less dependent on heavy rare earth elements for high-temperature performance than the alternative coarser-grained sintered NdFeB magnets. In particular, hot-pressed melt-spun magnets are an attractive low-cost solution for applications that require thermal stability up to 175-200 °C.

Effect of Sintering Atmosphere and Solution Treatment on Density, Microstructure and Tensile Properties of Duplex Stainless Steels Developed from Pre-alloyed Powders

NASA Astrophysics Data System (ADS)

Murali, Arun Prasad; Mahendran, Sudhahar; Ramajayam, Mariappan; Ganesan, Dharmalingam; Chinnaraj, Raj Kumar

2017-10-01

In this research, Powder Metallurgy (P/M) of Duplex Stainless Steels (DSS) of different compositions were prepared through pre-alloyed powders and elemental powders with and without addition of copper. The powder mix was developed by pot mill for 12 h to obtain the homogeneous mixture of pre-alloyed powder with elemental compositions. Cylindrical green compacts with the dimensions of 30 mm diameter and 12 mm height were compacted through universal testing machine at a pressure level of 560 ± 10 MPa. These green compacts were sintered at 1350 °C for 2 h in hydrogen and argon atmospheres. Some of the sintered stainless steel preforms were solution treated at 1050 °C followed by water quenching. The sintered as well as solution treated samples were analysed by metallography examination, Scanning Electron Microscopy and evaluation of mechanical properties. Ferrite content of sintered and solution treated DSS were measured by Fischer Ferritoscope. It is inferred that the hydrogen sintered DSS depicted better density (94% theoretical density) and tensile strength (695 MPa) than the argon sintered steels. Similarly the microstructure of solution treated DSS revealed existence of more volume of ferrite grains than its sintered condition. Solution treated hydrogen sintered DSS A (50 wt% 316L + 50 wt% 430L) exhibited higher tensile strength of 716 MPa and elongation of 17%, which are 10-13% increment than the sintered stainless steels.

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

Rabin, S.A.; Martin, M.M.; Lotts, A.L.

The fabricability of dispersion fuels using UO/sub 2/ or UC as the dispersoid and uranium combined with 10 to 15 wt% Mo as the matrix was investigated. Cores containing l7.8 wt% UO/sub 2/ dispersed in U-- 15 wt.% Mo were successfully fabricated to about 80% of theoretical density by cold pressing at 50 tsi, sintering at 1100 deg C, and cold coining at 50 tsi. Comparable results were obtained with UC as the dispersoid. Core fabrication results varied greatly with the type of matrix powder used. Occluded gases, pour density, and surface cleanliness bore important relations to the fabrication behaviormore » of powders. Suitable pressing and sintering results were obtained with prealloyed, calcium-reduced U--Mo powder and with molybdenum and calcium-reduced uranium as elemental powders. Shotted prealloyed powders were difficult to press and sinter, as were elemental and prealloyed powders prepared by hydriding. The cores containing UO/sub 2/ were picture-frame, hot-roll-clad as miniature plates. Molybdenum, Fansteel 82, and Zr--3 wt% Al were investigated as cladding materials. While each bonded well to itself, only the molybdenum-clad core, rolled at 1150 deg C to 10/1 reduction, resulted in dispersions free of ruptures and UO/sub 2/ fragmentation and in strong bonding to the core, evaluated by metallography, mechanical peel, and thermal shock tests. The matrix phase was homogeneous, but the UO/sub 2/ dispersoid showed stringering characteristic of cores worked by hot rolling. Core densities as high as 99% of theoretical were obtained. (auth)« less

Nitrogen doped microporous carbon by ZnCl2 activation of protein

NASA Astrophysics Data System (ADS)

Wilson, Praveen; Vijayan, Sujith; Prabhakaran, K.

2017-09-01

ZnCl2 activation of protein containing biomass has been studied for the preparation of N-doped activated carbon (NDC) using powdered dry fish as a source of protein. Nearly 52% increase in the yield of NDC is observed by activation with ZnCl2 due to an increase in the thermal stability of Zn2+-fish protein complex compared to the protein alone. The NDCs obtained are characterized by XRD, IR, XPS, Raman spectroscopy, SEM, TEM, elemental analysis and N2 adsorption-desorption studies. The activation at 550 °C produces NDC with the highest surface area and total pore volume of 1001 m2 g-1 and 0.719 cm3 g-1, respectively, at a ZnCl2 to fish powder weight ratio of 3. A maximum micropore volume of 0.273 cm3 g-1 is obtained at a ZnCl2 to fish powder weight ratio of 1:1. The N-content (12.4-5.2 wt%) decreases with an increase in activation temperature and ZnCl2 to fish powder weight ratio. The NDC obtained by activation at 550 °C at a ZnCl2 to fish powder weight ratio of 1:1 shows the maximum CO2 adsorption capacity of 2.4 and 3.73 mmol g-1 at 25 and 0 °C, respectively, at 1 atmosphere. The CO2 adsorption on the NDC shows excellent cyclic stability and high selectivity over nitrogen gas.

Influence of ammonium hydroxide solution on LiMn2O4 nanostructures prepared by modified chemical bath method

NASA Astrophysics Data System (ADS)

Koao, Lehlohonolo F.; Motloung, Setumo V.; Motaung, Tshwafo E.; Kebede, Mesfin A.

2018-04-01

LiMn2O4 (LMO) powders were prepared by modified chemical bath deposition (CBD) method by varying ammonium hydroxide solution (AHS). The volume of the AHS was varied from 5 to 120 mL in order to determine the optimum volume that is needed for preparation of LMO powders. The effect of AHS volume on the structure, morphology, and electrochemical properties of LMO powders was investigated. The X-ray diffraction (XRD) patterns of the LMO powders correspond to the cubic spinel LMO phase. It was found that the XRD peaks increased in intensity with increasing volume of the AHS up to 20 mL. The estimated average grain sizes calculated using the XRD patterns were found to be in the order of 66 ± 1 nm. It was observed that the estimated average grain sizes increased up to 20 mL of AHS. The scanning electron microscopy (SEM) results revealed that the AHS volume does not influence the surface morphology of the prepared nano-powders. Elemental energy dispersive (EDS) analysis mapping conducted on the samples revealed homogeneous distribution of Mn and O for the sample synthesized with 120 mL of AHS. The UV-Vis spectra showed a red shift with an increase in AHS up 20 mL. The cyclic voltammetry and galvanostatic charge/discharge cycle testing confirmed that 20 mL of AHS has superior lithium ion kinetics and electrochemical performance.

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.

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.

Synthesis and characterization of a prominent NLO active MOF of lead with 1,5-naphthalenedisulfonic acid

NASA Astrophysics Data System (ADS)

Prasad, S. Shibu; Sudarsanakumar, M. R.; Dhanya, V. S.; Suma, S.; Kurup, M. R. Prathapachandra

2018-09-01

A new metal-organic framework of lead, [Pb(1,5-nds)(H2O)3]n (1,5-nds = 1,5-naphthalenedisulfonate) having prominent nonlinear optical property has been prepared by single gel diffusion technique at ambient condition using sodium metasilicate. The second harmonic generation efficiency was analyzed using Kurtz and Perry powder method and was found to be 30 times as large as potassium dihydrogen phosphate (KDP). Single crystal X-ray diffraction studies reveal the crystal structure. The grown crystals were further characterized by elemental analysis, powder XRD study, thermogravimetry, FT-IR and UV-visible spectral studies. The Pb2S2O4 rings in the crystal structure form a 1D channel. Hydrogen bonding and π-π interactions provide additional stability to the compound. Photoluminescence studies were also carried out.

A novel specimen-preparing method using epoxy resin as binding material for LIBS analysis of powder samples.

PubMed

Shi, Linli; Lin, Qingyu; Duan, Yixiang

2015-11-01

In view of the inevitable preprocessing of powder samples for LIBS detection, epoxy resin glue was investigated for the first time as a binder of powder samples due to its superior property of improved performance in laser induced breakdown spectroscopy (LIBS) technique as a quantitative analytical tool. For comparative studies of the epoxy resin and traditional polyethylene (PE) pellets in soil, sample detection, the signal intensities of Fe (I) at 404.58 nm, Ca (I) at 443.57 nm, and Cr (I) at 453.52 nm, were studied and subsequently, the calibration curves for these elements were constructed using the standard samples with variable concentrations. The signal intensities of epoxy resin samples were, on average, about 2 times greater than those obtained with the traditional PE pellet samples. Meanwhile, the resin samples showed better R square values of 0.981, 0.985 and 0.979 for curves of Fe (I) 404.58 nm, Ca (I) 443.57 nm, and Cr (I) 453.52 nm, compared to the 0.974, 0.950 and 0.934, of the PE pellet samples. Furthermore, the former represented lower limits of detection (LOD) for Fe, Ca and Cr. These experimental results indicated that this proposed novel method based on epoxy resin can attach samples of properties of high homogeneity, cohesiveness, smoothness and hardness, which are conducive to system stability, testing accuracy and signal enhancement. This method can make LIBS more practical in powder sample analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Extraction and Physicochemical Characterization of a New Polysaccharide Obtained from the Fresh Fruits of Abelmoschus Esculentus

PubMed Central

Emeje, Martins; Isimi, Christiana; Byrn, Stephen; Fortunak, Joseph; Kunle, Olobayo; Ofoefule, Sabinus

2011-01-01

This paper is the first multi-scale characterization of the fluidize-dried gum extracted from the fresh fruits of the plant Abelmoschus esculentus. It describes the physical, thermal, sorptional and functional properties of this natural gum. Elemental analysis, scanning electron microscopy (SEM), particle size analysis, X-ray powder diffraction (XPRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transmittance infra red (FT-IR), and nuclear magnetic resonance (NMR) spectroscopy were used to characterize the gum sample. Abelmoschus Esculentus Gum (AEG) had a glass transition temperature (Tg) of 70°C and no melting peak. It showed a 14.91% loss in weight at 195°C. X-ray diffractogram showed numerous broad halos for AEG. Elemental analysis showed that AEG contains 39.5, 7.3, 51.8, and 1.4% carbon, hydrogen, oxygen and nitrogen respectively. The results obtained in this study established the fundamental characteristics of AEG and suggests its potential application in the food, cosmetic and pharmaceutical sectors. PMID:24250349

Thermal analysis, phase equilibria, and superconducting properties in magnesium boride and carbon doped magnesium boride

NASA Astrophysics Data System (ADS)

Bohnenstiehl, Scot David

In this work, the low temperature synthesis of MgB2 from Mg/B and MgH2/B powder mixtures was studied using Differential Scanning Calorimetry (DSC). For the Mg/B powder mixture, two exothermic reaction events were observed and the first reaction event was initiated by the decomposition of Mg(OH)2 on the surface of the magnesium powder. For the MgH 2/B powder mixture, there was an endothermic event at ˜375 °C (the decomposition of MgH2 into H2 and Mg) and an exothermic event ˜600 °C (the reaction of Mg and B). The Kissinger analysis method was used to estimate the apparent activation energy of the Mg and B reaction using DSC data with different furnace ramp rates. The limitations of MgB2 low temperature synthesis led to the development of a high pressure induction furnace that was constructed using a pressure vessel and an induction heating power supply. The purpose was to not only synthesize more homogeneous MgB2 samples, but also to determine whether MgB2 melts congruently or incongruently. A custom implementation of the Smith Thermal Analysis method was developed and tested on aluminum and AlB2, the closest analogue to MgB2. Measurements on MgB2 powder and a high purity Mg/B elemental mixture confirmed that MgB2 melts incongruently and decomposes into a liquid and MgB4 at ˜1445 °C at 10 MPa via peritectic decomposition. Another measurement using a Mg/B elemental mixture with impure boron suggested that ˜0.7 wt% carbon impurity in the boron raised the incongruent melting temperature to ˜1490-1500 °C. Lastly, the solubility limit for carbon in MgB2 was studied by making samples from B4C and Mg at 1530 °C, 1600 °C and 1700 °C in the high pressure furnace. All three samples had three phases: Mg, MgB2C2, and carbon doped MgB2. The MgB 2C2 and carbon doped MgB2 grain size increased with temperature and the 1700 °C sample had needle-like grains for both phases. The presence of the ternary phase, MgB2C2, suggested that the maximum doping limit for carbon in MgB2 had been reached. The 1530 °C sample was characterized by Electron Probe Microanalysis at the University of Oregon and the average carbon concentration was estimated to be ˜5.9 at%. Further investigation using TEM found MgO inclusions in the 1530 °C sample which were not detected with X-ray diffraction.

Ir-based refractory superalloys by pulse electric current sintering (PECS) process (II prealloyed powder)

NASA Astrophysics Data System (ADS)

Huang, C.; Yamabe-Mitarai, Y.; Harada, H.

2002-02-01

Five prealloyed powder samples prepared from binary Ir-based refractory superalloys were sintered at 1800 °C for 4 h by Pulse Electric Current Sintering (PECS). No metal loss was observed during sintering. The relative densities of the sintered specimens all exceeded 90% T.D. The best one was Ir-13% Hf with the density of 97.82% T.D. Phases detected in sintered samples were in accordance with the phase diagram as expected. Fractured surfaces were observed in two samples (Ir-13% Hf and Ir-15% Zr). Some improvements obtained by using prealloyed powders instead of elemental powders, which were investigated in the previous studies, were presented.

40 KG Sample of Fish-Clay from Stevns Klint, Denmark

NASA Astrophysics Data System (ADS)

Gwozdz, R.; Hansen, H. J.; Rasmussen, K. L.

1992-07-01

In March 1986 a 50-m-long exposure of the cliff at Stevns Klint fell down and exposed about 40 square meters of Fish Clay. Due to this extraordinary event we were able to pick by hand about 50 kg black KT boundary layer material. After drying, the material was homogenized using a wooden pestle and an agate mortar. The powdered material was sieved through 200 mesh nylon gauze. The fraction larger than 200 mesh was collected and powdered again in an agate mortar. After four repetitions the amount of material with grain size less than 200 mesh was about 40 kg. The fraction larger than 200 mesh was reduced to about 7 kg. The 40-kg powder was mixed in a rotating polyethylene drum for three weeks. The material was analyzed by instrumental neutron activation analysis, atomic absorption and X-ray fluorescence analysis for about 40 elements. INAA was made on 20 aliquots with weight about 300 mg, 20 aliquots with weight about 80 mg, and 30 with weights between 10 and 20 mg. The preliminary results show that our KT boundary sample (1) is very homogeneous, (2) is very close in composition to other K-T boundary clays analyzed by us or described in the literature, and (3) has an Ir concentration of 32 +- 2 ng/g. We hope that our Fish Clay sample (termed by us "Mesozoic Midnight") after analysis in other laboratories and by other analytical methods may qualify as reference material in analytical work on boundary clay material.

MTA-enriched nanocomposite TiO(2)-polymeric powder coatings support human mesenchymal cell attachment and growth.

PubMed

Shi, Wen; Mozumder, Mohammad Sayem; Zhang, Hui; Zhu, Jesse; Perinpanayagam, Hiran

2012-10-01

The objective of the study described in this paper was the development of novel polymer/ceramic nanocomposite coatings for implants through the application of ultrafine powder coating technology. Polyester resins were combined with µm-sized TiO(2) (25%) as the biocompatibility agent, nTiO(2) (0.5%) as the flow additive and mineral trioxide aggregates (ProRoot® MTA, 5%) as bioactive ceramics. Ultrafine powders were prepared and applied to titanium to create continuous polymeric powder coatings (PPCs) through the application of electrostatic ultrafine powder coating technology. Energy dispersive x-ray analysis confirmed that MTA had been incorporated into the PPCs, and elemental mapping showed that it had formed small clusters that were evenly distributed across the surface. Scanning electron microscopy (SEM) revealed continuous and smooth, but highly textured surface coatings that contrasted with the scalloped appearance of commercially pure titanium (cpTi) controls. Atomic force microscopy revealed intricate nano-topographies with an abundance of submicron-sized pits and nano-projections, evenly dispersed across their surfaces. Inverted fluorescence microscopy, SEM and cell counts showed that human embryonic palatal mesenchymal cells attached and spread out onto PPC and MTA-enriched PPCs within 24 h. Mitochondrial enzyme activity measured viable and metabolically active cells on all of the surfaces. After 72 h of growth, cell counts and metabolic activity were significantly higher (P < 0.05) on the grey-MTA enriched PPC surfaces, than on unmodified PPC and cpTi. The novel polymer/ceramic nanocomposites that were created with ultrafine powder coating technology were continuous, homogenous and nano-rough coatings that enhanced human mesenchymal cell attachment and growth.

A hydrometallurgical process for the recovery of terbium from fluorescent lamps: Experimental design, optimization of acid leaching process and process analysis.

PubMed

Innocenzi, Valentina; Ippolito, Nicolò Maria; De Michelis, Ida; Medici, Franco; Vegliò, Francesco

2016-12-15

Terbium and rare earths recovery from fluorescent powders of exhausted lamps by acid leaching with hydrochloric acid was the objective of this study. In order to investigate the factors affecting leaching a series of experiments was performed in according to a full factorial plan with four variables and two levels (4 2 ). The factors studied were temperature, concentration of acid, pulp density and leaching time. Experimental conditions of terbium dissolution were optimized by statistical analysis. The results showed that temperature and pulp density were significant with a positive and negative effect, respectively. The empirical mathematical model deducted by experimental data demonstrated that terbium content was completely dissolved under the following conditions: 90 °C, 2 M hydrochloric acid and 5% of pulp density; while when the pulp density was 15% an extraction of 83% could be obtained at 90 °C and 5 M hydrochloric acid. Finally a flow sheet for the recovery of rare earth elements was proposed. The process was tested and simulated by commercial software for the chemical processes. The mass balance of the process was calculated: from 1 ton of initial powder it was possible to obtain around 160 kg of a concentrate of rare earths having a purity of 99%. The main rare earths elements in the final product was yttrium oxide (86.43%) following by cerium oxide (4.11%), lanthanum oxide (3.18%), europium oxide (3.08%) and terbium oxide (2.20%). The estimated total recovery of the rare earths elements was around 70% for yttrium and europium and 80% for the other rare earths. Copyright © 2016 Elsevier Ltd. 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.

Uranium in NIMROC standard igneous rock samples

NASA Technical Reports Server (NTRS)

Rowe, M. W.; Herndon, J. M.

1976-01-01

Results are reported for analysis of the uranium in multiple samples of each of six igneous-rock standards (dunite, granite, lujavrite, norite, pyroxenite, and syenite) prepared as geochemical reference standards for elemental and isotopic compositions. Powdered rock samples were examined by measuring delayed neutron emission after irradiation with a flux of the order of 10 to the 13th power neutrons/sq cm per sec in a nuclear reactor. The measurements are shown to compare quite favorably with previous uranium determinations for other standard rock samples.

Porosity and mechanical properties of zirconium ceramics

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

Buyakova, S., E-mail: sbuyakova@ispms.tsc.ru; Kulkov, S.; Tomsk Polytechnic University

2015-11-17

Has been studied a porous ceramics obtained from ultra-fine powders. Porous ceramic ZrO{sub 2}(MgO), ZrO{sub 2}(Y{sub 2}O{sub 3}) powder was prepared by pressing and subsequent sintering of compacts homologous temperatures ranging from 0.63 to 0.56 during the isothermal holding duration of 1 to 5 hours. The porosity of ceramic samples was from 15 to 80%. The structure of the ceramic materials produced from plasma-sprayed ZrO{sub 2} powder was represented as a system of cell and rod structure elements. Cellular structure formed by stacking hollow powder particles can be easily seen at the images of fracture surfaces of obtained ceramics. Theremore » were three types of pores in ceramics: large cellular hollow spaces, small interparticle pores which are not filled with powder particles and the smallest pores in the shells of cells. The cells generally did not have regular shapes. The size of the interior of the cells many times exceeded the thickness of the walls which was a single-layer packing of ZrO{sub 2} grains. A distinctive feature of all deformation diagrams obtained in the experiment was their nonlinearity at low deformations which was described by the parabolic law. It was shown that the observed nonlinear elasticity for low deformation on deformation diagrams is due to mechanical instability of the cellular elements in the ceramic carcass.« less

Method of manufacturing metallic products such as sheet by cold working and flash anealing

DOEpatents

Hajaligol, Mohammad R.; Sikka, Vinod K.

2001-01-01

A metallic alloy composition is manufactured into products such as press formed or stamped products or rolled products such as sheet, strip, rod, wire or band by one or more cold working steps with intermediate or final flash annealing. The method can include cold rolling an iron, nickel or titanium aluminide alloy and annealing the cold worked product in a furnace by infrared heating. The flash annealing is preferably carried out by rapidly heating the cold worked product to an elevated temperature for less than one minute. The flash annealing is effective to reduce surface hardness of the cold worked product sufficiently to allow further cold working. The product to be cold worked can be prepared by casting the alloy or by a powder metallurgical technique such as tape casting a mixture of metal powder and a binder, roll compacting a mixture of the powder and a binder or plasma spraying the powder onto a substrate. In the case of tape casting or roll compaction, the initial powder product can be heated to a temperature sufficient to remove volatile components. The method can be used to form a cold rolled sheet which is formed into an electrical resistance heating element capable of heating to 900.degree. C. in less than 1 second when a voltage up to 10 volts and up to 6 amps is passed through the heating element.

Method of manufacturing metallic products such as sheet by cold working and flash annealing

DOEpatents

Hajaligol, Mohammad R.; Sikka, Vinod K.

2000-01-01

A metallic alloy composition is manufactured into products such as press formed or stamped products or rolled products such as sheet, strip, rod, wire or band by one or more cold working steps with intermediate or final flash annealing. The method can include cold rolling an iron, nickel or titanium aluminide alloy and annealing the cold worked product in a furnace by infrared heating. The flash annealing is preferably carried out by rapidly heating the cold worked product to an elevated temperature for less than one minute. The flash annealing is effective to reduce surface hardness of the cold worked product sufficiently to allow further cold working. The product to be cold worked can be prepared by casting the alloy or by a powder metallurgical technique such as tape casting a mixture of metal powder and a binder, roll compacting a mixture of the powder and a binder or plasma spraying the powder onto a substrate. In the case of tape casting or roll compaction, the initial powder product can be heated to a temperature sufficient to remove volatile components. The method can be used to form a cold rolled sheet which is formed into an electrical resistance heating element capable of heating to 900.degree. C. in less than 1 second when a voltage up to 10 volts and up to 6 amps is passed through the heating element.

Use of sol-gels as solid matrixes for simultaneous multielement determination by radio frequency glow discharge optical emission spectrometry: determinations of suspended particulate matter.

PubMed

Davis, W Clay; Knippel, Brad C; Cooper, Julia E; Spraul, Bryan K; Rice, Jeanette K; Smith, Dennis W; Marcus, R Kenneth

2003-05-15

A new approach for the analysis of particulate matter by radio frequency glow discharge optical emission spectrometry (rf-GD-OES) is described. Dispersion of the particles in a sol-gel sample matrix provides a convenient means of generating a thin film suitable for sputter-sampling into the discharge. Acid-catalyzed sol-gel glasses synthesized from tetramethyl orthosilicate were prepared and spun-cast on glass substrates. The resultant thin films on glass substrates were analyzed to determine the discharge operating conditions and resultant sputtering characteristics while a number of optical emission lines of the film components were monitored. Slurries of powdered standard reference materials NIST SRM 1884a (Portland Cement) and NIST SRM 2690 (Coal Fly Ash) dispersed in the sols were cast into films in the same manner. Use of the sol-gels as sample matrixes allows for background subtraction through the use of analytical blanks and may facilitate the generation of calibration curves via readily synthesized, matrix-matched analytical standards in solids analysis. Detection limits were determined for minor elements via the RSDB method to be in the range of 1-10 microg/g in Portland Cement and Coal Fly Ash samples for the elements Al, Fe, Mg, S, and Si. Values for Ca were in the range of 15-35 microg/g. This preliminary study demonstrates the possibility of incorporating various insoluble species, including ceramics and geological specimens in powder form, into a solid matrix for further analysis by either rf-GD-OES or MS.

Mineral contents and their solubility on calcium carbonat calcite nanocrystals from cockle shell powder (Anadara granosa Linn)

NASA Astrophysics Data System (ADS)

Widyastuti, S.; Pramushinta, I. A.

2018-03-01

Prepared and characterized calcium carbonat calcite nanocrystals improves solubility. Calcium carbonat calcite nanocrystals were synthesized using precipitation method from the waste of blood clam cockle shells (Anadara granosa Linn). This study was conducted to analyze mineral composition of nanocrystals calcium carbonat calcite cockle (Anadara granosa) shell for calcium fortification of food applications and to evaluate the solubilities of Calsium and Phospor. The sample of nanocrystals from cockle shells was evaluated to determine the content of 11 macro-and micro-elements. These elements are Calcium (Ca), Magnesium (Mg), Sodium (Na), Phosphorus (P), Potassium (K), Ferrum (Fe), Copper (Cu), Nickel (Ni), Zink (Zn), Boron (B) and Silica (Si)). Cockleshell powders were found to contain toxic elements below detectable levels. The solubilities of Calcium and Phospor were p<0.05.

Macroscopic X-ray Powder Diffraction Scanning: Possibilities for Quantitative and Depth-Selective Parchment Analysis.

PubMed

Vanmeert, Frederik; De Nolf, Wout; Dik, Joris; Janssens, Koen

2018-06-05

At or below the surface of painted works of art, valuable information is present that provides insights into an object's past, such as the artist's technique and the creative process that was followed or its conservation history but also on its current state of preservation. Various noninvasive techniques have been developed over the past 2 decades that can probe this information either locally (via point analysis) or on a macroscopic scale (e.g., full-field imaging and raster scanning). Recently macroscopic X-ray powder diffraction (MA-XRPD) mapping using laboratory X-ray sources was developed. This method can visualize highly specific chemical distributions at the macroscale (dm 2 ). In this work we demonstrate the synergy between the quantitative aspects of powder diffraction and the noninvasive scanning capability of MA-XRPD highlighting the potential of the method to reveal new types of information. Quantitative data derived from a 15th/16th century illuminated sheet of parchment revealed three lead white pigments with different hydrocerussite-cerussite compositions in specific pictorial elements, while quantification analysis of impurities in the blue azurite pigment revealed two distinct azurite types: one rich in barite and one in quartz. Furthermore, on the same artifact, the depth-selective possibilities of the method that stem from an exploitation of the shift of the measured diffraction peaks with respect to reference data are highlighted. The influence of different experimental parameters on the depth-selective analysis results is briefly discussed. Promising stratigraphic information could be obtained, even though the analysis is hampered by not completely understood variations in the unit cell dimensions of the crystalline pigment phases.

Single-step solubilization of milk samples with N,N-dimethylformamide for inductively coupled plasma-mass spectrometry analysis and classification based on their elemental composition.

PubMed

Azcarate, Silvana M; Savio, Marianela; Smichowski, Patricia; Martinez, Luis D; Camiña, José M; Gil, Raúl A

2015-10-01

A single-step procedure for trace elements analysis of milk samples is presented. Solubilization with small amounts of dymethylformamide (DMF) was assayed prior to inductively coupled plasma mass spectrometry (ICPMS) detection with a high efficiency sample introduction system. All main instrumental conditions were optimized in order to readily introduce the samples without matrix elimination. In order to assess and mitigate matrix effects in the determination of As, Cd, Co, Cu, Eu, Ga, Gd, Ge, Mn, Mo, Nb, Nd, Ni, Pb, Pr, Rb, Sm, S, Sr, Ta, Tb, V, Zn, and Zr, matrix matching calibration with (103)Rh as internal standard (IS) was performed. The obtained limits of detection were between 0.68 (Tb) and 30 (Zn) μg L(-1). For accuracy verification, certified Skim milk powder reference material (BCR 063R) was employed. The developed method was applied to trace elements analysis of commercially available milks. Principal components analysis was used to correlate the content of trace metals with the kind of milk, obtaining a classification according to adults, baby or baby fortified milks. The outcomes highlight a simple and fast approach that could be trustworthy for routine analysis, quality control and traceability of milks. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Additive Manufacturing of Nickel-Base Superalloy IN100 Through Scanning Laser Epitaxy

NASA Astrophysics Data System (ADS)

Basak, Amrita; Das, Suman

2018-01-01

Scanning laser epitaxy (SLE) is a laser powder bed fusion (LPBF)-based additive manufacturing process that uses a high-power laser to consolidate metal powders facilitating the fabrication of three-dimensional objects. In the present study, SLE is used to produce samples of IN100, a high-γ' non-weldable nickel-base superalloy on similar chemistry substrates. A thorough analysis is performed using various advanced material characterization techniques such as high-resolution optical microscopy, scanning electron microscopy, energy dispersive x-ray spectroscopy, and Vickers microhardness measurements to characterize and compare the quality of the SLE-fabricated IN100 deposits with the investment cast IN100 substrates. The results show that the IN100 deposits have a finer γ/γ' microstructure, weaker elemental segregation, and higher microhardness compared with the substrate. Through this study, it is demonstrated that the SLE process has tremendous potential in the repair and manufacture of gas turbine hot-section components.

Preparation of cermets

DOEpatents

Morgan, Chester S.

1978-01-01

Cermets are produced by the process of forming a physical mixture of a ceramic powder material with an elemental metal precursor compound and by decomposing the elemental metal precursor compound within the mixture. The decomposition step may be carried out either prior to or during a forming and densification step.

Application of powder metallurgy techniques to produce improved bearing elements for liquid rocket engines

NASA Technical Reports Server (NTRS)

Moracz, D. J.; Shipley, R. J.; Moxson, V. S.; Killman, R. J.; Munson, H. E.

1992-01-01

The objective was to apply powder metallurgy techniques for the production of improved bearing elements, specifically balls and races, for advanced cryogenic turbopump bearings. The materials and fabrication techniques evaluated were judged on the basis of their ability to improve fatigue life, wear resistance, and corrosion resistance of Space Shuttle Main Engine (SSME) propellant bearings over the currently used 440C. An extensive list of candidate bearing alloys in five different categories was considered: tool/die steels, through hardened stainless steels, cobalt-base alloys, and gear steels. Testing of alloys for final consideration included hardness, rolling contact fatigue, cross cylinder wear, elevated temperature wear, room and cryogenic fracture toughness, stress corrosion cracking, and five-ball (rolling-sliding element) testing. Results of the program indicated two alloys that showed promise for improved bearing elements. These alloys were MRC-2001 and X-405. 57mm bearings were fabricated from the MRC-2001 alloy for further actual hardware rig testing by NASA-MSFC.

Determination of refractive and volatile elements in sediment using laser ablation inductively coupled plasma mass spectrometry.

PubMed

Duodu, Godfred Odame; Goonetilleke, Ashantha; Allen, Charlotte; Ayoko, Godwin A

2015-10-22

Wet-milling protocol was employed to produce pressed powder tablets with excellent cohesion and homogeneity suitable for laser ablation (LA) analysis of volatile and refractive elements in sediment. The influence of sample preparation on analytical performance was also investigated, including sample homogeneity, accuracy and limit of detection. Milling in volatile solvent for 40 min ensured sample is well mixed and could reasonably recover both volatile (Hg) and refractive (Zr) elements. With the exception of Cr (-52%) and Nb (+26%) major, minor and trace elements in STSD-1 and MESS-3 could be analysed within ±20% of the certified values. Comparison of the method with total digestion method using HF was tested by analysing 10 different sediment samples. The laser method recovers significantly higher amounts of analytes such as Ag, Cd, Sn and Sn than the total digestion method making it a more robust method for elements across the periodic table. LA-ICP-MS also eliminates the interferences from chemical reagents as well as the health and safety risks associated with digestion processes. Therefore, it can be considered as an enhanced method for the analysis of heterogeneous matrices such as river sediments. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Tungsten carbide precursors as an example for influence of a binder on the particle formation in the nanosecond laser ablation of powdered materials.

PubMed

Holá, Markéta; Mikuska, Pavel; Hanzlíková, Renáta; Kaiser, Jozef; Kanický, Viktor

2010-03-15

A study of LA-ICP-MS analysis of pressed powdered tungsten carbide precursors was performed to show the advantages and problems of nanosecond laser ablation of matrix-unified samples. Five samples with different compositions were pressed into pellets both with silver powder as a binder serving to keep the matrix unified, and without any binder. The laser ablation was performed by nanosecond Nd:YAG laser working at 213 nm. The particle formation during ablation of both sets of pellets was studied using an optical aerosol spectrometer allowing the measurement of particle concentration in two size ranges (10-250 nm and 0.25-17 microm) and particle size distribution in the range of 0.25-17 microm. Additionally, the structure of the laser-generated particles was studied after their collection on a filter using a scanning electron microscope (SEM) and the particle chemical composition was determined by an energy dispersive X-ray spectroscope (EDS). The matrix effect was proved to be reduced using the same silver powdered binder for pellet preparation in the case of the laser ablation of powdered materials. The LA-ICP-MS signal dependence on the element content present in the material showed an improved correlation for Co, Ti, Ta and Nb of the matrix-unified samples compared to the non-matrix-unified pellets. In the case of W, the ICP-MS signal of matrix-unified pellets was influenced by the changes in the particle formation. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Modelling of the rotational moulding process for the manufacture of plastic products

NASA Astrophysics Data System (ADS)

Khoon, Lim Kok

The present research is mainly focused on two-dimensional non-linear thermal modelling, numerical procedures and software development for the rotational moulding process. The RotoFEM program is developed for the rotational moulding process using finite element procedures. The program is written in the MATLAB environment. The research includes the development of new slip flow models, phase change study, warpage study and process analyses. A new slip flow methodology is derived for the heat transfer problem inside the enclosed rotating mould during the heating stage of the tumbling powder. The methodology enables the discontinuous powder to be modelled by the continuous-based finite element method. The Galerkin Finite Element Method is incorporated with the lumped-parameter system and the coincident node technique in finding the multi-interacting heat transfer solutions inside the mould. Two slip flow models arise from the slip flow methodology; they are SDM (single-layered deposition method) and MDM (multi-layered deposition method). These two models have differences in their thermal description for the internal air energy balance and the computational procedure for the deposition of the molten polymer. The SDM model assumes the macroscopic deposition of the molten polymer bed exists only between the bed and the inner mould surface. On the other hand, the MDM model allows the layer-by-layer deposition of the molten polymer bed macroscopically. In addition, the latter has a more detailed heat transfer description for the internal air inside the mould during the powder heating cycle. In slip flow models, the semi-implicit approach has been introduced to solve the final quasi-equilibrium internal air temperature during the heating cycle. A notable feature of this slip flow methodology is that the slip flow models are capable of producing good results for the internal air at the heating powder stage, without the consideration of the powder movement and changeable powder mass. This makes the modelling of the rotational moulding process much simpler. In the simulation of the cooling stage in rotational moulding, the thermal aspects of the inherent warpage problem and external-internal cooling method have been explored. The predicted internal air temperature profiles have shown that the less apparent crystallization plateau in the experimental internal air in practice could be related to warpage. Various phase change algorithms have been reviewed and compared, and thus the most convenient and considerable effective algorithm is proposed. The dimensional analysis method, expressed by means of dimensionless combinations of physical, boundary, and time variables, is utilized to study the dependence of the key thermal parameters on the processing times of rotational moulding. Lastly, the predicted results have been compared with the experimental results from two different external resources. The predicted temperature profiles of the internal air, oven times and other process conditions are consistent with the available data.

Solid-state studies and antioxidant properties of the γ-cyclodextrin·fisetin inclusion compound.

PubMed

Pais, Joana M; Barroca, Maria João; Marques, Maria Paula M; Almeida Paz, Filipe A; Braga, Susana S

2017-01-01

Fisetin is a natural antioxidant with a wide range of nutraceutical properties, including antidiabetic, neuroprotecting, and suppression or prevention of tumors. The present work describes the preparation of a water-soluble, solid inclusion compound of fisetin with gamma-cyclodextrin (γ-CD), a cyclic oligosaccharide approved for human consumption. A detailed physicochemical analysis of the product is carried out using elemental analysis, powder X-ray diffraction (PXRD), Raman, infrared and 13 C{ 1 H} CP-MAS NMR spectroscopies, and thermal analysis (TGA) to verify fisetin inclusion and to present a hypothetical structural arrangement for the host-guest units. The antioxidant activity of the γ-CD·fisetin inclusion compound is evaluated by the DPPH assay.

Thermal Plasma Spheroidization of High-Nitrogen Stainless Steel Powder Alloys Synthesized by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Razumov, Nikolay G.; Popovich, Anatoly A.; Wang, QingSheng

2018-03-01

This paper presents the results of experimental studies on the treatment of Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys, synthesized by the mechanical alloying (MA) of elemental powders in the flow of a thermal plasma. Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys were prepared by MA in the attritor under an argon atmosphere. For spheroidization of Fe-23Cr-11Mn-1N high-nitrogen stainless steel powder alloys, the TekSphero 15 plant manufactured by Tekna Plasma Systems Inc was used. The studies have shown the possibility of obtaining Fe-23Cr-11Mn-1N high-nitrogen spherical powders steel alloys from the powder obtained by MA. According to the results of a series of experiments, it was found that the results of plasma spheroidization of powders essentially depend on the size of the fraction due to some difference in the particle shape and flowability, and on the gas regime of the plasma torch. It is established that during the plasma spheroidization process, some of the nitrogen leaves the alloy. The loss rate of nitrogen depends on the size of the initial particles.

A Nonvolume Preserving Plasticity Theory with Applications to Powder Metallurgy

NASA Technical Reports Server (NTRS)

Cassenti, B. N.

1983-01-01

A plasticity theory has been developed to predict the mechanical response of powder metals during hot isostatic pressing. The theory parameters were obtained through an experimental program consisting of hydrostatic pressure tests, uniaxial compression and uniaxial tension tests. A nonlinear finite element code was modified to include the theory and the results of themodified code compared favorably to the results from a verification experiment.

Analysis of 3D printing parameters of gears for hybrid manufacturing

NASA Astrophysics Data System (ADS)

Budzik, Grzegorz; Przeszlowski, Łukasz; Wieczorowski, Michal; Rzucidlo, Arkadiusz; Gapinski, Bartosz; Krolczyk, Grzegorz

2018-05-01

The paper deals with analysis and selection of parameters of rapid prototyping of gears by selective sintering of metal powders. Presented results show wide spectrum of application of RP systems in manufacturing processes of machine elements, basing on analysis of market in term of application of additive manufacturing technology in different sectors of industry. Considerable growth of these methods over the past years can be observed. The characteristic errors of printed model with respect to ideal one for each technique were pointed out. Special attention was paid to the method of preparation of numerical data CAD/STL/RP. Moreover the analysis of manufacturing processes of gear type elements was presented. The tested gears were modeled with different allowances for final machining and made by DMLS. Metallographic analysis and strength tests on prepared specimens were performed. The above mentioned analysis and tests were used to compare the real properties of material with the nominal ones. To improve the quality of surface after sintering the gears were subjected to final machining. The analysis of geometry of gears after hybrid manufacturing method was performed (fig.1). The manufacturing process was defined in a traditional way as well as with the aid of modern manufacturing techniques. Methodology and obtained results can be used for other machine elements than gears and constitutes the general theory of production processes in rapid prototyping methods as well as in designing and implementation of production.

Thermoelectric materials having porosity

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

Heremans, Joseph P.; Jaworski, Christopher M.; Jovovic, Vladimir

A thermoelectric material and a method of making a thermoelectric material are provided. In certain embodiments, the thermoelectric material comprises at least 10 volume percent porosity. In some embodiments, the thermoelectric material has a zT greater than about 1.2 at a temperature of about 375 K. In some embodiments, the thermoelectric material comprises a topological thermoelectric material. In some embodiments, the thermoelectric material comprises a general composition of (Bi.sub.1-xSb.sub.x).sub.u(Te.sub.1-ySe.sub.y).sub.w, wherein 0.ltoreq.x.ltoreq.1, 0.ltoreq.y.ltoreq.1, 1.8.ltoreq.u.ltoreq.2.2, 2.8.ltoreq.w.ltoreq.3.2. In further embodiments, the thermoelectric material includes a compound having at least one group IV element and at least one group VI element. In certain embodiments,more » the method includes providing a powder comprising a thermoelectric composition, pressing the powder, and sintering the powder to form the thermoelectric material.« less

Mechanical properties and microstructural evolution of vacuum hot-pressed titanium and Ti-6Al-7Nb alloy.

PubMed

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

2012-05-01

Hot-pressing is a powder metallurgy process where loose powder is loaded into a mould, usually of graphite, and sintered by the simultaneous application of high temperature and pressure. In this study elemental titanium and Ti-6Al-7Nb alloy powders are hot-pressed under different conditions in order to study the influence of the processing parameters on the microstructure and mechanical properties. The samples are characterised in terms of relative density, microstructure, XRD, percentage of interstitials, three-point bending test and hardness. Relative densities as high as 99% are obtained, the oxygen and carbon content remains almost constant but nitrogen percentage increases. This is due to the interaction with the BN coated mould and leads to the formation of a reacted layer in the surface, composed by different titanium compounds, which greatly affect the mechanical properties. Nevertheless, the removal of this reacted layer leads to an important improvement of the ductility, especially for elemental titanium. Copyright © 2012 Elsevier Ltd. All rights reserved.

Chemical composition of core samples from Newark Basin, a potential carbon sequestration site

NASA Astrophysics Data System (ADS)

Seltzer, A. M.; Yang, Q.; Goldberg, D.

2012-12-01

Injection of carbon dioxide into deep saline aquifers has been identified as a promising mitigation option of greenhouse gases, the successful management of which is considered to be one of the most urgent and important challenges. Given the high energy production in the New York metropolitan area, the Newark Basin region is considered to be a potential future sequestration site. However, the risk of an upward leak of sequestered CO2, especially to a shallow drinking water aquifer, is a key concern facing geological sequestration as a safe and viable mitigation option. In this study, we measured the chemical composition of 25 cores from various depths throughout Newark Basin as a precursor for an ex situ incubation experiment using these rock samples and aquifer water to simulate a leak event. Inductively coupled plasma mass spectrometry analysis of microwave-assisted digested rock powders and X-ray fluorescence analysis of the rock powders were conducted to obtain the concentrations of major and trace elements. Most of the major and trace elements show wide concentration ranges at one to two orders of magnitude. Understanding the chemical composition of these Newark Basin core samples is important not only for characterizing materials used for the later lab incubation, but also for gaining a broader understanding of the chemistry of the Newark Basin and profiling the region according to the varying risks associated with a leak of sequestered CO2 to a drinking water aquifer.

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

Muth, Thomas R; Yamamoto, Yukinori; Frederick, David Alan

ORNL undertook an investigation 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 priormore » to consolidation. The removal / 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 to achieve equivalent fusion welding success similar to that seen in wrought titanium produced via the Kroll process.« less

Synthesis and characterization of TiC nanopowders via sol-gel and subsequent carbothermal reduction process

NASA Astrophysics Data System (ADS)

Chen, Xu; Fan, Jinglian; Lu, Qiong

2018-06-01

TiC nanocrystalline powders were synthesized by in-situ carbothermic reduction of Ti-O-C precursor under vacuum atmosphere. And the Ti-O-C precursor was formed by sol-gel method from titanium butyrate (TBOT) and sucrose. To obtain stable sol, TBOT was directly added into mixed solution which contains water, sucrose, acetic acid (AcOH) and acetylacetone (ACAC). This procedure is more convenient and economical because it avoids the use of alcohol which is used as solvent in most reports of alkoxide hydrolysis sol-gel method. TG-DSC, XRD, FTIR and SEM/TEM were employed to analyze and characterize the product during the entire process. The phase composition and crystalline structure parameters of powders with different C/Ti molar ratio were investigated by Rietveld refinement method, and elemental quantitative analysis of the samples were performed. Furthermore, the optimal parameters of carbothermal reduction were obtained and the grain growth mechanism was demonstrated. The results show that TiC nanocrystalline powders (C/Ti molar ratio is 3.5 in the precursor) were synthesized at 1300 °C for 2 h, which have near standard lattice parameter, well crystallinity and fine average grain size ( 37.4 nm).

METHOD OF PREPARING A FUEL ELEMENT FOR A NUCLEAR REACTOR

DOEpatents

Hauth, J.J.; Anicetti, R.J.

1962-12-01

A method is described for preparing a fuel element for a nuclear reactor. According to the patent uranium dioxide is compacted in a metal tabe by directlng intense sound waves at the tabe prior to tamp packing or vibration compaction of the powder. (AEC)

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.

Synthesis, crystal growth, structural, thermal and optical properties of naphthalene picrate an organic NLO material.

PubMed

Chandramohan, A; Bharathikannan, R; Kandavelu, V; Chandrasekaran, J; Kandhaswamy, M A

2008-12-01

Crystalline substance of naphthalene picrate (NP) was synthesized and single crystals were grown using slow evaporation solution growth technique. The solubility of the naphthalene picrate complex was estimated using different solvents such as chloroform and benzene. The material was characterized by elemental analysis, powder X-ray diffraction (XRD), nuclear magnetic resonance (NMR) and fourier transform-infrared (FT-IR) techniques. The electronic absorption was studied through UV-vis spectrophotometer. Thermal behavior and stability of the crystal were studied using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The second harmonic generation (SHG) of the material was confirmed using Nd:YAG laser.

Dry powder segregation and flowability: Experimental and numerical studies

NASA Astrophysics Data System (ADS)

Ely, David R.

Dry powder blending is a very important industrial and physical process used in the production of numerous pharmaceutical dosage forms such as tablets, capsules, and dry powder aerosols. Key aspects of this unit operation are process monitoring and control. Process control is particularly difficult due to the complexity of particle-particle interactions, which arise from the adhesion/cohesion characteristics of interfaces and morphological characteristics such as particle size, shape, and dispersity. The effects of such characteristics need to be understood in detail in order to correlate individual particle properties to bulk powder properties. The present dissertation numerically and experimentally quantifies the mixing process to rationalize particle-particle interactions. In particular, near infrared spectroscopy (NIRS) was used to non-invasively characterize in real-time the blending processes and thus investigate the dynamics of blending under different operating conditions. A novel image analysis technique was developed to quantify the scale of segregation from images obtained non-destructively via near infrared chemical imaging (NIR-CI). Although NIR-CI data acquisition times are too long for real-time data collection, NIR-CI has an advantage, in that it provides the spatial distribution of the drug. Therefore, NIRS and NIR-CI are complementary techniques for investigating the complex process of blending dry powders and assessing end-product quality. Additionally, the discrete element method was used to investigate the effect of powder cohesion on the packing fraction. Simulations indicated an exponential relationship between the random loose packing fraction and cohesive forces. Specifically, the packing fraction decreased asymptotically with increased ratio of cohesive force to particle weight. Thus, increasing this force ratio above a critical value has negligible impact on the packing fraction. Such result directly impacts the Hausner ratio flowability measurement, which is directly related to the packing fraction. Two commonly used tests were compared to assess their utility: the rotational split-cell shear cell test and the Hausner ratio. The Hausner ratio proved to be better suited for characterizing the flowability of unconsolidated powders than the splitring shear cell. Results demonstrate that the optimal flowability test depends on the powder properties and the environment under which flow will be induced.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

PubMed

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

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

Rai, R.N., E-mail: rn_rai@yahoo.co.in; Kant, Shiva; Reddi, R.S.B.

Urea is an attractive material for frequency conversion of high power lasers to UV (for wavelength down to 190 nm), but its usage is hindered due to its hygroscopic nature, though there is no alternative organic NLO crystal which could be transparent up to 190 nm. The hygroscopic character of urea has been modified by making the solid solution (UCNB) of urea (U) and p-chloronitrobenzene (CNB). The formation of the solid solution of CNB in U is explained on the basis of phase diagram, powder XRD, FTIR, elemental analysis and single crystal XRD studies. The solubility of U, CNB andmore » UCNB in ethanol solution is evaluated at different temperatures. Transparent single crystals of UCNB are grown from its saturated solution in ethanol. Optical properties e.g., second harmonic generation (SHG), refractive index and the band gap for UCNB crystal were measured and their values were compared with the parent compounds. Besides modification in hygroscopic nature, UCNB has also shown the higher SHG signal and mechanical hardness in comparison to urea crystal. - Highlights: • The hygroscopic character of urea was modified by making the solid solution • Solid solution formation is support by elemental, powder- and single crystal XRD • Crystal of solid solution has higher SHG signal and mechanical stability. • Refractive index and band gap of solid solution crystal have determined.« less

Development of Powder Processing Models and Techniques for Meso-scale Devices: Perspirable Skin

DTIC Science & Technology

2008-03-31

of Powder Processing Models and Techniques for Meso-scale Devices: Perspirable Skin Contract Number ...Skin 5a. CONTRACT NUMBER 5b. GRANT NUMBER FA9550-05-1-0202 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Patrick Kwon, Michigan State University 5d...PROJECT NUMBER 5e. TASK NUMBER 5f. WORK UNIT NUMBER 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) Patrick Kwon Department of

FUEL COMPOSITION FOR NUCLEAR REACTORS

DOEpatents

Andersen, J.C.

1963-08-01

A process for making refractory nuclear fuel elements involves heating uranium and silicon powders in an inert atmosphere to 1600 to 1800 deg C to form USi/sub 3/; adding silicon carbide, carbon, 15% by weight of nickel and aluminum, and possibly also molybdenum and silicon powders; shaping the mixture; and heating to 1700 to 2050 deg C again in an inert atmosphere. Information on obtaining specific compositions is included. (AEC)

PROCESS OF FORMING POWDERED MATERIAL

DOEpatents

Glatter, J.; Schaner, B.E.

1961-07-14

A process of forming high-density compacts of a powdered ceramic material is described by agglomerating the powdered ceramic material with a heat- decompossble binder, adding a heat-decompossble lubricant to the agglomerated material, placing a quantity of the material into a die cavity, pressing the material to form a compact, pretreating the compacts in a nonoxidizing atmosphere to remove the binder and lubricant, and sintering the compacts. When this process is used for making nuclear reactor fuel elements, the ceramic material is an oxide powder of a fissionsble material and after forming, the compacts are placed in a cladding tube which is closed at its ends by vapor tight end caps, so that the sintered compacts are held in close contact with each other and with the interior wall of the cladding tube.

Study of Diffusion Bonding of 45 Steel through the Compacted Nickel Powder Layer

NASA Astrophysics Data System (ADS)

Zeer, G. M.; Zelenkova, E. G.; Temnykh, V. I.; Tokmin, A. M.; Shubin, A. A.; Koroleva, Yu. P.; Mikheev, A. A.

2018-02-01

The microstructure of the transition zone and powder spacer, the concentration distribution of chemical elements over the width of the diffusion-bonded joint, and microhardness of 45 steel-compacted Ni powder spacer-45 steel layered composites formed by diffusion bonding have been investigated. It has been shown that the relative spacer thickness χ < 0.06 is optimal for obtaining a high-quality joint has been formed under a compacting pressure of 500 MPa. The solid-state diffusion bonding is accompanied by sintering the nickel powder spacer and the formation of the transition zone between the spacer and steel. The transition zone consists of solid solution of nickel in the α-Fe phase and ordered solid solution of iron in nickel (FeNi3).

Characterization of ceramic powders by an X-ray measuring method

NASA Technical Reports Server (NTRS)

Ziegler, B.

1983-01-01

X-ray line broadening analysis gives quantitative data on structural changes of ceramic powders after different processing steps. Various Al2O3 powders were investigated and the following points are discussed on the basis of these results: X-ray line broadening analysis, structural changes during grinding, structural changes during annealing, influence of structural properties on sintering behavior and application of line broadening analysis to quality control of powders.

In search of the elusive IrB 2: Can mechanochemistry help?

DOE PAGES

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina; ...

2015-10-20

We produced hexagonal ReB 2-type IrB 2 diboride and orthorhombic IrB monoboride phases, that were previously unknown and saw them produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. Additionally, scanning electron microscopy and transmission electron microscopy were employed, along with XRD, to further characterize the microstructure of the phases produced.

Liquid-metal atomization for hot working preforms

NASA Technical Reports Server (NTRS)

Grant, N. J.; Pelloux, R. M.

1974-01-01

Rapid quenching of a liquid metal by atomization or splat cooling overcomes the major limitation of most solidification processes, namely, the segregation of alloying elements, impurities, and constituent phases. The cooling rates of different atomizing processes are related to the dendrite arm spacings and to the microstructure of the atomized powders. The increased solubility limits and the formation of metastable compounds in splat-cooled alloys are discussed. Consolidation of the powders by hot isostatic compaction, hot extrusion, or hot forging and rolling processes yields billets with properties equivalent to or better than those of the wrought alloys. The application of this powder processing technology to high-performance alloys is reviewed.

Hydrogen Decrepitation Press-Less Process recycling of NdFeB sintered magnets

NASA Astrophysics Data System (ADS)

Xia, Manlong; Abrahamsen, Asger B.; Bahl, Christian R. H.; Veluri, Badrinath; Søegaard, Allan I.; Bøjsøe, Poul

2017-11-01

A Hydrogen Decrepitation Press-Less Process (HD-PLP) recycling method for recycling of anisotropic NdFeB magnets is demonstrated. The method combines hydrogen decrepitation (HD) disintegration of the initial magnet, powder sieving and the Press-Less Process (PLP), where hydride powder is sintered in a graphite mold. Coercivities up to 534 kA/m were obtained in porous samples based on powder size d < 100 μm. Adding a ball milling step resulted in full density isotropic magnets for d > 100 μm. The coercivity reached Hci = 957 kA/m being 86% of the original N48M material without addition of rare earth elements.

In search of the elusive IrB 2: Can mechanochemistry help?

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

Xie, Zhilin; Blair, Richard G.; Orlovskaya, Nina

We produced hexagonal ReB 2-type IrB 2 diboride and orthorhombic IrB monoboride phases, that were previously unknown and saw them produced by mechanochemical syntheses. High energy ball milling of elemental Ir and B powder for 30 h, followed by annealing of the powder at 1050 °C for 48 h, resulted in the formation of the desired phases. Both traditional laboratory and high resolution synchrotron X-ray diffraction (XRD) analyses were used for phase identification of the synthesized powder. Additionally, scanning electron microscopy and transmission electron microscopy were employed, along with XRD, to further characterize the microstructure of the phases produced.

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.

Microstructural Evolution in Solution Heat Treatment of Gas-Atomized Al Alloy (7075) Powder for Cold Spray

NASA Astrophysics Data System (ADS)

Sabard, A.; de Villiers Lovelock, H. L.; Hussain, T.

2018-01-01

Cold gas dynamic spray is being explored as a repair technique for high-value metallic components, given its potential to produce pore and oxide-free deposits of between several micrometers and several millimeters thick with good levels of adhesion and mechanical strength. However, feedstock powders for cold spray experience rapid solidification if manufactured by gas atomization and hence can exhibit non-equilibrium microstructures and localized segregation of alloying elements. Here, we used sealed quartz tube solution heat treatment of a precipitation hardenable 7075 aluminum alloy feedstock to yield a consistent and homogeneous powder phase composition and microstructure prior to cold spraying, aiming for a more controllable heat treatment response of the cold spray deposits. It was shown that the dendritic microstructure and solute segregation in the gas-atomized powders were altered, such that the heat-treated powder exhibits a homogeneous distribution of solute atoms. Micro-indentation testing revealed that the heat-treated powder exhibited a mean hardness decrease of nearly 25% compared to the as-received powder. Deformation of the powder particles was enhanced by heat treatment, resulting in an improved coating with higher thickness ( 300 μm compared to 40 μm for untreated feedstock). Improved particle-substrate bonding was evidenced by formation of jets at the particle boundaries.

The analysis of disperse and elemental composition of dust from drobestry installations of foundry at the production of construction structures for altitude buildings

NASA Astrophysics Data System (ADS)

Ivanova, Irina; Golovina, Elena; Kulakov, Kirill; Sorokin, Andrey

2018-03-01

In the production of building structures for high-rise buildings, the dangerous and harmful factors of foundry production include high concentrations of dust and harmful gases released at various stages of the process. Disperse and elemental compositions of dust determine the hygienic state of the working area of the foundry. According to experts, the presence of dust of less than 10 microns in size in the air increases the danger of getting occupational diseases, such as pneumoconiosis (silicosis), bronchitis, dermatitis, conjunctivitis. The determination of the granulometric composition of the powder sample provided was carried out by the laser diffraction method realized on a laser particle analyzer Fritsch NanoTec «ANALISETTE 22».

Thermokinetic Modeling of Phase Transformation in the Laser Powder Deposition Process

NASA Astrophysics Data System (ADS)

Foroozmehr, Ehsan; Kovacevic, Radovan

2009-08-01

A finite element model coupled with a thermokinetic model is developed to predict the phase transformation of the laser deposition of AISI 4140 on a substrate with the same material. Four different deposition patterns, long-bead, short-bead, spiral-in, and spiral-out, are used to cover a similar area. Using a finite element model, the temperature history of the laser powder deposition (LPD) process is determined. The martensite transformation as well as martensite tempering is considered to calculate the final fraction of martensite, ferrite, cementite, ɛ-carbide, and retained austenite. Comparing the surface hardness topography of different patterns reveals that path planning is a critical parameter in laser surface modification. The predicted results are in a close agreement with the experimental results.

Influence of Powder Metallurgical Processing Routes on Phase Formations in a Multicomponent NbSi-Alloy

NASA Astrophysics Data System (ADS)

Seemüller, C.; Hartwig, T.; Mulser, M.; Adkins, N.; Wickins, M.; Heilmaier, M.

2014-09-01

Refractory metal silicide composites on the basis of Nbss-Nb5Si3 have been investigated as potential alternatives for nickel-base superalloys for years because of their low densities and good high-temperature strengths. NbSi-based composites are typically produced by arc-melting or casting. Samples in this study, however, were produced by powder metallurgy because of the potential for near net-shape component fabrication with very homogeneous microstructures. Either gas atomized powder or high-energy mechanically alloyed elemental powders were compacted by powder injection molding or hot isostatic pressing. Heat treatments were applied for phase stability evaluation. Slight compositional changes (oxygen, nitrogen, or iron) introduced by the processing route, i.e., powder production and consolidation, can affect phase formations and phase transitions during the process. Special focus is put on the distinction between different silicides (Nb5Si3 and Nb3Si) and silicide modifications (α-, β-, and γ-Nb5Si3), respectively. These were evaluated by x-ray diffraction and energy-dispersive spectroscopy measurements with the additional inclusion of thermodynamic calculations using the calculated phase diagram method.

Preparation of the Iron Oxide Red from the Converter Dust by the Magnetic Separation and Roasting Process

NASA Astrophysics Data System (ADS)

Guo, Z. J.; Li, S. Q.; Yang, C. Q.

2017-05-01

Preparation of iron oxide red (α-Fe2O3) from the converter dust by the superconductivity high gradient magnetic separation (S-HGMS) and roasting process was investigated in the paper. The basic properties of the dust were studied by the X Ray Fluorescence, the chemical analysis and the X Ray Diffraction methods. The results showed that the raw dust mainly contained elements of Fe‵O‵Si‵Ca, the iron content of the raw dust was 61.80%, and there were ferrous phases of Fe3O4, α-Fe2O3, Fe2(SiO4) and CaFe(Si2O6) in the raw dust. Under the optimum conditions of magnetic field intensity of 1.8T, the dispersion agent of 30mg/L and velocity of 500mL/min, the powders absorbed by the magnetic medium mainly contained Fe3O4 and α-Fe2O3, and the iron content of powders absorbed was up to 65.90%. The Fe2+ content of the powders absorbed under the optimum magnetic conditions dropped to 0.25% from 19.10% after roasting of fifty minutes, and the iron content of powders absorbed under the optimum magnetic conditions fell to 64% due to oxidation, and the Fe3O4 was removed. Finally the α-Fe2O3 content was up to 91.07% in the iron oxide red.

Preparation and certification of hijiki reference material, NMIJ CRM 7405-a, from the edible marine algae hijiki (Hizikia fusiforme).

PubMed

Narukawa, Tomohiro; Inagaki, Kazumi; Zhu, Yanbei; Kuroiwa, Takayoshi; Narushima, Izumi; Chiba, Koichi; Hioki, Akiharu

2012-02-01

A certified reference material, NMIJ CRM 7405-a, for the determination of trace elements and As(V) in algae was developed from the edible marine hijiki (Hizikia fusiforme) and certified by the National Metrology Institute of Japan (NMIJ), the National Institute of Advanced Industrial Science and Technology (AIST). Hijiki was collected from the Pacific coast in the Kanto area of Japan, and was washed, dried, powdered, and homogenized. The hijiki powder was placed in 400 bottles (ca. 20 g each). The concentrations of 18 trace elements and As(V) were determined by two to four independent analytical techniques, including (ID)ICP-(HR)MS, ICP-OES, GFAAS, and HPLC-ICP-MS using calibration solutions prepared from the elemental standard solution of Japan calibration service system (JCSS) and the NMIJ CRM As(V) solution, and whose concentrations are certified and SI traceable. The uncertainties of all the measurements and preparation procedures were evaluated. The values of 18 trace elements and As(V) in the CRM were certified with uncertainty (k = 2).

Time resolved fluorescence of cow and goat milk powder

NASA Astrophysics Data System (ADS)

Brandao, Mariana P.; de Carvalho dos Anjos, Virgílio; Bell., Maria José V.

2017-01-01

Milk powder is an international dairy commodity. Goat and cow milk powders are significant sources of nutrients and the investigation of the authenticity and classification of milk powder is particularly important. The use of time-resolved fluorescence techniques to distinguish chemical composition and structure modifications could assist develop a portable and non-destructive methodology to perform milk powder classification and determine composition. This study goal is to differentiate milk powder samples from cows and goats using fluorescence lifetimes. The samples were excited at 315 nm and the fluorescence intensity decay registered at 468 nm. We observed fluorescence lifetimes of 1.5 ± 0.3, 6.4 ± 0.4 and 18.7 ± 2.5 ns for goat milk powder; and 1.7 ± 0.3, 6.9 ± 0.2 and 29.9 ± 1.6 ns for cow's milk powder. We discriminate goat and cow powder milk by analysis of variance using Fisher's method. In addition, we employed quadratic discriminant analysis to differentiate the milk samples with accuracy of 100%. Our results suggest that time-resolved fluorescence can provide a new method to the analysis of powder milk and its composition.

Chemical composition and pharmacological significance of Anethum Sowa L. Root.

PubMed

Saleh-E-In, Md Moshfekus; Sultana, Nasim; Rahim, Md Matiur; Ahsan, Md Aminul; Bhuiyan, Md Nurul Huda; Hossain, Md Nur; Rahman, Md Mahbubar; Kumar Roy, Sudhangshu; Islam, Md Rabiul

2017-02-23

Medicinal herbs are used for the treatment of different ailments since antiquity. Different parts of Anethum sowa L. is used in folk medicine as a carminative for the treatment of flatulence, colic and hiccups of infants and children, antioxidant, antimicrobial and antispasmodic agent. The aim of our present study is to evaluate the chemical composition of the essential oil, proximate and elemental composition, amino acid, fatty acid profile and thermal behaviour of its root part as well as different pharmacological activities like antioxidant, antimicrobial and cytotoxicity of the root essential oil. The air-dried roots of Anethum sowa L. were subjected to hydro-distillation to yield the essential oil. The antioxidant activity of the essential oil was studied by DPPH radical scavenging activity. The antimicrobial activity was tested against four Gram-positive, six Gram-negative bacteria and four fungi species. The minimum inhibitory concentration (MIC) and Minimum bacterial concentration (MBC) for each examined microorganism were determined using the micro-dilution method. The LC 50 value of the oil was also evaluated by brine shrimp lethality assay. The subsequent proximate analysis was also done by AOAC methods. The elemental analysis of the root powder was analysed by ICP-MS, AAS and FP system. The fatty acid was extracted by hot and cold extraction method and the analyses were carried out by GC. The amino acid profile was done by the amino acid analyzer. The DTA, DTG and TG of the root powder were taken by the thermogravimetric analyzer. A total of 24 constituents was identified and quantified in the essential oil and its water extract portion by GC and GC-MS. Apiol (81.99 and 74.779%) was found the highest phenylpropanoid constituent followed by m-diaminobenzene (10.446 and 8.778%) in the essential oil and aqueous extract portion. On the other hand, β-butyrolactone (5.13%) and isobutyl acetone (3.73%) were found in the major constituents in the water extract part. The IC 50 value of the essential oil was found to be 3.07 mg/mL by DPPH radical assay methods. The LC 50 value of the brine shrimp cytotoxicity assay of the essential oil was observed at 0.81 μg/mL. The essential oil showed better activity on Gram-negative bacteria than Gram-positive bacteria and fungi. The proximate composition showed that root contained 5.29% ash, 2.01% protein, 54.09% crude fibre, 0.15% essential oil and 1.14% fatty oil for hot extract and 0.23% for cold extract on the dried basis. The palmitic (33.81 & 31.58%) and linoleic acid (30.03 & 23.79%) were the major saturated and unsaturated fatty acids in the cold and hot extracted root powder respectively. Ca (23,600 mg/kg), Mg (7620.33 mg/kg) and K (1286.15 mg/kg) were the most predominant elements followed by Ni (1187.30 mg/kg), Se (913.79 mg/kg), Li (317.84 mg/kg), Na (288.72 mg/kg) and Fe (206.88 mg/kg). The toxic elements were found to be within the permissible limit. Glutamic acid (19.37%), glycine (14.53%) and lysine (17.08%) were found as the major amino acids. The decomposition rates were obtained by TG, DTG and DTA curve of the powder sample at various temperature ranges. The results demonstrated that the root part of Anethum sowa L. is a rich source of mineral elements, essential amino acid and fatty acids. The essential oil is the highly potential as bioactive oil for pharmaceuticals and medical applications, possessing antioxidant, antimicrobial and cytotoxic activities. The thermal analysis suggested as a simple, effective and rapid method to characterize the Anethum sowa L. species as well as to assess for herbal formulation.

A new approach to assess the chemical composition of powder deposits damaging the stone surfaces of historical monuments.

PubMed

Fermo, Paola; Turrion, Raquel Gonzalez; Rosa, Mario; Omegna, Alessandra

2015-04-01

The issue of conservation of the monumental heritage worldwide is mainly related to atmospheric pollution that causes the degradation of stone surfaces. The powder deposits present on the stone monuments reflect the composition of the aerosol particulate matter (PM) to which the surfaces are exposed, so the chemical characterization of the outermost damaged layers is necessary in order to adopt mitigation measurements to reduce PM emissions. In the present paper, a new analytical approach is proposed to investigate the chemical composition of powder deposits present on Angera stone, a dolomitic rock used in the Richini courtyard, a masterpiece of Lombard Baroque and placed in Milan. Inorganic and organic components present in these deposits have been analyzed by IC (ion chromatography) and a new approach mainly bases on thermal analyses, respectively. Gypsum is the main inorganic constituent indicating a composition similar to that of black crusts, hard black patina covering the degraded building surfaces. Ammonium nitrate present in the powder is able to react with the stone substrate to form magnesium nitrate which can migrate into the porous stone. The carbonaceous fraction powder deposits (i.e. OC = Organic Carbon and EC = Elemental Carbon) have been quantified by a new simple thermal approach based on carbon hydrogen nitrogen (CHN) analysis. The presence of high concentration of EC confirms that the powder deposits are evolving to black crust. Low values of water-soluble organic carbon (WSOC, determined by total organic carbon-TOC), with respect to what is normally found in PM, may indicate a migration process of organic substances into the stone with a worsening of the conservation conditions. The presence of heavy metals of anthropogenic origin and acting as catalysts in the black crust formation process has been highlighted by SEM-EDS (electron microscopy coupled with an energy dispersive spectrometer) as well.

Trace impurities analysis of aluminum nanopowder and its air combustion product

NASA Astrophysics Data System (ADS)

Kabanov, Denis V.; Merkulov, Viktor G.; Mostovshchikov, Andrey V.; Ilyin, Alexander P.

2018-03-01

Neutron activation analysis (NAA) allows estimating micro-concentrations of chemicals and analyzes tens of elements at one measurement. In this paper we have used NAA to examine metal impurities in the electroexplosive aluminum nanopowder (ANP) and its air-combustion products produced by burning in crucibles in an electric and magnetic field and without application of fields. It has been revealed that in the air-combustion products impurities content is reduced. The presence of impurities in the ANP is associated with electric explosion technology (erosion of electrode and chamber materials) and with the previous development of various nanopowders in the composition of this electric explosive device. NAA is characterized by a high sensitivity and reproducibility to elements content and low metering error. According to the obtained results it has been concluded that NAA metering error does not exceed 10% in the wide concentration range, from 0.01 to 2100 ppm, particularly. Besides, there is high reproducibility of the method that has been proved on macro-elements of Ca (>1000 ppm), Fe (>2000 ppm), and micro-elements as Sm, U, Ce, Sb, Th, etc. (<0.9 ppm). It is recommended to use an individual unit for the production of pure metal powders for electric explosion and production of nanopowders, which is possible with mass production of nanopowders.

Ray tracing method for simulation of laser beam interaction with random packings of powders

NASA Astrophysics Data System (ADS)

Kovalev, O. B.; Kovaleva, I. O.; Belyaev, V. V.

2018-03-01

Selective laser sintering is a technology of rapid manufacturing of a free form that is created as a solid object by selectively fusing successive layers of powder using a laser. The motivation of this study is due to the currently insufficient understanding of the processes and phenomena of selective laser melting of powders whose time scales differ by orders of magnitude. To construct random packings from mono- and polydispersed solid spheres, the algorithm of their generation based on the discrete element method is used. A numerical method of ray tracing is proposed that is used to simulate the interaction of laser radiation with a random bulk packing of spherical particles and to predict the optical properties of the granular layer, the extinction and absorption coefficients, depending on the optical properties of a powder material.

Waste grape skins: evaluation of safety aspects for the production of functional powders and extracts for the food sector.

PubMed

Moncalvo, Alessandro; Marinoni, Laura; Dordoni, Roberta; Duserm Garrido, Guillermo; Lavelli, Vera; Spigno, Giorgia

2016-07-01

Skin powders and aqueous alcohol extracts were obtained from waste marcs from different grape varieties (Barbera, Nebbiolo, Pinot Noir, Chardonnay, Moscato and Müller-Thurgau). Both skins and extracts were analysed for the content of chemical contaminants: ochratoxin A (OTA), biogenic amines (BIAs), pesticides and metals. OTA was detected in low concentrations in Barbera, Moscato and Nebbiolo skins, but only in Barbera and Moscato extracts. Cadaverine, putrescine, ethanolamine and ethylamine were found in extracts at very low levels, while potential allergenic amines, tyramine and histamine, were never detected. Different pesticides were present in both skins and extracts. Pb and Cd were found in trace only in the powders, and K, Ca and Mg were the most abundant elements in both skin powders and extracts. Concentrations of the different contaminants were related to fibre content or total phenolics content of powders and extracts, respectively, in order to evaluate their use in the food sector.

Synthesis of Nano Sized Cr2AlC Powders by Molten Salt Method.

PubMed

Xiao, Dan; Zhu, Jianfeng; Wang, Fen; Tang, Yi

2015-09-01

Cr2AlC powders were successfully synthesized by molten salt method using Cr, Al and C as starting materials. The effects of the process parameters and amount of Al addition on the purity of the Cr2AlC powders were also investigated in details. The formation mechanism of Cr2AlC powders was investigated by XRD and DSC. The results indicated that intermediates of Cr7C3 and Cr- Al intermetallics, such as CrAl17, Cr2Al, Cr2Al8, were formed by the reactions among the initial elements, then the intermediates gradually transformed to Cr2AlC. From the fixed composition of Cr:Al:C = 2:1.2:1, high purity Cr2AlC powders could be obtained with an inorganic salt KCl as a solvent at 1250 degrees C for 60 min under argon atmosphere which was lower than that (generally 1450 degrees C) of conventional solid state reaction.

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.

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.

Laser Additive Manufacturing of Magnetic Materials

NASA Astrophysics Data System (ADS)

Mikler, C. V.; Chaudhary, V.; Borkar, T.; Soni, V.; Jaeger, D.; Chen, X.; Contieri, R.; Ramanujan, R. V.; Banerjee, R.

2017-03-01

While laser additive manufacturing is becoming increasingly important in the context of next-generation manufacturing technologies, most current research efforts focus on optimizing process parameters for the processing of mature alloys for structural applications (primarily stainless steels, titanium base, and nickel base alloys) from pre-alloyed powder feedstocks to achieve properties superior to conventionally processed counterparts. However, laser additive manufacturing or processing can also be applied to functional materials. This article focuses on the use of directed energy deposition-based additive manufacturing technologies, such as the laser engineered net shaping (LENS™) process, to deposit magnetic alloys. Three case studies are presented: Fe-30 at.%Ni, permalloys of the type Ni-Fe-V and Ni-Fe-Mo, and Fe-Si-B-Cu-Nb (derived from Finemet) alloys. All these alloys have been processed from a blend of elemental powders used as the feedstock, and their resultant microstructures, phase formation, and magnetic properties are discussed in this paper. Although these alloys were produced from a blend of elemental powders, they exhibited relatively uniform microstructures and comparable magnetic properties to those of their conventionally processed counterparts.

Synthesis and investigation of physico-chemical, antibacterial, biomymetic properties of silver and zinc containing hydroxyapatite

NASA Astrophysics Data System (ADS)

Zhuk, Ilya; Rasskazova, Lyudmila; Korotchenko, Natalia; Kozik, Vladimir; Kurzina, Irina

2017-11-01

In the work we carried out microwave synthesis of modified hydroxyapatites (HA) with different content of ions. A solid solution based on HA remains a single-phase sample when the calcium ions are substituted by silver and zinc ions up to 5 % by weight (0.5 mole fraction). The microstructure parameters, morphology and the particle powders size were studied by X-ray diffraction analysis, IR spectroscopy, and scanning electron microscopy (SEM). It is shown that the modification of HA by silver (AgHA) and zinc (ZnHA) ions increases the size of its particles, the degree of crystallinity, and the pore sizes of the samples while reducing their specific surface and uniformity of their forms. Elemental analysis and distribution of elements over the surface of HA, AgHA, and ZnHA powders were performed by X-ray spectral microanalysis (RSMA). The ratio of Ca/P is within the range of 1.66-1.77 and corresponds to the ratio of Ca/P in stoichiometric HA and the HA entering bone tissue. The ability of AgHA- and ZnHA-substrates to form on their surface a calcium-phosphate layer from the simulated body fluid (SBF) at 37 °C is determined. This ability decreases in the order: in ZnHA it is less than in AgHA, but greater than in HA. The antibacterial activity of the samples was analyzed. The AgHA sample has both bactericidal and persistent bacteriostatic properties in the case of direct contact with Escherichia coli cells.

Performance evaluation of laser induced breakdown spectroscopy in the measurement of liquid and solid samples

NASA Astrophysics Data System (ADS)

Bilge, Gonca; Sezer, Banu; Boyaci, Ismail Hakki; Eseller, Kemal Efe; Berberoglu, Halil

2018-07-01

Liquid analysis by using LIBS is a complicated process due to difficulties encountered during the collection of light and formation of plasma in liquid. To avoid these, some applications are performed such as aerosol formation and transforming liquid into solid state. However, performance of LIBS in liquid samples still remains a challenging issue. In this study, performance evaluation of LIBS and parameter optimizations in liquid and solid phase samples were performed. For this purpose, milk was chosen as model sample; milk powder was used as solid sample, and milk was used as liquid sample in the experiments. Different experimental setups have been constructed for each sampling technique, and optimizations were performed to determine suitable parameters such as delay time, laser energy, repetition rate and speed of rotary table for solid sampling technique, and flow rate of carrier gas for liquid sampling technique. Target element was determined as Ca, which is a critically important element in milk for determining its nutritional value and Ca addition. In optimum parameters, limit of detection (LOD), limit of quantification (LOQ) and relative standard deviation (RSD) values were calculated as 0.11%, 0.36% and 8.29% respectively for milk powders samples; while LOD, LOQ and RSD values were calculated as 0.24%, 0.81%, and 10.93% respectively for milk samples. It can be said that LIBS is an applicable method in both liquid and solid samples with suitable systems and parameters. However, liquid analysis requires much more developed systems for more accurate results.

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.

Syntheses, structures and luminescent properties of two novel Zn (II) coordination polymers

NASA Astrophysics Data System (ADS)

Huang, Ya-Ru; Gao, Ling-Ling; Wang, Xiao-Qing; Fan, Li-Ming; Hu, Tuo-Ping

2018-02-01

Two new coordination polymers, namely [Zn(TZMB)]n (1) and {[Zn(TZMB)](H2TZMB)]·(C2H5OH)0.5(H2O)2.5}n (2), (H2TZMB = 4,4‧-(1H-1,2,4-triazol-1-yl)methylene-bis(benzonic acid), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction analysis, elemental analysis (EA), IR spectrum analysis (IR), powder X-ray diffraction (PXRD), and thermogravimetric (TG) analysis. Single X-ray diffraction analysis reveals that complex 1 is a 3D 3,6-connected net with the point symbol of (6110.84)(63)2 and complex 2 is a 2D 3-connected net with the point symbol of (63). Furthermore, luminescent properties of complexes 1 and 2 were also investigated in detail.

Synthetic aspects, spectral, thermal studies and antimicrobial screening on bis(N,N-dimethyldithiocarbamato-S,S‧)antimony(III) complexes with oxo or thio donor ligands

NASA Astrophysics Data System (ADS)

Chauhan, H. P. S.; Carpenter, Jaswant; Joshi, Sapana

2014-09-01

The bis(N,N-dimethyldithiocarbamato-S,S‧)antimony(III) complexes have been obtained by the reaction of chloro bis(N,N-dimethyldithiocarbamato-S,S‧)antimony(III) with corresponding oxo or thio donor ligands such as sodium benzoate 1, sodium thioglycolate 2, phenol 3, sodium 1-propanethiolate 4, potassium thioacetate 5, sodium salicylate 6, ethane-1,2-dithiolate 7 and disodium oxalate 8. These complexes have been characterized by the physicochemical [melting point, molecular weight determination and elemental analysis (C, H, N, S and Sb)], spectral [UV-Visible, FT-IR, far IR, NMR (1H and 13C)], thermogravimetric (TG & DTA) analysis, ESI-Mass and powder X-ray diffraction studies. Thermogravimetric analysis of the complexes confirmed the final decomposition product as highly pure antimony sulfide (Sb2S3) and powder X-ray diffraction studies show that the complexes are in lower symmetry with monoclinic crystal lattice and nano-ranged particle size (11.51-20.82 nm). The complexes have also been screened against some bacterial and fungal strains for their antibacterial and antifungal activities and compared with standard drugs. These show that the complexes have greater activities against some human pathogenic bacteria and fungi than the activities of standard drugs.

Laser Induced Hydrogen Generation from Coal in Water

NASA Astrophysics Data System (ADS)

Seyitliyev, Dovletgeldi; Kholikov, Khomidkhodzha; Er, Ali

We report an alternative way of obtaining hydrogen using nanosecond laser pulses and various ranks of coal and coke. SEM-EDS analysis shows the atomic concentrations of elements on each of the powders which also is in good agreement with calorimeter analysis. Coal and coke powders were irradiated with 1064nm IR and 532 nm green Nd:YAG pulsed laser beam for 45 minutes. The volume of the total gas generated after irradiation of each rank was measured using the water displacement method. The amount of gas generated increased when using 532 nm compared to 1064 nm. Post-irradiation SEM images show structural differences with samples before irradiation. The amount of gas generation with respect to laser energy density shows nonlinear correlation. Generated gas concentrations were then analyzed using gas chromatography (GC). Hydrogen and carbon monoxide were the two most highly generated gases, and the efficiency of each rank of coal was determined by analyzing the hydrogen to carbon monoxide ratio. The highest efficiency rank was anthracite, with hydrogen to carbon monoxide ratio of 1.4. GC analysis also showed that the maximum hydrogen generation occurs at 100 mJ/pulse laser energy. The efficiency of each rank of coal was observed to correlate with carbon content. American Chemical Society Petroleum Research Fund.

Role of initial heat treatment of the ferrite component on magnetic properties in the composite of ferrimagnetic Co1.75Fe1.25O4 ferrite and non-magnetic BaTiO3 oxide

NASA Astrophysics Data System (ADS)

Bhowmik, R. N.; Kazhugasalamoorthy, S.; Sinha, A. K.

2017-12-01

We have prepared a composite of ferrimagnetic ferrite Co1.75Fe1.25O4 and non-magnetic oxide BaTiO3. The ferrite composition Co1.75Fe1.25O4 has been prepared by chemical co-precipitation and subsequently heated at different temperatures. The heat treated ferrite powder has been mixed with BaTiO3 powder with mass ratio 1:1 and the mixed powder has been finally heated at 1000 °C to form composite material. Structural phase of the composite material has been confirmed by high quality Synchrotron X-ray diffraction pattern and Micro-Raman spectra. The grain surface morphology and elemental composition have been studied by Scanning electron microscope and Energy dispersive X-ray analysis. The distribution of magnetic exchange interactions and blocking behavior of the ferrimagnetic grains in composite samples has been understood by analyzing the temperature and magnetic field dependence of dc magnetization. Finally, information on modified micro-structure and ferrimagnetic parameters in composite samples has been obtained as the variation of annealing temperature of the ferrite component before making composite.

Physicochemical properties, nutritional value and techno-functional properties of goldenberry (Physalis peruviana) waste powder concise title: Composition of goldenberry juice waste.

PubMed

Mokhtar, Sayed M; Swailam, Hesham M; Embaby, Hassan El-Sayed

2018-05-15

Goldenberry waste powder, contained 5.87% moisture, 15.89% protein, 13.72% fat, 3.52% ash, 16.74% dietary fiber and 61% carbohydrates. Potassium (560 mg/100 g) was the predominant element followed by sodium (170 mg/100 g) and phosphorus (130 mg/100 g). Amino acid analysis gave high levels of cystine/methionine, histidine and tyrosine/phenylalanine. Goldenberry waste powder had good levels of the techno-functional properties including water absorption index, swelling index, foaming capacity and stability (3.38 g/g, 5.24 ml/g, 4.09 and 72.0%, respectively). Fatty acids profile showed that linoleic acid was the predominant fatty acid followed by oleic, palmitic and stearic acids. Iodine value (109.5 g/100 g of oil), acid value (2.36 mg KOH/g of oil), saponification value (183.8 mg KOH/g of oil), peroxide value (8.2 meq/kg of oil) and refractive index (1.4735) were comparable to those of soybean and sunflower oils. Goldenberry waste oil exhibited absorbance in the UV range at 100-400 nm. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Sanghapi, Hervé K.; Jain, Jinesh; Bol'shakov, Alexander; Lopano, Christina; McIntyre, Dustin; Russo, Richard

2016-08-01

In this study laser induced breakdown spectroscopy (LIBS) is used for elemental characterization of outcrop samples from the Marcellus Shale. Powdered samples were pressed to form pellets and used for LIBS analysis. Partial least squares regression (PLS-R) and univariate calibration curves were used for quantification of analytes. The matrix effect is substantially reduced using the partial least squares calibration method. Predicted results with LIBS are compared to ICP-OES results for Si, Al, Ti, Mg, and Ca. As for C, its results are compared to those obtained by a carbon analyzer. Relative errors of the LIBS measurements are in the range of 1.7 to 12.6%. The limits of detection (LODs) obtained for Si, Al, Ti, Mg and Ca are 60.9, 33.0, 15.6, 4.2 and 0.03 ppm, respectively. An LOD of 0.4 wt.% was obtained for carbon. This study shows that the LIBS method can provide a rapid analysis of shale samples and can potentially benefit depleted gas shale carbon storage research.

Structural and electrical properties of Li4Ti5O12 anode material for lithium-ion batteries

NASA Astrophysics Data System (ADS)

Vikram Babu, B.; Vijaya Babu, K.; Tewodros Aregai, G.; Seeta Devi, L.; Madhavi Latha, B.; Sushma Reddi, M.; Samatha, K.; Veeraiah, V.

2018-06-01

In this work we investigate Li4Ti5O12 (LTO) anode material synthesized by conventional solid state reaction method calcined at 850 °C for 16 h. Thermal analysis reveals the temperature dependence of the material properties. The phase composition, micro-morphology and elemental analysis of the compound are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectra (EDS) respectively. The results of XRD pattern possessed cubic spinel structure with space group Fd-3m. The morphological features of the powder sample are in the range of 1.1 μm. The EDS spectra confirm the constituent elemental composition of the sample. Electrical conductivity measurement at different frequencies and temperatures had been carried out; and at room temperature it is found to be 5.96 × 10-7 S/cm. Besides, for the different frequencies applied, the activation energies were calculated and obtained to be in the range of 0.2-0.4 eV.

Exploring a Multiphysics Resolution Approach for Additive Manufacturing

NASA Astrophysics Data System (ADS)

Estupinan Donoso, Alvaro Antonio; Peters, Bernhard

2018-06-01

Metal additive manufacturing (AM) is a fast-evolving technology aiming to efficiently produce complex parts while saving resources. Worldwide, active research is being performed to solve the existing challenges of this growing technique. Constant computational advances have enabled multiscale and multiphysics numerical tools that complement the traditional physical experimentation. In this contribution, an advanced discrete-continuous concept is proposed to address the physical phenomena involved during laser powder bed fusion. The concept treats powder as discrete by the extended discrete element method, which predicts the thermodynamic state and phase change for each particle. The fluid surrounding is solved with multiphase computational fluid dynamics techniques to determine momentum, heat, gas and liquid transfer. Thus, results track the positions and thermochemical history of individual particles in conjunction with the prevailing fluid phases' temperature and composition. It is believed that this methodology can be employed to complement experimental research by analysis of the comprehensive results, which can be extracted from it to enable AM processes optimization for parts qualification.

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.

Synthesis, antimicrobial, antioxidant and molecular docking studies of thiophene based macrocyclic Schiff base complexes

NASA Astrophysics Data System (ADS)

Rathi, Parveen; Singh, D. P.

2015-11-01

The macrocyclic complexes of pharmaceutical importance with trivalent transition metals have been synthesized by [1 + 1] condensation of succinyldihydrazide and thiophenedicarboxaldehyde, via template method, resulting in the formation of the complex [MLX] X2; where L is (C10H10N4O2S), a macrocyclic ligand, M = Cr (III) and Fe (III) and X = Cl-, CH3COO- or NO3- . These complexes have been characterized with the help of elemental analyses, molar conductance measurements, magnetic susceptibility measurements, ultraviolet, infrared, far infrared, electron spin resonance, mass spectral studies and powder x-ray diffraction analysis. On the basis of all these studies, mononuclear complexes having 1:2 electrolytic nature with a five coordinated square pyramidal geometry have been proposed. Powder diffraction XRD indicates the presence of triclinic crystal system with p bravais lattice for the representative complex. All the metal complexes have also been explored for their in vitro antimicrobial and antioxidant activities.

Tungsten tetraboride, an inexpensive superhard material

PubMed Central

Mohammadi, Reza; Lech, Andrew T.; Xie, Miao; Weaver, Beth E.; Yeung, Michael T.; Tolbert, Sarah H.; Kaner, Richard B.

2011-01-01

Tungsten tetraboride (WB4) is an interesting candidate as a less expensive member of the growing group of superhard transition metal borides. WB4 was successfully synthesized by arc melting from the elements. Characterization using powder X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDX) indicates that the as-synthesized material is phase pure. The zero-pressure bulk modulus, as measured by high-pressure X-ray diffraction for WB4, is 339 GPa. Mechanical testing using microindentation gives a Vickers hardness of 43.3 ± 2.9 GPa under an applied load of 0.49 N. Various ratios of rhenium were added to WB4 in an attempt to increase hardness. With the addition of 1 at.% Re, the Vickers hardness increased to approximately 50 GPa at 0.49 N. Powders of tungsten tetraboride with and without 1 at.% Re addition are thermally stable up to approximately 400 °C in air as measured by thermal gravimetric analysis. PMID:21690363

[Determination of lead and cadmium contents in chicken granules and gourmet powder].

PubMed

Shi, Min; Hao, Ai-guo; Zhu, Li-zun

2005-02-01

Through atomic absorption detector, the contents of Pb and Cd in chicken granules and gourmet powder were determined. From the result it was found that there are differing contents of pollutant elements, i. e. 0.00-10.00 microg x mL(-1) for Pb and 0.00-4.00 microg x mL(-1) for Cd, respectively. The relative standard deviations of Pb and Cd are 3.15% and 4.26%, respectively. At the same time, a recovery experiment for Pb and Cd in chicken granules and gourmet powder were performed, and the recoveries are 96.7%-102.1% for Pb and 91.9%-107.6% for Cd, respectively.

Surface modification of titania powder P25 with phosphate and phosphonic acids--effect on thermal stability and photocatalytic activity.

PubMed

Djafer, Lahcène; Ayral, André; Boury, Bruno; Laine, Richard M

2013-03-01

Phosphorus is frequently reported as a doping element for TiO(2) as photocatalyst; however, the previously reported methods used to prepare P-doped TiO(2) do not allow control over the location of the phosphorus either in the bulk or at the surface or both. In this study, we report on the surface modification of Evonik P25 with phosphonic (H(3)PO(3)) and octylphosphonic acid [C(8)H(17)-PO(OH)(2)], done to limit the introduction of phosphorus only to the photocatalyst surface. The effect of this element on the thermal behavior and photocatalytic properties is reported through characterization using elemental analyses, solid state (31)P NMR, X-ray powder diffraction, N(2) porosimetry, dilatometry, etc. Thus, the objective of the work reported here is to focus on the role(s) that phosphorus plays only at TiO(2) crystallite surfaces. For comparison, other samples were treated with phosphoric acid. Copyright © 2012 Elsevier Inc. All rights reserved.

Finite Element Simulation of Residual Stress Development in Thermally Sprayed Coatings

NASA Astrophysics Data System (ADS)

Elhoriny, Mohamed; Wenzelburger, Martin; Killinger, Andreas; Gadow, Rainer

2017-04-01

The coating buildup process of Al2O3/TiO2 ceramic powder deposited on stainless-steel substrate by atmospheric plasma spraying has been simulated by creating thermomechanical finite element models that utilize element death and birth techniques in ANSYS commercial software and self-developed codes. The simulation process starts with side-by-side deposition of coarse subparts of the ceramic layer until the entire coating is created. Simultaneously, the heat flow into the material, thermal deformation, and initial quenching stress are computed. The aim is to be able to predict—for the considered spray powder and substrate material—the development of residual stresses and to assess the risk of coating failure. The model allows the prediction of the heat flow, temperature profile, and residual stress development over time and position in the coating and substrate. The proposed models were successfully run and the results compared with actual residual stresses measured by the hole drilling method.

Mineral content of Chinese medicinal herbs used as diuretic treatments for Taiwanese children.

PubMed

Chen, Chien-Yi

2005-01-01

Eighteen major, minor and trace elements in 12 Chinese medicinal herbs commonly consumed by Taiwanese Children as diuretics were determined by instrumental neutron activation analysis (INAA). Dried and powdered herb samples were irradiated in a neutron flux of ca. 2 x 10(12) n/cm2 s under separate short and long irradiation schemes. Lichen (IAEA-336) was used as the reference standard, and tomato leaves (NIST-SRM 1570a) were employed for cross-checking the accuracy of the results. INAA was shown to be a reliable multi-element analytical method for determining the content of both toxicologically and nutritionally important minerals in Chinese medicinal herbs. Determined elements were present in the dried herbs in concentrations ranging from 10(4) to 10(-3) microg/g. The mineral contents and the maximum daily intake values of the tested herbs were compared with published values and with the recommended daily intakes for Taiwanese children as specified by the World Health Organization.

Synthesis and characterization of barium hexaferrite with manganese (Mn) doping material as anti-radar

NASA Astrophysics Data System (ADS)

Susilawati, Doyan, Aris; Khalilurrahman

2017-01-01

Have been successfully synthesized barium powder doping Manganese hexaferrite with the expected potential as anti-radar material. Synthesis was done by using the co-precipitation method, the variation of the variable x concentrations used were 0; 0.2; 0.4; and 0.6 and calcined at temperatures of 400, 600 and 800°C. Characterization powders of hexaferrite have used XRD (X-Ray Diffraction), SEM (Scanning Electron Microscopy), TEM (Transmission Electron Microscopy), LCR (inductance, capacitance, and resistance) meter, and VSM (Vibrating Sample Magnetometer). The higher the concentration and temperature of calcinations given affect the color of the powder. The test results using XRD indicates that it has formed barium hexaferrite phase with a hexagonal crystal structure. Tests using SEM showed that all the constituent elements barium powder hexaferrite by doping Manganese powders have been spread evenly. XRD test results were confirmed by a test using a TEM showing the crystal structure and the powder was sized nano particles. The results from the LCR meter showed that the barium powder hexaferrite by doping Manganese that has been synthesized classified in semiconductor materials. The result from VSM showed that the value of coercivity magnetic powder doped barium hexaferrite Manganese is smaller when compared with barium hexaferrite without doping and belong to the soft magnetic. Based on the results of the synthesis and characterization, we can conclude that the barium powder heksaferrite by doping Manganese potential as a material anti-radar.

[Protecting Safety During Dust Fires and Dust Explosions - The Example of the Formosa Fun Coast Water Park Accident].

PubMed

Hsieh, Ming-Hong; Wu, Jia-Wun; Li, Ya-Cing; Tang, Jia-Suei; Hsieh, Chun-Chien

2016-02-01

This paper will explore the fire and explosion characteristics of cornstarch powder as well as strategies for protecting the safety of people who are involved a dust fire or dust explosion. We discuss the 5 elements of dust explosions and conduct tests to analyze the fire and explosion characteristics of differently colored powders (yellow, golden yellow, pink, purple, orange and green). The results show that, while all of the tested powders were difficult to ignite, low moisture content was associated with significantly greater risks of ignition and flame spread. We found the auto-ignition temperature (AIT) of air-borne cornstarch powder to be between 385°C and 405°C, with yellow-colored cornstarch powder showing the highest AIT and pink-colored cornstarch powder showing the lowest AIT. The volume resistivity of all powder samples was approximately 108 Ω.m, indicating that they were nonconductive. Lighters and cigarettes are effective ignition sources, as their lit temperatures are higher than the AIT of cornstarch powder. In order to better protect the safety of individuals at venues where cornstarch powder is released, explosion control measures such as explosion containment facilities, vents, and explosion suppression and isolation devices should be installed. Furthermore, employees that work at these venues should be better trained in explosion prevention and control measures. We hope this article is a reminder to the public to recognize the fire and explosion characteristics of flammable powders as well as the preventive and control measures for dust explosions.

The 'North American shale composite' - Its compilation, major and trace element characteristics

NASA Technical Reports Server (NTRS)

Gromet, L. P.; Dymek, R. F.; Haskin, L. A.; Korotev, R. L.

1984-01-01

North American shale composite (NASC) major element composition and compilation are presented, together with rare earth element (REE) redeterminations obtained by high precision analytical methods. The major element composition of the NASC compares closely with other average shale compositions, and significant portions of the REE and some other trace elements are contained in minor phases. The uneven REE distribution in NASC powder appears to yield the heterogeneity in analyzed aliquants. REE distributions of detrital sediments may to some extent be dependent on their minor mineral assemblages and the sedimentological factors controlling these assemblages.

Floral Biosynthesis of Mn3O4 and Fe2O3 Nanoparticles Using Chaenomeles sp. Flower Extracts for Efficient Medicinal Applications

NASA Astrophysics Data System (ADS)

Karunakaran, Gopalu; Jagathambal, Matheswaran; Kolesnikov, Evgeny; Dmitry, Arkhipov; Ishteev, Artur; Gusev, Alexander; Kuznetsov, Denis

2017-08-01

Manganese oxide (Mn3O4) and iron oxide (Fe2O3) nanoparticles were successfully synthesized with the flower extracts of Chaenomeles sp. This is the first ever approach to synthesize nanoparticles from Chaenomeles sp. flower extracts. The organic molecules present in the flower extracts actively converted the nitrate precursor into its corresponding nanoparticles. The organic molecules that are involved in the synthesis of nanoparticles are identified using different phytochemical and gas chromatography-mass spectrometry analyses. The identified components are glycosides, alkaloids, terpenoids, saponins, flavonoids, quinines, and steroids. The structural and chemical compositions of the synthesized powder were also analyzed. The x-ray powder diffraction analysis revealed that the particles show tetragonal and rhombohedral crystalline phases. The Fourier transform infrared spectroscopy analysis showed the functional groups that are involved in the reduction of nitrates into the corresponding nanoparticles. Energy-dispersive x-ray spectroscopy analysis confirmed the presence of the elements in the synthesized nanoparticles. Transmission electron microscopy images showed the formation of spherical nanoparticles with an average size of 30-100 nm. Antioxidant analysis showed that the synthesized nanoparticles had excellent antioxidant potential. The antibacterial study showed that they inhibit the growth of harmful bacteria such as Pseudomonas aeruginosa and Streptococcus pyogenes. Thus, this study proposes a new eco-friendly and nontoxic method to synthesize nanoparticles for medicinal applications.

Method of forming a hardened surface on a substrate

DOEpatents

Branagan, Daniel J.

2010-08-31

The invention includes a method of producing a hard metallic material by forming a mixture containing at least 55% iron and at least one of B, C, Si and P. The mixture is formed into an alloy and cooled to form a metallic material having a hardness of greater than about 9.2 GPa. The invention includes a method of forming a wire by combining a metal strip and a powder. The metal strip and the powder are rolled to form a wire containing at least 55% iron and from two to seven additional elements including at least one of C, Si and B. The invention also includes a method of forming a hardened surface on a substrate by processing a solid mass to form a powder, applying the powder to a surface to form a layer containing metallic glass, and converting the glass to a crystalline material having a nanocrystalline grain size.

PowderSim: Lagrangian Discrete and Mesh-Free Continuum Simulation Code for Cohesive Soils

NASA Technical Reports Server (NTRS)

Johnson, Scott; Walton, Otis; Settgast, Randolph

2013-01-01

PowderSim is a calculation tool that combines a discrete-element method (DEM) module, including calibrated interparticle-interaction relationships, with a mesh-free, continuum, SPH (smoothed-particle hydrodynamics) based module that utilizes enhanced, calibrated, constitutive models capable of mimicking both large deformations and the flow behavior of regolith simulants and lunar regolith under conditions anticipated during in situ resource utilization (ISRU) operations. The major innovation introduced in PowderSim is to use a mesh-free method (SPH-based) with a calibrated and slightly modified critical-state soil mechanics constitutive model to extend the ability of the simulation tool to also address full-scale engineering systems in the continuum sense. The PowderSim software maintains the ability to address particle-scale problems, like size segregation, in selected regions with a traditional DEM module, which has improved contact physics and electrostatic interaction models.

Hardfacing material

DOEpatents

Branagan, Daniel J [Iona, ID

2012-01-17

A method of producing a hard metallic material by forming a mixture containing at least 55% iron and at least one of boron, carbon, silicon and phosphorus. The mixture is formed into an alloy and cooled to form a metallic material having a hardness of greater than about 9.2 GPa. The invention includes a method of forming a wire by combining a metal strip and a powder. The metal strip and the powder are rolled to form a wire containing at least 55% iron and from two to seven additional elements including at least one of C, Si and B. The invention also includes a method of forming a hardened surface on a substrate by processing a solid mass to form a powder, applying the powder to a surface to form a layer containing metallic glass, and converting the glass to a crystalline material having a nanocrystalline grain size.

PROCESSING OF RADIOACTIVE WASTE

DOEpatents

Allemann, R.T.; Johnson, B.M. Jr.

1961-10-31

A process for concentrating fission-product-containing waste solutions from fuel element processing is described. The process comprises the addition of sugar to the solution, preferably after it is made alkaline; spraying the solution into a heated space whereby a dry powder is formed; heating the powder to at least 220 deg C in the presence of oxygen whereby the powder ignites, the sugar is converted to carbon, and the salts are decomposed by the carbon; melting the powder at between 800 and 900 deg C; and cooling the melt. (AEC) antidiuretic hormone from the blood by the liver. Data are summarized from the following: tracer studies on cardiovascular functions; the determination of serum protein-bound iodine; urinary estrogen excretion in patients with arvanced metastatic mammary carcinoma; the relationship between alheroclerosis aad lipoproteins; the physical chemistry of lipoproteins; and factors that modify the effects of densely ionizing radia

Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

2013-02-01

NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

High Density Hydrogen Storage System Demonstration Using NaAlH4 Based Complex Compound Hydrides

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

Daniel A. Mosher; Xia Tang; Ronald J. Brown

2007-07-27

This final report describes the motivations, activities and results of the hydrogen storage independent project "High Density Hydrogen Storage System Demonstration Using NaAlH4 Based Complex Compound Hydrides" performed by the United Technologies Research Center under the Department of Energy Hydrogen Program, contract # DE-FC36-02AL67610. The objectives of the project were to identify and address the key systems technologies associated with applying complex hydride materials, particularly ones which differ from those for conventional metal hydride based storage. This involved the design, fabrication and testing of two prototype systems based on the hydrogen storage material NaAlH4. Safety testing, catalysis studies, heat exchangermore » optimization, reaction kinetics modeling, thermochemical finite element analysis, powder densification development and material neutralization were elements included in the effort.« less

KEY COMPARISON: Final report of the CCQM-K56: Ca, Fe, Zn and Cu in whole fat soybean powder

NASA Astrophysics Data System (ADS)

Liandi, Ma; Qian, Wang

2010-01-01

The CCQM-K56 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM as a follow-up to completed pilot study CCQM-P64 to test the abilities of national metrology institutes to measure the amount content of nutritious elements in whole fat soybean powder. A pilot study CCQM-P64.1 was conducted in parallel with this key comparison. The National Institute of Metrology (NIM), P. R. China, acted as the coordinating laboratory. Eleven NIMs participated in CCQM-K56. Four elements - Ca, Fe, Zn and Cu - in different concentration levels have been studied. Different measurement methods (IDMS, ICP-MS, ICP-OES, AAS and INAA) and the microwave digestion method were used. The agreement of the results of CCQM-K56 is very good, and obviously better than that of the original P64. It shows that the capability of all of the participants had been promoted from the original pilot study to this key comparison. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).

THE MANUFACTURE OF FUEL ELEMENTS OF THE ARGONAUT TYPE

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

Kittl, J.; Machado, R.E.; Mazza, J.A.

1958-06-10

The conditions required for the manufacture of the RA-1 Argonant type fuel elements are investigated. The fuel elements are in the form of a plate which is manufactured by the extrusion of a presintered mass of U/sub 3/O/sub 8/ (20% enriched) in an aluminum matrix. Steps in the investigation were obtention and specification of U/sub 3/O/sub 8/ and Al in powder form for testing, filling, and extrusion tests, finishing of the fuel elements, and computation of U/sub 3/O/sub 8/ content. (W.D.M.)

Finite element method analysis of cold forging for deformation and densification of Mo alloyed sintered steel

NASA Astrophysics Data System (ADS)

Kamakoshi, Y.; Nishida, S.; Kanbe, K.; Shohji, I.

2017-10-01

In recent years, powder metallurgy (P/M) materials have been expected to be applied to automobile products. Then, not only high cost performance but also more strength, wear resistance, long-life and so on are required for P/M materials. As an improvement method of mechanical properties of P/M materials, a densification is expected to be one of effective processes. In this study, to examine behaviours of the densification of Mo-alloyed sintered steel in a cold-forging process, finite element method (FEM) analysis was performed. Firstly, a columnar specimen was cut out from the inner part of a sintered specimen and a load-stroke diagram was obtained by the compression test. 2D FEM analysis was performed using the obtained load-stroke diagram. To correct the errors of stress between the porous mode and the rigid-elastic mode of analysis software, the analysis of a polynominal approximation was performed. As a result, the modified true stress-true strain diagram was obtained for the sintered steel with the densification. Afterwards, 3D FEM analysis of backward extrusion was carried out using the modified true stress-true strain diagram. It was confirmed that both the shape and density of the sintered steel analyzed by new FEM analysis that we suggest correspond well with experimental ones.

Improving feeding powder distribution to the compaction zone in the roller compaction.

PubMed

Yu, Mingzhe; Omar, Chalak; Schmidt, Alexander; Litster, James D; Salman, Agba D

2018-07-01

In the roller compaction process, powder flow properties have a significant influence on the uniformity of the ribbon properties. The objective of this work was to improve the powder flow in the feeding zone by developing novel feeding guiders which are located in the feeding zone close to the rollers in the roller compactor (side sealing system). Three novel feeding guiders were designed by 3D printing and used in the roller compactor, aiming to control the amount of powder passing across the roller width. The new feeding guiders were used to guide more powder to the sides between the rollers and less powder to the centre comparing to the original feeding elements. Temperature profile and porosity across the ribbon width indicated the uniformity of the ribbon properties. Using the novel feeding guiders resulted in producing ribbons with uniform temperature profile and porosity distribution across the ribbon width. The design of the feeding guiders contributed to improving the tensile strength of the ribbons produced from the compaction stage as well as reducing the fines produced from the crushing stage. Copyright © 2018 Elsevier B.V. All rights reserved.

Transport and deposition of cohesive pharmaceutical powders in human airway

NASA Astrophysics Data System (ADS)

Wang, Yuan; Chu, Kaiwei; Yu, Aibing

2017-06-01

Pharmaceutical powders used in inhalation therapy are in the size range of 1-5 microns and are usually cohesive. Understanding the cohesive behaviour of pharmaceutical powders during their transportation in human airway is significant in optimising aerosol drug delivery and targeting. In this study, the transport and deposition of cohesive pharmaceutical powders in a human airway model is simulated by a well-established numerical model which combines computational fluid dynamics (CFD) and discrete element method (DEM). The van der Waals force, as the dominant cohesive force, is simulated and its influence on particle transport and deposition behaviour is discussed. It is observed that even for dilute particle flow, the local particle concentration in the oral to trachea region can be high and particle aggregation happens due to the van der Waals force of attraction. It is concluded that the deposition mechanism for cohesive pharmaceutical powders, on one hand, is dominated by particle inertial impaction, as proven by previous studies; on the other hand, is significantly affected by particle aggregation induced by van der Waals force. To maximum respiratory drug delivery efficiency, efforts should be made to avoid pharmaceutical powder aggregation in human oral-to-trachea airway.

BONDING ALUMINUM METALS

DOEpatents

Noland, R.A.; Walker, D.E.

1961-06-13

A process is given for bonding aluminum to aluminum. Silicon powder is applied to at least one of the two surfaces of the two elements to be bonded, the two elements are assembled and rubbed against each other at room temperature whereby any oxide film is ruptured by the silicon crystals in the interface; thereafter heat and pressure are applied whereby an aluminum-silicon alloy is formed, squeezed out from the interface together with any oxide film, and the elements are bonded.

Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument

NASA Technical Reports Server (NTRS)

Chipera, S. J.; Vaniman, D. T.; Bish, D. L.; Sarrazin, P.; Feldman, S.; Blake, D. F.; Bearman, G.; Bar-Cohen, Y.

2004-01-01

A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Two novel FeII-oxalate architectures: Solvent-free synthesis, structures, thermal and magnetic studies

NASA Astrophysics Data System (ADS)

Li, Jin-Hua; Liu, Hui; Wei, Li; Wang, Guo-Ming

2015-10-01

Two novel FeII-oxalate framework with the formulas of [NH4][FeIILi3(C2O4)3] (1) and [NH4]2[FeII(C2O4)2]·H2O (2) have been prepared by an oxalic acid flux approach and structurally characterized by IR, elemental analysis, thermogravimetric analysis, single-crystal and powder X-ray diffraction. Heterometallic compound 1 displays a three-dimensional (3D) framework with a pto topology, while homometallic compound 2 features a pillar-layer architecture with a hms topology. Thermal analysis indicates that the two compounds can be stable up to 300 °C and 200 °C, respectively. Magnetic investigations suggest that the FeII ions in 1 and 2 exhibit weak magnetic exchange interactions.

Luminescent silver(I) tert-butylethynide compounds with nicotinic/isonicotinic acid as ligands

NASA Astrophysics Data System (ADS)

Xie, Yi-Ming; Fan, Yue-Yue; Lin, Fu-Lin; Hu, Ting; Liu, Jia; Lu, Can-Zhong

2017-12-01

Solvothermal reaction of tBuC≡CAg, AgBF4 and nicotinic/isonicotinic acid in acetonitrile afforded two new silver(I) tert-butylethynide double salts, namely [(tBuC≡CAg)(AgL1)3] (HL1 = nicotinic acid) (1) and [(tBuC≡CAg)(AgL1)2] (HL2 = isonicotinic acid) (2). These compounds have been characterized by elemental analysis, infrared spectra, single-crystal X-ray analysis, X-ray powder diffraction, thermogravimetric analysis, UV-visible absorption spectra, and luminescent measurement. 1 exhibits a two-dimensional coordination network, and 2 features a three-dimensional coordination architecture. Luminescence measurements indicate that 1 shows a fluorescent emission band centered at 568 nm, and 2 exhibits an intense emission maximum at 550 nm and a shoulder peak at 436 nm.

Bifunctional 3D porous Cu(I) metal-organic framework with gas sorption and luminescent properties

NASA Astrophysics Data System (ADS)

Xing, Guang'en; Zhang, Yan; Cao, Xiulian

2017-10-01

A new Cu(I) metal-organic framework, namely [Cu(L)]2n·n(H2O) (1 HL = 5-(4-Pyridyl)-1H-tetrazole), has been successfully synthesized via the solvothermal reactions of CuI and 5-(4-Pyridyl)-1H-tetrazole ligand, and further characterized by elemental analysis, powder X-ray diffraction analysis, thermal analysis and single crystal X-ray structural analysis. The L- ligand displays a μ4-N2, N3, N4, N5 coordination mode bridging Cu(I) ions into a 3D porous framework with the opened 1D channels filled by the lattice water molecules. Gas sorption investigations indicated that compound 1 can selectively adsorb CO2 over N2 at 298 K, and luminescent properties investigations revealed that compound 1 features luminescent sensing function for nitrobenzene.

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

Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

NASA Astrophysics Data System (ADS)

Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

2018-04-01

A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

Cold Spray Aluminum–Alumina Cermet Coatings: Effect of Alumina Content

NASA Astrophysics Data System (ADS)

Fernandez, Ruben; Jodoin, Bertrand

2018-04-01

Deposition behavior and deposition efficiency were investigated for several aluminum-alumina mixture compositions sprayed by cold spray. An increase in deposition efficiency was observed. Three theories postulated in the literature, explaining this increase in deposition efficiency, were investigated and assessed. Through finite element analysis, the interaction between a ceramic particle peening an impacting aluminum particle was found to be a possible mechanism to increase the deposition efficiency of the aluminum particle, but a probability analysis demonstrated that this peening event is too unlikely to contribute to the increment in deposition efficiency observed. The presence of asperities at the substrate and deposited layers was confirmed by a single-layer deposition efficiency measurement and proved to be a major mechanism in the increment of deposition efficiency of the studied mixtures. Finally, oxide removal produced by the impact of ceramic particles on substrate and deposited layers was evaluated as the complement of the other effects and found to also play a major role in increasing the deposition efficiency. It was found that the coatings retained approximately half of the feedstock powder alumina content. Hardness tests have shown a steady increase with the coating alumina content. Dry wear tests have revealed no improvement in wear resistance in samples with an alumina content lower than 22 wt.% compared to pure aluminum coatings. Adhesion strength showed a steady improvement with increasing alumina content in the feedstock powder from 18.5 MPa for pure aluminum coatings to values above 70 MPa for the ones sprayed with the highest feedstock powder alumina content.

Powder formation of {gamma} uranium-molybdenum alloys via hydration-dehydration

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

Vaz de Oliveira, Fabio Branco; Durazzo, Michelangelo; Fontenele Urano de Carvalho, Elita

2008-07-15

Gamma uranium-molybdenum alloys has been considered as fuel phase in plate type fuel elements for MTR reactors, mainly due to their acceptable performance under irradiation and metallurgical processing. To its use as a dispersion phase in aluminum matrix, a necessary step is the conversion of the as cast structure into powder, and one of the techniques considered at IPEN / CNEN - Brazil is HDH (hydration-dehydration). The alloys were produced by the induction melting technique, and samples were obtained from the alloys for the thermal treatments, under constant flow of hydrogen, for temperatures varying from 400 deg C to 600more » deg C and times from 1 to 4 hours, followed by dehydration. A preliminary characterization of the powders was made and the curves of mass variation versus time were obtained and related to the powder characteristics. This paper describes the first results on the development of the technology to the powder formation of the (5 to 10) % weight molybdenum {gamma}-UMo alloys, and discusses some of its aspects, mainly those related to the {gamma} {yields} {alpha} equilibrium data. (author)« less

Elemental composition study of heavy metal (Ni, Cu, Zn) in riverbank soil by electrokinetic-assisted phytoremediation using XRF and SEM/EDX

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

Jamari, Suhailly; Embong, Zaidi; Bakar, Ismail

Electrokinetic (EK)-assisted phytoremediation is one of the methods that have a big potential in enhancing the ability of plant uptake in soils remediation process. This research was conducted to investigate the difference in elemental composition concentration of riverbank soil and the change of pH between pre- and post-phytoremediation under the following condition: 1) control or as-receive sample; 2) Dieffenbachia spp plant with EK system (a pair of EK electrodes connected to a direct current (DC) power supply). After the electrodes were connected to a magnitude of 6V/cm{sup −1} electric field for 4 hours/day, the soil and plant samples were analyzedmore » using and X-ray Fluorescence Spectrometer (XRF) and Scanning Electron Microscope / Energy Dispersive X-ray Spectroscopy (SEM/EDX). The SEM/EDX analysis showed that concentration of elemental composition (Ni, Cu and Zn) in post-phytoremediation plant powder samples had increase while elemental concentrations in the post-phytoremediation soil samples were decreased. XRF analysis presented a variation in soil elemental composition concentration from anode to cathode where the concentration near anode region increased while decreased near the cathode region. A significant changes in soil pH were obtained where the soil pH increase in cathode region while decrease in anode region. The results reveal that the assistance of EK in phytoremediation process has increase the efficiency of plant uptake.« less

Fabrication of Thermoelectric Mg2Si by Mechanofusion and Pulsed Electric Current Sintering

NASA Astrophysics Data System (ADS)

Nanko, M.; Abe, H.; Takeda, M.; Homma, T.; Abe, H.; Kondo, A.; Naito, M.

2011-03-01

Mg2Si is a promising thermoelectric material because it is composed of non-toxic and "ubiquitous" elements, and development of an efficient production process for bulk Mg2Si is important for the fabrication of thermoelectric devices. The mechanofusion (MF) process, which is an attrition type milling process, is attractive in terms of ease of use and collection of powder materials, in addition to a reduced risk of contamination since it requires no milling medium. In the present study, the MF process was applied to produce Mg2Si powder, and pulsed electric current sintering (PECS) was then used to densify the powder. The density, microstructure and thermoelectric properties of the final bulk product were evaluated.

Compton suppression method and epithermal NAA in the determination of nutrients and heavy metals in Nigerian food and beverages.

PubMed

Ahmed, Y A; Landsberger, S; O'Kelly, D J; Braisted, J; Gabdo, H; Ewa, I O B; Umar, I M; Funtua, I I

2010-10-01

We used in this study Compton suppression method and epithermal neutron activation analysis to determine the concentration of nutrients and heavy metals in Nigerian food and beverages. The work was performed at the University of Texas TRIGA Reactor by short, medium, and long irradiation protocols, using thermal flux of 1.4x10(12)n cm(-2)s(-1) and epithermal flux of 1.4x10(11)n cm(-2)s(-1). Application of Compton suppression method has reduced interferences from Compton scattered photons thereby allowing easy evaluation of Na, Cl, Ca, Cu, Mn, Mg, Co, Cr, Rb, Fe, and Se. The epithermal NAA method has enabled determination of Cd, As, Ba, Sr, Br, I, and V with little turn-around time. Quality Control and Quality Assurance of the method was tested by analyzing four Standard Reference Materials (non-fat powdered milk, apple leaves, citrus leaves, and peach leaves) obtained from National Institute for Standards and Technology. Our results show that sorghum, millet, and maize have high values of Zn, Mn, Fe, low values of Cd, As, and Se. Powdered milks, rice, beans, and soybeans were found to have moderate amounts of all the elements. Tobacco recorded high content of Cd, Mn, and As, whereas tea, tsobo leaves, Baobab leaves, and okro seed have more As values than others. However, biscuits, macaroni, spaghetti, and noodles show lower concentrations of all the elements. The distribution of these nutrients and heavy metals in these food and beverages shows the need to fortify biscuits and pastas with micro and macro-nutrients and reduce the use of tobacco, tea, tsobo leaves, Baobab leaves, and Okro seed to avoid intake of heavy elements. Copyright 2010 Elsevier Ltd. All rights reserved.

Research of polishing process to control the iron contamination on the magnetorheological finished KDP crystal surface.

PubMed

Chen, Shaoshan; Li, Shengyi; Peng, Xiaoqiang; Hu, Hao; Tie, Guipeng

2015-02-20

A new nonaqueous and abrasive-free magnetorheological finishing (MRF) method is adopted for processing a KDP crystal. MRF polishing is easy to result in the embedding of carbonyl iron (CI) powders; meanwhile, Fe contamination on the KDP crystal surface will affect the laser induced damage threshold seriously. This paper puts forward an appropriate MRF polishing process to avoid the embedding. Polishing results show that the embedding of CI powders can be avoided by controlling the polishing parameters. Furthermore, on the KDP crystal surface, magnetorheological fluids residua inevitably exist after polishing and in which the Fe contamination cannot be removed completely by initial ultrasonic cleaning. To solve this problem, a kind of ion beam figuring (IBF) polishing is introduced to remove the impurity layer. Then the content of Fe element contamination and the depth of impurity elements are measured by time of flight secondary ion mass spectrometry. The measurement results show that there are no CI powders embedding in the MRF polished surface and no Fe contamination after the IBF polishing process, respectively. That verifies the feasibility of MRF polishing-IBF polishing (cleaning) for processing a KDP crystal.

Preparation of Cu2ZnSnS4 nano-crystalline powder by mechano-chemical method

NASA Astrophysics Data System (ADS)

Alirezazadeh, Farzaneh; Sheibani, Saeed; Rashchi, Fereshteh

2018-01-01

Copper zinc tin sulfide (Cu2ZnSnS4, CZTS) is one of the most promising ceramic materials as an absorber layer in solar cells due to its suitable band gap, high absorption coefficient and non-toxic and environmental friendly constituent elements. In this work, nano-crystalline CZTS powder was synthesized by mechanical milling. Elemental powders of Cu, Zn, Sn and were mixed in atomic ratio of 2:1:1:4 according to the stoichiometry of Cu2ZnSnS4 and then milled in a planetary high energy ball mill under argon atmosphere. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and diffusion reflectance spectroscopy (DRS). XRD results confirm the formation of single-phase CZTS with kesterite structure after 20 h of milling. Also, the mean crystallite size was about 35 nm. SEM results show that after 20 h of milling, the product has a relatively uniform particle size distribution. Optical properties of the product indicate that the band gap of prepared CZTS is 1.6 eV which is near to the optimum value for photovoltaic solar cells showing as a light absorber material in solar energy applications.

Dielectric relaxation in AC powder electroluminescent devices

NASA Astrophysics Data System (ADS)

Zhang, Shuai; Su, Haibin; Tan, Chuan Seng; Wong, Terence Kin Shun; Teo, Ronnie Jin Wah

2017-01-01

The dielectric properties of AC powder electroluminescent devices were measured and analyzed using complex impedance spectroscopy to determine the relaxation processes occurring within the devices. The relaxation processes identified were ascribed to the electrode polarization caused by ion accumulation at the electrode/resin interfaces, the Maxwell-Wagner-Sillars effects at the (ZnS or BaTiO3) particle/resin interfaces, and the dipolar reorientation of polymer chains in the resin matrix. Each relaxation process was represented by its corresponding equivalent circuit component. Space charge polarization at the electrodes were represented by a Warburg element, a resistor, and a constant phase element. The resin matrix, ZnS/resin and BaTiO3/resin interfaces could each be modeled by a resistor and a capacitor in parallel. The simulated equivalent circuits for three different printed structures showed good fitting with their experimental impedance results.

Diffusion of Siderophile Elements in Iron Meteorites

NASA Astrophysics Data System (ADS)

Watson, H. C.; Watson, E. B.

2001-12-01

Preliminary results for diffusion of siderophile elements (Cu, Os, Pd, Re, Os, and Mo) in an iron meteorite analog were obtained at 1400° C and 1GPa from diffusion couple experiments in a piston-cylinder apparatus. Alloys were prepared by synthesizing mixtures of pure metal powders. The alloys were made from a 90 wt% Fe and 10 wt% Ni base mixture, and approximately 1wt% of the various siderophile elements was added (individually) to the same base mixture to make the doped alloys. The powders were packed in pre-drilled holes (~1 mm dia. by 8 mm deep) in MgO cylinders, and run in a piston cylinder apparatus at 1400° C and 1GPa for 48 hours. The resulting homogeneous alloys were then sectioned into wafers approximately 1mm thick, and the faces were polished to prepare for the diffusion experiments. A diffusion couple experiment was conducted by mating a pure alloy wafer and a doped wafer, and placing the couple into an MgO capsule for pressurization and heating in the piston cylinder. The duration of the diffusion experiments ranged from 33 hours to 72 hours. Upon run completion, the diffusion couples were extracted, sectioned lengthwise, and polished for analysis. Diffusion profiles were measured using an electron microprobe. From these experiments it was found that at 1400° C and 1GPa the diffusion coefficient of Os is 1.6E-14 m2/s, the diffusion coefficient of Re is 2.8E-14 m2/s, for Pd it is 9.2E-14 m2/s, for Cu it is 1.2E-13 m2/s, and for Mo it is 2.3E-13 m2/s. These preliminary results raise the possibility that significant diffusive fraction of siderophile elements may occur in metal-silicate systems that fail to equilibrate fully, or under disequilibrium crystallization in pure metal systems.

Employing linear tetranuclear [Zn4(COO)4(OH)2] clusters as building subunits to construct a new Zn(II) coordination polymer with tunable luminescent properties

NASA Astrophysics Data System (ADS)

Li, Wu-Wu; Zhang, Zun-Ting

2016-02-01

A new Zn(II) coordination polymer, [Zn2(btc) (biimpy) (OH)]n (1 H3btc = 1,3,5-benzenetricarboxylic acid, biimpy = 2,6-bis(1-imdazoly)pyridine) has been successfully synthesized and characterized by elemental analysis, powder single crystal X-ray diffraction analyses. Compound 1 features a 3D framework employing linear tetranuclear [Zn4(COO)4(OH)2] cluster as building subunits. Topological analysis reveals it represents a (3,10)-connected structural topology by viewing btc3-, linear tetranuclear clusters and biimpy as 3-connected nodes, 10-connected nodes, linear linkers, respectively. Moreover, the thermal stability and luminescent property of compound 1 have been well investigated.

Bringing a Chemical Laboratory Named Sam to Mars on the 2011 Curiosity Rover

NASA Technical Reports Server (NTRS)

Mahaffy, P. R.; Bleacher, L.; Jones, A.; Conrad, P. G.; Cabane, M.; Webster, C. R.; Atreya, S. A.; Manning, H.

2010-01-01

An important goal of upcoming missions to Mars is to understand if life could have developed there. The task of the Sample Analysis at Mars (SAM) suite of instruments [1] and the other Curiosity investigations [2] is to move us steadily toward that goal with an assessment of the habitability of our neighboring planet through a series of chemical and geological measurements. SAM is designed to search for organic compounds and inorganic volatiles and measure isotope ratios. Other instruments on Curiosity will provide elemental analysis and identify minerals. SAM will analyze both atmospheric samples and gases evolved from powdered rocks that may have formed billions of years ago with Curiosity providing access to interesting sites scouted by orbiting cameras and spectrometers.

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.

Synthesis, spectroscopic characterization, electrochemistry and biological evaluation of some binuclear transition metal complexes of bicompartmental ONO donor ligands containing benzo[b]thiophene moiety

NASA Astrophysics Data System (ADS)

Mahendra Raj, K.; Vivekanand, B.; Nagesh, G. Y.; Mruthyunjayaswamy, B. H. M.

2014-02-01

A series of new binucleating Cu(II), Co(II), Ni(II) and Zn(II) complexes of bicompartmental ligands with ONO donor were synthesized. The ligands were obtained by the condensation of 3-chloro-6-substituted benzo[b]thiophene-2-carbohydrazides and 4,6-diacetylresorcinol. The synthesized ligands and their complexes were characterized by elemental analysis and various spectroscopic techniques. Elemental analysis, IR, 1H NMR, ESI-mass, UV-Visible, TG-DTA, magnetic measurements, molar conductance and powder-XRD data has been used to elucidate their structures. The bonding sites are the oxygen atom of amide carbonyl, azomethine nitrogen and phenolic oxygen for ligands 1 and 2. The binuclear nature of the complexes was confirmed by ESR spectral data. TG-DTA studies for some complexes showed the presence of coordinated water molecules and the final product is the metal oxide. All the complexes were investigated for their electrochemical activity, only the Cu(II) complexes showed the redox property. Cu(II) complexes were square planar, whereas Co(II), Ni(II) and Zn(II) complexes were octahedral. Powder-XRD pattern have been studied in order to test the degree of crystallinity of the complexes and unit cell calculations were made. In order to evaluate the effect of antimicrobial activity of metal ions upon chelation, both the ligands and their metal complexes were screened for their antibacterial and antifungal activities by minimum inhibitory concentration (MIC) method. The results showed that the metal complexes were found to be more active than free ligands. The DNA cleaving capacities of all the complexes were analyzed by agarose gel electrophoresis method against supercoiled plasmid DNA. Among the compounds tested for antioxidant capacity, ligand 1 displayed excellent activity than its metal complexes.

Plasma methods of obtainment of multifunctional composite materials, dispersion-hardened by nanoparticles

NASA Astrophysics Data System (ADS)

Sizonenko, O. N.; Grigoryev, E. G.; Zaichenko, A. D.; Pristash, N. S.; Torpakov, A. S.; Lipyan, Ye V.; Tregub, V. A.; Zholnin, A. G.; Yudin, A. V.; Kovalenko, A. A.

2016-04-01

The new approach in developed plasma methods consists in that dispersionhardening additives (TiC, TiB2 in particular) are not mechanically added to powder mixture as additional component, as in conventional methods, but are instead synthesized during high voltage electric discharges (HVED) in disperse system “hydrocarbon liquid - powder” preservation of ultrafine structure is ensured due to use of spark plasma sintering (SPS) as a consolidation method. HVED in disperse system “hydrocarbon liquid - powder” due to impact of plasma discharge channel, electromagnetic fields, shock waves mechanical impact, hydro flows and volume microcavitation leads to synthesis of nanocarbon, metal powders dispersion and synthesis of micro- (from 10-6 to 10-7 m) and nanosized (from 10-7 to 10-9 m) composite powders of hardening phases. SPS is the passage of pulsed current (superposition of direct and alternating current) through powder with the simultaneous mechanical compressing. The formation of plasma is initiated in gaseous phase that fills gaps between particles. SPS allows targeted control of grain growth rate and thus allows obtainment of multifunctional composite materials dispersion hardened by nanoparticles. Processes of HVED synthesis of micro- and nanosized powders of new compositions from elemental metal powders and their mixtures with the subsequent application of high-speed SPS of obtained powders create conditions for increase of strength (by 10 - 20%), hardness and wear-resistance (by 30 - 60%) of obtained materials.

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.

Characterization of Metal Powders Used for Additive Manufacturing.

PubMed

Slotwinski, J A; Garboczi, E J; Stutzman, P E; Ferraris, C F; Watson, S S; Peltz, M A

2014-01-01

Additive manufacturing (AM) techniques can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process.

On the nature and origin of the oxalate package in Solanum sisymbriifolium anthers.

PubMed

Burrieza, Hernán Pablo; López-Fernández, María Paula; Láinez, Verónica; Montenegro, Teresita; Maldonado, Sara

2010-11-01

This is a detailed study carried out in Solanum sisymbriifolium Lam. on the development of the circular cell cluster (CCC) during crystal deposition, as well as the composition of the crystals. Light microscopy and scanning and transmission electron microscopy (TEM) were used to characterize tissue throughout anther development. Energy dispersive X-ray analysis (EDAX) allowed the determination of the elemental composition of crystals that form in the CCC region, and infrared and x-ray diffraction analysis were used to specify the crystal salt composition. TEM analysis revealed that the crystals originated simultaneously within the vacuoles in association with a paracrystalline protein. Prior to the appearance of protein within vacuoles, protein paracrystals were visible in both rough endoplasmic reticulum and vesicles with ribosomes on their membranes. In vacuoles, paracrystals constitute nucleation sites for druse crystals formation. EDAX revealed that C, O, and Ca were the main elements, and K, Cl, Mg, P, S, and Si, the minor elements. X-ray powder diffraction of crystals detected the predominant presence of calcium oxalate, but also vestiges of calcite, quartz, and sylvite. The calcium oxalate coexisted in the three chemical forms, that is, whewellite, weddellite, and caoxite. Infrared spectrophotometry identified bands that characterize O-C-O, H-O, C-H bonds, all of calcium oxalate, and Si-O-Si, of quartz. These results were compared with studies of anthers carried out in other Solanaceae genera.

[Analysis and characterization of Belamcanda chinensis with space mutagenesis breeding by X-ray fluorescence analysis and X-ray diffraction].

PubMed

Guan, Ying; Ding, Xi-Feng; Wang, Wen-Jing; Guo, Xi-Hua; Zhu, Yan-Ying

2008-02-01

The contents of various elements in the fourth generation Belamcanda chinensis (L.) DC. with space mutagenesis breeding were analyzed and characterized. X-ray fluorescence spectrum analysis (XRF) and powder X-ray diffraction (PXRD) were applied jointly. It was found that the content of K element in the space flight mutagenesis increases 1.03 and 0.31 times, Mg enhances 1.44 and 0.06 times, but Al reduces 38.5% and 85.5% respectively compared to the contents in the ground group and the comparison group, while those of Ca, Mn and Fe enhance 0.95, 0.30 and 0.29 times respectively contrasted to the ground group. Besides, there was discovered the crystal of whewellite in the Belamcanda chinensis (L.) DC. and the content in the ground group is less than that of the outer space and the outer space group, which in turn is less than that of the comparison group. It is concluded that the contents of mineral elements indispensable to body in the space group are closer or superior to the comparison, group as compared to the ground group. In the present paper, a quick and simple appraising method is offered, which may be of great significance to the popularization of the planting outer space Chinese traditional medicine to filtrate more excellent breed and set up norm of quality appraisal.

pXRF quantitative analysis of the Otowi Member of the Bandelier Tuff: Generating large, robust data sets to decipher trace element zonation in large silicic magma chambers

NASA Astrophysics Data System (ADS)

Van Hoose, A. E.; Wolff, J.; Conrey, R.

2013-12-01

Advances in portable X-Ray fluorescence (pXRF) analytical technology have made it possible for high-quality, quantitative data to be collected in a fraction of the time required by standard, non-portable analytical techniques. Not only do these advances reduce analysis time, but data may also be collected in the field in conjunction with sampling. Rhyolitic pumice, being primarily glass, is an excellent material to be analyzed with this technology. High-quality, quantitative data for elements that are tracers of magmatic differentiation (e.g. Rb, Sr, Y, Nb) can be collected for whole, individual pumices and subsamples of larger pumices in 4 minutes. We have developed a calibration for powdered rhyolite pumice from the Otowi Member of the Bandelier Tuff analyzed with the Bruker Tracer IV pXRF using Bruker software and influence coefficients for pumice, which measures the following 19 oxides and elements: SiO2, TiO2, Al2O3, FeO*, MnO, CaO, K2O, P2O5, Zn, Ga, Rb, Sr, Y, Zr, Nb, Ba, Ce, Pb, and Th. With this calibration for the pXRF and thousands of individual powdered pumice samples, we have generated an unparalleled data set for any single eruptive unit with known trace element zonation. The Bandelier Tuff of the Valles-Toledo Caldera Complex, Jemez Mountains, New Mexico, is divided into three main eruptive events. For this study, we have chosen the 1.61 Ma, 450 km3 Otowi Member as it is primarily unwelded and pumice samples are easily accessible. The eruption began with a plinian phase from a single source located near center of the current caldera and deposited the Guaje Pumice Bed. The initial Unit A of the Guaje is geochemically monotonous, but Units B through E, co-deposited with ignimbrite show very strong chemical zonation in trace elements, progressing upwards through the deposits from highly differentiated compositions (Rb ~350 ppm, Nb ~200 ppm) to less differentiated (Rb ~100 ppm, Nb ~50 ppm). Co-erupted ignimbrites emplaced during column collapse show similar trace element zonation. The eruption culminated in caldera collapse after transitioning from a single central vent to ring fracture vents. Ignimbrites deposited at this time have lithic breccias and chaotic geochemical profiles. The geochemical discrepancy between early and late deposits warrants detailed, high-resolution sampling and analysis in order to fully understand the dynamics behind zonation processes. Samples were collected from locations that circumvent the caldera and prepared and analyzed in the field and the laboratory with the pXRF. Approximately 2,000 pumice samples will complete this unprecedented data set, allowing detailed reconstruction of trace element zonation around all sides of the Valles Caldera. These data are then used to constrain models of magma chamber processes that produce trace element zonation and how it is preserved in the deposits after a catastrophic, caldera-forming eruption.

Synchrotron WAXS and XANES studies of silica (SiO2) powders synthesized from Indonesian natural sands

NASA Astrophysics Data System (ADS)

Muchlis, Khairanissa; Aini Fauziyah, Nur; Soontaranon, Siriwat; Limpirat, Wanwisa; Pratapa, Suminar

2017-01-01

In this study, we have investigated polymorphic silica (SiO2) powders using, Wide Angle X-ray Scattering (WAXS) and X-Ray Absorption Near Edge Spectroscopy (XANES), laboratory X-Ray Diffraction (XRD) instruments. The WAXS and XANES spectra were collected using synchrotron radiation at Synchrotron Light Research Institute (SLRI), Nakhon Ratchasima, Thailand. The silica powders were obtained by processing silica sand from Tanah Laut, South Kalimantan, Indonesia. Purification process of silica sand was done by magnetic separation and immersion with HCl. The purification step was needed to reduce impurity or undesirable non Si elements. Three polymorphs of silica were produced, i.e. amorphous phase (A), quartz (B), and cristobalite (C). WAXS profile for each phase was presented in terms of intensity vs. 2θ prior to analyses. Both XRD (λCuKα=1.54056 Å) and WAXS (λ=1.09 Å) patttern show that (1) A sample contains no crystallites, (2) B sample is monophasic, contains only quartz, and (3) C sample contains cristobalite and trydimite. XRD quantitative analysis using Rietica gave 98,8 wt% cristobalite, while the associated WAXS data provided 98.7 wt% cristobalite. Si K-edge XANES spectra were measured at energy range 1840 to 1920 eV. Qualitatively, the pre-edge and edge features for all phases are similar, but their main peaks in the post-edge region are different.

Phase analysis of ZrO2-SiO2 systems synthesized through Ball milling mechanical activations

NASA Astrophysics Data System (ADS)

Nurlaila, Rizka; Musyarofah, Muwwaqor, Nibras Fuadi; Triwikantoro, Kuswoyo, Anton; Pratapa, Suminar

2017-01-01

Zircon powders have been produced from raw materials of amorphous zirconia and amorphous silica powders obtained from natural zircon sand of Kalimantan Tengah, Indonesia. Synthesis process was started with the extraction of zircon powder to produce sodium silicate solution and pure zircon powder. The amorphous zirconia and silica powders were prepared by alkali fusion and co-precipitation techniques. The powders were mixed using a planetary ball mill, followed by a calcination of various holding time of 3, 10, and 15 h. Phase characterization was done using X-Ray Diffraction (XRD) technique and analysis of the diffraction data was carried out using Rietica and MAUD software. The identified phases after the calcination were zircon, tetragonal zirconia, and cristobalite. The highest zircon content was obtained in the sample calcinated for15 hours - reaching 99.66 %wt. Crystallite size analysis revealed that the samples calcinated for 3, 10, and 15 h exhibited zircon crystal size of 176 (1) nm, 191 (1) nm and 233 (1) nm respectively.

A dietary strategy for the management of artemether-lumefantrine-induced cardiovascular and renal toxicity.

PubMed

Asiedu-Gyekye, Isaac Julius; Seidu, Mahmood Abdulai; N'guessan, Banga Benoit; Frimpong-Manso, Samuel; Sarkodie, Joseph Edusei; Adjei, Samuel; Kutu, Schevadnazy; Osei-Little, Joseph; Nyarko, Alexander Kwadwo; Debrah, Philip

2016-09-06

Unsweetened natural cocoa has antimalarial properties. Unsweetened natural cocoa powder (UNCP), obtained as a result of the removal of cocoa butter from a cocoa bean protects against malaria episodes. Cocoa powder, which is prepared after removal of the cocoa butter, contains about 1.9 % theobromine and 0.21 % caffeine. Concomitant consumption of cocoa and artemether/lumefantrine (A/L) is a common practice in Ghana, West Africa. This study seeks to determine the elemental composition of UNCP and its protective effect on the heart and kidney against (A/L) administration. Energy dispersive x-ray fluorescence spectroscopy was used to detect the quality and quantity of the elemental composition in UNCP. Thereafter, 30 nonmalarious male guinea pigs were divided into five groups of six animals each. One group was administered with 75 mg/kg body weight A/L only and another group distilled water (control group). The rest received 300 mg/kg, 900 mg/kg and 1500 mg/kg body weight UNCP for 14 days orally and A/L for the last 3 days (ie day 11 to day 14). Biochemical and histopathological examinations were carried out after euthanisation of the animals. A total of thirty-eight (38) micro and macro elements were detected with the ED-XRF. Macro elements like sodium (Na), magnesium (Mg), aluminium (Al), phosphorus (P), chlorine (Cl), potassium (K), calcium (Ca), manganese (Mn) and iron (Fe) and micro elements like chromium (Cr), copper (Cu), zinc (Zn), arsenic (As), and lead (Pb) were identified and evaluated. Biochemical analysis revealed increases in HDL levels (p>0.05) while there were decreases in LDL levels (p>0.05), creatine kinase and AST levels (P<0.05) in animals that received UNCP compared to A/L only administered group. Urea levels reduced significantly by 53 % (p<0.05) in group that received 1500 mg/kg UNCP. Histopathological examinations of the heart and kidney buttressed the protective effects of cocoa administration. The percentage of recommended daily allowance of UNCP for chromium is 3750 % for men and 5250 % for women while % RDA for copper corresponds to 103.6 % in both sexes. UNCP proved to possess cardioprotective and renoprotective potential during artemether-lumefantrine administration.

Analysis of the mechanical behavior of a titanium scaffold with a repeating unit-cell substructure.

PubMed

Ryan, Garrett; McGarry, Patrick; Pandit, Abhay; Apatsidis, Dimitrios

2009-08-01

Titanium scaffolds with controlled microarchitecture have been developed for load bearing orthopedic applications. The controlled microarchitecture refers to a repeating array of unit-cells, composed of sintered titanium powder, which make up the scaffold structure. The objective of this current research was to characterize the mechanical performance of three scaffolds with increasing porosity, using finite element analysis (FEA) and to compare the results with experimental data. Scaffolds were scanned using microcomputed tomography and FEA models were generated from the resulting computer models. Macroscale and unit-cell models of the scaffolds were created. The material properties of the sintered titanium powders were first evaluated in mechanical tests and the data used in the FEA. The macroscale and unit-cell FEA models proved to be a good predictor of Young's modulus and yield strength. Although macroscale models showed similar failure patterns and an expected trend in UCS, strain at UCS did not compare well with experimental data. Since a rapid prototyping method was used to create the scaffolds, the original CAD geometries of the scaffold were also evaluated using FEA but they did not reflect the mechanical properties of the physical scaffolds. This indicates that at present, determining the actual geometry of the scaffold through computed tomography imaging is important. Finally, a fatigue analysis was performed on the scaffold to simulate the loading conditions it would experience as a spinal interbody fusion device.

Understanding the Different Effects of Inhaler Design on the Aerosol Performance of Drug-Only and Carrier-Based DPI Formulations. Part 1: Grid Structure.

PubMed

Leung, Cassandra Ming Shan; Tong, Zhenbo; Zhou, Qi Tony; Chan, John Gar Yan; Tang, Patricia; Sun, Siping; Yang, Runyu; Chan, Hak-Kim

2016-09-01

The design of a dry powder inhaler device has significant influence on aerosol performance; however, such influence may be different between the drug-only and carrier-based formulations. The present study aims to examine the potential difference on the dispersion between these distinct types of formulations, using Aerolizer(®) as a model inhaler with the original or modified (cross-grid) designs. A coupled CFD-discrete element method analysis was employed to determine the flow characteristics and particle impaction. Micronized salbutamol sulphate as a drug-only formulation and three lactose carrier-based formulations with various drug-to-carrier weight ratios 1:5, 1:10 and 1:100 were used. The in vitro aerosolization performance was assessed by a next-generation impactor operating at 100 L/min. Using the original device, FPFloaded was reduced from 47.5 ± 3.8% for the drug-only formulation to 31.8 ± 0.7%, 32.1 ± 0.7% and 12.9 ± 1.0% for the 1:5, 1:10 and 1:100 formulations, respectively. With the cross-grid design, powder-mouthpiece impaction was increased, which caused not only powder deagglomeration but also significant drug retention (doubling or more) in the mouthpiece, and the net result is a significant decrease in FPFloaded to 36.8 ± 1.2%, 20.9 ± 2.6% and 21.9 ± 1.5% for the drug-only, 1:5 and 1:10 formulations, respectively. In contrast, the FPFloaded of the 1:100 formulation remained the same at 12.1 ± 1.3%, indicating the increased mouthpiece drug retention was compensated by increased drug detachment from carriers caused by increased powder-mouthpiece impaction. In conclusion, this study has elucidated different effects and the mechanism on the aerosolization of varied dry powder inhaler formulations due to the grid design.

Clusters of Monoisotopic Elements for Calibration in (TOF) Mass Spectrometry

NASA Astrophysics Data System (ADS)

Kolářová, Lenka; Prokeš, Lubomír; Kučera, Lukáš; Hampl, Aleš; Peňa-Méndez, Eladia; Vaňhara, Petr; Havel, Josef

2017-03-01

Precise calibration in TOF MS requires suitable and reliable standards, which are not always available for high masses. We evaluated inorganic clusters of the monoisotopic elements gold and phosphorus (Au n +/Au n - and P n +/P n -) as an alternative to peptides or proteins for the external and internal calibration of mass spectra in various experimental and instrumental scenarios. Monoisotopic gold or phosphorus clusters can be easily generated in situ from suitable precursors by laser desorption/ionization (LDI) or matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Their use offers numerous advantages, including simplicity of preparation, biological inertness, and exact mass determination even at lower mass resolution. We used citrate-stabilized gold nanoparticles to generate gold calibration clusters, and red phosphorus powder to generate phosphorus clusters. Both elements can be added to samples to perform internal calibration up to mass-to-charge ( m/z) 10-15,000 without significantly interfering with the analyte. We demonstrated the use of the gold and phosphorous clusters in the MS analysis of complex biological samples, including microbial standards and total extracts of mouse embryonic fibroblasts. We believe that clusters of monoisotopic elements could be used as generally applicable calibrants for complex biological samples.

Hydrometallurgical separation of rare earth elements, cobalt and nickel from spent nickel-metal-hydride batteries

NASA Astrophysics Data System (ADS)

Rodrigues, Luiz Eduardo Oliveira Carmo; Mansur, Marcelo Borges

The separation of rare earth elements, cobalt and nickel from NiMH battery residues is evaluated in this paper. Analysis of the internal content of the NiMH batteries shows that nickel is the main metal present in the residue (around 50% in weight), as well as potassium (2.2-10.9%), cobalt (5.1-5.5%), rare earth elements (15.3-29.0%) and cadmium (2.8%). The presence of cadmium reveals that some Ni-Cd batteries are possibly labeled as NiMH ones. The leaching of nickel and cobalt from the NiMH battery powder with sulfuric acid is efficient; operating variables temperature and concentration of H 2O 2 has no significant effect for the conditions studied. A mixture of rare earth elements is separated by precipitation with NaOH. Finally, solvent extraction with D2EHPA (di-2-ethylhexyl phosphoric acid) followed by Cyanex 272 (bis-2,4,4-trimethylpentyl phosphinic acid) can separate cadmium, cobalt and nickel from the leach liquor. The effect of the main operating variables of both leaching and solvent extraction steps are discussed aiming to maximize metal separation for recycling purposes.

Pulsed—Laser Deposition Of Oxide Thin Films And Laser—Induced Breakdown Spectroscopy Of Multi—Element Materials

NASA Astrophysics Data System (ADS)

Pedarnig, Johannes D.

2010-10-01

New results of the Linz group on pulsed—laser deposition (PLD) of oxide thin films and on laser—induced breakdown spectroscopy (LIBS) of multi-element materials are reported. High-Tc superconducting (HTS) films with enhanced critical current density Jc are produced by laser ablation of novel nano-composite ceramic targets. The targets contain insulating nano-particles that are embedded into the YBa2Cu3O7 matrix. Epitaxial double-layers of lithium-doped and aluminum-doped ZnO are deposited on r-cut sapphire substrates. Acoustic over-modes in the GHz range are excited by piezoelectric actuation of layers. Smooth films of rare-earth doped glass are produced by F2—laser ablation. The transport properties of HTS thin films are modified by light—ion irradiation. Thin film nano—patterning is achieved by masked ion beam irradiation. LIBS is employed to analyze trace elements in industrial iron oxide powder and reference polymer materials. Various trace elements of ppm concentration are measured in the UV/VIS and vacuum-UV spectral range. Quantitative LIBS analysis of major components in oxide materials is performed by calibration-free methods.

Ballistic Characterization of the Scalability of Magnesium Alloy AMX602

DTIC Science & Technology

2015-07-01

Powder Metallurgy 4 5. Fabrication Procedure 4 6. Mechanical Property Analysis 5 7. Ballistic Experimental Procedures 6 8. Ballistic Experimental...compositions of noncombustive Mg alloy powders 4. Powder Metallurgy The powder was consolidated at room temperature using a 2,000-kN hydraulic press...evaluation of advanced powder metallurgy magnesium alloys for dynamic applications. Aberdeen Proving Ground (MD): Army Research Laboratory (US); 2009 May

Numerical Simulation of Sintering Process in Ceramic Powder Injection Moulded Components

NASA Astrophysics Data System (ADS)

Song, J.; Barriere, T.; Liu, B.; Gelin, J. C.

2007-05-01

A phenomenological model based on viscoplastic constitutive law is presented to describe the sintering process of ceramic components obtained by powder injection moulding. The parameters entering in the model are identified through sintering experiments in dilatometer with the proposed optimization method. The finite element simulations are carried out to predict the density variations and dimensional changes of the components during sintering. A simulation example on the sintering process of hip implant in alumina has been conducted. The simulation results have been compared with the experimental ones. A good agreement is obtained.

Electrical relaxation, optical and magnetic studies of nanocrystalline lithium ferrite synthesized by different chemical routes

NASA Astrophysics Data System (ADS)

Cheruku, Rajesh; Govindaraj, G.; Vijayan, Lakshmi

2017-12-01

The nanocrystalline lithium ferrite was synthesized by wet chemical methods such as solution combustion technique, sol-gel, and hydrothermal for a comparative study. Different characterization techniques like x-ray powder diffraction and thermal analysis were employed to confirm the structure and phase. Temperature-dependent Raman analysis was employed to classify the phonon modes associated with precise atomic motions existing in the synthesized materials. Morphology of sample surface was explored by scanning electron microscopy, and elemental analysis was done by energy dispersive spectroscopy analysis. The nanocrystalline nature of the materials was confirmed through transmission electron microscopy. Magnetic properties of these samples were explored through a vibrating sample magnetometer. Ac electrical impedance spectroscopy data were investigated using two Cole-Cole functions, and activation energies were calculated for all materials. Among them, solution combustion prepared lithium ferrite shows the highest conductivity and lowest activation energy.

Synthesis of CaCu3Ti4O12 by modified Sol-gel method with Hydrothermal process

NASA Astrophysics Data System (ADS)

Masingboon, C.; Rungruang, S.

2017-09-01

CaCu3Ti4O12 powders were synthesized by modified Sol-gel method with Hydrothermal process using Ca(NO3)2· 4H2O, Cu(NO3)2·3H2O, Ti(OC3H7)4 and freshly extracted egg white (ovalbumin) in aqueous medium. The precursor was calcined at 800, 900 and 1000 °C in air for 8 h to obtain nanocrystalline powders of CaCu3Ti4O12. The calcined CaCu3Ti4O12 powders were characterized by XRD, TEM and EDX. The XRD results indicated that all calcined samples have a typical perovskite CaCu3Ti4O12 structure and a small amount of CaTiO3, CuO and TiO2. TEM micrographs showed particle size 100 - 500 nm and EDX results showed elements of CaCu3Ti4O12 powders have calcium, copper, titanium and oxygen.

Ultrasonic-assisted preparation of nano eggshell powder: a novel catalyst in green and high efficient synthesis of 2-aminochromenes.

PubMed

Mosaddegh, Elaheh

2013-11-01

The nano eggshell powder (NESP) has been prepared by ultrasound irradiation and used as a novel and biodegradable catalyst with high catalytic activity and reusability in green synthesis of 2-aminochromenes via condensation of α- or β-phathol, malononitrile and aromatic aldehydes at 120 °C under solvent-free conditions. The reaction proceeds to completion within 10-35 min in 91-98% yield. Nano eggshell catalyst was characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and X-ray fluorescence, thermal gravimetric, surface area and elemental analyses. In addition, the catalytic activity and chemical structure of nano-sized eggshell were compared with pure CaCO3. Copyright © 2013 Elsevier B.V. All rights reserved.

Design of Wear-Resistant Austenitic Steels for Selective Laser Melting

NASA Astrophysics Data System (ADS)

Lemke, J. N.; Casati, R.; Lecis, N.; Andrianopoli, C.; Varone, A.; Montanari, R.; Vedani, M.

2018-03-01

Type 316L stainless steel feedstock powder was modified by alloying with powders containing carbide/boride-forming elements to create improved wear-resistant austenitic alloys that can be readily processed by Selective Laser Melting. Fe-based alloys with high C, B, V, and Nb contents were thus produced, resulting in a microstructure that consisted of austenitic grains and a significant amount of hard carbides and borides. Heat treatments were performed to modify the carbide distribution and morphology. Optimal hard-phase spheroidization was achieved by annealing the proposed alloys at 1150 °C for 1 hour followed by water quenching. The total increase in hardness of samples containing 20 pct of C/B-rich alloy powder was of 82.7 pct while the wear resistance could be increased by a factor of 6.

[Advances in studies on bear bile powder].

PubMed

Zhou, Chao-fan; Gao, Guo-jian; Liu, Ying

2015-04-01

In this paper, a detailed analysis was made on relevant literatures about bear bile powder in terms of chemical component, pharmacological effect and clinical efficacy, indicating bear bile powder's significant pharmacological effects and clinical application in treating various diseases. Due to the complex composition, bear bile powder is relatively toxic. Therefore, efforts shall be made to study bear bile powder's pharmacological effects, clinical application, chemical composition and toxic side-effects, with the aim to provide a scientific basis for widespread reasonable clinical application of bear bile powder.

FGM (Functionally Graded Material) Thermal Barrier Coatings for Hypersonic Structures - Design and Thermal Structural Analysis

DTIC Science & Technology

2007-06-29

than others. It was found that TZ-3Y-E, which is a partially stabilised zirconia powder , was particularly suitable. The percentage of ceramic powder...layered coatings The current ceramic powder that was being used was a fully stabilised zirconia powder TZ-0Y. However a readily available powder...TZ-3Y-E, partially stabilised zirconia powder , was available and utilised. These tests consisted of a combination of 3, 4 and 5 layers. In the

Characterization of Metal Powders Used for Additive Manufacturing

PubMed Central

Slotwinski, JA; Garboczi, EJ; Stutzman, PE; Ferraris, CF; Watson, SS; Peltz, MA

2014-01-01

Additive manufacturing (AM) techniques1 can produce complex, high-value metal parts, with potential applications as critical parts, such as those found in aerospace components. The production of AM parts with consistent and predictable properties requires input materials (e.g., metal powders) with known and repeatable characteristics, which in turn requires standardized measurement methods for powder properties. First, based on our previous work, we assess the applicability of current standardized methods for powder characterization for metal AM powders. Then we present the results of systematic studies carried out on two different powder materials used for additive manufacturing: stainless steel and cobalt-chrome. The characterization of these powders is important in NIST efforts to develop appropriate measurements and standards for additive materials and to document the property of powders used in a NIST-led additive manufacturing material round robin. An extensive array of characterization techniques was applied to these two powders, in both virgin and recycled states. The physical techniques included laser diffraction particle size analysis, X-ray computed tomography for size and shape analysis, and optical and scanning electron microscopy. Techniques sensitive to structure and chemistry, including X-ray diffraction, energy dispersive analytical X-ray analysis using the X-rays generated during scanning electron microscopy, and X-Ray photoelectron spectroscopy were also employed. The results of these analyses show how virgin powder changes after being exposed to and recycled from one or more Direct Metal Laser Sintering (DMLS) additive manufacturing build cycles. In addition, these findings can give insight into the actual additive manufacturing process. PMID:26601040

Enhanced method of magnetic powder alignment for production of PLP Nd-Fe-B magnets

NASA Astrophysics Data System (ADS)

Popov, A. G.; Golovnia, O. A.; Protasov, A. V.

2017-04-01

It is demonstrated how the high degree of powder alignment in PLP magnets can be achieved by loading the powder into a container placed in a magnetic field of moderate strength. The strip-cast alloy with a composition of 30.00 Nd, 1.95 Dy, 66.42 Fe, 0.99 B, 0.54 Co, 0.1 Ga (wt%) was subjected to hydrogen decrepitation and then milled in a vibratory mill in toluene to an average particle size of 2.9 μm determined by the FSSS method. The powder was compacted in the magnetic field of 0.2 - 1.2 T to the filling density 2.6 - 3.2×103 kg/m3. It is shown that loading the powder into a container placed in a magnetic field enhances the degree of powder alignment in sintered Nd-Fe-B magnets produced from non-pressed powder. At the filling density less than 3.2×103 kg/m3, the density of magnets is high but insufficient, because of the formation of magnetostatic chains of particles, which impedes the powder compaction. The simulation by the discrete-element method qualitatively proves that the magnetostatic interaction of the chains of particles that are formed in the course of loading in the magnetic field stimulates a decrease in the density of the sintered magnets and its non-uniform distribution over the sample. As a result of the optimization of the parameters of the alignment and compaction of the powder loaded in a magnetic field, PLP magnets with Br ≥1.34 T, Hc ≥950 kA/m, (BH)max ≥340 kJ/m3, and the degree of alignment exceeding 96% were produced.

A New Dusts Sensor for Cultural Heritage Applications Based on Image Processing

PubMed Central

Proietti, Andrea; Leccese, Fabio; Caciotta, Maurizio; Morresi, Fabio; Santamaria, Ulderico; Malomo, Carmela

2014-01-01

In this paper, we propose a new sensor for the detection and analysis of dusts (seen as powders and fibers) in indoor environments, especially designed for applications in the field of Cultural Heritage or in other contexts where the presence of dust requires special care (surgery, clean rooms, etc.). The presented system relies on image processing techniques (enhancement, noise reduction, segmentation, metrics analysis) and it allows obtaining both qualitative and quantitative information on the accumulation of dust. This information aims to identify the geometric and topological features of the elements of the deposit. The curators can use this information in order to design suitable prevention and maintenance actions for objects and environments. The sensor consists of simple and relatively cheap tools, based on a high-resolution image acquisition system, a preprocessing software to improve the captured image and an analysis algorithm for the feature extraction and the classification of the elements of the dust deposit. We carried out some tests in order to validate the system operation. These tests were performed within the Sistine Chapel in the Vatican Museums, showing the good performance of the proposed sensor in terms of execution time and classification accuracy. PMID:24901977

Dicoumarol complexes of Cu(II) based on 1,10-phenanthroline: Synthesis, X-ray diffraction studies, thermal behavior and biological evaluation

NASA Astrophysics Data System (ADS)

Dholariya, Hitesh R.; Patel, Ketan S.; Patel, Jiten C.; Patel, Kanuprasad D.

2013-05-01

A series of Cu(II) complexes containing dicoumarol derivatives and 1, 10-phenanthroline have been synthesized. Structural and spectroscopic properties of ligands were studied on the basis of mass spectra, NMR (1H and 13C) spectra, FT-IR spectrophotometry and elemental analysis, while physico-chemical, spectroscopic and thermal properties of mixed ligand complexes have been studied on the basis of infrared spectra, mass spectra, electronic spectra, powder X-ray diffraction, elemental analysis and thermogravimetric analysis. X-ray diffraction study suggested the suitable octahedral geometry for hexa-coordinated state. The kinetic parameters such as order of reaction (n), energy of activation (Ea), entropy (S*), pre-exponential factor (A), enthalpy (H*) and Gibbs free energy (G*) have been calculated using Freeman-Carroll method. Ferric-reducing antioxidant power (FRAP) of all complexes were measured. All the compounds were screened for their antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Streptococcus pyogenes and Bacillus subtilis, while antifungal activity against Candida albicans and Aspergillus niger have been carried out. Also compounds against Mycobacterium tuberculosis shows clear enhancement in the anti-tubercular activity upon copper complexation.

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.

Composites of aluminum alloy and magnesium alloy with graphite showing low thermal expansion and high specific thermal conductivity

NASA Astrophysics Data System (ADS)

Oddone, Valerio; Boerner, Benji; Reich, Stephanie

2017-12-01

High thermal conductivity, low thermal expansion and low density are three important features in novel materials for high performance electronics, mobile applications and aerospace. Spark plasma sintering was used to produce light metal-graphite composites with an excellent combination of these three properties. By adding up to 50 vol.% of macroscopic graphite flakes, the thermal expansion coefficient of magnesium and aluminum alloys was tuned down to zero or negative values, while the specific thermal conductivity was over four times higher than in copper. No degradation of the samples was observed after thermal stress tests and thermal cycling. Tensile strength and hardness measurements proved sufficient mechanical stability for most thermal management applications. For the production of the alloys, both prealloyed powders and elemental mixtures were used; the addition of trace elements to cope with the oxidation of the powders was studied.

Characterization of the chemical variation of feed coal and coal combustion products from a power plant utilizing low sulfur Powder River Basin coal

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

Affolter, R.H.; Brownfield, M.E.; Cathcart, J.D.

2000-07-01

The US Geological Survey and the University of Kentucky Center for Applied Energy Research, in collaboration with an Indiana utility, are studying a coal-fired power plant burning Powder River Basin coal. This investigation involves a systematic study of the chemical and mineralogical characteristics of feed coal and coal combustion products (CCPs) from a 1,300-megawatt (MW) power unit. The main goal of this study is to characterize the temporal chemical variability of the feed coal, fly ash, and bottom ash by looking at the major-, minor-, and trace-element compositions and their associations with the feed coal mineralogy. Emphasis is also placedmore » on the abundance and modes of occurrence of elements of potential environmental concern that may affect the utilization of these CCPs and coals.« less

Composites of aluminum alloy and magnesium alloy with graphite showing low thermal expansion and high specific thermal conductivity

PubMed Central

Oddone, Valerio; Boerner, Benji; Reich, Stephanie

2017-01-01

Abstract High thermal conductivity, low thermal expansion and low density are three important features in novel materials for high performance electronics, mobile applications and aerospace. Spark plasma sintering was used to produce light metal–graphite composites with an excellent combination of these three properties. By adding up to 50 vol.% of macroscopic graphite flakes, the thermal expansion coefficient of magnesium and aluminum alloys was tuned down to zero or negative values, while the specific thermal conductivity was over four times higher than in copper. No degradation of the samples was observed after thermal stress tests and thermal cycling. Tensile strength and hardness measurements proved sufficient mechanical stability for most thermal management applications. For the production of the alloys, both prealloyed powders and elemental mixtures were used; the addition of trace elements to cope with the oxidation of the powders was studied. PMID:28458742

Composites of aluminum alloy and magnesium alloy with graphite showing low thermal expansion and high specific thermal conductivity.

PubMed

Oddone, Valerio; Boerner, Benji; Reich, Stephanie

2017-01-01

High thermal conductivity, low thermal expansion and low density are three important features in novel materials for high performance electronics, mobile applications and aerospace. Spark plasma sintering was used to produce light metal-graphite composites with an excellent combination of these three properties. By adding up to 50 vol.% of macroscopic graphite flakes, the thermal expansion coefficient of magnesium and aluminum alloys was tuned down to zero or negative values, while the specific thermal conductivity was over four times higher than in copper. No degradation of the samples was observed after thermal stress tests and thermal cycling. Tensile strength and hardness measurements proved sufficient mechanical stability for most thermal management applications. For the production of the alloys, both prealloyed powders and elemental mixtures were used; the addition of trace elements to cope with the oxidation of the powders was studied.

Boron nitride insulating material

DOEpatents

Morgan, Jr., Chester S.; Cavin, O. Burl; McCulloch, Reginald W.; Clark, David L.

1978-01-01

High temperature BN-insulated heaters for use as fuel pin simulators in reactor thermal hydraulic test facility studies comprise a cylindrical housing and a concentric heating element disposed within the housing and spaced apart from the housing to define an annular region therebetween. The annular region contains BN for providing electrical resistance and thermal conductivity between the housing and the heating element. The fabrication method of this invention comprises the steps of cold pressing BN powder at a pressure of 20 to 80,000 psig and a dwell time of at least 0.1-3 seconds to provide hollow cylindrical preforms of suitable dimensions for insertion into the annular region, the BN powder having a tap density of about 0.6-1.1 g/cm.sup.3 and an orientation ratio of at least about 100/3.5. The preforms are inserted into the annular region and crushed in place.

Effect of Powder-Feeding Modes During Plasma Spray on the Properties of Tungsten Carbide Composite Coatings

NASA Astrophysics Data System (ADS)

Zhong, Yi-ming; Du, Xiao-dong; Wu, Gang

2017-05-01

A WC-reinforced composite coating was fabricated on the surface of 45 steel samples by plasma, cladding process with WC powder added to the molten pool synchronously or in the tail of the molten pool. The microstructure, phase composition, and element distribution in the coating were analyzed. The results show that the undissolved WC particles and crystallized carbide (WC, W2C) were distributed uniformly in the sub-eutectic matrix in both cases. Fewer of the WC particles are dissolved in the matrix when they are injected into the tail of the molten pool. There are fewer needle-like tungsten carbide formations seen in the composite coating fabricated by back-feeding process than in that formed by synchronous feeding. The former results in a finer microstructure and a higher concentration gradient of elements near the interface between the WC particles and the coating matrix.

METHOD OF FABRICATING A URANIUM-ZIRCONIUM HYDRIDE REACTOR CORE

DOEpatents

Weeks, I.F.; Goeddel, W.V.

1960-03-22

A method is described of evenly dispersing uranlum metal in a zirconium hydride moderator to produce a fuel element for nuclear reactors. According to the invention enriched uranium hydride and zirconium hydride powders of 200 mesh particle size are thoroughly admixed to form a mixture containing 0.1 to 3% by weight of U/sup 235/ hydride. The mixed powders are placed in a die and pressed at 100 tons per square inch at room temperature. The resultant compacts are heated in a vacuum to 300 deg C, whereby the uranium hydride deoomposes into uranium metal and hydrogen gas. The escaping hydrogen gas forms a porous matrix of zirconium hydride, with uramum metal evenly dispersed therethrough. The advantage of the invention is that the porosity and uranium distribution of the final fuel element can be more closely determined and controlled than was possible using prior methods of producing such fuel ele- ments.

Structural diversity of silver (I) azine complexes - Effect of substituents and counter anions

NASA Astrophysics Data System (ADS)

Patra, Goutam Kumar; Mukherjee, Anindita; Mitra, Partha; Adarsh, N. N.

2011-08-01

Three new Ag(I) complexes, 1, 2, and 3 of two azine ligands diacetyl dihydrazone ( L1) and benzil dihydrazone ( L2) have been synthesized and characterized by single crystal X-ray diffraction studies (for 2 and 3), X-ray powder diffraction studies( 1 and 2), elemental analyses, IR and UV-VIS spectroscopy and TGA analysis. They represent one-dimensional polymeric assemblies and discrete dinuclear Ag(I) complex depending on functionality of the ligands and the counter anions. Tetrahedral as well as square pyramidal coordination motifs of the silver (I) ions have been observed in the supramolecular designing of such hybrid organic-inorganic materials.

Crystallinity and compositional changes in carbonated apatites: Evidence from 31P solid-state NMR, Raman, and AFM analysis

NASA Astrophysics Data System (ADS)

McElderry, John-David P.; Zhu, Peizhi; Mroue, Kamal H.; Xu, Jiadi; Pavan, Barbara; Fang, Ming; Zhao, Guisheng; McNerny, Erin; Kohn, David H.; Franceschi, Renny T.; Holl, Mark M. Banaszak; Tecklenburg, Mary M. J.; Ramamoorthy, Ayyalusamy; Morris, Michael D.

2013-10-01

Solid-state (magic-angle spinning) NMR spectroscopy is a useful tool for obtaining structural information on bone organic and mineral components and synthetic model minerals at the atomic-level. Raman and 31P NMR spectral parameters were investigated in a series of synthetic B-type carbonated apatites (CAps). Inverse 31P NMR linewidth and inverse Raman PO43-ν1 bandwidth were both correlated with powder XRD c-axis crystallinity over the 0.3-10.3 wt% CO32- range investigated. Comparison with bone powder crystallinities showed agreement with values predicted by NMR and Raman calibration curves. Carbonate content was divided into two domains by the 31P NMR chemical shift frequency and the Raman phosphate ν1 band position. These parameters remain stable except for an abrupt transition at 6.5 wt% carbonate, a composition which corresponds to an average of one carbonate per unit cell. This near-binary distribution of spectroscopic properties was also found in AFM-measured particle sizes and Ca/P molar ratios by elemental analysis. We propose that this transition differentiates between two charge-balancing ion-loss mechanisms as measured by Ca/P ratios. These results define a criterion for spectroscopic characterization of B-type carbonate substitution in apatitic minerals.

Synthesis, structural and vibrational studies on mixed alkali metal gadolinium double tungstate, K1-xNaxGd(WO4)2

NASA Astrophysics Data System (ADS)

Durairajan, A.; Thangaraju, D.; Moorthy Babu, S.

2013-02-01

Mixed alkali double tungstates K1-xNaxGd(WO4)2 (KNGW) (0 ⩽ x ⩽ 1) were synthesized by solid state reaction using sodium doped monoclinic KGd(WO4)2 (KGW). Synthesized KNGW powders were characterized using powder X-ray diffraction (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and Raman analysis. DTA analysis confirms that the melting point of the KGW matrix increases from 1063 °C to 1255 °C with increasing sodium content. The Powder XRD analyses reveal that mixed phases were observed up to 40 wt.% of Na in the KGW matrix above that percentage there is domination of scheelite structure in the synthesized powder. Polyhedral type, bi-pyramidal shape and spheroid shape morphology was observed for KGW, NKGW and NGW powders respectively. The Raman analysis was carried out to understand the vibrational characteristic changes with mixing of sodium ions in the KGW matrix.

Effect of Magnesium Content and Processing Conditions on Phase Formation and Stability in Mg2+ δ Si0.3Sn0.7

NASA Astrophysics Data System (ADS)

Goyal, Gagan K.; Dasgupta, T.

2018-03-01

Mg2+ δ Si0.3Sn0.7 compositions with nominal Mg content of δ = 0, 0.2 are synthesized using a single-step quartz tube reaction method with different heating rates and holding times. The resulting powders are sintered using a uniaxial induction hot press under similar conditions to produce near-dense compacts. The effect of Mg content and processing conditions on the phase formation and its stability are studied using x-ray diffraction measurements, scanning electron microscopy (SEM) with elemental mapping and compositional analysis using energy dispersive spectroscopy (EDS). Results indicate that with sufficient Mg content and shorter synthesis time, the powder remains single phasic; however, prolonged heat treatment during synthesis results in Mg loss and causes the system to become biphasic. Compaction results in single-phase formation in all the specimens. This is attributed to the removal of the low-melting secondary Sn-rich phases present in the system. The decomposition of the specimens depends on the Mg content after the compaction step with a δ around - 0.15 necessary to preserve the single phase. The decomposition also results in Mg enrichment of the matrix (due to formation of elemental Sn), thereby acting as a self-healing mechanism. Annealing the dense products at 773 K for 24 h in static vacuum is carried out. Progressive Mg loss is observed resulting in degradation of the specimen.

An Experimental Investigation of Effects of Fluxes (Na3AlF6 and K2TiF6), Element Alloys (Mg), and Composite Powders ((Al + TiC)CP and (Al + B4C)CP) on Distribution of Particles and Phases in Al-B4C and Al-TiC Composites

NASA Astrophysics Data System (ADS)

Mazaheri, Younes; Emadi, Rahmatollah; Meratian, Mahmood; Zarchi, Mehdi Karimi

2017-04-01

The wettability, incorporation, and gravity segregation of TiC and B4C particles into molten aluminum are important problems in the production of Al-TiC and Al-B4C composites by the casting techniques. In order to solve these problems, different methods consisting of adding the Na3AlF6 and K2TiF6 fluxes and Mg (as the alloying element) into the molten aluminum and injection of the (Al + TiC)CP and (Al + B4C)CP composite powders instead of B4C and TiC particles are evaluated. In this work, the conditions of sample preparation, such as particle addition temperature, stirring speed, and stirring time, are determined after many studies and tests. Microstructural characterizations of samples are investigated by scanning electron microscopy equipped with energy dispersive spectroscopy (EDS) and X-ray diffractometry. The results show better distribution and incorporation of TiCp and B4Cp in aluminum matrix when the fluxes are used, as well as EDS analysis of the interface between the matrix and reinforcement-strengthened formation of the different phases such as Al4C3 in the Al-TiC composites and Al3BC, TiB2 in the Al-B4C composites.

Analysis of ultrasonic effect on powder and application to radioactive sample compaction

NASA Astrophysics Data System (ADS)

Kim, Jungsoon; Sim, Minseop; Kim, Jihyang; Kim, Moojoon

2018-07-01

The effect of ultrasound on powder compaction was analyzed. The decreasing in the friction coefficient of the powder sample is derived theoretically. The compaction rate was improved by the ultrasound. We applied the effect to the compaction of environmental radioactive soil samples. From γ-ray spectroscopy analysis, more radionuclides could be detectable in the sample compacted with ultrasound.

Thermal treatment and ammoniacal leaching for the recovery of valuable metals from spent lithium-ion batteries.

PubMed

Chen, Yongming; Liu, Nannan; Hu, Fang; Ye, Longgang; Xi, Yan; Yang, Shenghai

2018-05-01

The recycling of spent commercial lithium-ion batteries (LIBs) generates numerous environmental and economic benefits. In this research, a thermal treatment-ammoniacal leaching process is proposed to recover valuable metals from cathode active powder. Based on the thermal behavior by TG-DSC analysis, the cathode active powder is calcined at 300 °C and 550 °C in air atmosphere, and the crystalline phase characterization indicates that a new phase of Co 3 O 4 appears in the cathode active powder calcined at 550 °C, which signifies that the layer structure of LiCoO 2 collapses. The valence of manganese increases to form Li 4 Mn 5 O 12 in spinel structure of LiMn 2 O 4 . Using calcined cathode powder as feed material, ammoniacal leaching is carried out in (NH 4 ) 2 SO 4 -(NH 4 ) 2 SO 3 solution. Under the optimum conditions, Ni, Co, Mn and Li can be completely leached out with efficiencies of 98%, 81%, 92% and 98%, respectively. However, with the increase of ammonia concentration, the leaching efficiency of Mn decreases dramatically to 4% due to the formation of double salts. It is found that Co and Mn can be precipitated into residues in the form of (NH 4 ) 2 Co(SO 4 ) 2 ·H 2 O, (NH 4 ) 2 Mn(SO 3 ) 2 ·H 2 O and (NH 4 ) 2 Mn(SO 4 ) 2 ·6H 2 O under different leaching parameters. Based on the corresponding relationship between the leaching efficiency and phase evolution of object element, selective leaching can be achieved by controlling the formation of double salts. Copyright © 2018 Elsevier Ltd. All rights reserved.

Characterization of magnetite (Fe3O4) minerals from natural iron sand of Bonto Kanang Village Takalar for ink powder (toner) application

NASA Astrophysics Data System (ADS)

Fahlepy, M. R.; Tiwow, V. A.; Subaer

2018-03-01

This research is about magnetite’s characterization (Fe3O4) from natural iron sands of Bonto Kanang Village, District of Takalar for ink powder (toner) application. This study aims to determine the process parameters to obtain magnetite of high purity degree and to observe its physical characteristics as a supporting toner material which synthesized through co-precipitation method. The iron sand was first separated by the magnetic technique and dissolved into HCl solution before conducting the precipitation process. Precipitation was done by dripping ammonium hydroxide (NH4OH). The precipitated powder was dried at 100°C, and then calcined at 400°C. The purity degree and magnetite mineral grain size were analyzed by XRD and SEM-EDS. The EDS elemental test before and after precipitation shown an increase of iron oxide composition from 66.70% to 87.76%. Diffractogram of XRD before and after precipitation showed Fe3O4 compounds with magnetite phase of 59% and 98%, respectively. The crystal structure iron sand powder structure before and after precipitation is cubic with each lattice parameters a = b = c = 8.384971 Å, V = 589.528423 Å3 and a = b = c = 8.386829 Å and V = 589.920291 Å3 when angle α = β = γ = 90°. SEM images (using SE and HV 20kV) showed inhomogeneous magnetite morphology. The magnetite phase percentage that obtained based on the XRD analysis gives information that magnetite precipitation has been successfully performed with high degree of purity. The material obtained can be applied as a support toner material.

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.

Synthesis and characterization of ZnO–CuO nanocomposites powder by modified perfume spray pyrolysis method and its antimicrobial investigation

NASA Astrophysics Data System (ADS)

Saravanakkumar, D.; Sivaranjani, S.; Kaviyarasu, K.; Ayeshamariam, A.; Ravikumar, B.; Pandiarajan, S.; Veeralakshmi, C.; Jayachandran, M.; Maaza, M.

2018-03-01

Pure ZnO, ZnO–CuO nanocomposites can be synthesized by using a modified perfume spray pyrolysis method (MSP). The crystallite size of the nanoparticles (NPs) has been observed by X-ray diffraction pattern and is nearly 36 nm. Morphological studies have been analyzed by using Field Emission Scanning Electron Microscopy (FESEM) and its elemental analysis was reported by Elemental X-ray Analysis (EDX); these studies confirmed that ZnO and CuO have hexagonal structure and monoclinic structure respectively. Fourier Transform Infrared (FTIR) spectra revealed that the presence of functional frequencies of ZnO and CuO were observed at 443 and 616 cm‑1. The average bandgap value at 3.25 eV using UV–vis spectra for the entitled composite has described a blue shift that has been observed here. The antibacterial study against both gram positive and negative bacteria has been studied by the disc diffusion method. To the best of our knowledge, it is the first report on ZnO–CuO nanocomposite synthesized by a modified perfume spray pyrolysis method.

Iodinated curcumin bearing dermal cream augmented drug delivery, antimicrobial and antioxidant activities.

PubMed

Manchanda, Gagandeep; Sodhi, Rupinder Kaur; Jain, Upendra Kumar; Chandra, Ramesh; Madan, Jitender

2018-01-01

Curcumin (Cur) exhibits weak microbicidal activity owing to high lipophilicity and low cell permeability. Therefore, in the present investigation, Cur was iodinated using elemental iodine (I 2 ) to synthesise Cur-I 2 powder that was later formulated as Cur-I 2 dermal cream and characterised in vitro for antimicrobial and antioxidant activities. Electrophilic addition of I 2 saturated the olefinic bonds of Cur, as confirmed by UV/visible spectroscopy, FT-IR, 1 H NMR and DSC techniques. In addition, in vitro skin permeation and retention analysis indicated that Cur-I 2 cream followed the first order and Higuchi model for drug release through the rat skin. The minimum inhibitory concentration (MIC) of Cur-I 2 powder was measured to be 60 and 90 µg/ml significantly (p < 0.05) lower than 150 and 120 µg/ml of Cur against Staphylococcus aureus and Escherichia coli, respectively. Moreover, Cur-I 2 also exhibited strong antioxidant potential. Cur-I 2 cream warrants further in vivo study to scale up the technology for clinical translation.

Synthesis and characterization of Ti-27.5Nb alloy made by CLAD® additive manufacturing process for biomedical applications.

PubMed

Fischer, M; Laheurte, P; Acquier, P; Joguet, D; Peltier, L; Petithory, T; Anselme, K; Mille, P

2017-06-01

Biocompatible beta-titanium alloys such as Ti-27.5(at.%)Nb are good candidates for implantology and arthroplasty applications as their particular mechanical properties, including low Young's modulus, could significantly reduce the stress-shielding phenomenon usually occurring after surgery. The CLAD® process is a powder blown additive manufacturing process that allows the manufacture of patient specific (i.e. custom) implants. Thus, the use of Ti-27.5(at.%)Nb alloy formed by CLAD® process for biomedical applications as a mean to increase cytocompatibility and mechanical biocompatibility was investigated in this study. The microstructural properties of the CLAD-deposited alloy were studied with optical microscopy and electron back-scattered diffraction (EBSD) analysis. The conservation of the mechanical properties of the Ti-27.5Nb material after the transformation steps (ingot-powder atomisation-CLAD) were verified with tensile tests and appear to remain close to those of reference material. Cytocompatibility of the material and subsequent cell viability tests showed that no cytotoxic elements are released in the medium and that viable cells proliferated well. Copyright © 2017 Elsevier B.V. All rights reserved.

Biosorption of Cu(II) by powdered anaerobic granular sludge from aqueous medium.

PubMed

Zhou, Xu; Chen, Chuan; Wang, Aijie; Jiang, Guangming; Liu, Lihong; Xu, Xijun; Yuan, Ye; Lee, Duu-Jung; Ren, Nanqi

2013-01-01

Copper(II) biosorption processes by two pre-treated powdered anaerobic granular sludges (PAGS) (original sludges were methanogenic anaerobic granules and denitrifying sulfide removal (DSR) anaerobic granules) were investigated through batch tests. Factors affecting the biosorption process, such as pH, temperature and initial copper concentrations, were examined. Also, the physico-chemical characteristics of the anaerobic sludge were analyzed by Fourier transform infrared spectroscopy, scanning electron microscopy image, surface area and elemental analysis. A second-order kinetic model was applied to describe the biosorption process, and the model could fit the biosorption process. The Freundlich model was used for describing the adsorption equilibrium data and could fit the equilibrium data well. It was found that the methanogenic PAGS was more effective in Copper(II) biosorption process than the DSR PAGS, whose maximum biosorption capacity was 39.6% lower. The mechanisms of the biosorption capacities for different PAGS were discussed, and the conclusion suggested that the environment and biochemical reactions during the growth of biomass may have affected the structure of the PAGS. The methanogenic PAGS had larger specific surface area and more biosorption capacity than the DSR PAGS.

Effect of thermal annealing on the structural and optical properties of Cu2FeSnS4 thin films grown by vacuum evaporation method

NASA Astrophysics Data System (ADS)

Oueslati, H.; Rabeh, M. Ben; Kanzari, M.

2018-02-01

In this work, the effect of different types of thermal annealing on the properties of Cu2FeSnS4 (CFTS) thin films deposited by thermal evaporation at room temperature on glass substrate were investigated. CFTS powder was synthesized by direct melting of the constituent elements taken in stoichiometry compositions. The X-ray diffraction experimental data indicating that the Cu2FeSnS4 powder illustrating a stannite structure in space group I\\bar {4}2m. From the XRD analysis we have found that the polycrystalline CFTS thin film was only obtained by thermal annealed in sulfur atmosphere under a high vacuum of 400 °C temperature during 2 h. Optical study reveals that the thin films have relatively high absorption coefficients (≈ 105cm-1) and the values of optical band gap energy ranged between 1.38 and 1.48 eV. Other optical parameters were evaluated according to the models of Wemple Di-Domenico and Spitzer-Fan. Finally, hot probe measurements of CFTS thin films reveal p-type conductivity.

Glove powder's carrying capacity for latex protein: analysis using the ASTM ELISA test.

PubMed

Beezhold, D; Horton, K; Hickey, V; Daddona, J; Kostyal, D

2003-01-01

Glove donning powders carry latex proteins and disperse them into the workplace environment. We have used the ASTM D6499 ELISA to quantify the amount of latex antigen bound to and carried by glove powders. We could differentiate between a small amount of protein actually bound to the powders and a larger amount carried by the powder. Enhanced binding of a major allergen, Hev b 5, to the starch powders was demonstrated by Western blot. The D6499 ELISA is able to measure total latex antigen, soluble and powder bound, simultaneously without the need to centrifuge the samples.

Hydrogen and elemental carbon production from natural gas and other hydrocarbons

DOEpatents

Detering, Brent A.; Kong, Peter C.

2002-01-01

Diatomic hydrogen and unsaturated hydrocarbons are produced as reactor gases in a fast quench reactor. During the fast quench, the unsaturated hydrocarbons are further decomposed by reheating the reactor gases. More diatomic hydrogen is produced, along with elemental carbon. Other gas may be added at different stages in the process to form a desired end product and prevent back reactions. The product is a substantially clean-burning hydrogen fuel that leaves no greenhouse gas emissions, and elemental carbon that may be used in powder form as a commodity for several processes.

Microstructure and compression properties of 3D powder printed Ti-6Al-4V scaffolds with designed porosity: Experimental and computational analysis.

PubMed

Barui, Srimanta; Chatterjee, Subhomoy; Mandal, Sourav; Kumar, Alok; Basu, Bikramjit

2017-01-01

The osseointegration of metallic implants depends on an effective balance among designed porosity to facilitate angiogenesis, tissue in-growth and bone-mimicking elastic modulus with good strength properties. While addressing such twin requirements, the present study demonstrates a low temperature additive manufacturing based processing strategy to fabricate Ti-6Al-4V scaffolds with designed porosity using inkjet-based 3D powder printing (3DPP). A novel starch-based aqueous binder was prepared and the physico-chemical parameters such as pH, viscosity, and surface tension were optimized for drop-on-demand (DOD) based thermal inkjet printing. Micro-computed tomography (micro-CT) of sintered scaffolds revealed a 57% total porosity in homogeneously porous scaffold and 45% in the gradient porous scaffold with 99% interconnectivity among the micropores. Under uniaxial compression testing, the strength of homogeneously porous and gradient porous scaffolds were ~47MPa and ~90MPa, respectively. The progressive failure in homogeneously porous scaffold was recorded. In parallel to experimental measurements, finite element (FE) analyses have been performed to study the stress distribution globally and also locally around the designed pores. Consistent with FE analyses, a higher elastic modulus was recorded with gradient porous scaffolds (~3GPa) than the homogenously porous scaffolds (~2GPa). While comparing with the existing literature reports, the present work, for the first time, establishes 'direct powder printing methodology' of Ti-6Al-4V porous scaffolds with biomedically relevant microstructural and mechanical properties. Also, a new FE analysis approach, based on the critical understanding of the porous architecture using micro-CT results, is presented to realistically predict the compression response of porous scaffolds. Copyright © 2016 Elsevier B.V. All rights reserved.

Zr 2Ir 6B with an eightfold superstructure of the cubic perovskite-like boride ZrIr 3B 0.5: Synthesis, crystal structure and bonding analysis

NASA Astrophysics Data System (ADS)

Hermus, Martin; Fokwa, Boniface P. T.

2010-04-01

Single phase powder samples and single crystals of Zr 2Ir 6B were successfully synthesized by arc-melting the elements in a water-cooled copper crucible under an argon atmosphere. Superstructure reflections were observed both on powder and on single crystal diffraction data, leading to an eightfold superstructure of ZrIr 3B x phase. The new phase, which has a metallic luster, crystallizes in space group Fm3¯m (no. 225) with the lattice parameters a=7.9903(4) Å, V=510.14(4) Å 3. Its crystal structure was refined on the basis of powder as well as single crystal data. The single crystal refinement converged to R1=0.0239 and w R2=0.0624 for all 88 unique reflections and 6 parameters. Zr 2Ir 6B is isotypic to Ti 2Rh 6B and its structure can be described as a defect double perovskite, A2BB' O6, where the A site is occupied by zirconium, the B site by boron, the O site by iridium but the B' site is vacant, leading to the formation of empty and boron-filled octahedral Ir 6 clusters. According to the result of tight-binding electronic structure calculations, Ir-B and Ir-Zr interactions are mainly responsible for the structural stability of the phase. According to COHP bonding analysis, the strongest bonding occurs for the Ir-B contacts, and the Ir-Ir bonding within the empty clusters is two times stronger than that in the BIr 6 octahedra.

Effect of process control agent on the porous structure and mechanical properties of a biomedical Ti-Sn-Nb alloy produced by powder metallurgy.

PubMed

Nouri, A; Hodgson, P D; Wen, C E

2010-04-01

The influence of different amounts and types of process control agent (PCA), i.e., stearic acid and ethylene bis-stearamide, on the porous structure and mechanical properties of a biomedical Ti-16Sn-4Nb (wt.%) alloy was investigated. Alloy synthesis was performed on elemental metal powders using high-energy ball milling for 5h. Results indicated that varying the PCA content during ball milling led to a drastic change in morphology and particle-size distribution of the ball-milled powders. Porous titanium alloy samples sintered from the powders ball milled with the addition of various amounts of PCA also revealed different pore morphology and porosity. The Vickers hardness of the sintered titanium alloy samples exhibited a considerable increase with increasing PCA content. Moreover, the addition of larger amounts of PCA in the powder mixture resulted in a significant increase in the elastic modulus and peak stress for the sintered porous titanium alloy samples under compression. It should also be mentioned that the addition of PCA introduced contamination (mainly carbon and oxygen) into the sintered porous product. Crown Copyright 2009. Published by Elsevier Ltd. All rights reserved.

Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

NASA Astrophysics Data System (ADS)

Kara, P.; Csetényi, L. J.; Borosnyói, A.

2016-04-01

In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

New technique for the direct analysis of food powders confined in a small hole using transversely excited atmospheric CO(2) laser-induced gas plasma.

PubMed

Khumaeni, Ali; Ramli, Muliadi; Deguchi, Yoji; Lee, Yong Inn; Idris, Nasrullah; Kurniawan, Koo Hendrik; Lie, Tjung Jie; Kagawa, Kiichiro

2008-12-01

Taking advantage of the differences between the interactions of transversely excited atmospheric (TEA) CO(2) lasers with metal and with organic powder, a new technique for the direct analysis of food powder samples has been developed. In this technique, the powder samples were placed into a small hole with a diameter of 2 mm and a depth of 3 mm and covered by a metal mesh. The TEA CO(2) laser (1500 mJ, 200 ns) was focused on the powder sample surfaces, passing through the metal mesh, at atmospheric pressure in nitrogen gas. It is hypothesized that the small hole functions to confine the powder particles and suppresses the blowing-off of sample, while the metal mesh works as the source of electrons to initiate the strong gas breakdown plasma. The confined powder particles are then ablated by laser irradiation and the ablated particles move into the strong gas breakdown plasma region to be atomized and excited; this method cannot be applied for the case of Nd:YAG lasers because in such case the metal mesh itself was ablated by the laser irradiation. A quantitative analysis of a milk powder sample containing different concentrations of Ca was successfully demonstrated, resulting in a good linear calibration curve with high precision.

Synthesis of Ti-Ta alloys with dual structure by incomplete diffusion between elemental powders.

PubMed

Liu, Yong; Li, Kaiyang; Wu, Hong; Song, Min; Wang, Wen; Li, Nianfeng; Tang, Huiping

2015-11-01

In this work, powder metallurgical (PM) Ti-Ta alloys were sintered using blended elemental powders. A dual structure, consisting of Ti-rich and Ta-rich zones, was formed due to the insufficient diffusion between Ti and Ta powders. The microstructure, mechanical properties and in vitro biological properties of the alloys were studied. Results indicated that the alloys have inhomogenous microstructures and compositions, but the grain structures were continuous from the Ti-rich zone to the Ta-rich zone. The Ta-rich zone exhibited a much finer grain size than the Ti-rich zone. The alloys had a high relative density in the range of 95-98%, with the porosity increasing with the content of Ta due to the increased difficulty in sintering and the formation of Kirkendall pores. The alloys had a good combination of low elastic modulus and high tensile strength. The strength of alloys was almost doubled compared to that of the ingot metallurgy alloys with the same compositions. The low elastic modulus was due to the residual pores and the alloying effect of Ta, while the high tensile strength resulted from the strengthening effects of solid solution, fine grain size and α phase. The alloys had a high biocompatibility due to the addition of Ta, and were suitable for the attachment of cells due to the surface porosity. It was also indicated that PM Ti-(20-30)Ta alloys are promising for biomedical applications after the evaluations of both the mechanical and the biological properties. Copyright © 2015 Elsevier Ltd. All rights reserved.

Growth, optical, ICP and thermal studies of nonlinear optical single crystal: Sodium acid phthalate (NaAP)

NASA Astrophysics Data System (ADS)

Mahadevan, M.; Arivanandhan, M.; Elangovan, K.; Anandan, P.; Ramachandran, K.

2017-07-01

Good quality single crystals of sodium acid phthalate (NaAP) were grown by slow evaporation technique. Single crystal X-ray diffraction study of the grown crystal reveals that the crystal belongs to orthorhombic system with space group B2ab. Fourier transform infrared spectrum confirms the presence of the functional groups of the grown material. Inductively coupled plasma emission spectroscopy analysis is used to confirm the presence of Na element in the sample. Thermal analysis of the NaAP crystal shows that the crystal is stable up to 140°C. Optical transmittance of the grown crystal was recorded in the wavelength range from 200 and 800 nm using UV-Vis-NIR spectrophotometer. The second harmonic generation of NaAP was analysed using Kurtz powder technique.

Laer-induced Breakdown Spectroscopy Instrument for Element Analysis of Planetary Surfaces

NASA Technical Reports Server (NTRS)

Blacic, J.; Pettit, D.; Cremers, D.; Roessler, N.

1993-01-01

One of the most fundamental pieces of information about any planetary body is the elemental and mineralogical composition of its surface materials. We are developing an instrument to obtain such data at ranges of up to several hundreds of meters using the technique of Laser-Induced Breakdown Spectroscopy (LIBS). We envision our instrument being used from a spacecraft in close rendezvous with small bodies such as comets and asteroids, or deployed on surface-rover vehicles on large bodies such as Mars and the Moon. The elemental analysis is based on atomic emission spectroscopy of a laser-induced plasma or spark. A pulsed, diode pumped Nd:YAG laser of several hundred millijoules optical energy is used to vaporize and electronically excite the constituent elements of a rock surface remotely located from the laser. Light emitted from the excited plasma is collected and introduced to the entrance slit of a small grating spectrometer. The spectrally dispersed spark light is detected with either a linear photo diode array or area CCD array. When the latter detector is used, the optical and spectrometer components of the LIBS instrument can also be used in a passive imaging mode to collect and integrate reflected sunlight from the same rock surface. Absorption spectral analysis of this reflected light gives mineralogical information that provides a remote geochemical characterization of the rock surface. We performed laboratory calibrations in air and in vacuum on standard rock powders to quantify the LIBS analysis. We performed preliminary field tests using commercially available components to demonstrate remote LIBS analysis of terrestrial rock surfaces at ranges of over 25 m, and we have demonstrated compatibility with a six-wheeled Russian robotic rover vehicle. Based on these results, we believe that all major and most minor elements expected on planetary surfaces can be measured with absolute accuracy of 10-15 percent and much higher relative accuracy. We have performed preliminary systems analysis of a LIBS instrument to evaluate probable mass and power requirements; results of this analysis are summarized.

Equal channel angular pressing of powder processed Al6061/SiC nano metal matrix composites and study of its wear properties

NASA Astrophysics Data System (ADS)

Bongale, Arunkumar M.; Kumar, Satish

2018-03-01

Nano Metal Matrix Composites were fabricated by a novel approach by combining powder metallurgy and equal channel angular pressing (ECAP) using aluminium alloy 6061 (Al6061) as matrix phase and 2, 4 and 6 wt% of silicon carbide nanoparticles (SiCnp) as reinforcements. Alloying elements of Al6061 in their elemental form are blended together using high energy planetary ball mill and calculated wt% of SiCnp were mixed with it. Thus formed composite powder mixture is compacted in a uniaxial compaction die and then subjected to ECAP up to three passes. Density and porosity of samples were estimated using Archimedes’ principle. Pin on disc setup is used to evaluate the wear properties of the composites under different speed and loading conditions. Tests revealed that increase in wt% of SiCnp reduces the wear rate of the composites whereas increasing the load and speed increases wear rate of the composite samples. SEM micrographs of worn surfaces indicated different types of wear mechanism responsible for wear of the specimens under different testing conditions. Also, wt% of SiCnp and the number of passes through ECAP were found to increase the hardness value of the composite material.

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury

PubMed Central

Li, Cen; Yang, Hongxia; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao

2016-01-01

Zuotai (gTso thal) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100–800 nm, which commonly further aggregate into 1–30 μm loosely amorphous particles. XRD test shows that β-HgS, S8, and α-HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai, and it would play a positive role in interpreting this mysterious Tibetan drug. PMID:27738409

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

PubMed

Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

2016-01-01

Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

To evaluate the effect of various magnesium stearate polymorphs using powder rheology and thermal analysis.

PubMed

Okoye, Patrick; Wu, Stephen H; Dave, Rutesh H

2012-12-01

The effects of magnesium stearate (MgSt) polymorphs-anhydrate (MgSt-A), monohydrate (MgSt-M), and dihydrate (MgSt-D)-on rheological properties of powders were evaluated using techniques such as atomic analysis and powder rheometry. Additional evaluation was conducted using thermal analysis, micromeritics, and tableting forces. In this study, binary ratios of neat MgSt polymorphs were employed as lubricants in powder blends containing acetaminophen (APAP), microcrystalline cellulose (MCC), and lactose monohydrate (LAC-M). Powder rheometry was studied using permeability, basic flow energy (BFE), density, and porosity analysis. Thermal conductivity and differential scanning calorimetric analysis of MgSt polymorphs were employed to elucidate MgSt effect on powder blends. The impact of MgSt polymorphs on compaction characteristics were analyzed via tablet compression forces. Finally, the distribution of atomized magnesium (Mg) ions as a function of intensity was evaluated using laser-induced breakdown spectroscopy (LIBS) on tablets. The results from LIBS analysis indicated the dependency of the MgSt polymorphic forms on the atomized Mg ion intensity, with higher Mg ion intensity suggesting higher lubricity index (i.e. greater propensity to over-lubricate). The results from lubricity index suggested the tendency of blends to over-lubricate based on the MgSt polymorphic forms. Finally, tableting forces suggested that MgSt-D and MgSt-A offered processing benefits such as lower ejection and compression forces, and that MgSt-M showed the most stable compression force in single or combined polymorphic ratios. These results suggested that the initial moisture content, crystal arrangement, intra- and inter-molecular packing of the polymorphs defined their effects on the rheology of lubricated powders.

Mg(1 + x)Ir(1 - x) (x = 0, 0.037 and 0.054), a binary intermetallic compound with a new orthorhombic structure type determined from powder and single-crystal X-ray diffraction.

PubMed

Cerný, Radovan; Renaudin, Guillaume; Favre-Nicolin, Vincent; Hlukhyy, Viktor; Pöttgen, Rainer

2004-06-01

The new binary compound Mg(1 + x)Ir(1 - x) (x = 0-0.054) was prepared by melting the elements in the Mg:Ir ratio 2:3 in a sealed tantalum tube under an argon atmosphere in an induction furnace (single crystals) or by annealing cold-pressed pellets of the starting composition Mg:Ir 1:1 in an autoclave under an argon atmosphere (powder sample). The structure was independently solved from high-resolution synchrotron powder and single-crystal X-ray data: Pearson symbol oC304, space group Cmca, lattice parameters from synchrotron powder data a = 18.46948 (6), b = 16.17450 (5), c = 16.82131 (5) A. Mg(1 + x)Ir(1 - x) is a topologically close-packed phase, containing 13 Ir and 12 Mg atoms in the asymmetric unit, and has a narrow homogeneity range. Nearly all the atoms have Frank-Kasper-related coordination polyhedra, with the exception of two Ir atoms, and this compound contains the shortest Ir-Ir distances ever observed. The solution of a rather complex crystal structure from powder diffraction, which was fully confirmed by the single-crystal method, shows the power of powder diffraction in combination with the high-resolution data and the global optimization method.

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

Hou, Xian; Li, Yan, E-mail: liyan-nwnu@163.com; Yan, Jian-Jun

Highlights: • Kesterite CZTS nanocrystal powder was synthesized by one-pot method. • First successful use CZTS nanocrystal powder as photocatalyst. • CZTS shows an efficient photocatalysis under visible light irradiation. • CZTS photocatalyst having excellent stability. - Abstract: Cu{sub 2}ZnSnS{sub 4}, as a very promising p-type semiconductor material, has been extensively used in the study of solar cells owing to its suitable band gap (1.1–1.5 eV), large absorption coefficient of 10{sup 4} cm{sup −1} in the visible spectrum, good photo stability, nontoxicity and relative abundance of the component elements. In this paper, we have successfully synthesized p-type kesterite Cu{sub 2}ZnSnS{submore » 4} nanocrystal powder by facile one-pot method, and made our first successful attempt to use Cu{sub 2}ZnSnS{sub 4} nanocrystal powder as a photocatalyst to degradation methyl orange under visible-light irradiation. The exciting results show that in the visible light region, Cu{sub 2}ZnSnS{sub 4} nanocrystal powder possesses an excellent photocatalytic performance of K = 0.0317 min{sup −1}, nearly about 6 times of well known commercial P25 titania powder performance under the same conditions, which suggests that the p-type kesterite Cu{sub 2}ZnSnS{sub 4} nanocrystal would be a promising candidate of photocatalyst.« less

Production of coconut protein powder from coconut wet processing waste and its characterization.

PubMed

Naik, Aduja; Raghavendra, S N; Raghavarao, K S M S

2012-07-01

Virgin coconut oil (VCO) has been gaining popularity in recent times. During its production, byproducts such as coconut skim milk and insoluble protein are obtained which are underutilized or thrown away to the environment at present. This study deals with utilization of these byproducts to obtain a value-added product, namely, coconut protein powder. When coconut milk was subjected to centrifugation, three phases, namely, fat phase (coconut cream), aqueous phase (coconut skim milk), and solid phase (insoluble protein) were obtained. The coconut skim milk and insoluble protein were mixed and homogenized before spray drying to obtain a dehydrated protein powder. The proximate analysis of the powder showed high protein content (33 % w/w) and low fat content (3 % w/w). Protein solubility was studied as a function of pH and ionic content of solvent. Functional properties such as water hydration capacity, fat absorption capacity, emulsifying properties, wettability, and dispersibility of coconut protein powder were evaluated along with morphological characterization, polyphenol content, and color analysis. Coconut protein powder has shown to have good emulsifying properties and hence has potential to find applications in emulsified foods. Sensory analysis showed high overall quality of the product, indicating that coconut protein powder could be a useful food ingredient.

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.

Discrimination of smokeless powders by headspace SPME-GC-MS and SPME-GC-ECD, and the potential implications upon training canine detection of explosives

NASA Astrophysics Data System (ADS)

Harper, Ross J.; Almirall, Jose R.; Furton, Kenneth G.

2005-05-01

This presentation will provide an odour analysis of a variety of smokeless powders & communicate the rapid SPME-GC-ECD method utilized. This paper will also discuss the implications of the headspace analysis of Smokeless Powders upon the choice of training aids for Explosives Detection Canines. Canine detection of explosives relies upon the dogs" ability to equate finding a given explosive odour with a reward, usually in the form of praise or play. The selection of explosives upon which the dogs are trained thus determines which explosives the canines can and potentially cannot find. Commonly, the training is focussed towards high explosives such as TNT and Composition 4, and the low explosives such as Black and Smokeless Powders are added often only for completeness. Powder explosives constitute a major component of explosive incidents throughout the US, and canines trained to detect explosives must be trained across the entire range of powder products. Given the variability in the manufacture and product make-up many smokeless powders do not share common odour chemicals, giving rise to concerns over the extensiveness of canine training. Headspace analysis of a selection of Smokeless Powders by Solid Phase Microextraction Gas Chromatography using Mass Spectrometry (SPME-GC-MS) and Electron Capture Detectors (SPME-GC-ECD) has highlighted significant differences in the chemical composition of the odour available from different brands. This suggests that greater attention should be paid towards the choice of Powder Explosives when assigning canine training aids.

Selenium recovery from kiln powder of cement manufacturing by chemical leaching and bioreduction.

PubMed

Soda, S; Hasegawa, A; Kuroda, M; Hanada, A; Yamashita, M; Ike, M

2015-01-01

A novel process by using chemical leaching followed by bacterial reductive precipitation was proposed for selenium recovery from kiln powder as a byproduct of cement manufacturing. The kiln powder at a slurry concentration of 10 w/v% with 0.25 M Na2CO3 at 28°C produced wastewater containing about 30 mg-Se/L selenium. The wastewater was diluted four-fold and adjusted to pH 8.0 as preconditioning for bioreduction. A bacterial strain Pseudomonas stutzeri NT-I, capable of reducing selenate and selenite into insoluble elemental selenium, could recover about 90% selenium from the preconditioned wastewater containing selenium of 5 mg-Se/L when supplemented with lactate or glycerol. The selenium concentrations in the treated wastewater were low around the regulated effluent concentration of 0.1 mg-Se/L in Japan.

X-Ray Diffraction Study of Elemental Erbium to 65 GPa

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

Pravica, M.G.; Lipinska-Kalita, K.; Quine, Z.

2006-02-02

We have investigated phase transitions in elemental erbium in a diamond anvil cell up to 65 GPa using x-ray powder diffraction methods. We present preliminary evidence of a series of phase transitions that appear to follow the expected hcp {yields} Sm-type {yields} dhcp {yields} distorted fcc sequence. In particular, we believe that we have evidence for the predicted dhcp {yields} distorted fcc transition between 43 GPa and 65 GPa.

METHOD FOR THE PREPARATION OF STABLE ACTINIDE METAL OXIDE-CONTAINING SLURRIES AND OF THE OXIDES THEREFOR

DOEpatents

Hansen, R.S.; Minturn, R.E.

1958-02-25

This patent deals with a method of preparing actinide metal oxides of a very fine particle size and of forming stable suspensions therefrom. The process consists of dissolving the nitrate of the actinide element in a combustible organic solvent, converting the solution obtained into a spray, and igniting the spray whereby an oxide powder is obtained. The oxide powder is then slurried in an aqueous soiution of a substance which is adsorbable by said oxides, dspersed in a colloid mill whereby a suspension is obtained, and electrodialyzed until a low spectiic conductance is reached.

Study of alumina-trichite reinforcement of a nickel-based matric by means of powder metallurgy

NASA Technical Reports Server (NTRS)

Walder, A.; Hivert, A.

1982-01-01

Research was conducted on reinforcing nickel based matrices with alumina trichites by using powder metallurgy. Alumina trichites previously coated with nickel are magnetically aligned. The felt obtained is then sintered under a light pressure at a temperature just below the melting point of nickel. The halogenated atmosphere technique makes it possible to incorporate a large number of additive elements such as chromium, titanium, zirconium, tantalum, niobium, aluminum, etc. It does not appear that going from laboratory scale to a semi-industrial scale in production would create any major problems.

A review of micro-powder injection moulding as a microfabrication technique

NASA Astrophysics Data System (ADS)

Attia, Usama M.; Alcock, Jeffrey R.

2011-04-01

Micro-powder injection moulding (µPIM) is a fast-developing micro-manufacturing technique for the production of metal and ceramic components. Shape complexity, dimensional accuracy, replication fidelity, material variety combined with high-volume capabilities are some of the key advantages of the technology. This review assesses the capabilities and limitations of µPIM as a micro-manufacturing technique by reviewing the latest developments in the area and by considering potential improvements. The basic elements of the process chain, variant processes and simulation attempts are discussed and evaluated. Challenges and research gaps are highlighted, and potential areas for improvement are presented.

TSX-PLUS MULTI-TASKING UPGRADE FOR THE NICOLET L-11 POWDER DIFFRACTION SYSTEM.

USGS Publications Warehouse

Fitzpatrick, J.; Queen, David L.

1985-01-01

In August of 1982, a single-user, dual-translator, automated powder diffraction system was purchased by the Denver Research Institute for use on project work in the Chemical and Materials Sciences Division. Within a short period of time, the system had already become saturated with users. Scheduling conflicts arose. In view of these problems, an answer was sought in the form of hardware and software changes which would allow many users access to the system simultaneously. A low-cost, minimum impact solution was eventually found. The elements of the solution are reported.

XAP, a program for deconvolution and analysis of complex X-ray spectra

USGS Publications Warehouse

Quick, James E.; Haleby, Abdul Malik

1989-01-01

The X-ray analysis program (XAP) is a spectral-deconvolution program written in BASIC and specifically designed to analyze complex spectra produced by energy-dispersive X-ray analytical systems (EDS). XAP compensates for spectrometer drift, utilizes digital filtering to remove background from spectra, and solves for element abundances by least-squares, multiple-regression analysis. Rather than base analyses on only a few channels, broad spectral regions of a sample are reconstructed from standard reference spectra. The effects of this approach are (1) elimination of tedious spectrometer adjustments, (2) removal of background independent of sample composition, and (3) automatic correction for peak overlaps. Although the program was written specifically to operate a KEVEX 7000 X-ray fluorescence analytical system, it could be adapted (with minor modifications) to analyze spectra produced by scanning electron microscopes, electron microprobes, and probes, and X-ray defractometer patterns obtained from whole-rock powders.

Synthesis and characterization of ligational behavior of curcumin drug towards some transition metal ions: Chelation effect on their thermal stability and biological activity

NASA Astrophysics Data System (ADS)

Refat, Moamen S.

2013-03-01

Complexes of Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with curcumin ligand as antitumor activity were synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-Vis, IR, Raman, ESR, 1H-NMR spectroscopy, X-ray diffraction analysis of powdered samples and thermal analysis, and screened for antimicrobial activity. The IR spectral data suggested that the ligand behaves as a monobasic bidentate ligand towards the central metal ion with an oxygen's donor atoms sequence of both sbnd OH and Cdbnd O groups under keto-enol structure. From the microanalytical data, the stoichiometry of the complexes 1:2 (metal:ligand) was found. The ligand and their metal complexes were screened for antibacterial activity against Escherichia Coli, Staphylococcus aureus, Bacillus subtilis and Pseudomonas aeruginosa and fungicidal activity against Aspergillus flavus and Candida albicans.

Dietary Cocoa Powder Improves Hyperlipidemia and Reduces Atherosclerosis in apoE Deficient Mice through the Inhibition of Hepatic Endoplasmic Reticulum Stress.

PubMed

Guan, Hua; Lin, Yan; Bai, Liang; An, Yingfeng; Shang, Jianan; Wang, Zhao; Zhao, Sihai; Fan, Jianglin; Liu, Enqi

2016-01-01

Cocoa powder is rich in flavonoids, which have many beneficial effects on human health, including antioxidative and anti-inflammatory effects. The aim of our study was to investigate whether the intake of cocoa powder has any influence on hyperlipidemia and atherosclerosis and examine the underlying molecular mechanisms. We fed apoE knockout mice a Western diet supplemented with either 0.2% (low group) or 2% (high group) cocoa powder for 12 weeks. The groups fed dietary cocoa powder showed a significant reduction in both plasma cholesterol levels and aortic atherosclerosis compared to the control group. Analysis of mRNA profiling of aortic atherosclerotic lesions revealed that the expression of several genes related to apoptosis, lipid metabolism, and inflammation was significantly reduced, while the antiapoptotic gene Bcl2 was significantly increased in the cocoa powder group compared to the control. RT-PCR analysis along with Western blotting revealed that a diet containing cocoa powder inhibited the expression of hepatic endoplasmic reticulum stress. These data suggest that cocoa powder intake improves hyperlipidemia and atherosclerosis, and such beneficial effects are possibly mediated through the suppression of hepatic endoplasmic reticulum stress.

Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES.

PubMed

Matschat, Ralf; Hassler, Jürgen; Traub, Heike; Dette, Angelika

2005-12-01

The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and used to determine the repeatability and the reproducibility (expressed as standard deviations) of both methods. The calculation was carried out according to the related standard. The results are specified and discussed in this paper, as are the optimized analytical conditions determined and used by the authors of this paper. For both methods, the repeatability relative standard deviations were <25%, usually ~10%, and the reproducibility relative standard deviations were <35%, usually ~15%. These results were regarded as satifactory for both methods intended for rapid analysis of materials for which decomposition is difficult and time-consuming. Also described are some results from an interlaboratory comparison used to certify one of the materials that had been previously used for validation in both interlaboratory comparisons. Thirty laboratories (from eight countries) participated in this interlaboratory comparison for certification. As examples, accepted results are shown from laboratories that used ETV ICP OES or DC arc OES and had performed calibrations by using solutions or oxides, respectively. The certified mass fractions of the certified reference materials were also compared with the mass fractions determined in the interlaboratory comparisons performed within the framework of method standardization. Good agreement was found for most of the analytes.

Gas-Phase Combustion Synthesis of Aluminum Nitride Powder

NASA Technical Reports Server (NTRS)

Axelbaum, R. L.; Lottes, C. R.; Huertas, J. I.; Rosen, L. J.

1996-01-01

Due to its combined properties of high electrical resistivity and high thermal conductivity aluminum nitride (AlN) is a highly desirable material for electronics applications. Methods are being sought for synthesis of unagglomerated, nanometer-sized powders of this material, prepared in such a way that they can be consolidated into solid compacts having minimal oxygen content. A procedure for synthesizing these powders through gas-phase combustion is described. This novel approach involves reacting AlCl3, NH3, and Na vapors. Equilibrium thermodynamic calculations show that 100% yields can be obtained for these reactants with the products being AlN, NaCl, and H2. The NaCl by-product is used to coat the AlN particles in situ. The coating allows for control of AlN agglomeration and protects the powders from hydrolysis during post-flame handling. On the basis of thermodynamic and kinetic considerations, two different approaches were employed to produce the powder, in co-flow diffusion flame configurations. In the first approach, the three reactants were supplied in separate streams. In the second, the AlCl3 and NH3 were premixed with HCl and then reacted with Na vapor. X-ray diffraction (XRD) spectra of as-produced powders show only NaCl for the first case and NaCl and AlN for the second. After annealing at 775 C tinder dynamic vacuum, the salt was removed and XRD spectra of powders from both approaches show only AlN. Aluminum metal was also produced in the co-flow flame by reacting AlCl3 with Na. XRD spectra of as-produced powders show the products to be only NaCl and elemental aluminum.

Compliant high temperature seals for dissimilar materials

DOEpatents

Rynders, Steven Walton; Minford, Eric; Tressler, Richard Ernest; Taylor, Dale M.

2001-01-01

A high temperature, gas-tight seal is formed by utilizing one or more compliant metallic toroidal ring sealing elements, where the applied pressure serves to activate the seal, thus improving the quality of the seal. The compliant nature of the sealing element compensates for differences in thermal expansion between the materials to be sealed, and is particularly useful in sealing a metallic member and a ceramic tube art elevated temperatures. The performance of the seal may be improved by coating the sealing element with a soft or flowable coating such as silver or gold and/or by backing the sealing element with a bed of fine powder. The material of the sealing element is chosen such that the element responds to stress elastically, even at elevated temperatures, permitting the seal to operate through multiple thermal cycles.

Effect of acidity on the citrate-nitrate combustion synthesis of alumina-zirconia composite powder

NASA Astrophysics Data System (ADS)

Chandradass, J.; Kim, Ki Hyeon

2009-12-01

Alumina-zirconia composite powders were produced by sol-gel autocombustion. 20 wt.% ZrO2-Al2O3 mixture precursor solutions were chelated by citric acid ions at different pH. DTA analysis shows sluggish decomposition at low pH, whereas there was rapid decomposition at high pH = 9. XRD patterns of the calcined powders showed that well crystallized powder with 100 % tetragonal phase and α-alumina phase is produced when pH = 0.58 (without ammonia addition). TEM characterization of composite powders revealed homogenous distribution of nanosized zirconia particles in the alumina matrix. FTIR analysis shows peaks at 590 cm-1 and 454 cm-1, which are identified as the characteristic absorption bands of Zr-O and Al-O.

Quantitative prediction of the bitterness suppression of elemental diets by various flavors using a taste sensor.

PubMed

Miyanaga, Yohko; Inoue, Naoko; Ohnishi, Ayako; Fujisawa, Emi; Yamaguchi, Maki; Uchida, Takahiro

2003-12-01

The purpose of the study was to develop a method for the quantitative prediction of the bitterness suppression of elemental diets by various flavors and to predict the optimum composition of such elemental diets for oral administration using a multichannel taste sensor. We examined the effects of varying the volume of water used for dilution and of adding varying quantities of five flavors (pineapple, apple, milky coffee, powdered green tea, and banana) on the bitterness of the elemental diet, Aminoreban EN. Gustatory sensation tests with human volunteers (n = 9) and measurements using the artificial taste sensor were performed on 50 g Aminoreban EN dissolved in various volumes (140), 180, 220, 260, 300, 420, 660, 1140, and 2100 ml) of water, and on 50 g Aminoreban EN dissolved in 180 ml of water with the addition of 3-9 g of various flavors for taste masking. In gustatory sensation tests, the relationship between the logarithmic values of the volumes of water used for dilution and the bitterness intensity scores awarded by the volunteers proved to be linear. The addition of flavors also reduced the bitterness of elemental diets in gustatory sensation tests; the magnitude of this effect was, in decreasing order, apple, pineapple, milky coffee, powdered green tea, and banana. With the artificial taste sensor, large changes of membrane potential in channel 1, caused by adsorption (CPA values, corresponding to a bitter aftertaste), were observed for Aminoreban EN but not for any of the flavors. There was a good correlation between the CPA values in channel 1 and the results of the human gustatory tests, indicating that the taste sensor is capable of evaluating not only the bitterness of Aminoreban EN itself but also the bitterness-suppressing effect of the five flavors, which contained many elements such as organic acids and flavor components, and the effect of dilution (by water) on this bitterness. Using regression analysis of data derived from the taste sensor and from human gustatory data for four representative points, we were able to predict the bitterness of 50 g Aminoreban EN solutions diluted with various volumes of water (14-300 ml), with or without the addition of a selected flavor. Even though this prediction method does not offer perfect simulation of human taste sensations, the artificial taste sensor may be useful for predicting the bitterness intensity of elemental diets containing various flavors in the absence of results from full gustatory sensation tests.

Hydrologic Reconnaissance of Wetland-Bird Habitat in Areas With Potential to be Influenced by Water Produced During Coalbed Methane Production in the Northern Powder River Basin, MT

NASA Astrophysics Data System (ADS)

Custer, S. G.; Sojda, R. S.

2003-12-01

The removal and disposal of ground water during production of coalbed methane has the potential to influence wetland-bird habitat in the Powder River Basin. Office analysis of wetland areas was conducted on National Wetland Inventory maps and Digital Orthophoto Quadrangles along the Tongue and Powder rivers in the northern Powder River Basin, Montana. Selected sites were palustrine emergent, large enough to be important to waterbirds, part of a wetland complex, not dependent on artificial water regimes, in an area with high potential for coalbed methane production, and judged to be accessible in the field. Several promising wetland areas were selected for field examination. Field investigation suggests that the most promising wetlands in oxbow cutoffs would not be productive sites. Only facultative not obligate wetland plants were observed, the topographic position of the wetlands suggested that flooding would be infrequent, and the stream flow would likely dilute the effect of produced water adjacent to these rivers. Fortuitously wetland-bird habitat not recognized on the National Wetland Inventory maps and Digital Orthophoto Quadrangles was observed along Rosebud Creek during the field reconnaissance. This habitat is not continuous. The lack of continuity is reflected in the soil surveys as well as in the reconnaissance field nvestigation. The Alluvial Land soil series corresponds to observed wetland areas but the extent of the wetland-bird habitat varies substantially within the soil unit. When the Korchea series is present, extensive wetland-bird habitat is not observed. Field and aerial photo analysis suggests that the presence of the habitat may be controlled by beaver, and/or by stratigraphic and structural elements that influence stream erosion. Human modification of the stream for irrigation purposes may impact habitat continuity in some areas. The "Rosebud" type wetland-bird habitat may have the potential to be influenced by coalbed methane water production and warrants further more detailed investigation to determine the areal extent of the habitat, to determine the factors that control the distribution of intermittent wetland-bird-habitat areas, and to better model whether and how water produced during coalbed methane development might influence wetland-bird habitat.

A new titanium based alloy Ti-27Nb-13Zr produced by powder metallurgy with biomimetic coating for use as a biomaterial.

PubMed

Mendes, Marcio W D; Ágreda, Carola G; Bressiani, Ana H A; Bressiani, José C

2016-06-01

Titanium alloys are widely used in biomedical applications due to their excellent properties such as high strength, good corrosion resistance and biocompatibility. Titanium alloys with alloying elements such as Nb and Zr are biocompatible and have Young's modulus close to that of human bone. To increase the bioactivity of titanium alloy surfaces is used chemical treatment with NaOH followed by immersion in simulated body fluid (SBF). The purpose of this study was to produce the alloy Ti-27Nb-13Zr with low Young's modulus by powder metallurgy using powders produced by the HDH process. The formation of biomimetic coatings on samples immersed in SBF for 3, 7, 11 and 15 days was evaluated. Characterization of the coating was performed by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and scanning electron microscope. The microstructure and composition of the alloy were determined using SEM and XRD, while the mechanical properties were evaluated by determining the elastic modulus and the Vickers microhardness. The sintered alloys were composed of α and β phases, equiaxed grains and with density around 97.8% of its theoretical density. The Vickers microhardness and elasticity modulus of the alloy were determined and their values indicate that this alloy can be used as a biomaterial. Analysis of the coating revealed the presence of calcium phosphate layers on samples immersed for >3 days in the SBF solution. Copyright © 2016 Elsevier B.V. All rights reserved.

Numerical Analysis of the Effect of Particle Shape and Adhesion on the Segregation of Powder Mixtures

NASA Astrophysics Data System (ADS)

Alizadeh Behjani, Mohammadreza; Hassanpour, Ali; Ghadiri, Mojtaba; Bayly, Andrew

2017-06-01

Segregation of granules is an undesired phenomenon in which particles in a mixture separate from each other based on the differences in their physical and chemical properties. It is, therefore, crucial to control the homogeneity of the system by applying appropriate techniques. This requires a fundamental understanding of the underlying mechanisms. In this study, the effect of particle shape and cohesion has been analysed. As a model system prone to segregation, a ternary mixture of particles representing the common ingredients of home washing powders, namely, spray dried detergent powders, tetraacetylethylenediamine, and enzyme placebo (as the minor ingredient) during heap formation is modelled numerically by the Discrete Element Method (DEM) with an aim to investigate the effect of cohesion/adhesion of the minor components on segregation quality. Non-spherical particle shapes are created in DEM using the clumped-sphere method based on their X-ray tomograms. Experimentally, inter particle adhesion is generated by coating the minor ingredient (enzyme placebo) with Polyethylene Glycol 400 (PEG 400). The JKR theory is used to model the cohesion/adhesion of coated enzyme placebo particles in the simulation. Tests are carried out experimentally and simulated numerically by mixing the placebo particles (uncoated and coated) with the other ingredients and pouring them in a test box. The simulation and experimental results are compared qualitatively and quantitatively. It is found that coating the minor ingredient in the mixture reduces segregation significantly while the change in flowability of the system is negligible.

Geochemical processes controlling selenium in ground water after mining, Powder River Basin, Wyoming, U.S.A.

USGS Publications Warehouse

Naftz, D.L.; Rice, J.A.

1989-01-01

Geochemical data for samples of overburden from three mines in the Powder River Basin indicate a statistically significant (0.01 confidence level) positive correlation (r = 0.74) between Se and organic C. Results of factor analysis with varimax rotation on the major and trace element data from the rock samples indicate large (>50) varimax loadings for Se in two of the three factors. In Factor 1, the association of Se with constituents common to detrital grains indicates that water transporting the detrital particles into the Powder River Basin also carried dissolved Se. The large (>50) varimax loadings of Se and organic C in Factor 2 probably are due to the organic affinities characteristic of Se. Dissolved Se concentrations in water samples collected at one coal mine are directly related to the dissolved organic C concentrations. Hydrophilic acid concentrations in the water samples from the mine ranged from 35 to 43% of the total dissolved organic C, and hydrophobic acid concentrations ranged from 40 to 49% of the total dissolved organic C. The largest dissolved organic C concentrations in water from the same mine (34-302 mg/l), coupled with the large proportion of acidic components, may saturate adsorption sites on geothite and similar minerals that comprise the aquifer material, thus decreasing the extent of selenite (SeO32-) adsorption as a sink for Se as the redox state of ground water decreases. ?? 1989.

Effect of polymer coating on the osseointegration of CP-Ti dental implant

NASA Astrophysics Data System (ADS)

Al-Hassani, Emad; Al-Hassani, Fatima; Najim, Manar

2018-05-01

Modifications achieved coatings of titanium samples were investigated in order to improve their surface characteristics so as to facilitate bio-integration. Chitosan coating was use for commercial pure Ti alloys manufactured by two different methods in which commercial pure titanium rod converted in form of implant screw by using wire cut machine and lathe, second method included the used of powder technology for producing the implant screws. The coating process of chitosan polymer was carried out using advance technology (electrospnning process) to create fibrous structure from Nano to micro scale of the chitosan on the implant surface which result in a bioactive surface. The characterization includes; microstructure observation, surface chemical composition analysis (EDS), surface roughness (AFM), and the histological analysis. from the SEM No morphological differences were observed among the implants surfaces except for some inconsiderable morphological differences that results from the manufacturing process, by using EDX analysis the surfaces chemical compositions were completely changed and there was large decrease in the percentage of titanium element at the surface which indicates that the surface is covered with chitosan and had a new surface composition and topography. The sample was produced by powder technology process have higher roughness (845.36 nm) than sample produced by machining without any surface treatment (531.7nm),finally The histological view of implant samples after 4weeks of implantation, showed active bone formation in all implant surface which give clear indication of tissue acceptance.

The synthesis and the spectroscopic, thermal, and structural properties of the M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) clathrate (M = Co, Ni, Cd and Hg)

NASA Astrophysics Data System (ADS)

Kartal, Zeki; Yavuz, Abdülkerim

2018-03-01

In this study, the clathrates of fumarate-tetracyanonickel-dioxane, given by the formula M2[(fumarate)Ni(CN)4]·2(1,4-Dioxane) (M = Co, Ni, Cd and Hg), have been obtained for the first time through chemical methods. These clathrates have been characterized by elemental, thermal, FT-IR, and FT-Raman spectroscopies. The parameters of structures of clathrates have been determined by X-ray powder diffraction. The thermal behaviors of these clathrates have been also investigated by thermo-gravimetric analysis (TGA), differential thermal analysis (DTA), and derivative thermal gravimetric analysis (DTG) in the range of 20-900 °C. X-ray powder diffraction data have been recorded at ambient temperature in the 2θ range 5-50°. The FT-IR and FT-Raman spectra of clathrates have been recorded in the region of 4000-400 cm-1 and 4000-100 cm-1, respectively. The results of the spectral and thermal analyses of the newly synthesized clathrates of fumarate-tetracyanonickel-dioxane suggest that these clathrates are new examples of the Hofmann-type dioxane clathrates. In our study, the Hofmann-type dioxane clathrates, which are formed by bounding electrons of oxygen-donor atoms of fumarate ion ligand molecule to transition metal atoms, consist of the corrugated |M-Ni(CN)4|∞ polymeric layers, which are held in parallel through the chain of (-M-fumarate-M-).

Removal of residual particulate matter from filter media

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

Almlie, Jay C.; Miller, Stanley J.

A method for removing residual filter cakes that remain adhered to a filter after typical particulate removal methodologies have been employed, such as pulse-jet filter element cleaning, for all cleanable filters used for air pollution control, dust control, or powder control.

Removal of residual particulate matter from filter media

DOEpatents

Almlie, Jay C; Miller, Stanley J

2014-11-11

A method for removing residual filter cakes that remain adhered to a filter after typical particulate removal methodologies have been employed, such as pulse-jet filter element cleaning, for all cleanable filters used for air pollution control, dust control, or powder control.

Denudation of metal powder layers in laser powder bed fusion processes

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

Matthews, Manyalibo J.; Guss, Gabe; Khairallah, Saad A.

Understanding laser interaction with metal powder beds is critical in predicting optimum processing regimes in laser powder bed fusion additive manufacturing of metals. In this work, we study the denudation of metal powders that is observed near the laser scan path as a function of laser parameters and ambient gas pressure. We show that the observed depletion of metal powder particles in the zone immediately surrounding the solidified track is due to a competition between outward metal vapor flux directed away from the laser spot and entrainment of powder particles in a shear flow of gas driven by a metalmore » vapor jet at the melt track. Between atmospheric pressure and ~10 Torr of Ar gas, the denuded zone width increases with decreasing ambient gas pressure and is dominated by entrainment from inward gas flow. The denuded zone then decreases from 10 to 2.2 Torr reaching a minimum before increasing again from 2.2 to 0.5 Torr where metal vapor flux and expansion from the melt pool dominates. In addition, the dynamics of the denudation process were captured using high-speed imaging, revealing that the particle movement is a complex interplay among melt pool geometry, metal vapor flow, and ambient gas pressure. The experimental results are rationalized through finite element simulations of the melt track formation and resulting vapor flow patterns. The results presented here represent new insights to denudation and melt track formation that can be important for the prediction and minimization of void defects and surface roughness in additively manufactured metal components.« less

Denudation of metal powder layers in laser powder bed fusion processes

DOE PAGES

Matthews, Manyalibo J.; Guss, Gabe; Khairallah, Saad A.; ...

2016-05-20

Understanding laser interaction with metal powder beds is critical in predicting optimum processing regimes in laser powder bed fusion additive manufacturing of metals. In this work, we study the denudation of metal powders that is observed near the laser scan path as a function of laser parameters and ambient gas pressure. We show that the observed depletion of metal powder particles in the zone immediately surrounding the solidified track is due to a competition between outward metal vapor flux directed away from the laser spot and entrainment of powder particles in a shear flow of gas driven by a metalmore » vapor jet at the melt track. Between atmospheric pressure and ~10 Torr of Ar gas, the denuded zone width increases with decreasing ambient gas pressure and is dominated by entrainment from inward gas flow. The denuded zone then decreases from 10 to 2.2 Torr reaching a minimum before increasing again from 2.2 to 0.5 Torr where metal vapor flux and expansion from the melt pool dominates. In addition, the dynamics of the denudation process were captured using high-speed imaging, revealing that the particle movement is a complex interplay among melt pool geometry, metal vapor flow, and ambient gas pressure. The experimental results are rationalized through finite element simulations of the melt track formation and resulting vapor flow patterns. The results presented here represent new insights to denudation and melt track formation that can be important for the prediction and minimization of void defects and surface roughness in additively manufactured metal components.« less

Toxic metal levels in cocoa powder and chocolate by ICP-MS method after microwave-assisted digestion.

PubMed

Lo Dico, Gianluigi Maria; Galvano, Fabio; Dugo, Giacomo; D'ascenzi, Carlo; Macaluso, Andrea; Vella, Antonio; Giangrosso, Giuseppe; Cammilleri, Gaetano; Ferrantelli, Vincenzo

2018-04-15

The Commission Regulation (EC) Regulation N. 488/2014, established the concentration limits for cadmium in specific products based on cocoa and chocolate products as from January 2019. Based on this information there is a need to determine ultratrace levels of elements that might be presents in cocoa and chocolate products. In this work, the concentrations of Arsenic, Antimony, Cadmium, Chromium, Lead, Selenium and Vanadium were evaluated in cocoa powder and chocolate by the validation of an ICP-MS method. Good selectivity/specificity, recovery, repeatability and within-laboratory reproducibility, LOD, LOQ, range of linearity, standard measurement uncertainty parameters for method validation were achieved, in accordance with Commission Regulation. The cocoa powder revealed the maximum metal concentrations of 0.303 ± 0.035 mg/kg for cadmium, 1.228 ± 0.146 mg/kg for lead and 0.094 ± 0.013 mg/kg for arsenic. A significant difference was found between cocoa powder and chocolate samples (p < .05). Copyright © 2017 Elsevier Ltd. All rights reserved.

Modeling picking on pharmaceutical tablets

NASA Astrophysics Data System (ADS)

Swaminathan, Shrikant

Tablets are the most popular solid dosage form in the pharmaceutical industry because they are cheap to manufacture, chemically and mechanically stable and easy to transport and fairly easy to control dosage. Pharmaceutical tableting operations have been around for decades however the process is still not well understood. One of the common problems faced during the production of pharmaceutical tablets by powder compaction is sticking of powder to the punch face, This is known as 'sticking'. A more specialized case of sticking is picking when the powder is pulled away form the compact in the vicinity of debossed features. In the pharmaceutical industry, picking is solved by trial and error which is an expensive, labor intensive and time consuming affair. The objective of this work was to develop, validate, and implement a modeling framework for predicting picking in powder compacts. The model was developed in Abaqus a commercially available finite element package. The resulting model was used to investigate the influence of debossed feature geometry viz. the stroke angle and degree of pre-pick, and, influence of lubricant on picking. (Abstract shortened by ProQuest.).

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

NASA Astrophysics Data System (ADS)

Santhanam, Priya Radhi

Mechanical milling is a widely used technique for powder processing in various areas. In this work, a scale-up model for describing this ball milling process is developed. The thesis is a combination of experimental and modeling efforts. Initially, Discrete Element Model (DEM) is used to describe energy transfer from milling tools to the milled powder for shaker, planetary, and attritor mills. The rolling and static friction coefficients are determined experimentally. Computations predict a quasisteady rate of energy dissipation, E d, for each experimental configuration. It is proposed that the milling dose defined as a product of Ed and milling time, t, divided by the mass of milled powder, mp characterizes the milling progress independently of the milling device or milling conditions used. Once the milling dose is determined for one experimental configuration, it can be used to predict the milling time required to prepare the same material in any milling configuration, for which Ed is calculated. The concept is validated experimentally for DEM describing planetary and shaker mills. For attritor, the predicted Ed includes substantial contribution from milling tool interaction events with abnormally high forces (>103 N). The energy in such events is likely dissipated to heat or plastically deform milling tools rather than refine material. Indeed, DEM predictions for the attritor correlate with experiments when such events are ignored in the analysis. With an objective of obtaining real-time indicators of milling progress, power, torque, and rotation speed of the impeller of an attritor mill are measured during preparation of metal matrix composite powders in the subsequent portion of this thesis. Two material systems are selected and comparisons made between in-situ parameters and experimental milling progress indicators. It is established that real-time measurements can certainly be used to describe milling progress. However, they need to be interpreted carefully depending on hardness of brittle component relative to milling media. To improve the DEM model of the attritor mill, it is desired to avoid the removal of unrealistic, high-force events using an approach that would not predict such events in the first place. It is observed that during experiments in attritor, balls may jam causing an increased resistance to the impeller's rotation. The impeller may instantaneously slow down, quickly returning to its pre-set rotation rate. Previous DEM models did not account for such rapid changes in the impeller's rotation. In this work, this relationship between impeller's torque and rotation rate is obtained experimentally and introduced in DEM. As a result, predicted Ed, are shown to correlate well with the experimental data. Finally, a methodology is proposed combining an experiment and its DEM description enabling one to identify the appropriate interaction parameters for powder systems. The experiment uses a miniature vibrating hopper and can be applied to characterize the powder flow for variety of materials. The hopper is designed to hold up to 20,000 particles of 50-mum diameter, which can be directly described in DEM. Based on comparison of discharge rate from experiments and model, all 6 interaction parameters were analyzed and the ideal conditions identified for Zirconia beads. The values of these parameters for powders are generally not the same as those established for macroscopic bodies. In addition, effects of some other experimental parameters such as particle size distribution and amplitude of vibration are also investigated.

Spectral Interferences Manganese (Mn) - Europium (Eu) Lines in X-Ray Fluorescence Spectrometry Spectrum

NASA Astrophysics Data System (ADS)

Tanc, Beril; Kaya, Mustafa; Gumus, Lokman; Kumral, Mustafa

2016-04-01

X-ray fluorescence (XRF) spectrometry is widely used for quantitative and semi quantitative analysis of many major, minor and trace elements in geological samples. Some advantages of the XRF method are; non-destructive sample preparation, applicability for powder, solid, paste and liquid samples and simple spectrum that are independent from chemical state. On the other hand, there are some disadvantages of the XRF methods such as poor sensitivity for low atomic number elements, matrix effect (physical matrix effects, such as fine versus course grain materials, may impact XRF performance) and interference effect (the spectral lines of elements may overlap distorting results for one or more elements). Especially, spectral interferences are very significant factors for accurate results. In this study, semi-quantitative analyzed manganese (II) oxide (MnO, 99.99%) was examined. Samples were pelleted and analyzed with XRF spectrometry (Bruker S8 Tiger). Unexpected peaks were obtained at the side of the major Mn peaks. Although sample does not contain Eu element, in results 0,3% Eu2O3 was observed. These result can occur high concentration of MnO and proximity of Mn and Eu lines. It can be eliminated by using correction equation or Mn concentration can confirm with other methods (such as Atomic absorption spectroscopy). Keywords: Spectral Interferences; Manganese (Mn); Europium (Eu); X-Ray Fluorescence Spectrometry Spectrum.

Rapid identification of pearl powder from Hyriopsis cumingii by Tri-step infrared spectroscopy combined with computer vision technology

NASA Astrophysics Data System (ADS)

Liu, Siqi; Wei, Wei; Bai, Zhiyi; Wang, Xichang; Li, Xiaohong; Wang, Chuanxian; Liu, Xia; Liu, Yuan; Xu, Changhua

2018-01-01

Pearl powder, an important raw material in cosmetics and Chinese patent medicines, is commonly uneven in quality and frequently adulterated with low-cost shell powder in the market. The aim of this study is to establish an adequate approach based on Tri-step infrared spectroscopy with enhancing resolution combined with chemometrics for qualitative identification of pearl powder originated from three different quality grades of pearls and quantitative prediction of the proportions of shell powder adulterated in pearl powder. Additionally, computer vision technology (E-eyes) can investigate the color difference among different pearl powders and make it traceable to the pearl quality trait-visual color categories. Though the different grades of pearl powder or adulterated pearl powder have almost identical IR spectra, SD-IR peak intensity at about 861 cm- 1 (v2 band) exhibited regular enhancement with the increasing quality grade of pearls, while the 1082 cm- 1 (v1 band), 712 cm- 1 and 699 cm- 1 (v4 band) were just the reverse. Contrastly, only the peak intensity at 862 cm- 1 was enhanced regularly with the increasing concentration of shell powder. Thus, the bands in the ranges of (1550-1350 cm- 1, 730-680 cm- 1) and (830-880 cm- 1, 690-725 cm- 1) could be exclusive ranges to discriminate three distinct pearl powders and identify adulteration, respectively. For massive sample analysis, a qualitative classification model and a quantitative prediction model based on IR spectra was established successfully by principal component analysis (PCA) and partial least squares (PLS), respectively. The developed method demonstrated great potential for pearl powder quality control and authenticity identification in a direct, holistic manner.

Rapid identification of pearl powder from Hyriopsis cumingii by Tri-step infrared spectroscopy combined with computer vision technology.

PubMed

Liu, Siqi; Wei, Wei; Bai, Zhiyi; Wang, Xichang; Li, Xiaohong; Wang, Chuanxian; Liu, Xia; Liu, Yuan; Xu, Changhua

2018-01-15

Pearl powder, an important raw material in cosmetics and Chinese patent medicines, is commonly uneven in quality and frequently adulterated with low-cost shell powder in the market. The aim of this study is to establish an adequate approach based on Tri-step infrared spectroscopy with enhancing resolution combined with chemometrics for qualitative identification of pearl powder originated from three different quality grades of pearls and quantitative prediction of the proportions of shell powder adulterated in pearl powder. Additionally, computer vision technology (E-eyes) can investigate the color difference among different pearl powders and make it traceable to the pearl quality trait-visual color categories. Though the different grades of pearl powder or adulterated pearl powder have almost identical IR spectra, SD-IR peak intensity at about 861cm -1 (v 2 band) exhibited regular enhancement with the increasing quality grade of pearls, while the 1082cm -1 (v 1 band), 712cm -1 and 699cm -1 (v 4 band) were just the reverse. Contrastly, only the peak intensity at 862cm -1 was enhanced regularly with the increasing concentration of shell powder. Thus, the bands in the ranges of (1550-1350cm -1 , 730-680cm -1 ) and (830-880cm -1 , 690-725cm -1 ) could be exclusive ranges to discriminate three distinct pearl powders and identify adulteration, respectively. For massive sample analysis, a qualitative classification model and a quantitative prediction model based on IR spectra was established successfully by principal component analysis (PCA) and partial least squares (PLS), respectively. The developed method demonstrated great potential for pearl powder quality control and authenticity identification in a direct, holistic manner. Copyright © 2017. Published by Elsevier B.V.

Bifunctional air electrodes containing elemental iron powder charging additive

DOEpatents

Liu, Chia-tsun; Demczyk, Brian G.; Gongaware, Paul R.

1982-01-01

A bifunctional air electrode for use in electrochemical energy cells is made, comprising a hydrophilic layer and a hydrophobic layer, where the hydrophilic layer essentially comprises a hydrophilic composite which includes: (i) carbon; (ii) elemental iron particles having a particle size of between about 25 microns and about 700 microns diameter; (iii) an oxygen evolution material; (iv) a nonwetting agent; and (v) a catalyst, where at least one current collector is formed into said composite.

X-ray diffraction study of elemental erbium to 70 GPa

NASA Astrophysics Data System (ADS)

Pravica, Michael G.; Romano, Edward; Quine, Zachary

2005-12-01

We have investigated phase transitions in elemental erbium in a diamond anvil cell (DAC) up to 70GPa using angular-dispersive x-ray powder diffraction methods. We present evidence of a series of phase transitions that appear to follow the anticipated hcp→Sm-type→doublehcp(dhcp)→distorted fcc sequence. In particular, we present evidence for the predicted dhcp→distorted fcc transition above 63GPa . Equation of state data are also presented up to 70GPa .

Phase analysis of Košice meteorite: Preliminary results

NASA Astrophysics Data System (ADS)

Sitek, J.; Dekan, J.; Degmová, J.; Sedlačková, K.

2012-10-01

Meteorite fall was observed by the Košice town in Slovakia in February 2010 and it was classified as an ordinary chondrite H5. The samples were prepared in powder form scratched from the surface. Mossbauer spectra were measured at room temperature and liquid nitrogen temperature. Spectra consist of components related to iron-bearing phases with different content. Non-magnetic part was fitted with three quadrupole doublets. According to its parameters, we identified olivine, pyroxene, and traces of Fe3+ phases. Magnetic part consists of an iron-rich Fe-Ni alloy with hyperfine magnetic field similar to kamacite α-Fe(Ni,Co) and troilite. Main elements were also determined by X-ray fluorescence spectroscopy.

Simultaneous Measurement of Zinc, Copper, Lead and Cadmium in Baby Weaning Food and Powder Milk by DPASV.

PubMed

Sadeghi, Naficeh; Oveisi, Mohammad Reza; Jannat, Behrooz; Hajimahmoodi, Mannan; Behfar, Abdolazim; Behzad, Masoomeh; Norouzi, Narges; Oveisi, Morvarid; Jannat, Behzad

2014-01-01

Apart from the breast milk, infant formula and baby weaning food have a special role in infant diet. Infants and young children are very susceptible to amount of trace elements. Copper and zinc are two elements that add in infant food. Lead and cadmium are heavy metals that enter to food chain unavoidably. DPASV is a benefit and applicable method for measurement of trace elements in food products. In this study, concentration of zinc, copper, lead and cadmium in four brands of baby food (rice and wheat based) and powder milk was analyzed with DPASV and polarograph set. Total Mean ± SE of zinc, copper, lead and cadmium in baby foods (n = 240) were 11.86 ± 1.474 mg/100g, 508.197 ± 83.154 μg/100g, 0.445 ± 0.006, 0.050 ± 0.005 mg/Kg respectively. Also these amount in powder milk (n = 240) were 3.621± 0.529 mg/100g, 403.822 ± 133.953 μg/100g, 0.007 ± 0.003, 0.060 ± 0.040 mg/Kg respectively. Zinc level in baby food type I was higher than lablled value (P = 0.030), but in other brands was not difference. Concentration of copper in all of samples was in labeled range (P > 0.05). In each four products, level of lead and cadmium were lower than the standard limit (P < 0.05). Amount of zinc and lead in baby food I, had difference versus other products. Concentration of zinc, camium in baby food type I, was higher than type II (P = 0.043, 0.001 respectively). Concentration of lead and cadmium in baby food type II, was higher than infant formulas, but are in standard limit.

TC17 titanium alloy laser melting deposition repair process and properties

NASA Astrophysics Data System (ADS)

Liu, Qi; Wang, Yudai; Zheng, Hang; Tang, Kang; Li, Huaixue; Gong, Shuili

2016-08-01

Due to the high manufacturing cost of titanium compressor blisks, aero engine repairing process research has important engineering significance and economic value. TC17 titanium alloy is a rich β stable element dual α+β phase alloy whose nominal composition is Ti-5Al-2Sn-2Zr-4Mo-4Cr. It has high mechanical strength, good fracture toughness, high hardenability and a wide forging-temperature range. Through a surface response experiment with different laser powers, scanning speeds and powder feeding speeds, the coaxial powder feeding laser melting deposition repair process is studied for the surface circular groove defects. In this paper, the tensile properties, relative density, microhardness, elemental composition, internal defects and microstructure of the laser-repaired TC17 forging plate are analyzed. The results show that the laser melting deposition process could realize the form restoration of groove defect; tensile strength and elongation could reach 1100 MPa and 10%, which could reach 91-98% that of original TC17 wrought material; with the optimal parameters (1000 W-25 V-8 mm/s), the microhardness of the additive zone, the heat-affected zone and base material is evenly distributed at 370-390 HV500. The element content difference between the additive zone and base material is less than ±0.15%. Due to the existence of the pores 10 μm in diameter, the relative density could reach 99%, which is mainly inversely proportional to the powder feeding speed. The repaired zone is typically columnar and dendrite crystal, and the 0.5-1.5 mm-deep heat-affected zone in the groove interface is coarse equiaxial crystal.

An analysis of un-dissolved powders of instant powdered soup by using ultrasonographic image

NASA Astrophysics Data System (ADS)

Kawaai, Yukinori; Kato, Kunihito; Yamamoto, Kazuhiko; Kasamatsu, Chinatsu

2008-11-01

Nowadays, there are many instant powdered soups around us. When we make instant powdered soup, sometimes we cannot dissolve powders perfectly. Food manufacturers want to improve this problem in order to make better products. Therefore, they have to measure the state and volume of un-dissolved powders. Earlier methods for analyzing removed the un-dissolved powders from the container, the state of the un-dissolved power was changed. Our research using ultrasonographic image can measure the state of un-dissolved powders with no change by taking cross sections of the soup. We then make 3D soup model from these cross sections of soup. Therefore we can observe the inside of soup that we do not have ever seen. We construct accurate 3D model. We can visualize the state and volume of un-dissolved powders with analyzing the 3D soup models.

The use of glass powder in making batako

NASA Astrophysics Data System (ADS)

Nursyamsi, N.; Indrawan, I.

2018-02-01

Along with the increase in construction materials, innovation is needed to lessen the use of them, and one of them is by using cement [1]. In this research, it is reduced by glass powder; the reason for using it as the substitution of cement is that some chemical elements in cement are similar to those in glass powder such as SiO2, A12o3, Fe2O3, and CaO. The glass powder used was the one who passed sieve no. 100 and was hampered in sieve no. 200. It passed sieve no. 200 with its composition of 0%, 10%, 15%, 20%, 25%, and 30% from the volume of the use of cement. The specimen would treat within 28 days before the testing of compressive strength, water absorption, and tensile strength [2]. The variation which produced optimum result would mix with the foaming agent as the material for reducing the weight of the specimen. After that, the test of compressive strength, water absorption, and tensile strength on the installment of batako walls were done. The data analyzed by using SNI 02-0349-1989[3] reference about concrete brick for wall installment. The variation of 20% of glass powder passing sieve no. 200 gave optimum result. A specimen of the variation on glass powder of 20% which passed sieve no. 200 and the foaming agent was higher than the compressive strength of the specimen which used glass powder substitution of 0% of passing sieve no. 200 and foaming agent. The compressive strength of batako walls which used the batako construction with glass powder substitution of 20% of passing sieve no. 200 and the foaming agent was also higher than the compressive strength of the assaying object which used glass powder substitution of 0% of passing sieve no. 200 and foaming agent.

Numerical modelling of powder caking at REV scale by using DEM

NASA Astrophysics Data System (ADS)

Guessasma, Mohamed; Silva Tavares, Homayra; Afrassiabian, Zahra; Saleh, Khashayar

2017-06-01

This work deals with numerical simulation of powder caking process caused by capillary condensation phenomenon. Caking consists in unwanted agglomeration of powder particles. This process is often irreversible and not easy to predict. To reproduce mechanism involved by caking phenomenon we have used the Discrete Elements Method (DEM). In the present work, we mainly focus on the role of capillary condensation and subsequent liquid bridge formation within a granular medium exposed to fluctuations of ambient relative humidity. Such bridges cause an attractive force between particles, leading to the formation of a cake with intrinsic physicochemical and mechanical properties. By considering a Representative Elementary Volume (REV), the DEM is then performed by means of a MULTICOR-3D software tacking into account the properties of the cake (degree of saturation) in order to establish relationships between the microscopic parameters and the macroscopic behaviour (tensile strength).

Study of soft magnetic iron cobalt based alloys processed by powder injection molding

NASA Astrophysics Data System (ADS)

Silva, Aline; Lozano, Jaime A.; Machado, Ricardo; Escobar, Jairo A.; Wendhausen, Paulo A. P.

As a near net shape process, powder injection molding (PIM) opens new possibilities to process Fe-Co alloys for magnetic applications. Due to the fact that PIM does not involve plastic deformation of the material during processing, we envisioned the possibility of eliminating vanadium (V), which is generally added to Fe-Co alloys to improve the ductility in order to enable its further shaping by conventional processes such as forging and cold rolling. In our investigation we have found out two main futures related to the elimination of V, which lead to a cost-benefit gain in manufacturing small magnetic components where high-saturation induction is needed at low frequencies. Firstly, the elimination of V enables the achievement of much better magnetic properties when alloys are processed by PIM. Secondly, a lower sintering temperature can be used when the alloy is processed starting with elemental Fe and Co powders without the addition of V.

The influence of sintering temperature on microstructure and mechanical properties of Ni-Al intermetallics fabricated by SPS

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

Thömmes, A., E-mail: thoemmes.alexander@gmail.com; Shevtsova, L. I., E-mail: edeliya2010@mail.ru; Laptev, I. S., E-mail: ilya-laptev-nstu@mail.ru

2015-10-27

In the present study PN85Yu15 was used as elemental powder to produce a sintered compound with Ni3Al as main phase. The Spark Plasma Sintering (SPS) technique is used to compact the powders. The powder was sintered in a temperature range between 1000°C and 1150°C to observe the influence of the sintering temperature on the microstructure and the mechanical properties. The microstructure was observed with optical microscope (OM), the phase composition was characterized by X-ray diffraction (XRD) technique. Density and microhardness were observed and compared the values with the results of other researchers. The compressive-, density- and microhardness tests show asmore » clear result that with increasing the sintering temperature nearly all properties become better and also the microstructure studies show that porous places become less.« less

Cleaner Production of Ti Powder by a Two-Stage Aluminothermic Reduction Process

NASA Astrophysics Data System (ADS)

Zhao, Kun; Wang, Yaowu; Feng, Naixiang

2017-10-01

A two-stage aluminothermic reduction process for preparing Ti powder under vacuum conditions using Na2TiF6 was investigated. An Al-Ti master alloy and a clean cryolite were simultaneously obtained as co-products. The first-stage reduction was an exothermic process that occurred at approximately 660°C. The Al and O contents of the Ti powder product were 0.18 wt.% and 0.35 wt.%, respectively, with an average particle size <74 μm. Ti(IV), Ti(III), and metallic Ti were present in the Ti-containing cryolite produced by the first-stage reduction, at a total content of approximately 3.13 wt.%. After second-stage reduction, the Ti elemental contents of the clean cryolite were reduced to 0.002 wt.%. The Al-Ti master alloy obtained by second-stage reduction was composed of Al and TiAl3. The mechanisms involved in these reduction processes were also examined.

Powder metallurgy bearings for advanced rocket engines

NASA Technical Reports Server (NTRS)

Fleck, J. N.; Killman, B. J.; Munson, H.E.

1985-01-01

Traditional ingot metallurgy was pushed to the limit for many demanding applications including antifriction bearings. New systems require corrosion resistance, better fatigue resistance, and higher toughness. With conventional processing, increasing the alloying level to achieve corrosion resistance results in a decrease in other properties such as toughness. Advanced powder metallurgy affords a viable solution to this problem. During powder manufacture, the individual particle solidifies very rapidly; as a consequence, the primary carbides are very small and uniformly distributed. When properly consolidated, this uniform structure is preserved while generating a fully dense product. Element tests including rolling contact fatigue, hot hardness, wear, fracture toughness, and corrosion resistance are underway on eleven candidate P/M bearing alloys and results are compared with those for wrought 440C steel, the current SSME bearing material. Several materials which offer the promise of a significant improvement in performance were identified.

High temperature Ir segregation in Ir-B ceramics: Effect of oxygen presence on stability of IrB 2 and other Ir-B phases

DOE PAGES

Xie, Zhilin; Terracciano, Anthony C.; Cullen, David A.; ...

2015-05-13

The formation of IrB 2, IrB 1.35, IrB 1.1 and IrB monoboride phases in the Ir–B ceramic nanopowder was confirmed during mechanochemical reaction between metallic Ir and elemental B powders. The Ir–B phases were analysed after 90 h of high energy ball milling and after annealing of the powder for 72 h at 1050°C in vacuo. The iridium monoboride (IrB) orthorhombic phase was synthesised experimentally for the first time and identified by powder X-ray diffraction. Additionally, the ReB 2 type IrB 2 hexagonal phase was also produced for the first time and identified by high resolution transmission electron microscope. Irmore » segregation along disordered domains of the boron lattice was found to occur during high temperature annealing. Furthermore, these nanodomains may have useful catalytic properties.« less

Complex doping chemistry owing to Mn incorporation in nanocrystalline anatase TiO2 powders.

PubMed

Guo, Meilan; Gao, Yun; Shao, G

2016-01-28

Mn-doped TiO2 powders with a wide range of nominal doping levels were fabricated using a one-step hydrothermal method followed by 400 °C annealing. Anatase powders with a uniform size distribution below 10 nm were obtained. The maximum solubility of Mn in the TiO2 lattice was around 30%, beyond which the Mn3O4 compound appeared as a secondary phase. The optical absorption edges for Mn-doped anatase TiO2 were red-shifted effectively through increasing Mn content. Alloying chemistry and associated elemental valences were elaborated through combining X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and theoretical simulation in the framework of density functional theory (DFT). The results showed that the Mn species exhibited mixed valence states of 3+ and 4+ in anatase TiO2, with the latter being the key to remarkable photocatalytic performance.

Synthesis of Nano-Crystalline Gamma-TiAl Materials

NASA Technical Reports Server (NTRS)

Hales, Stephen J.; Vasquez, Peter

2003-01-01

One of the principal problems with nano-crystalline materials is producing them in quantities and sizes large enough for valid mechanical property evaluation. The purpose of this study was to explore an innovative method for producing nano-crystalline gamma-TiAl bulk materials using high energy ball milling and brief secondary processes. Nano-crystalline powder feedstock was produced using a Fritsch P4(TM) vario-planetary ball mill recently installed at NASA-LaRC. The high energy ball milling process employed tungsten carbide tooling (vials and balls) and no process control agents to minimize contamination. In a collaborative effort, two approaches were investigated, namely mechanical alloying of elemental powders and attrition milling of pre-alloyed powders. The objective was to subsequently use RF plasma spray deposition and short cycle vacuum hot pressing in order to effect consolidation while retaining nano-crystalline structure in bulk material. Results and discussion of the work performed to date are presented.

Investigations in Producing Porous NiAl by Combustion Synthesis

NASA Astrophysics Data System (ADS)

Zhong, Songming

In recent years, nickel aluminide (NiAl) intermetallic foam, which combines the advantages of nickel-based alloy and metallic foam, has attracted great attention due to its extraordinary properties. In this present work, nickel aluminide (NiAl) foam has been reactively processed from elemental powder (nickel and aluminium) with different types and percentage of volume of a foaming agent (TiH2 or CaCO3), using a combustion synthesis (CS) approach. Most of the previous research has focused on producing close-cell NiAl intermetallic foam; however, this paper presents a new combustion synthesis process to fabricate a hybrid open-cell and close-cell NiAl intermetallic foam. Mixed elemental powder was compacted at moderate pressure generating closed and open porosity with green compact; as a result, part of the liberated gas could escape from the sample, which resulted in producing open-cell pores, in addition, closed cell pores in the product. The effect of foaming agent type and volume percentage on the product is discussed. An increase in volume percentage of TiH2 was found to have beneficial effects on increasing porosity; however, with the increase of volume percentage of CaCO3, there is a big drop in porosity because the low viscosity under high temperature makes more liberated gas escape and pores collapse. According to XRD and EDX analysis, despite the present of multiple phases in samples, NiAl was still the major phase. Hardness measurement shows that high hardness value was obtained at sample of low grain size, hardness value increases with decreasing grain size.

Synthesis and characterization of α-cobalt hydroxide nanobelts

NASA Astrophysics Data System (ADS)

Tian, L.; Zhu, J. L.; Chen, L.; An, B.; Liu, Q. Q.; Huang, K. L.

2011-08-01

α-Cobalt hydroxide was synthesized by a facile hydrothermal process from Co(Ac)2 and NH3·H2O in the presence of 1,3-propanediol. The large-scale-prepared cobalt hydroxide has a uniform nanobelt morphology with a considerably high aspect-ratio more than 20 which may be advantageous for exploration of their physicochemical properties. This synthetic method is convenient, economical, and controllable. The samples were characterized by powder X-ray diffraction, energy dispersive spectrum, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, CHN element analysis, thermogravimetric and differential-thermogravimetric analysis, which revealed the compound is lamellar structural cobalt organic-inorganic hybrid with the chemical formula of Co(OH)1.49(NH3)0.01(CO3 2-)0.22(Ac-)0.07(H2O)0.11 and single-crystalline.

Magneto-structural studies of sol-gel synthesized nanocrystalline manganese substituted nickel ferrites

NASA Astrophysics Data System (ADS)

Pandav, R. S.; Patil, R. P.; Chavan, S. S.; Mulla, I. S.; Hankare, P. P.

2016-11-01

Nanocrystalline NiFe2-xMnxO4 (2≥x≥0) ferrites were prepared by sol-gel method. X-ray diffraction patterns reveal that synthesized compounds are in single phase cubic spinel lattice for all the composition. The surface morphology of all the samples were studied by scanning electron microscopy. The particle size measured from transmission electron microscopy and X-ray diffraction patterns confirms the nanosized dimension of the as-prepared powder. The elemental analysis was carried out by energy dispersive X-ray analysis technique. Magnetic properties such as saturation magnetization, coercivity and remanence are studied as a function of increasing Mn concentration at room temperature. The saturation magnetization shows a decreasing trend with increase in Mn content. The substitution of manganese in the nickel ferrite affects the structural and magnetic properties of cubic spinels.

Synthesis of nanostructured vanadium powder by high-energy ball milling: X-ray diffraction and high-resolution electron microscopy characterization

NASA Astrophysics Data System (ADS)

Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran

2016-10-01

Vanadium metal powders, ball milled with different surfactants viz., stearic acid, KCl and NaCl, have been studied by X-ray diffraction and transmission electron microscopy. The surfactants alter the microstructural and morphological characteristics of the powders. Ball milling with stearic acid results in solid-state amorphization, while powders milled with KCl yield vanadium-tungsten carbide nanocomposite mixtures. NaCl proved to be an excellent surfactant for obtaining nanostructured fusion-grade vanadium powders. In order to understand the reaction mechanism behind any interstitial addition in the ball-milled powders, CHNOS analysis was performed.

Coercivity enhancement of sintered Nd-Fe-B magnets by chemical bath deposition

NASA Astrophysics Data System (ADS)

Zhang, Qiushuang; Guo, Shuai; Yang, Xiao; Zeng, Jiling; Cao, Xuejing; Chen, Renjie; Yan, Aru

2018-05-01

The chemical bath deposition (CBD) method is used to diffuse the heavy rare earth element in order to obtain the high coercivity magnets with low heavy rare earth element. The jet mill powders are soaked in the alcohol suspension of Dy(CH3CHOHCH3)3 (Dy-ipa) so that Nd2Fe14B powder particles are surrounded by Dy-ipa homogeneously. By adding 1.0 wt. % Dy, the coercivity of magnet is increased from 14.47 kOe to 17.55 kOe with slight reduction of remanence after grain boundary diffusion (GBD) in the sintering and annealing processes. The temperature coefficient of coercivity optimizes from -0.629 %/°C to -0.605 %/°C as well as that of remanence improves from -0.108 %/°C to -0.100 %/°C. The CBD method is helpful for thermal stability and alignment either. The relation between the microstructure and the coercivity has been studied systematically.

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

The synthesis of ternary acetylides with tellurium: Li 2 TeC 2 and Na 2 TeC 2

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

Németh, Károly; Unni, Aditya K.; Kalnmals, Christopher

The synthesis of ternary acetylides Li 2TeC 2 and Na 2TeC 2 is presented as the first example of ternary acetylides with metalloid elements instead of transition metals. The synthesis was carried out by the direct reaction of the corresponding bialkali acetylides with tellurium powder in liquid ammonia. Alternatively, the synthesis of Na 2TeC 2 was also carried out by the direct reaction of tellurium powder and two equivalents of NaC 2H in liquid ammonia leading to Na 2TeC 2 and acetylene gas through an equilibrium containing the assumed NaTeC 2H molecules besides the reactants and the products. The resultingmore » disordered crystalline materials were characterized by X-ray diffraction and Raman spectroscopy. Implications of these new syntheses on the synthesis of other ternary acetylides with metalloid elements and transition metals are also discussed.« less

Adsorption of oils, heavy metals and dyes by recovered carbon powder from spent pot liner of aluminum smelter plant.

PubMed

Mazumder, B; Devi, Sasmita Rani

2008-07-01

Aluminum smelter plants employ Hall-Heroult electrolysis cells for electrolysis of molten cryolite to recover aluminum metal by electrolysis. These cells use carbon cathode blocks as a lining material inside. At the end of service life of the cells, pot lines are discarded and new carbon blocks are laid for fresh charging. These used carbon cathode blocks, known as spent pot liners, are heavily infested with toxic elements such as fluoride, cyanide, alkali, etc. Therefore, their disposal in open field poses great environmental risk. A simple process has been developed for decontamination of these spent pot liners and to recover its carbon value. The experiments indicated that this carbon, in the form of fine powder (around 20 micron in size) can absorb toxic elements like heavy metals, dyes, oils, etc. to a great extent and thus can be used for mitigating environmental pollution occuring due to various toxic wastes.

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

Crucial role of molecular planarity on the second order nonlinear optical property of pyridine based chalcone single crystals

NASA Astrophysics Data System (ADS)

Menezes, Anthoni Praveen; Jayarama, A.; Ng, Seik Weng

2015-05-01

An efficient nonlinear optical material 2E-3-(4-bromophenyl)-1-(pyridin-3-yl) prop-2-en-1-one (BPP) was synthesized and single crystals were grown using slow evaporation solution growth technique at room temperature. Grown crystal had prismatic morphology and its structure was confirmed by various spectroscopic studies, elemental analysis, and single crystal X-ray diffraction (XRD) technique. The single crystal XRD of the crystal showed that BPP crystallizes in monoclinic system with noncentrosymmetric space group P21 and the cell parameters are a = 5.6428(7) Å, b = 3.8637(6) Å, c = 26.411(2) Å, β = 97.568(11) deg and v = 575.82(12) Å3. The UV-Visible spectrum reveals that the crystal is optically transparent and has high optical energy band gap of 3.1 eV. The powder second harmonic generation efficiency (SHG) of BPP is 6.8 times that of KDP. From thermal analysis it is found that the crystal melts at 139 °C and decomposes at 264 °C. High optical transparency down to blue region, higher powder SHG efficiency and better thermal stability than that of urea makes this chalcone derivative a promising candidate for SHG applications. Furthermore, effect of molecular planarity on SHG efficiency and role of pyridine ring adjacent to carbonyl group in forming noncentrosymmetric crystal systems of chalcone family is also discussed.

[Studies on the brand traceability of milk powder based on NIR spectroscopy technology].

PubMed

Guan, Xiao; Gu, Fang-Qing; Liu, Jing; Yang, Yong-Jian

2013-10-01

Brand traceability of several different kinds of milk powder was studied by combining near infrared spectroscopy diffuse reflectance mode with soft independent modeling of class analogy (SIMCA) in the present paper. The near infrared spectrum of 138 samples, including 54 Guangming milk powder samples, 43 Netherlands samples, and 33 Nestle samples and 8 Yili samples, were collected. After pretreatment of full spectrum data variables in training set, principal component analysis was performed, and the contribution rate of the cumulative variance of the first three principal components was about 99.07%. Milk powder principal component regression model based on SIMCA was established, and used to classify the milk powder samples in prediction sets. The results showed that the recognition rate of Guangming milk powder, Netherlands milk powder and Nestle milk powder was 78%, 75% and 100%, the rejection rate was 100%, 87%, and 88%, respectively. Therefore, the near infrared spectroscopy combined with SIMCA model can classify milk powder with high accuracy, and is a promising identification method of milk powder variety.

Structural changes during milling of aluminum oxide powders

NASA Technical Reports Server (NTRS)

Ziepler, G.

1984-01-01

The mechanical activation of four fused corundum powders and a calcined Al2O3 powder was studied. The milled powders were characterized by their structural properties, crystallite size, and lattice distortions. Structural changes during milling, detected by X-ray line broadening analysis, gave information about the enhanced activity of the powders caused by the lattice distortions and by the decreasing crystallite size during milling. The structural changes during milling, under the same milling conditions, can be quite different for the same ceramic material, but with different characteristics in the as received state.

A Comparative Biocompatibility Analysis of Ternary Nitinol Alloys

PubMed Central

Haider, Waseem; Munroe, Norman; Pulletikurthi, Chandan; Singh Gill, Puneet K.; Amruthaluri, Sushma

2009-01-01

Nitinol alloys are rapidly being utilized as the material of choice in a variety of applications in the medical industry. It has been used for self-expanding stents, graft support systems, and various other devices for minimally invasive interventional and endoscopic procedures. However, the biocompatibility of this alloy remains a concern to many practitioners in the industry due to nickel sensitivity experienced by many patients. In recent times, several new Nitinol alloys have been introduced with the addition of a ternary element. Nevertheless, there is still a dearth of information concerning the biocompatibility and corrosion resistance of these alloys. This study compared the biocompatibility of two ternary Nitinol alloys prepared by powder metallurgy (PM) and arc melting (AM) and critically assessed the influence of the ternary element. ASTM F 2129-08 cyclic polarization in vitro corrosion tests were conducted to evaluate the corrosion resistance in phosphate buffered saline (PBS). The growth of endothelial cells on NiTi was examined using optical microscopy. PMID:19956791

A Comparative Biocompatibility Analysis of Ternary Nitinol Alloys

NASA Astrophysics Data System (ADS)

Haider, Waseem; Munroe, Norman; Pulletikurthi, Chandan; Gill, Puneet K. Singh; Amruthaluri, Sushma

2009-08-01

Nitinol alloys are rapidly being utilized as the material of choice in a variety of applications in the medical industry. It has been used for self-expanding stents, graft support systems, and various other devices for minimally invasive interventional and endoscopic procedures. However, the biocompatibility of this alloy remains a concern to many practitioners in the industry due to nickel sensitivity experienced by many patients. In recent times, several new Nitinol alloys have been introduced with the addition of a ternary element. Nevertheless, there is still a dearth of information concerning the biocompatibility and corrosion resistance of these alloys. This study compared the biocompatibility of two ternary Nitinol alloys prepared by powder metallurgy (PM) and arc melting (AM) and critically assessed the influence of the ternary element. ASTM F 2129-08 cyclic polarization in vitro corrosion tests were conducted to evaluate the corrosion resistance in phosphate buffered saline (PBS). The growth of endothelial cells on NiTi was examined using optical microscopy.

A Comparative Biocompatibility Analysis of Ternary Nitinol Alloys.

PubMed

Haider, Waseem; Munroe, Norman; Pulletikurthi, Chandan; Singh Gill, Puneet K; Amruthaluri, Sushma

2009-08-01

Nitinol alloys are rapidly being utilized as the material of choice in a variety of applications in the medical industry. It has been used for self-expanding stents, graft support systems, and various other devices for minimally invasive interventional and endoscopic procedures. However, the biocompatibility of this alloy remains a concern to many practitioners in the industry due to nickel sensitivity experienced by many patients. In recent times, several new Nitinol alloys have been introduced with the addition of a ternary element. Nevertheless, there is still a dearth of information concerning the biocompatibility and corrosion resistance of these alloys. This study compared the biocompatibility of two ternary Nitinol alloys prepared by powder metallurgy (PM) and arc melting (AM) and critically assessed the influence of the ternary element. ASTM F 2129-08 cyclic polarization in vitro corrosion tests were conducted to evaluate the corrosion resistance in phosphate buffered saline (PBS). The growth of endothelial cells on NiTi was examined using optical microscopy.

Influence of Cobalt on the Properties of Load-Sensitive Magnesium Alloys

PubMed Central

Klose, Christian; Demminger, Christian; Mroz, Gregor; Reimche, Wilfried; Bach, Friedrich-Wilhelm; Maier, Hans Jürgen; Kerber, Kai

2013-01-01

In this study, magnesium is alloyed with varying amounts of the ferromagnetic alloying element cobalt in order to obtain lightweight load-sensitive materials with sensory properties which allow an online-monitoring of mechanical forces applied to components made from Mg-Co alloys. An optimized casting process with the use of extruded Mg-Co powder rods is utilized which enables the production of magnetic magnesium alloys with a reproducible Co concentration. The efficiency of the casting process is confirmed by SEM analyses. Microstructures and Co-rich precipitations of various Mg-Co alloys are investigated by means of EDS and XRD analyses. The Mg-Co alloys' mechanical strengths are determined by tensile tests. Magnetic properties of the Mg-Co sensor alloys depending on the cobalt content and the acting mechanical load are measured utilizing the harmonic analysis of eddy-current signals. Within the scope of this work, the influence of the element cobalt on magnesium is investigated in detail and an optimal cobalt concentration is defined based on the performed examinations. PMID:23344376

Solvents effect on photoluminescence of nitrogen incorporated graphene oxide using light emitting diode as an excitation source

NASA Astrophysics Data System (ADS)

Kumara, K.; Shetty, T. C. S.; Patil, P. S.; Dharmaprakash, S. M.

2018-05-01

The present study investigates linear and third order nonlinear optical (TNLO) properties of nitrogen incorporated graphene oxide (NGO). A simple pyrolysis method is followed to obtain NGO powder which is soluble in polar aprotic and protic solvents. The normalized emission intensity of NGO for aprotic solvents shows better than polar protic solvents. The surface morphology and element analysis of NGO displayed a leaf like morphology and the elemental compositions of carbon, nitrogen and oxygen in NGO respectively. TNLO property of NGO is investigated by employing z-scan technique in which a continuous wave of wavelength 632.8 nm from He-Ne source was used. This investigation reveals the reverse saturation behaviour and negative nonlinear refractive (NLR) index in NGO. Negative NLR index sign arises mainly from local heating of solvents during continuous interactions of NGO with laser beam. The photoluminescence and TNLO data recorded for NGO revealed its potentiality for bio-sensing, bio-imaging and optoelectronic applications.

SEM-EDX analysis of an unknown "known" white powder found in a shipping container from Peru

NASA Astrophysics Data System (ADS)

Albright, Douglas C.

2009-05-01

In 2008, an unknown white powder was discovered spilled inside of a shipping container of whole kernel corn during an inspection by federal inspectors in the port of Baltimore, Maryland. The container was detained and quarantined while a sample of the powder was collected and sent to a federal laboratory where it was screened using chromatography for the presence of specific poisons and pesticides with negative results. Samples of the corn kernels and the white powder were forwarded to the Food and Drug Administration, Forensic Chemistry Center for further analysis. Stereoscopic Light Microscopy (SLM), Scanning Electron Microscopy/Energy Dispersive X-ray Spectrometry (SEM/EDX), and Polarized Light Microscopy/Infrared Spectroscopy (PLM-IR) were used in the analysis of the kernels and the unknown powder. Based on the unique particle analysis by SLM and SEM as well as the detection of the presence of aluminum and phosphorous by EDX, the unknown was determined to be consistent with reacted aluminum phosphide (AlP). While commonly known in the agricultural industry, aluminum phosphide is relatively unknown in the forensic community. A history of the use and acute toxicity of this compound along with some very unique SEM/EDX analysis characteristics of aluminum phosphide will be discussed.

Effect of boron addition on injection molded 316L stainless steel: mechanical, corrosion properties and in vitro bioactivity.

PubMed

Bayraktaroglu, Esra; Gulsoy, H Ozkan; Gulsoy, Nagihan; Er, Ozay; Kilic, Hasan

2012-01-01

The research was investigated the effect of boron additions on sintering characteristics, mechanical, corrosion properties and biocompatibility of injection molded austenitic grade 316L stainless steel. Addition of boron is promoted to get high density of sintered 316L stainless steels. The amount of boron plays a role in determining the sintered microstructure and all properties. In this study, 316L stainless steel powders have been used with the elemental NiB powders. A feedstock containing 62.5 wt% powders loading was molded at different injection molded temperature. The binders were completely removed from molded components by solvent and thermal debinding at different temperature. The debinded samples were sintered at different temperature for 60 min. Mechanical property, microstructural characterization and electrochemical property of the sintered samples were performed using tensile testing, hardness, optical, scanning electron microscopy and electrochemical corrosion experiments. 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. Results of study showed that sintered 316L and 316L with NiB addition samples exhibited high mechanical and corrosion properties in a physiological environment. Especially, 316L with NiB addition can be used in some bioapplications.

Preliminary Determination of the Temperature Dependence of Siderophile Element Diffusion in Iron Meteorites at 1GPa

NASA Astrophysics Data System (ADS)

Watson, H. C.; Watson, B.

2002-05-01

Preliminary results for diffusion of siderophile elements (Cu, Pd, Re, Os, and Mo) in an iron meteorite analog were obtained at temperatures ranging from 1175° C to 1400° C and 1GPa from diffusion couple experiments in a piston-cylinder apparatus. Alloys were prepared by synthesizing mixtures of pure metal powders. The alloys were made from a 90 wt% Fe and 10 wt% Ni base mixture, and approximately 1wt% of the various siderophile elements was added (individually) to the same base mixture to make the doped alloys. The powders were packed in pre-drilled holes ( ~1 mm diameter by 8 mm deep) in MgO cylinders, and run in a piston cylinder apparatus at 1400° C and 1GPa for 48 hours. The resulting homogeneous alloys were then sectioned into wafers approximately 1mm thick, and the faces were polished to prepare for the diffusion experiments. A diffusion couple experiment was conducted by mating a pure alloy wafer and a doped wafer, and placing the couple into an MgO capsule for pressurization and heating in the piston cylinder. The duration of the diffusion experiments ranged from 12 hours to 100 hours. Upon run completion, the diffusion couples were extracted, sectioned lengthwise, and polished for analysis. Diffusion profiles were measured using standard electron microprobe techniques. Preliminary Arrhenius relations have been found as follows: DMo=2.12E-1+/-0.20 m2/s exp(390.86+/-40.46 kJ/mol/RT) DCu=1.37E-3+/-1.25E-3 m2/s exp(315.24+/-31.64 kJ/mol/RT) DPd=2.40E-5+/-2.40E-5 m2/s exp(269.64+/-87.49 kJ/mol/RT) Diffusion coefficients have also been found for Re and Os at 1325° C. They are: DRe=7.89E-15+/-6.70 m2/s and DOs=9.69E-15+/-8.24 m2/s

The first 3-D LaIII-SrII heterometallic complex: Synthesis, structure and luminescent properties

NASA Astrophysics Data System (ADS)

Hong, Zhiwei; Ran, Jingwen; Li, Tao; Chen, Yanmei

2016-10-01

The first 3-D LaIII-SrII heterometallic complex, namely [La2Sr(pda)4(H2O)4]n·6nH2O (1, H2pda = pyridine-2,6-dicarboxylic acid), has been successfully synthesized under solvothermal conditions. Single crystal X-ray diffraction analysis reveals that complex 1 features a 3-D porous framework and displays a new topology. The crystal structure can be simplified to a 4,6-connected 3-D network with Schläfli symbol of {34·42·88·9}2{34·42}. The crystals also have been characterized by X-ray powder diffraction, elemental analysis, thermal analysis, and IR spectroscopy. The infrared spectral analysis indicates that complex 1 is a carboxylate coordinated compound, several water molecules exist in the compound. The thermal study shows that there are ten water molecules in the crystal structure. The luminescent property has also been investigated. It shows a blue-purple fluorescence emission.

Trace metal assay of U(3)O(8) powder by electrothermal AAS.

PubMed

Page, A G; Godbole, S V; Kulkarni, M J; Porwal, N K; Shelar, S S; Joshi, B D

1983-10-01

Methods have been developed for the direct determination of Ag, Ca, K., Li, Mg, Na, Pb, Sn and Zn in U(3)O(8) powder samples by electrothermal AAS. Nanogram and lower amounts of these elements have been determined with a relative standard deviation of 6-16% in mg amounts of sample (either alone or mixed with an equal weight of graphite). The results for NBL reference samples were in reasonable agreement with the certified values. X-Ray diffraction studies on the residues left from the graphite mixtures after the atomization cycle, confirmed the formation of uranium carbide (UC(2)).

Amino Acids Aided Sintering for the Formation of Highly Porous FeAl Intermetallic Alloys

PubMed Central

Karczewski, Krzysztof; Stepniowski, Wojciech J.

2017-01-01

Fabrication of metallic foams by sintering metal powders mixed with thermally degradable compounds is of interest for numerous applications. Compounds releasing gaseous nitrogen, minimizing interactions between the formed gases and metallic foam by diluting other combustion products, were applied. Cysteine and phenylalanine, were used as gas releasing agents during the sintering of elemental Fe and Al powders in order to obtain metallic foams. Characterization was carried out by optical microscopy with image analysis, scanning electron microscopy with energy dispersive spectroscopy, and gas permeability tests. Porosity of the foams was up to 42 ± 3% and 46 ± 2% for sintering conducted with 5 wt % cysteine and phenylalanine, respectively. Chemical analyses of the formed foams revealed that the oxygen content was below 0.14 wt % and the carbon content was below 0.3 wt %. Therefore, no brittle phases could be formed that would spoil the mechanical stability of the FeAl intermetallic foams. The gas permeability tests revealed that only the foams formed in the presence of cysteine have enough interconnections between the pores, thanks to the improved air flow through the porous materials. The foams formed with cysteine can be applied as filters and industrial catalysts. PMID:28773106

Postsynthetic Functionalization of Mg-MOF-74 with Tetraethylenepentamine: Structural Characterization and Enhanced CO2 Adsorption.

PubMed

Su, Xiao; Bromberg, Lev; Martis, Vladimir; Simeon, Fritz; Huq, Ashfia; Hatton, T Alan

2017-03-29

Postsynthetic functionalization of magnesium 2,5-dihydroxyterephthalate (Mg-MOF-74) with tetraethylenepentamine (TEPA) resulted in improved CO 2 adsorption performance under dry and humid conditions. XPS, elemental analysis, and neutron powder diffraction studies indicated that TEPA was incorporated throughout the MOF particle, although it coordinated preferentially with the unsaturated metal sites located in the immediate proximity to the surface. Neutron and X-ray powder diffraction analyses showed that the MOF structure was preserved after amine incorporation, with slight changes in the lattice parameters. The adsorption capacity of the functionalized amino-Mg-MOF-74 (TEPA-MOF) for CO 2 was as high as 26.9 wt % versus 23.4 wt % for the original MOF due to the extra binding sites provided by the multiunit amines. The degree of functionalization with the amines was found to be important in enhancing CO 2 adsorption, as the optimal surface coverage improved performance and stability under both pure CO 2 and CO 2 /H 2 O coadsorption, and with partially saturated surface coverage, optimal CO 2 capacity could be achieved under both wet and dry conditions by a synergistic binding of CO 2 to the amines as well as metal centers.

Develop Techniques for Ion Implantation of PLZT for Adaptive Optics

DTIC Science & Technology

1989-11-01

WL-TR-89-26 FIGURES (Continued) Fizure Page 20 EDX elemental spectrum from perovskite region of the sample shown in Fig. 15. 65 21 EDX elemental...pyroelectric response. 126 84 Result of doping PZT with La and Mn (Ref. 7). 127 85 APW results along the lin for several perovskite - type compounds and ReO 2...structure of the calcined powder was analyzed and shown to be mainly the hexagonal/rhombohedral phase within 17 WL-TR-89-26 the perovskite structure of

X-ray diffraction study of elemental erbium to 70 GPa

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

Pravica, Michael G.; Romano, Edward; Quine, Zachary

2005-12-01

We have investigated phase transitions in elemental erbium in a diamond anvil cell (DAC) up to 70 GPa using angular-dispersive x-ray powder diffraction methods. We present evidence of a series of phase transitions that appear to follow the anticipated hcp{yields}Sm-type{yields}double hcp (dhcp){yields}distorted fcc sequence. In particular, we present evidence for the predicted dhcp{yields}distorted fcc transition above 63 GPa. Equation of state data are also presented up to 70 GPa.

Demonstration of the B4C/NaIO4/PTFE Delay in the U.S. Army Hand-Held Signal

DTIC Science & Technology

2015-05-20

Figure 1. Partial cross section diagram of a hand-held signal showing the rocket motor , delay element, expelling charge, and pyrotechnic payload as...The black powder-based rocket motor , consisting of propellant pellets (G) encased in a cardboard tube, contains an axial core hole to accommodate the...that ignites the rocket motor . Simultaneously, the delay element is ignited and burns for an interval (preferably 5−6 s) before it ignites the black

Semiconducting icosahedral boron arsenide crystal growth for neutron detection

NASA Astrophysics Data System (ADS)

Whiteley, C. E.; Zhang, Y.; Gong, Y.; Bakalova, S.; Mayo, A.; Edgar, J. H.; Kuball, M.

2011-03-01

Semiconducting icosahedral boron arsenide, B12As2, is an excellent candidate for neutron detectors, thermoelectric converters, and radioisotope batteries, for which high quality single crystals are required. Thus, the present study was undertaken to grow B12As2 crystals by precipitation from metal solutions (nickel) saturated with elemental boron (or B12As2 powder) and arsenic in a sealed quartz ampoule. B12As2 crystals of 10-15 mm were produced when a homogeneous mixture of the three elements was held at 1150 °C for 48-72 h and slowly cooled (3.5 °C/h). The crystals varied in color and transparency from black and opaque to clear and transparent. X-ray topography (XRT), and elemental analysis by energy dispersive X-ray spectroscopy (EDS) confirmed that the crystals had the expected rhombohedral structure and chemical stoichiometry. The concentrations of residual impurities (nickel, carbon, etc.) were low, as measured by Raman spectroscopy and secondary ion mass spectrometry (SIMS). Additionally, low etch-pit densities (4.4×107 cm-2) were observed after etching in molten KOH at 500 °C. Thus, the flux growth method is viable for growing large, high-quality B12As2 crystals.

Spectral analysis of allogeneic hydroxyapatite powders

NASA Astrophysics Data System (ADS)

Timchenko, P. E.; Timchenko, E. V.; Pisareva, E. V.; Vlasov, M. Yu; Red'kin, N. A.; Frolov, O. O.

2017-01-01

In this paper we discuss the application of Raman spectroscopy to the in vitro analysis of the hydroxyapatite powder samples produced from different types of animal bone tissue during demineralization process at various acid concentrations and exposure durations. The derivation of the Raman spectrum of hydroxyapatite is attempted by the analysis of the pure powders of its known constituents. Were experimentally found spectral features of hydroxyapatite, based on analysis of the line amplitude at wave numbers 950-965 cm-1 ((PO4)3- (ν1) vibration) and 1065-1075 cm-1 ((CO3)2-(ν1) B-type replacement). Control of physicochemical properties of hydroxyapatite was carried out by Raman spectroscopy. Research results are compared with an infrared Fourier spectroscopy.

Effects of milling media on the fabrication of melt-derived bioactive glass powder for biomaterial application

NASA Astrophysics Data System (ADS)

Ibrahim, Nurul Farhana; Mohamad, Hasmaliza; Noor, Siti Noor Fazliah Mohd

2016-12-01

The present work aims to study the effects of using different milling media on bioactive glass produced through melt-derived method for biomaterial application. The bioactive glass powder based on SiO2-CaO-Na2O-P2O5 system was fabricated using two different types of milling media which are tungsten carbide (WC) and zirconia (ZrO2) balls. However, in this work, no P2O5 was added in the new composition. XRF analysis indicated that tungsten trioxide (WO3) was observed in glass powder milled using WC balls whereas ZrO2 was observed in glass powder milled using ZrO2 balls. Amorphous structure was detected with no crystalline peak observed through XRD analysis for both glass powders. FTIR analysis confirmed the formation of silica network with the existence of functional groups Si-O-Si (bend), Si-O-Si (tetrahedral) and Si-O-Si (stretch) for both glass powders. The results revealed that there was no significant effect of milling media on amorphous silica network glass structure which shows that WC and zirconia can be used as milling media for bioactive glass fabrication without any contamination. Therefore, the fabricated BG can be tested safely for bioactivity assessment in biological fluids environment.

Characterization of powdered fish heads for bone graft biomaterial applications.

PubMed

Oteyaka, Mustafa Ozgür; Unal, Hasan Hüseyin; Bilici, Namık; Taşçı, Eda

2013-01-01

The aim of this study was to define the chemical composition, morphology and crystallography of powdered fish heads of the species Argyrosomus regius for bone graft biomaterial applications. Two sizes of powder were prepared by different grinding methods; Powder A (coarse, d50=68.5 µm) and Powder B (fine, d50=19.1 µm). Samples were analyzed using X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), thermogravimetry (TG), and energy dispersive X-ray spectroscopy (EDS). The powder was mainly composed of aragonite (CaCO3) and calcite (CaCO3). The XRD pattern of Powder A and B matched standard aragonite and calcite patterns. In addition, the calcium oxide (CaO) phase was found after the calcination of Powder A. Thermogravimetry analysis confirmed total mass losses of 43.6% and 47.3% in Powders A and B, respectively. The microstructure of Powder A was mainly composed of different sizes and tubular shape, whereas Powder B showed agglomerated particles. The high quantity of CaO and other oxides resemble the chemical composition of bone. In general, the powder can be considered as bone graft after transformation to hydroxyapatite phase.

Micro structrual characterization and analysis of ball milled silicon carbide

NASA Astrophysics Data System (ADS)

Madhusudan, B. M.; Raju, H. P.; Ghanaraja., S.

2018-04-01

Mechanical alloying has been one of the prominent methods of powder synthesis technique in solid state involving cyclic deformation, cold welding and fracturing of powder particles. Powder particles in this method are subjected to greater mechanical deformation due to the impact of ball-powder-ball and ball-powder-container collisions that occurs during mechanical alloying. Strain hardening and fracture of particles decreases the size of the particles and creates new surfaces. The objective of this Present work is to use ball milling of SiC powder for different duration of 5, 10, 15 and 20 hours by High energy planetary ball milling machine and to evaluate the effect of ball milling on SiC powder. Micro structural Studies using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD) and EDAX has been investigated.

Bimodal metal micro-nanopowders for powder injection molding

NASA Astrophysics Data System (ADS)

Pervikov, Aleksandr; Rodkevich, Nikolay; Glazkova, Elena; Lerner, Marat

2017-12-01

The paper studies a bimodal metal powder composition designed to prepare feedstock for powder injection molding, as well as microstructure and porosity of sintered pats. Two kinds of metal powder compositions are used, in particular, a mixture of micro- and nanopowders and a bimodal powder prepared with dispersion of steel wire. The feedstock is prepared by mixing a bimodal metal powder composition with acetylacetone and paraffin wax. The microstructure of the debound parts is observed by scanning electron microscopy. The sintered parts are characterized by density measurements and metallographic analysis. The technique of the metal powder composition proves to affect the characteristics of sintered parts. Nanoparticles are shown in the interstitial spaces among the microparticles upon mixing micro- and nanopowders, but the regular distribution of nanoparticles on the surface of microparticles is observed in the bimodal powder providing the reduction of the porosity of sintered parts and increasing the density to the proper density of steel.

Identification of goat milk powder by manufacturer using multiple chemical parameters.

PubMed

McLeod, Rebecca J; Prosser, Colin G; Wakefield, Joshua W

2016-02-01

Concentrations of multiple elements and ratios of stable isotopes of carbon and nitrogen were measured and combined to create a chemical fingerprint of production batches of goat whole milk powder (WMP) produced by different manufacturers. Our objectives were to determine whether or not differences exist in the chemical fingerprint among samples of goat WMP produced at different sites, and assess temporal changes in the chemical fingerprint in product manufactured at one site. In total, 58 samples of goat WMP were analyzed by inductively coupled plasma-mass spectrometry as well as isotope ratio mass spectrometry and a suite of 13 elements (Li, Na, Mg, K, Ca, Mn, Cu, Zn, Rb, Sr, Mo, Cs, and Ba), δ(13)C, and δ(15)N selected to create the chemical fingerprint. Differences in the chemical fingerprint of samples between sites and over time were assessed using principal components analysis and canonical analysis of principal coordinates. Differences in the chemical fingerprints of samples between production sites provided a classification success rate (leave-one-out classification) of 98.1%, providing a basis for using the approach to test the authenticity of product manufactured at a site. Within one site, the chemical fingerprint of samples produced at the beginning of the production season differed from those produced in the middle and late season, driven predominantly by lower concentrations of Na, Mg, K, Mn, and Rb, and higher concentrations of Ba and Cu. This observed temporal variability highlights the importance of obtaining samples from throughout the season to ensure a representative chemical fingerprint is obtained for goat WMP from a single manufacturing site. The reconstitution and spray drying of samples from one manufacturer by the other manufacturer enabled the relative influence of the manufacturing process on the chemical fingerprint to be examined. It was found that such reprocessing altered the chemical fingerprint, although the degree of alteration varied among samples and individual elements. The findings of this study support the use of trace elements and stable isotope ratios to test the authenticity of goat WMP, which can likely be applied to other dairy goat products. This approach could be used test to the factory of origin (and potentially batch of origin) of products in the supply chain, thus providing the ability to audit the supply chain and monitor for fraudulent activity. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

The spectroscopic detection of exogenous material in fingerprints after development with powders and recovery with adhesive lifters.

PubMed

West, Matthew J; Went, Michael J

2008-01-15

The application of powders to fingerprints has long been established as an effective and reliable method for developing latent fingerprints. The powders adhere to the ridge pattern of the fingerprint only, thus allowing the image to be visualised. Fingerprints developed in situ at a crime scene routinely undergo lifting with specialist tapes to facilitate subsequent laboratory analysis. As with all recovered evidence these samples would be stored in evidence bags to allow secure transit from the scene to the laboratory and also to preserve the chain of evidence. In this paper, the application of Raman spectroscopy for the analysis of exogenous material in latent fingerprints is reported for contaminated fingerprints that had been treated with powders and also subsequently lifted with adhesive tapes. A selection of over the counter (OTC) analgesics were used as samples for the analysis and contaminated fingerprints were deposited on clean glass slides. The application of aluminium or iron based powders to contaminated fingerprints did not interfere with the Raman spectra obtained for the contaminants. In most cases background fluorescence attributed to the sebaceous content of the latent fingerprint was reduced by the application of the powder thus reducing spectral interference. Contaminated fingerprints developed with powders and then lifted with lifting tapes were also examined. The combination of these two techniques did not interfere with the successful analysis of exogenous contaminants by Raman spectroscopy. The lifting process was repeated using hinge lifters. As the hinge lifters exhibited strong Raman bands the spectroscopic analysis was more complex and an increase in the number of exposures to the detector allowed for improved clarification. Raman spectra of developed and lifted fingerprints recorded through evidence bags were obtained and it was found that the detection process was not compromised in any way. Although the application of powders did not interfere with the detection process the time taken to locate the contaminant was increased due to the physical presence of more material within the fingerprint. The presence of interfering Raman bands from lifting tapes is another potential complication. This, however, could be removed by spectral subtraction or by the choice of lifting tapes that have only weak Raman bands.

Sequential changes of main components in different kinds of milk powders using two-dimensional infrared correlation analysis

NASA Astrophysics Data System (ADS)

Zhou, Qun; Sun, Su-Qin; Yu, Lu; Xu, Chang-Hua; Noda, Isao; Zhang, Xin-Rong

2006-11-01

Infrared (IR) spectroscopy and two-dimensional (2D) correlation IR spectroscopy are shown to offer some information about stability and shelf life of milk powders without separation and extraction of individual components in this paper. Temperature has been chosen as the perturbation to monitor the infrared behavior of various milk powders, namely, whole milk powder (WMP), sweet whole milk powder (Sweet WMP), low-fat milk powder (LFMP), and skim milk powder (SMP). The sequential order of changes in protein, fat and carbohydrates (mainly lactose) in milk powders is studied for the first time. The protein changes before the sucrose in WMP, whereas the sucrose changes before the protein in Sweet WMP under temperature perturbation. It is also found that in SMP, carbohydrate changes prior to protein whereas in LFMP and WMP protein changes first as the temperature is increased. The conclusion can provide some useful reference to understand the thermal stability of milk powders.

Effects of packaging materials on the aroma stability of Thai 'tom yam' seasoning powder as determined by descriptive sensory analysis and gas chromatography-mass spectrometry.

PubMed

Leelaphiwat, Pattarin; Harte, Janice B; Auras, Rafael A; Ong, Peter Kc; Chonhenchob, Vanee

2017-04-01

Changes in the aroma characteristics of Thai 'tom yam' seasoning powder, containing lemongrass, galangal and kaffir lime leaf, as affected by different packaging materials were assessed using quantitative descriptive analysis (QDA) and gas chromatography-mass spectrometry (GC-MS). The descriptive aroma attributes for lemongrass, galangal and kaffir lime leaf powders were developed by the QDA panel. The mixed herb and spice seasoning powder was kept in glass jars closed with different packaging materials (Nylon 6, polyethylene terephthalate (PET) and polylactic acid (PLA)) stored at 38 °C (accelerated storage condition), and evaluated by the trained QDA panel during storage for 49 days. The descriptive words for Thai 'tom yam' seasoning powder developed by the trained panelists were lemongrass, vinegary and leafy for lemongrass, galangal and kaffir lime leaf dried powder, respectively. The aroma intensities significantly (P ≤ 0.05) decreased with increased storage time. However, the intensity scores for aroma attributes were not significantly (P > 0.05) different among the packaging materials studied. The major components in Thai 'tom yam' seasoning powder, quantified by GC-MS, were estragole, bicyclo[3.1.1]heptane, β-bisabolene, benzoic acid and 2-ethylhexyl salicylate. The concentrations of major aroma compounds significantly (P ≤ 0.05) decreased with storage time. Aroma stability of Thai 'tom yam' powder can be determined by descriptive sensory evaluation and GC-MS analysis. Nylon, PET and PLA exhibited similar aroma barrier properties against key aroma compounds in Thai 'tom yam'. This information can be used for prediction of aroma loss through packaging materials during storage of Thai 'tom yam'. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Coal Quality and Major, Minor, and Trace Elements in the Powder River, Green River, and Williston Basins, Wyoming and North Dakota

USGS Publications Warehouse

Stricker, Gary D.; Flores, Romeo M.; Trippi, Michael H.; Ellis, Margaret S.; Olson, Carol M.; Sullivan, Jonah E.; Takahashi, Kenneth I.

2007-01-01

The U.S. Geological Survey (USGS), in cooperation with the Wyoming Reservoir Management Group (RMG) of the Bureau of Land Management (BLM) and nineteen independent coalbed methane (CBM) gas operators in the Powder River and Green River Basins in Wyoming and the Williston Basin in North Dakota, collected 963 coal samples from 37 core holes (fig. 1; table 1) between 1999 and 2005. The drilling and coring program was in response to the rapid development of CBM, particularly in the Powder River Basin (PRB), and the needs of the RMG BLM for new and more reliable data for CBM resource estimates and reservoir characterization. The USGS and BLM entered into agreements with the gas operators to drill and core Fort Union coal beds, thus supplying core samples for the USGS to analyze and provide the RMG with rapid, real-time results of total gas desorbed, coal quality, and high pressure methane adsorption isotherm data (Stricker and others, 2006). The USGS determined the ultimate composition of all coal core samples; for selected samples analyses also included proximate analysis, calorific value, equilibrium moisture, apparent specific gravity, and forms of sulfur. Analytical procedures followed those of the American Society of Testing Materials (ASTM; 1998). In addition, samples from three wells (129 samples) were analyzed for major, minor, and trace element contents. Ultimate and proximate compositions, calorific value, and forms of sulfur are fundamental parameters in evaluating the economic value of a coal. Determining trace element concentrations, along with total sulfur and ash yield, is also essential to assess the environmental effects of coal use, as is the suitability of the coal for cleaning, gasification, liquefaction, and other treatments. Determination of coal quality in the deeper part (depths greater than 1,000 to 1,200 ft) of the PRB (Rohrbacher and others, 2006; Luppens and others, 2006) is especially important, because these coals are targeted for future mining and development. This report contains summary tables, histograms, and isopleth maps of coal analyses. Details of the compositional internal variability of the coal beds are based on the continuous vertical sampling of coal sequences, including beds in the deeper part of the PRB. Such sampling allows for close comparisons of the compositions of different parts of coal beds as well as within the same coal beds at different core hole locations within short distances of each other.

Assessment of Alternative [U] and [Th] Zircon Standards for SIMS

NASA Astrophysics Data System (ADS)

Monteleone, B. D.; van Soest, M. C.; Hodges, K.; Moore, G. M.; Boyce, J. W.; Hervig, R. L.

2009-12-01

The quality of in situ (U-Th)/He zircon dates is dependent upon the accuracy and precision of spatially distributed [U] and [Th] measurements on often complexly zoned zircon crystals. Natural zircon standards for SIMS traditionally have been used to obtain precise U-Pb ages rather than precise U and Th concentration. [U] and [Th] distributions within even the most homogeneous U-Pb age standards are not sufficient to make good microbeam standards (i.e., yield good precision: 2σ < 5%) for (U-Th)/He dates. In the absence of sufficiently homogeneous natural zircon crystals, we evaluate the use of the NIST 610 glass standard and a synthetic polycrystalline solid “zircon synrock” made by powdering and pressing natural zircon crystals at 2 GPa and 1100°C within a 13 mm piston cylinder for 24 hours. SIMS energy spectra and multiple spot analyses help assess the matrix-dependence of secondary ion emission and [U] and [Th] homogeneity of these materials. Although spot analyses on NIST 610 glass yielded spatially consistent ratios of 238U/30Si and 232Th/30Si (2σ = 2%, n = 14), comparison of energy spectra collected on glass and zircon reveal significant differences in U, UO, Th, and ThO ion intensities over the range of initial kinetic energies commonly used for trace element analyses. Computing [U] and [Th] in zircon using NIST glass yields concentrations that vary by more than 10% for [U] and [Th], depending on the initial kinetic energy and ion mass (elemental, oxide, or sum of elemental and oxide) used for the analysis. The observed effect of chemistry on secondary ion energy spectra suggests that NIST glass cannot be used as a standard for trace [U] and [Th] in zircon without a correction factor (presently unknown). Energy spectra of the zircon synrock are similar to those of natural zircon, suggesting matrix compatibility and therefore potential for accurate standardization. Spot analyses on the zircon powder pellets, however, show that adequate homogeneity of [U] and [Th] (2σ = 37% and 33% for 238U/30Si and 232Th/30Si, respectively, n = 8) has yet to be achieved. Modeling shows that homogenization of [U] and [Th] within these pellets requires preparation of powders with <2 micron sized particles, which has yet to be achieved in sample preparation. Thus, the zircon synrock pellet remains a viable potential [U], [Th] standard, although the preparation of a sufficiently fine grained, homogeneous pellet is a work in progress.

The suitability of common compressibility equations for characterizing plasticity of diverse powders.

PubMed

Paul, Shubhajit; Sun, Changquan Calvin

2017-10-30

The analysis of powder compressibility data yields useful information for characterizing compaction behavior and mechanical properties of powders, especially plasticity. Among the many compressibility equations proposed in powder compaction research, the Heckel equation and the Kawakita equation are the most commonly used, despite their known limitations. Systematic evaluation of the performance in analyzing compressibility data suggested the Kuentz-Leuenberger equation is superior to both the Heckel equation and the Kawakita equation for characterizing plasticity of powders exhibiting a wide range of mechanical properties. Copyright © 2017 Elsevier B.V. All rights reserved.

Identification and evaluation of composition in food powder using point-scan Raman spectral imaging

USDA-ARS?s Scientific Manuscript database

This study used Raman spectral imaging coupled with self-modeling mixture analysis (SMA) for identification of three components mixed into a complex food powder mixture. Vanillin, melamine, and sugar were mixed together at 10 different concentration levels (spanning 1% to 10%, w/w) into powdered non...

Effect of powder compaction on radiation-thermal synthesis of lithium-titanium ferrites

NASA Astrophysics Data System (ADS)

Surzhikov, A. P.; Lysenko, E. N.; Vlasov, V. A.; Malyshev, A. V.; Korobeynikov, M. V.; Mikhailenko, M. A.

2017-01-01

Effect of powder compaction on the efficiency of thermal and radiation-thermal synthesis of lithium-substituted ferrites was investigated by X-Ray diffraction and specific magnetization analysis. It was shown that the radiation-thermal heating of compacted powder reagents mixture leads to an increase in efficiency of lithium-titanium ferrites synthesis.

Direct analysis of herbal powders by pipette-tip electrospray ionization mass spectrometry.

PubMed

Wang, Haixing; So, Pui-Kin; Yao, Zhong-Ping

2014-01-27

Conventional electrospray ionization mass spectrometry (ESI-MS) is widely used for analysis of solution samples. The development of solid-substrate ESI-MS allows direct ionization analysis of bulky solid samples. In this study, we developed pipette-tip ESI-MS, a technique that combines pipette tips with syringe and syringe pump, for direct analysis of herbal powders, another common form of samples. We demonstrated that various herbal powder samples, including herbal medicines and food samples, could be readily online extracted and analyzed using this technique. Various powder samples, such as Rhizoma coptidis, lotus plumule, great burdock achene, black pepper, Panax ginseng, roasted coffee beans, Fructus Schisandrae Chinensis and Fructus Schisandrae Sphenantherae, were analyzed using pipette-tip ESI-MS and quality mass spectra with stable and durable signals could be obtained. Both positive and negative ion modes were attempted and various compounds including amino acids, oligosaccharides, glycosides, alkaloids, organic acids, ginosensides, flavonoids and lignans could be detected. Principal component analysis (PCA) based on the acquired mass spectra allowed rapid differentiation of closely related herbal species. Copyright © 2013 Elsevier B.V. All rights reserved.

MERCURY OXIDATION PROMOTED BY A SELECTIVE CATALYTIC REDUCTION CATALYST UNDER SIMULATED POWDER RIVER BASIN COAL COMBUSTION CONDITIONS

EPA Science Inventory

A bench-scale reactor consisting of a natural gas burner and an electrically heated reactor housing a selective catalytic reduction (SCR) catalyst was constructed for studying elemental mercury oxidation under SCR conditions. A low sulfur Power River Basin (PRB) coal combustion ...

STUDY OF MERCURY OXIDATION BY SCR CATALYST IN AN ENTRAINED-FLOW REACTOR UNDER SIMULATED PRB CONDITIONS

EPA Science Inventory

A bench-scale entrained-flow reactor system was constructed for studying elemental mercury oxidation under selective catalytic reduction (SCR) reaction conditions. Simulated flue gas was doped with fly ash collected from a subbituminous Powder River Basin (PRB) coal-fired boiler ...

A novel structure of gel grown strontium cyanurate crystal and its structural, optical, electrical characterization

NASA Astrophysics Data System (ADS)

Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Gopakumar, N.; Babu, K. Rajendra

2017-12-01

Strontium cyanurate crystals with novel structure and unique optical property like mechanoluminescence have been grown by conventional gel method. Transparent crystals were obtained. The single crystal X-ray diffraction analysis reveals the exquisite structure of the grown crystal. The crystal is centrosymmetric and has a three dimensional polymeric structure. The powder X ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal were identified by Fourier transform infrared spectroscopy. Elemental analysis confirmed the composition of the complex. A study of thermal properties was done by thermo gravimetric analysis and differential thermal analysis. The optical properties like band gap, refractive index and extinction coefficient were evaluated from the UV visible spectral analysis. The etching study was done to reveal the dislocations in the crystal which in turn explains mechanoluminescence emission. The mechanoluminescence property exhibited by the crystal makes it suitable for stress sensing applications. Besides being a centrosymmetric crystal, it also exhibits NLO behavior. Dielectric properties were studied and theoretical calculations of Fermi energy, valence electron plasma energy, penn gap and polarisability have been done.

Microstructural Evolution of AlCoCrFeNiSi High-Entropy Alloy Powder during Mechanical Alloying and Its Coating Performance

PubMed Central

Fu, Ming; Xiong, Wei

2018-01-01

High-entropy alloys (HEAs) are promising structural materials due to their excellent comprehensive performances. The use of mechanically alloyed powders to deposit HEA coatings through atmospheric plasma spraying (APS) is an effective approach that can broaden the application areas of the HEAs. In this paper, a ductility–brittleness AlCoCrFeNiSi system was chosen as an object of study, and the detailed evolution of the surface morphology, particle size distribution, and microstructure of the powder during mechanical alloying was investigated. An AlCoCrFeNiSi HEA coating was deposited using powder milled for 10 h, which can be used as an ideal feedstock for APS. The surface morphology, microstructure, microhardness, and wear behavior of the coating at room temperature were investigated. The results showed that as the milling time increased, the particle size first increased, and then decreased. At the milling time of 10 h, simple body-centered cubic (BCC) and face-centered cubic (FCC) solid solution phases were formed. After spraying, the lamellar structure inside a single particle disappeared. An ordered BCC phase was detected, and the diffraction peaks of the Si element also disappeared, which indicates that phase transformation occurred during plasma spraying. A transmission electron microscopy analysis showed that nanometer crystalline grains with a grain size of about 30 nm existed in the APS coating. For the coating, an average microhardness of 612 ± 41 HV was obtained. Adhesive wear, tribo-oxidation wear, and slight abrasion wear took place during the wear test. The coating showed good wear resistance, with a volume wear rate of 0.38 ± 0.08 × 10−4 mm3·N−1·m−1, which makes it a promising coating for use in abrasive environments. PMID:29473872

Effects of forming temperature and sintering rate to the final properties of FeCuAl powder compacts formed through uniaxial die compaction process

NASA Astrophysics Data System (ADS)

Rahman, M. M.; Ismail, M. A.; Sopyan, I.; Rahman, H. Y.

2018-01-01

This paper presents the outcomes of an experimental investigation on the effects of forming temperature and sintering schedule to the final characteristics of FeCuAl powder mass formed at different temperature and sintered at different schedule. A lab-scale uni-axial die compaction rig was designed and fabricated which enabled the compaction of powder mass at room temperature as well as elevated temperature. Iron (Fe) powder ASC 100.29 was mechanically mixed with other elemental powders, namely copper (Cu), and aluminum (Al) for 60 minutes and compacted at three different temperature, i.e., 30°C, 150°C, and 200°C by applying 425 MPa of simultaneous downward and upward axial loading to generate green compacts. The as-pressed samples were inspected visually and the defect-free green compacts were subsequently sintered in an argon gas fired furnace at 800°C for 60 min at three different heating/cooling rates, i.e., 5, 10, and 15°C/min, respectively. The sintered samples were then characterised for their physical, electrical, and mechanical properties. The microstructures of the sintered samples were also analysed. The results revealed that a forming temperature of 150°C and a sintering rate of 10°C/min could produce a product with better characteristics.

Consolidation processing parameters and alternative processing methods for powder metallurgy Al-Cu-Mg-X-X alloys

NASA Technical Reports Server (NTRS)

Sankaran, K. K.

1987-01-01

The effects of varying the vacuum degassing parameters on the microstructure and properties of Al-4Cu-1Mg-X-X (X-X = 1.5Li-0.2Zr or 1.5Fe-0.75Ce) alloys processed from either prealloyed (PA) or mechanically alloyed (M) powder, and consolidated by either using sealed aluminum containers or containerless vacuum hot pressing were studied. The consolidated billets were hot extruded to evaluate microstructure and properties. The MA Li-containing alloy did not include Zr, and the MA Fe- and Ce-containing alloy was made from both elemental and partially prealloyed powder. The alloys were vacuum degassed both above and below the solution heat treatment temperature. While vacuum degassing lowered the hydrogen content of these alloys, the range over which the vacuum degassing parameters were varied was not large enough to cause significant changes in degassing efficiency, and the observed variations in the mechanical properties of the heat treated alloys were attributed to varying contributions to strengthening by the sub-structure and the dispersoids. Mechanical alloying increased the strength over that of alloys of similar composition made from PA powder. The inferior properties in the transverse orientation, especially in the Li-containing alloys, suggested deficiencies in degassing. Among all of the alloys processed for this study, the Fe- and Ce-containing alloys made from MA powder possessed better combinations of strength and toughness.

Quantification of Tribocharging of Pharmaceutical Powders in V-Blenders: Experiments, Multiscale Modeling, and Simulations.

PubMed

Naik, Shivangi; Hancock, Bruno; Abramov, Yuriy; Yu, Weili; Rowland, Martin; Huang, Zhonghui; Chaudhuri, Bodhisattwa

2016-04-01

Pharmaceutical powders are very prone to electrostatic charging by colliding and sliding contacts. In pharmaceutical formulation processes, particle charging is often a nuisance and can cause problems in the manufacture of products, such as affecting powder flow, fill, and dose uniformity. For a fundamental understanding of the powder triboelectrification, it is essential to study charge transfer under well-defined conditions. Hence, all experiments in the present study were conducted in a V-blender located inside a glove box with a controlled humidity of 20%. To understand tribocharging, different contact surfaces, namely aluminum, Teflon, poly methyl methacrylate, and nylon were used along with 2 pharmaceutical excipients and 2 drug substances. For the pharmaceutical materials, the work function values were estimated using MOPAC, a semiempirical molecular orbital package which has been previously used for the solid-state studies and molecular structure predictions. For a mechanistic understanding of tribocharging, a discrete element model incorporating charge transfer and electrostatic forces was developed. An effort was made to correlate tribocharging of pharmaceutical powders to properties such as cohesive energy density and surface energy. The multiscale model used is restricted as it considers only spherical particles with smooth surfaces. It should be used judiciously for other experimental assemblies because it does not represent a full validation of a tightly integrated model. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Bulk Al-Al3Zr composite prepared by mechanical alloying and hot extrusion for high-temperature applications

NASA Astrophysics Data System (ADS)

Pourkhorshid, E.; Enayati, M. H.; Sabooni, S.; Karimzadeh, F.; Paydar, M. H.

2017-08-01

Bulk Al/Al3Zr composite was prepared by a combination of mechanical alloying (MA) and hot extrusion processes. Elemental Al and Zr powders were milled for up to 10 h and heat treated at 600°C for 1 h to form stable Al3Zr. The prepared Al3Zr powder was then mixed with the pure Al powder to produce an Al-Al3Zr composite. The composite powder was finally consolidated by hot extrusion at 550°C. The mechanical properties of consolidated samples were evaluated by hardness and tension tests at room and elevated temperatures. The results show that annealing of the 10-h-milled powder at 600°C for 1 h led to the formation of a stable Al3Zr phase. Differential scanning calorimetry (DSC) results confirmed that the formation of Al3Zr began with the nucleation of a metastable phase, which subsequently transformed to the stable tetragonal Al3Zr structure. The tension yield strength of the Al-10wt%Al3Zr composite was determined to be 103 MPa, which is approximately twice that for pure Al (53 MPa). The yield stress of the Al/Al3Zr composite at 300°C is just 10% lower than that at room temperature, which demonstrates the strong potential for the prepared composite to be used in high-temperature structural applications.

Development of Nanomaterials for Nuclear Energetics

NASA Astrophysics Data System (ADS)

Petrunin, V. F.

Structure and properties peculiarities of the nanocrystalline powders give the opportunity to design new and to develop a modernization of nuclear energy industry materials. It was shown experimentally, that addition of 5-10% uranium dioxide nanocrystalline powder to traditional coarse powder allows to decrease the sintering temperature or to increase the fuel tablets size of grain. Similar perspectives for the technology of neutron absorbing tablets of control-rod modernization are shown by nanopowder of dysprosium hafnate changing instead now using boron carbide. It is powders in nanocrystalline state get an opportunity to sinter them and to receive compact tablet with 8,2-8,4 g/cm2 density for automatic defence system of nuclear reactor. Resource of dysprosium hafnate ceramics can be 18-20 years instead 4-5 years for boron carbide. To step up the radiation-damage stability of fuel element jacket material was suggested to strengthen a heat-resistant ferrite-martensite steel by Y2O3 nanocrystalline powder addition. Nanopowder with size of particles 560 nm and crystallite size 9 nm was prepeared by chemical coprecipitation method. To make lighter the container for transport and provisional disposal of exposed fuel from nuclear reactor a new boron-aluminium alloy called as boral was developed. This composite armed with nanopowders of boron-containing materials and heavy metals oxides can replace succesburnt-up corrosion-resistant steels.

Gas-to-particle conversion in the particle precipitation-aided chemical vapor deposition process II. Synthesis of the perovskite oxide yttrium chromite

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

Dieten, V.E.J. van; Dekker, J.P.; Hurkmans, E.J.

1993-11-01

In the particle precipitation-aided chemical vapor deposition process, an aerosol is formed in the gas phase at elevated temperatures. The particles are deposited on a cooled substrate. Coherent layers with a controlled porosity can be obtained by a simultaneous heterogeneous reaction, which interconnects the deposited particles. The synthesis of submicrometer powder of the perovskite oxide yttrium chromite (YCrO[sub 3]) by gas to particle conversion, which is the first step of the PP-CVD process, has been investigated, and preliminary results are shown. The powders have been synthesized using yttrium trichloride vapor (YCl[sub 3]), chromium trichloride vapor (CrCl[sub 3]), and steam andmore » oxygen as reactants. The influence of the input molar ratio of the elements on the composition and characteristics of the powders has been investigated. Phase composition has been determined by X-ray diffraction (XRD). The powders have been characterized by transmission electron microscopy (TEM) and sedimentation field flow fractionation (SF[sup 3]). At a reaction temperature of 1283 K the powders consist of the chromium sesquioxide (Cr[sub 2]O[sub 3]), or a mixture of Cr[sub 2]O[sub 3] and YCrO[sub 3]. At stoichiometeric input amounts of metal chlorides and steam the formation of YCrO[sub 3] seems to be favored. 19 refs., 6 figs., 3 tabs.« less

Characterization of derived natural hydroxyapatite (HAp) obtained from different types of tilapia fish bones and scales

NASA Astrophysics Data System (ADS)

Fara, A. N. K. A.; Abdullah, H. Z.

2015-07-01

Hydroxyapatite, (HAp), Ca10(PO4)6(OH)2, is recognised as a biomaterial that is widely used for bone implant due to its chemical and structural similarity to the mineral components in human bone and enamel. The elements of HAp are primarily composed of calcium and phosphorus molar ratio of calcium to phosphorous is 1.67 capable to promote bone in-growth into prosthetic implant. Enormous amounts of by-product waste produced from fish factories generated an undesirable environmental impact. Thus, this study was conducted to obtain natural biological HAp from different types of tilapia fish bones and scales from fishery waste. Therefore, fish bones and scales can be as cheap source to produce biological HAp for medical applications. For this purpose, fish bones and scales of tilapia fish were boiled at 100°C to remove adhering meat and other impurities. Later, fish bones and scales were separated into several groups and subjected to different calcination temperatures of 800° C and 900° C for 3h respectively. Afterward, all calcined samples were crushed to form a fine powder. The XRD result revealed the presence of derived Hapfrom the samples powder and were identical with standard Hap. Thermo Gravimetric Analysis was carried out to show the thermal stability of the HAp powder from different types of fish bones and scales. SEM results show porous structure appeared in calcined samples compared to raw samples. The findings are the promising alternative to produce calcium and phosphorus from fishery wastes that beneficial to medical applications.

Simulation of Laser Additive Manufacturing and its Applications

NASA Astrophysics Data System (ADS)

Lee, Yousub

Laser and metal powder based additive manufacturing (AM), a key category of advanced Direct Digital Manufacturing (DDM), produces metallic components directly from a digital representation of the part such as a CAD file. It is well suited for the production of high-value, customizable components with complex geometry and the repair of damaged components. Currently, the main challenges for laser and metal powder based AM include the formation of defects (e.g., porosity), low surface finish quality, and spatially non-uniform properties of material. Such challenges stem largely from the limited knowledge of complex physical processes in AM especially the molten pool physics such as melting, molten metal flow, heat conduction, vaporization of alloying elements, and solidification. Direct experimental measurement of melt pool phenomena is highly difficult since the process is localized (on the order of 0.1 mm to 1 mm melt pool size) and transient (on the order of 1 m/s scanning speed). Furthermore, current optical and infrared cameras are limited to observe the melt pool surface. As a result, fluid flows in the melt pool, melt pool shape and formation of sub-surface defects are difficult to be visualized by experiment. On the other hand, numerical simulation, based on rigorous solution of mass, momentum and energy transport equations, can provide important quantitative knowledge of complex transport phenomena taking place in AM. The overarching goal of this dissertation research is to develop an analytical foundation for fundamental understanding of heat transfer, molten metal flow and free surface evolution. Two key types of laser AM processes are studied: a) powder injection, commonly used for repairing of turbine blades, and b) powder bed, commonly used for manufacturing of new parts with complex geometry. In the powder injection simulation, fluid convection, temperature gradient (G), solidification rate (R) and melt pool shape are calculated using a heat transfer and fluid flow model, which solves the mass, momentum and energy transport equations using the volume of fluid (VOF) method. These results provide quantitative understanding of underlying mechanisms of solidification morphology, solidification scale and deposit side bulging. In particular, it is shown that convective mixing alters solidification conditions (G and R), cooling trend and resultant size of primary dendrite arm spacing. Melt pool convexity in multiple layer LAM is associated not only with the convex shape of prior deposit but also with Marangoni flow. Lastly, it is shown that the lateral width of bulge is possibly controlled by the type of surface tension gradient. It is noted that laser beam spot size in the powder injection AM is about 2 mm and it melts hundreds of powder particles. Hence, the injection of individual particles is approximated by a lumped mass flux into the molten pool. On the other hand, for laser powder bed AM, the laser beam spot size is about 100 microm and thus it only melts a few tens of particles. Therefore, resolution of individual powder particles is essential for the accurate simulation of laser powder bed AM. To obtain the powder packing information in the powder bed, dynamic discrete element simulation (DEM) is used. It considers particle-particle interactions during packing to provide the quantitative structural powder bed properties such as particle arrangement, size and packing density, which is then an inputted as initial geometry for heat transfer and fluid flow simulation. This coupled 3D transient transport model provides a high spatial resolution while requiring less demanding computation. The results show that negatively skewed particle size distribution, faster scanning speed, low power and low packing density worsen the surface finish quality and promote the formation of balling defects. Taken together, both powder injection and powder bed models have resulted in an improved quantitative understanding of heat transfer, molten metal flow and free surface evolution. Furthermore, the analytical foundation that is developed in this dissertation provides the temperature history in AM, a prerequisite for predicting the solid-state phase transformation kinetics, residual stresses and distortion using other models. Moreover, it can be integrated with experimental monitoring and sensing tools to provide the capability of controlling melt pool shape, solidification microstructure, defect formation and surface finish.

Preparation of Mo-Re-C samples containing Mo{sub 7}Re{sub 13}C with the β-Mn-type structure by solid state reaction of planetary-ball-milled powder mixtures of Mo, Re and C, and their crystal structures and superconductivity

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

Oh-ishi, Katsuyoshi, E-mail: oh-ishi@kc.chuo-u.ac.jp; Nagumo, Kenta; Tateishi, Kazuya

Mo-Re-C compounds containing Mo{sub 7}Re{sub 13}C with the β-Mn structure were synthesized with high-melting-temperature metals Mo, Re, and C powders using a conventional solid state method with a planetary ball milling machine instead of the arc melting method. Use of the ball milling machine was necessary to obtain Mo{sub 7}Re{sub 13}C with the β-Mn structure using the solid state method. Almost single-phase Mo{sub 7}Re{sub 13}C with a trace of impurity were obtained using the synthesis method. By XRF and lattice parameter measurements on the samples, Fe element existed in the compound synthesized using the planetary ball milling machine with amore » pot and balls made of steel, though Fe element was not detected in the compound synthesized using a pot and balls made of tungsten carbide. The former compound containg the Fe atom did not show superconductivity but the latter compound without the Fe atom showed superconductivity at 6.1 K. - Graphical abstract: Temperature dependence of the magnetic susceptibility measured under 10 Oe for the superconducting PBM-T samples without Fe element and non-superconducting PBM-S with Fe element. The inset is the enlarged view of the data for the PBM-S sample.« less

Meso-scale investigation of anaerobic chemical reactivity of Ti-Al-B powder mixtures under impact loading

NASA Astrophysics Data System (ADS)

Gonzales, Manny; Gurumurthy, Ashok; Gokhale, Arun; Thadhani, Naresh N.

2011-06-01

Impact-initiated anaerobic chemical reactions in Ti-Al-B reactive powder mixtures under uniaxial stress conditions are investigated using a coupled experimental/computational approach. In particular, we characterize the effects of bulk composition on the threshold impact energy to initiate reaction using rod-on-anvil type tests performed on Ti-Al-B powder compacts. Statistical volume elements (SVEs) of different bulk compositions of the powder mixtures are analyzed using the continuum hydrocode CTH to quantify the effects of strain confinement and load configuration on the overall energy of the structure. These SVEs are also validated using one-point correlation functions to characterize the volume fraction and surface area of the constituents. Based on the deformation profiles from the continuum simulations, we investigate the effect of particle size distribution and clustering of Ti and B on the threshold energy required for observed reactivity. The deformation and threshold kinetic energy of the simulated system is compared with published values of the activation energy for Ti+B reactions and Al combustion in air to assess the extent of their impact-initiated reactivity. Funded by DTRA grant No. HDTRA1-10-1-0038

In vitro bioactivity of a biocomposite fabricated from HA and Ti powders by powder metallurgy method.

PubMed

Ning, C Q; Zhou, Y

2002-07-01

Traditionally, hydroxyapatite was used as a coating material on titanium substrate by various techniques. In the present work, a biocomposite was successfully fabricated from hydroxyapatite and titanium powders by powder metallurgy method. Bioactivity of the composite in a simulated body fluid (SBF) was investigated. Main crystal phases of the as-fabricated composite are found to be Ti2O, CaTiO3, CaO, alpha-Ti and a TiP-like phase. When the composite is immersed in the simulated body fluid for a certain time, a poor-crystallized, calcium-deficient, carbonate-containing apatite film will form on the surface of the composite. The time required to induce apatite nucleation is within 2 h. In addition, the apatite is also incorporated with a little magnesium and chlorine element. It is found that Ti2O has the ability to induce the formation of bone-like apatite in the SBF. And a dissolve of the CaO phase could also provide favorable conditions for the apatite formation, by forming open pores on the surface of the composite and increasing the degree of supersaturation of the SBF with respect to the apatite.

Thermal dynamic behavior during selective laser melting of K418 superalloy: numerical simulation and experimental verification

NASA Astrophysics Data System (ADS)

Chen, Zhen; Xiang, Yu; Wei, Zhengying; Wei, Pei; Lu, Bingheng; Zhang, Lijuan; Du, Jun

2018-04-01

During selective laser melting (SLM) of K418 powder, the influence of the process parameters, such as laser power P and scanning speed v, on the dynamic thermal behavior and morphology of the melted tracks was investigated numerically. A 3D finite difference method was established to predict the dynamic thermal behavior and flow mechanism of K418 powder irradiated by a Gaussian laser beam. A three-dimensional randomly packed powder bed composed of spherical particles was established by discrete element method. The powder particle information including particle size distribution and packing density were taken into account. The volume shrinkage and temperature-dependent thermophysical parameters such as thermal conductivity, specific heat, and other physical properties were also considered. The volume of fluid method was applied to reconstruct the free surface of the molten pool during SLM. The geometrical features, continuity boundaries, and irregularities of the molten pool were proved to be largely determined by the laser energy density. The numerical results are in good agreement with the experiments, which prove to be reasonable and effective. The results provide us some in-depth insight into the complex physical behavior during SLM and guide the optimization of process parameters.

Application of metal hydride paper to simple pressure generator for use in soft actuator systems.

PubMed

Ino, Shuichi; Sakaki, Kouji; Hosono, Minako; Doi, Kouki; Shimada, Shigenobu; Chikai, Manabu

2015-01-01

Metal hydride (MH) actuators have a simple structure and a number of features that make them attractive for use in rehabilitation engineering and assistive technology. The MH actuator provides a high power-to-weight ratio, high-strain actuation, human-compatible softness, and noiseless operation, while being environmentally benign. On the other hand, there remain technical challenges to be overcome to improve the MH actuator regarding its speed of operation and energy efficiency, given the low heat conductivity of the MH powder that is used as the pressure generator for soft actuation. To overcome the issues of low heat conductivity and the handling of MH powder, we developed an MH paper, which is a special paper incorporating MH powder and carbon fiber, for use as a new pressure-generating element for a soft MH actuator system. In addition, the basic properties and structure of the proposed MH paper were investigated through scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and several thermodynamic experiments. The results of these experiments showed that the hydrogen absorption and desorption rates of the MH paper were significantly higher than those of the MH powder around room temperature.

Enhanced Kinetics of Electrochemical Hydrogen Uptake and Release by Palladium Powders Modified by Electrochemical Atomic Layer Deposition

DOE PAGES

Benson, David M.; Tsang, Chu F.; Sugar, Joshua Daniel; ...

2017-04-28

One method for the formation of nanofilms of materials, is Electrochemical atomic layer deposition (E-ALD), one atomic layer at a time. It uses the galvanic exchange of a less noble metal, deposited using underpotential deposition (UPD), to produce an atomic layer of a more noble element by reduction of its ions. This process is referred to as surface limited redox replacement and can be repeated in a cycle to grow thicker deposits. Previously, we performed it on nanoparticles and planar substrates. In the present report, E-ALD is applied for coating a submicron-sized powder substrate, making use of a new flowmore » cell design. E-ALD is used to coat a Pd powder substrate with different thicknesses of Rh by exchanging it for Cu UPD. Furthermore, cyclic voltammetry and X-ray photoelectron spectroscopy indicate an increasing Rh coverage with increasing numbers of deposition cycles performed, in a manner consistent with the atomic layer deposition (ALD) mechanism. Cyclic voltammetry also indicated increased kinetics of H sorption and desorption in and out of the Pd powder with Rh present, relative to unmodified Pd.« less

Physical characteristics and aerosolization performance of insulin dry powders for inhalation prepared by a spray drying method.

PubMed

You, Yu; Zhao, Min; Liu, Guangli; Tang, Xing

2007-07-01

The objective of this study was to investigate the influence of formulation excipients on the physical characteristics and aerosolization performance of insulin dry powders for inhalation. Insulin dry powders were prepared by a spray drying technique using excipients such as sugars (trehalose, lactose and dextran), mannitol and amino acids (L-leucine, glycine and threonine). High performance liquid chromatography and the mouse blood glucose method were used for determination of the insulin content. The powder properties were determined and compared by scanning electron microscopy, thermo-gravimetric analysis and size distribution analysis by a time-of-flight technique. The in-vitro aerosolization behaviour of the powders was assessed with an Aerolizer inhaler using a twin-stage impinger. Powder yield and moisture absorption were also determined. Results showed that there was no noticeable change in insulin content in any of the formulations by both assay methods. All powders were highly wrinkled, with median aerodynamic diameters of 2-4 microm, and consequently suitable for pulmonary administration. The tapped density was reduced dramatically when glycine was added. The powders containing mannitol, with or without L-leucine, were less sensitive to moisture. The highest respirable fraction of 67.3 +/- 1.3% was obtained with the formulation containing L-leucine, in contrast to formulations containing glycine and threonine, which had a respirable fraction of 11.2 +/- 3.9% and 23.5 +/- 2.5%, respectively. In addition, powders with good physical properties were achieved by the combination of insulin and trehalose. This study suggests that L-leucine could be used to enhance the aerosolization behaviour of the insulin dry powders for inhalation, and trehalose could potentially be used as an excipient in the formulations.

Optical Properties of Natural Minerals in the Far-Infrared

NASA Astrophysics Data System (ADS)

Long, Larry Lavern

The reflectivity of natural mineral powders were measured in the far infrared. The complex indices of refraction were then determined by Kramers-Kronig analysis or dispersive analysis. The samples were constructed by pressing the powdered sample into a 13 mm diameter pellet. A few of the samples that were measured were kaolin, illite, and montmorillonite, clay samples that could not be obtained in large single crystals. For calcite and gypsum crystals a comparison between the single crystal measurements and powder measurements was done to determine the effect of sample preparation on the measured spectra.

Establishing powder-handling workflow practices and standard operating procedures: compounding pharmacy and safety.

PubMed

Prince, Bryan; Lundevall, Jeremy

2014-01-01

This is an ongoing discussion and analysis of powder-handling safety in the compounding pharmacy laboratory that started in the November/December 2013 issue of the International Journal of Pharmaceutical Compounding. In the previous technical article, we established that most chemical powders handled during compounding procedures have an established occupational exposure limits and that powders are micronized during manipulation. All micronized powders handled on an open bench create health hazards to the technicians and create a potential for cross-contamination to the lab environment. Proper identification of the chemical hazard and established standard operating procedures in direct correlation to Good Lab Practices when working inside a powder hood will positively improve the compounding pharmacy's work environment.

Fungus mediated biosynthesis of WO3 nanoparticles using Fusarium solani extract

NASA Astrophysics Data System (ADS)

Kavitha, N. S.; Venkatesh, K. S.; Palani, N. S.; Ilangovan, R.

2017-05-01

Currently nanoparticles were synthesized by emphasis bioremediation process due to less hazardous, eco-friendly and imperative applications on biogenic process. Fungus mediated biosynthesis strategy has been developed to prepare tungsten oxide nanoflakes (WO3, NFs) using the plant pathogenic fungus F.solani. The powder XRD pattern revealed the monoclinic crystal structure with improved crystalline nature of the synthesized WO3 nanoparticles. FESEM images showed the flake-like morphology of WO3, with average thickness and length around 40 nm and 300 nm respectively. The Raman spectrum of WO3 NFs showed their characteristic vibration modes that revealed the defect free nature of the WO3 NFs. Further, the elemental analysis indicated the stoichiometric composition of WO3 phase.

Chemical systematics of the Shergotty meteorite and the composition of its parent body (Mars)

NASA Technical Reports Server (NTRS)

Laul, J. C.; Smith, M. R.; Waenke, H.; Jagoutz, E.; Dreibus, G.

1986-01-01

Sixty elements in two bulk samples of Shergotty meteorite and 30 elements in various mineral separates of Shergotty were identified, using mainly INAA and RNAA techniques. In addition, elements leached out from powdered samples of Shergotty and EETA 79001 meteorites by 0.1 N HCl, as well as the elements of their residues, were analyzed. The results have indicated that Shergotty meteorite is homogeneous in its major element composition, but heterogeneous with respect to large-ion lithophile elements, such as K, Ba, Sr, Zr, Hf, Ta, Th, and rare-earth elements (REEs). It is even more heterogeneous with respect to volatile elements, such as Cd, Te, Tl, and Bi, and the siderophiles Au and Ag. The REE patterns of the Shergotty and EETA 79001 residues are identical, indicating that the parent magmas of both meteorites are compositionally similar. However, their leachate (phosphate) patterns are different, suggesting two components for the Shergotty, one of which is similar to the EETA 79001 leachate.

Modified Chaihu Shugan Powder for Functional Dyspepsia: Meta-Analysis for Randomized Controlled Trial

PubMed Central

Yang, Nan; Jiang, Xuehua; Hu, Zhiqiang; Wang, Ling; Song, Minxian

2013-01-01

Context. Modified Chaihu Shugan powder (MCSP) is a popular traditional Chinese herbal formula for functional dyspepsia, which is revised from Chaihu Shugan San and recorded in a medical classic works of China. However, its role and effect in treating functional dyspepsia have not been well established. Objective. To assess the effect and safety of modified Chaihu Shugan powder for functional dyspepsia. Methods. We searched the published and unpublished studies up to August 2012. Only RCTs of modified Chaihu Shugan powder with or without prokinetic drugs versus prokinetic drugs in the patients diagnosed with functional dyspepsia were included. Results. Twenty-two clinical trials involving 1998 participants were included. There were evidences that modified Chaihu Shugan powder (RR = 1.20, 95%, CI 1.14 to 1.27) and modified Chaihu Shugan powder plus prokinetic drugs (RR = 1.18, 95%, CI 1.11 to 1.25) were significantly better treatment options than prokinetic drugs alone in improving symptoms. No serious adverse events were described in the included trials. Conclusions. This meta-analysis showed that modified Chaihu Shugan powder alone or in combination with prokinetic drugs might be more effective than prokinetic drugs alone. However, with poor methodological quality, all the included trials were at high risk of bias. Further large-scale high-quality trials are required for assessment. PMID:23762161

Cleansing orthodontic brackets with air-powder polishing: effects on frictional force and degree of debris.

PubMed

Leite, Brisa Dos Santos; Fagundes, Nathalia Carolina Fernandes; Aragón, Mônica Lídia Castro; Dias, Carmen Gilda Barroso Tavares; Normando, David

2016-01-01

Debris buildup on the bracket-wire interface can influence friction. Cleansing brackets with air-powder polishing can affect this process. The aim of this study was to evaluate the frictional force and amount of debris remaining on orthodontic brackets subjected to prophylaxis with air-powder polishing. Frictional force and debris buildup on the surface of 28 premolar brackets were evaluated after orthodontic treatment. In one hemiarch, each bracket was subjected to air-powder polishing (n = 14) for five seconds, while the contralateral hemiarch (n = 14) served as control. Mechanical friction tests were performed and images of the polished bracket surfaces and control surfaces were examined. Wilcoxon test was applied for comparative analysis between hemiarches at p < 0.05. Brackets that had been cleaned with air-powder polishing showed lower friction (median = 1.27 N) when compared to the control surfaces (median = 4.52 N) (p < 0.01). Image analysis showed that the control group exhibited greater debris buildup (median = 2.0) compared with the group that received prophylaxis with air-powder polishing (median = 0.5) (p < 0.05). Cleansing orthodontic brackets with air-powder polishing significantly reduces debris buildup on the bracket surface while decreasing friction levels observed during sliding mechanics.

Properties and Applications of High Emissivity Composite Films Based on Far-Infrared Ceramic Powder

PubMed Central

Xiong, Yabo; Huang, Shaoyun; Wang, Wenqi; Liu, Xinghai; Li, Houbin

2017-01-01

Polymer matrix composite materials that can emit radiation in the far-infrared region of the spectrum are receiving increasing attention due to their ability to significantly influence biological processes. This study reports on the far-infrared emissivity property of composite films based on far-infrared ceramic powder. X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, thermogravimetric analysis, and X-ray powder diffractometry were used to evaluate the physical properties of the ceramic powder. The ceramic powder was found to be rich in aluminum oxide, titanium oxide, and silicon oxide, which demonstrate high far-infrared emissivity. In addition, the micromorphology, mechanical performance, dynamic mechanical properties, and far-infrared emissivity of the composite were analyzed to evaluate their suitability for strawberry storage. The mechanical properties of the far-infrared radiation ceramic (cFIR) composite films were not significantly influenced (p ≥ 0.05) by the addition of the ceramic powder. However, the dynamic mechanical analysis (DMA) properties of the cFIR composite films, including a reduction in damping and shock absorption performance, were significant influenced by the addition of the ceramic powder. Moreover, the cFIR composite films showed high far-infrared emissivity, which has the capability of prolonging the storage life of strawberries. This research demonstrates that cFIR composite films are promising for future applications. PMID:29186047

Properties and Applications of High Emissivity Composite Films Based on Far-Infrared Ceramic Powder.

PubMed

Xiong, Yabo; Huang, Shaoyun; Wang, Wenqi; Liu, Xinghai; Li, Houbin

2017-11-29

Polymer matrix composite materials that can emit radiation in the far-infrared region of the spectrum are receiving increasing attention due to their ability to significantly influence biological processes. This study reports on the far-infrared emissivity property of composite films based on far-infrared ceramic powder. X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, thermogravimetric analysis, and X-ray powder diffractometry were used to evaluate the physical properties of the ceramic powder. The ceramic powder was found to be rich in aluminum oxide, titanium oxide, and silicon oxide, which demonstrate high far-infrared emissivity. In addition, the micromorphology, mechanical performance, dynamic mechanical properties, and far-infrared emissivity of the composite were analyzed to evaluate their suitability for strawberry storage. The mechanical properties of the far-infrared radiation ceramic (cFIR) composite films were not significantly influenced ( p ≥ 0.05) by the addition of the ceramic powder. However, the dynamic mechanical analysis (DMA) properties of the cFIR composite films, including a reduction in damping and shock absorption performance, were significant influenced by the addition of the ceramic powder. Moreover, the cFIR composite films showed high far-infrared emissivity, which has the capability of prolonging the storage life of strawberries. This research demonstrates that cFIR composite films are promising for future applications.

Synthesis of imine bond containing insoluble polymeric ligand and its transition metal complexes, structural characterization and catalytic activity on esterification reaction.

PubMed

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Saribiyik, Oguz Yunus; Yildiz, Emel; Serin, Selahattin

2017-01-01

In this study, synthesis of insoluble polymeric ligand (L) and its transition metal complexes [Cu(L)Cl 2 ]·2H 2 O (1) , [Co(L)Cl 2 (H 2 O) 2 ] (2) and [Ni(L)Cl 2 (H 2 O) 2 ] (3) , having the azomethine groups, were synthesized by the condensation reactions of the diamines and dialdehydes. The structural properties were characterized by the analytical and spectroscopic methods using by elemental analysis, Fourier Transform Infrared, Thermo Gravimetric Analysis, Powder X-ray Diffraction, magnetic susceptibility and Inductively Coupled Plasma. The solubilities of the synthesized polymeric materials were also investigated and found as insoluble some organic and inorganic solvents. Additionally, their catalytic performance was carried out for the esterification reaction of acetic acid and butyl acetate. The highest conversion rate is 75.75% by using catalyst 1 . The esterification of butanol gave butyl acetate with 100% selectivity.

Pyrolytic synthesis and luminescence of porous lanthanide Eu-MOF.

PubMed

Jin, Guangya; Liu, Zhijian; Sun, Hongfa; Tian, Zhiyong

2016-02-01

A lanthanide metal coordination polymer [Eu2(BDC)3(DMSO)(H2O)] was synthesized by the reaction of europium oxide with benzene-1,3-dicarboxylic acid (H2BDC) in a mixed solution of dimethyl sulfoxide (DMSO) and water under hydrothermal conditions. The crystal structure of Eu2(BDC)3(DMSO)(H2O) was characterized by X-ray diffraction (XRD). Thermo-gravimetric analysis of Eu2(BDC)3(DMSO)(H2O) indicated that coordinated DMSO and H2O molecules could be removed to create Eu2(BDC)3(DMSO)(H2O)-py with permanent microporosity, which was also verified by powder XRD (PXRD) and elemental analysis. Both Eu2(BDC)3(DMSO)(H2O) and Eu2(BDC)3(DMSO)(H2O)-py showed mainly Eu-based luminescence and had characteristic emissions in the range 550-700 nm. Copyright © 2015 John Wiley & Sons, Ltd.

Quinoline derivative containing monomeric and polymeric metal carboxylates: Synthesis, crystal structure and gas adsorption study over a 2D layered framework

NASA Astrophysics Data System (ADS)

Gayen, Saikat; Saha, Debraj; Koner, Subratanath

2018-06-01

A new supramolecular metal-carboxylate framework [Co(mqc)2]n (1), and another monomeric compound [Zn (mqc)2(H2O)] (2) (mqcH = 4-methoxy 2-quinolinecarboxylic acid) have been synthesized solvothermally and characterized by single crystal X-ray diffraction, elemental analysis, IR spectra, UV-vis spectra, powdered X-ray diffraction (PXRD) and thermogravimetric analysis. Compound 1 is a 2D coordination polymer, extended to a 3D porous supramolecular network having void space in between 2D layers. Compound 1 exhibits gas uptake capacity of N2, H2, CO2 and CH4 like small gas molecules in which moderately high uptake of H2 and CO2 takes place among the 2D MOFs. While the Zn variety, compound 2 features a one-dimensional chain like structure through strong intermolecular hydrogen-bonding.

Synthesis and structural characterization of CdS nanoparticles using nitrogen adducts of mixed diisopropylthiourea and dithiolate derivatives of Cd(II) complexes

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2015-07-01

[Cd(diptu)2(ced)], [Cd(diptu)2(ced)(bpy)], [Cd(diptu)2(ced)(phen)], (where diptu = diisopropyl thiourea; ced = 1-cyano-1-carboethoxylethylene-2,2‧-dithiolate; bpy = 2,2‧-bipyridine and phen = 1,10-phenanthroline) have been prepared and used as single source precursors for the preparation of hexadecylamine capped CdS nanoparticles. The precursor complexes were characterized by elemental analysis, FTIR and TGA. The structural properties of the nanoparticles were investigated using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy techniques (SEM). The optical properties of the nanoparticles were studied using UV-Visible and photoluminescence spectroscopy. The XRD analysis showed that the nanoparticles were indexed to the hexagonal phase of CdS and the TEM results showed CdS nanoparticles with average crystallite sizes of 4.00-8.80 nm.