Microstructure and physical properties of laser Zn modified amorphous-nanocrystalline coating on a titanium alloy

NASA Astrophysics Data System (ADS)

Li, Jia-Ning; Gong, Shui-Li; Shi, Yi-Ning; Suo, Hong-Bo; Wang, Xi-Chang; Deng, Yun-Hua; Shan, Fei-Hu; Li, Jian-Quan

2014-02-01

A Zn modified amorphous-nanocrystalline coating was fabricated on a Ti-6Al-4V alloy by laser cladding of the Co-Ti-B4C-Zn-Y2O3 mixed powders. Such coating was researched by means of a scanning electron microscope (SEM) and a high resolution transmission electron microscope (HRTEM), etc. Experimental results indicated that the Co5Zn21 and TiB2 nanocrystalline phases were produced through in situ metallurgical reactions, which blocked the motion of dislocation, and TiB2 grew along (010), (111) and (024). The Co5Zn21 nanocrystals were produced attached to the ceramics, which mainly consisted of the Co nanoparticles embedded in a heterogeneous zinc, and had varied crystalline orientations.

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.

Grain growth in nanocrystalline iron and Fe-Al alloys

NASA Astrophysics Data System (ADS)

Mirzadeh, Hamed; Zomorodian, Amir

2010-02-01

The effects of the annealing temperature and time, cryomilling in liquid nitrogen, and the addition of aluminum powder on the thermal stability and grain growth behavior of nanocrystalline iron were modeled using the Artificial Neural Network (ANN) technique. The developed model can be used as a guide for the quantification of the grain growth by considering the effects of annealing temperature and time. The model also quantified the effect of Al on the thermal stability of cryomilled nanocrystalline Fe. The model results showed that the cryomilling of Fe has a tangible effect on the stabilization of the nanostructure.

The Cold Gas-Dynamic Spray and Characterization of Microcrystalline and Nanocrystalline Copper Alloys

DTIC Science & Technology

2012-12-01

cold gas-dynamic spray process are well understood, the effects of feedstock powder microstructure and composition on the deposition process remain...The Relationship between Powder Zinc Content and Porosity .....74  5.  Compositional Variability as a Side Effect of the Cold Spray Deposition Process ...to expect in cold spray deposited copper coatings based on common spray parameters. Ning et

Nanocrystalline Al7075 + 1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering

PubMed Central

Málek, Přemysl; Minárik, Peter; Chráska, Tomáš; Novák, Pavel; Průša, Filip

2017-01-01

The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm) with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM)/8 h) resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm) along with the dissolution of the intermetallic phases. Milling led to an increase in the powder’s microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS) exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al3Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder. PMID:28930192

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

Nanostructured Fe-Cr Alloys for Advanced Nuclear Energy Applications

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

Scattergood, Ronald O.

2016-04-26

We have completed research on the grain-size stabilization of model nanostructured Fe14Cr base alloys at high temperatures by the addition of non-equilibrium solutes. Fe14Cr base alloys are representative for nuclear reactor applications. The neutron flux in a nuclear reactor will generate He atoms that coalesce to form He bubbles. These can lead to premature failure of the reactor components, limiting their lifetime and increasing the cost and capacity for power generation. In order to mitigate such failures, Fe14Cr base alloys have been processed to contain very small nano-size oxide particles (less than 10 nm in size) that trap He atomsmore » and reduce bubble formation. Theoretical and experimental results indicate that the grain boundaries can also be very effective traps for He atoms and bubble formation. An optimum grain size will be less than 100 nm, ie., nanocrystalline alloys must be used. Powder metallurgy methods based on high-energy ball milling can produce Fe-Cr base nanocrystalline alloys that are suitable for nuclear energy applications. The problem with nanocrystalline alloys is that excess grain-boundary energy will cause grains to grow at higher temperatures and their propensity for He trapping will be lost. The nano-size oxide particles in current generation nuclear alloys provide some grain size stabilization by reducing grain-boundary mobility (Zener pinning – a kinetic effect). However the current mitigation strategy minimizing bubble formation is based primarily on He trapping by nano-size oxide particles. An alternate approach to nanoscale grain size stabilization has been proposed. This is based on the addition of small amounts of atoms that are large compared to the base alloy. At higher temperatures these will diffuse to the grain boundaries and will produce an equilibrium state for the grain size at higher temperatures (thermodynamic stabilization – an equilibrium effect). This would be preferred compared to a kinetic effect, which is not based on an equilibrium state. The PI and coworkers have developed thermodynamic-based models that can be used to select appropriate solute additions to Fe14Cr base alloys to achieve a contribution to grain-size stabilization and He bubble mitigation by the thermodynamic effect. All such models require approximations and the proposed research was aimed at alloy selection, processing and detailed atomic-level microstructure evaluations to establish the efficacy of the thermodynamic effect. The outcome of this research shows that appropriate alloy additions can produce a contribution from the thermodynamic stabilization effect. Furthermore, due to the oxygen typically present in nominally high purity elemental powders used for powder metallurgy processing, the optimum results obtained appeared as a synergistic combination of nano-size oxide particle pinning kinetic effect and the grain-boundary segregation thermodynamic effect.« less

Influence of temperature on AC conductivity of nanocrystalline CuAlO2

NASA Astrophysics Data System (ADS)

Prakash, T.

2012-07-01

Nanocrystalline CuAlO2 was synthesized by mechanical alloying of Cu2O and α-Al2O3 powders in the molar ratio of 1:1 for 20 h in toluene medium with tungsten carbide balls and vials using planetary ball mill. The ball milling was carried out at 300 rpm with a ball to powder weight ratio of 10:1 and then annealed at 1373 K in a platinum crucible for 20 h to get CuAlO2 phase with average crystallite size 45 nm. Complex impedance spectroscopic measurement in the frequency region 1 Hz to 10 MHz between the temperatures 333 to 473 K was carried out for nanocrystalline CuAlO2 sample. The obtained complex impedance data was analyzed for AC conductivities, DC and AC conductivities correlations and crossover frequencies ( f co ). The BNN (Barton, Nakajima and Namikawa) relation was applied to understand the correlation between DC and AC conductivities. The observed experimental results were discussed in the paper.

Preparation, deformation, and failure of functional Al-Sn and Al-Sn-Pb nanocrystalline alloys

NASA Astrophysics Data System (ADS)

Noskova, N. I.; Vil'Danova, N. F.; Filippov, Yu. I.; Churbaev, R. V.; Pereturina, I. A.; Korshunov, L. G.; Korznikov, A. V.

2006-12-01

Changes in the structure, hardness, mechanical properties, and friction coefficient of Al-30% Sn, Al-15% Sn-25% Pb, and Al-5% Sn-35% Pb (wt %) alloys subjected to severe plastic deformation by equal-channel angular pressing (with a force of 40 tonne) and by shear at a pressure of 5 GPa have been studied. The transition into the nanocrystalline state was shown to occur at different degrees of plastic deformation. The hardness exhibits nonmonotonic variations, namely, first it increases and subsequently decreases. The friction coefficient of the Al-30% Sn, Al-15% Sn-25% Pb, and Al-5% Sn-35% Pb alloys quenched from the melt was found to be 0.33; the friction coefficients of these alloys in the submicrocrystalline state (after equal-channel angular pressing) equal 0.24, 0.32, and 0.35, respectively. The effect of disintegration into nano-sized powders was found to occur in the Al-15% Sn-25% Pb, and Al-5% Sn-35% Pb alloys after severe plastic deformation to ɛ = 6.4 and subsequent short-time holding.

Microstructural Evolution and Mechanical Properties of Nanointermetallic Phase Dispersed Al65Cu20Ti15 Amorphous Matrix Composite Synthesized by Mechanical Alloying and Hot Isostatic Pressing

NASA Astrophysics Data System (ADS)

Roy, D.; Mitra, R.; Ojo, O. A.; Lojkowski, W.; Manna, I.

2011-08-01

The structure and mechanical properties of nanocrystalline intermetallic phase dispersed amorphous matrix composite prepared by hot isostatic pressing (HIP) of mechanically alloyed Al65Cu20Ti15 amorphous powder in the temperature range 573 K to 873 K (300 °C to 600 °C) with 1.2 GPa pressure were studied. Phase identification by X-ray diffraction (XRD) and microstructural investigation by transmission electron microscopy confirmed that sintering in this temperature range led to partial crystallization of the amorphous powder. The microstructures of the consolidated composites were found to have nanocrystalline intermetallic precipitates of Al5CuTi2, Al3Ti, AlCu, Al2Cu, and Al4Cu9 dispersed in amorphous matrix. An optimum combination of density (3.73 Mg/m3), hardness (8.96 GPa), compressive strength (1650 MPa), shear strength (850 MPa), and Young's modulus (182 GPa) were obtained in the composite hot isostatically pressed ("hipped") at 773 K (500 °C). Furthermore, these results were compared with those from earlier studies based on conventional sintering (CCS), high pressure sintering (HPS), and pulse plasma sintering (PPS). HIP appears to be the most preferred process for achieving an optimum combination of density and mechanical properties in amorphous-nanocrystalline intermetallic composites at temperatures ≤773 K (500 °C), while HPS is most suited for bulk amorphous alloys. Both density and volume fraction of intermetallic dispersoids were found to influence the mechanical properties of the composites.

High temperature coercive field behavior of Fe-Zr powder

NASA Astrophysics Data System (ADS)

Mishra, Debabrata; Perumal, A.; Srinivasan, A.

2009-04-01

We report the investigation of high temperature coercive field behavior of Fe80Zr20 nanocrystalline alloy powder having two-phase microstructure prepared by mechanical alloying process. Thermomagnetization measurement shows the presence of two different magnetic phase transitions corresponding to the amorphous matrix and nonequilibrium Fe(Zr) solid solution. Temperature dependent coercivity exhibits a sharp increase in its value close to the Curie temperature of the amorphous matrix. This feature is attributed to the loss of intergranular ferromagnetic exchange coupling between the nanocrystallites due to the paramagnetic nature of the amorphous matrix. The temperature dependent coercive field behavior is ascribed to the variations in both the effective anisotropy and the exchange stiffness constant with temperature.

Synthesis and characterization of nanocrystalline Al 2024-B4C composite powders by mechanical alloying

NASA Astrophysics Data System (ADS)

Varol, T.; Canakci, A.

2013-06-01

In the present work, the effect of milling parameters on the morphology and microstructure of nanostructure Al2024-B4C composite powders obtained by mechanical alloying (MA) was studied. The effects of milling time and B4C content on the morphology, microstructure and particle size of nanostructure Al2024-B4C composite powders have been investigated. Different amounts of B4C particles (0, 5, 10 and 20 wt.%) were mixed with Al2024 powders and milled in a planetary ball mill for 30, 60, 120, 300, 420 and 600 min. Al 2024-B4C composite powders were characterized using a scanning electron microscope (SEM), laser particle-size analyzer, X-ray diffraction analysis (XRD) and the Vickers microhardness test. The results showed that the nanostructure Al2024-B4C composite powders were produced when they were milled for 600 min. The size of composite powder in the milled powder mixture was affected by the milling time and content of B4C particles. Moreover, it was observed that when MA reached a steady state, the properties of composite powders were stabilized.

High-Temperature Stability and Grain Boundary Complexion Formation in a Nanocrystalline Cu-Zr Alloy

NASA Astrophysics Data System (ADS)

Khalajhedayati, Amirhossein; Rupert, Timothy J.

2015-12-01

Nanocrystalline Cu-3 at.% Zr powders with ~20 nm average grain size were created with mechanical alloying and their thermal stability was studied from 550-950°C. Annealing drove Zr segregation to the grain boundaries, which led to the formation of amorphous intergranular complexions at higher temperatures. Grain growth was retarded significantly, with 1 week of annealing at 950°C, or 98% of the solidus temperature, only leading to coarsening of the average grain size to 54 nm. The enhanced thermal stability can be connected to both a reduction in grain boundary energy with doping as well as the precipitation of ZrC particles. High mechanical strength is retained even after these aggressive heat treatments, showing that complexion engineering may be a viable path toward the fabrication of bulk nanostructured materials with excellent properties.

Microstructure, Mechanical Properties, and Two-Body Abrasive Wear Behavior of Cold-Sprayed 20 vol.% Cubic BN-NiCrAl Nanocomposite Coating

NASA Astrophysics Data System (ADS)

Luo, Xiao-Tao; Yang, Er-Juan; Shang, Fu-Lin; Yang, Guan-Jun; Li, Chen-Xin; Li, Chang-Jiu

2014-10-01

20 vol.% cubic boron nitride (cBN) dispersoid reinforced NiCrAl matrix nanocomposite coating was prepared by cold spray using mechanically alloyed nanostructured composite powders. The as-sprayed nanocomposite coating was annealed at a temperature of 750 °C to enhance the inter-particle bonding. Microstructure of spray powders and coatings was characterized. Vickers microhardness of the coatings was measured. Two-body abrasive wear behavior of the coatings was examined on a pin-on-disk test. It was found that, in mechanically alloyed composite powders, nano-sized and submicro-sized cBN particles are uniformly distributed in nanocrystalline NiCrAl matrix. Dense coating was deposited by cold spray at a gas temperature of 650 °C with the same phases and grain size as those of the starting powder. Vickers hardness test yielded a hardness of 1063 HV for the as-sprayed 20 vol.% cBN-NiCrAl coating. After annealed at 750 °C for 5 h, unbonded inter-particle boundaries were partially healed and evident grain growth of nanocrystalline NiCrAl was avoided. Wear resistance of the as-sprayed 20 vol.% cBN-NiCrAl nanocomposite coating was comparable to the HVOF-sprayed WC-12Co coating. Annealing of the nanocomposite coating resulted in the improvement of wear resistance by a factor of ~33% owing to the enhanced inter-particle bonding. Main material removal mechanisms during the abrasive wear are also discussed.

Preparation of high-quality ultrathin transmission electron microscopy specimens of a nanocrystalline metallic powder.

PubMed

Riedl, Thomas; Gemming, Thomas; Mickel, Christine; Eymann, Konrad; Kirchner, Alexander; Kieback, Bernd

2012-06-01

This article explores the achievable transmission electron microscopy specimen thickness and quality by using three different preparation methods in the case of a high-strength nanocrystalline Cu-Nb powder alloy. Low specimen thickness is essential for spatially resolved analyses of the grains in nanocrystalline materials. We have found that single-sided as well as double-sided low-angle Ar ion milling of the Cu-Nb powders embedded into epoxy resin produced wedge-shaped particles of very low thickness (<10 nm) near the edge. By means of a modified focused ion beam lift-out technique generating holes in the lamella interior large micrometer-sized electron-transparent regions were obtained. However, this lamella displayed a higher thickness at the rim of ≥30 nm. Limiting factors for the observed thicknesses are discussed including ion damage depths, backscattering, and surface roughness, which depend on ion type, energy, current density, and specimen motion. Finally, sections cut by ultramicrotomy at low stroke rate and low set thickness offered vast, several tens of square micrometers uniformly thin regions of ∼10-nm minimum thickness. As major drawbacks, we have detected a thin coating on the sections consisting of epoxy deployed as the embedding material and considerable nanoscale thickness variations. Copyright © 2011 Wiley Periodicals, Inc.

Powder metallurgical low-modulus Ti-Mg alloys for biomedical applications.

PubMed

Liu, Yong; Li, Kaiyang; Luo, Tao; Song, Min; Wu, Hong; Xiao, Jian; Tan, Yanni; Cheng, Ming; Chen, Bing; Niu, Xinrui; Hu, Rong; Li, Xiaohui; Tang, Huiping

2015-11-01

In this work, powder metallurgical (PM) Ti-Mg alloys were prepared using combined techniques of mechanical alloying and spark plasma sintering. The alloys mainly consist of super saturations of Mg in Ti matrix, and some laminar structured Ti- and Mg-rich phases. The PM Ti-Mg alloys contain a homogeneous mixtures of nanocrystalline Mg and Ti phases. The novel microstructures result in unconventional mechanical and biological properties. It has been shown that the PM Ti-Mg alloys have a much lower compression modulus (36-50GPa) compared to other Ti alloys, but still remain a very high compressive strength (1500-1800MPa). In addition, the PM Ti-Mg alloys show good biocompatibility and bioactivity. Mg can dissolve in the simulated body fluids, and induce the formation of the calcium phosphate layer. The compression modulus of PM Ti-Mg alloys decreases with the amount of Mg, while the bioactivity increases. Although the corrosion resistance of Ti-Mg alloys decreases with the content of Mg, the alloys still show good stability in simulated body fluid under electrochemical conditions. The indirect and direct cytotoxicity results show that PM Ti-Mg alloys have a good biocompatibility to NIH-3T3 cells. Therefore, the PM Ti-Mg alloys are promising candidates in biomedical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Fabrication, microstructure, properties and deformation mechanisms of a nanocrystalline aluminum-iron-chromium-titanium alloy by mechanical alloying

NASA Astrophysics Data System (ADS)

Luo, Hong

A multi-phase nanocrystalline Al93Fe3Cr2Ti 2 alloy containing 30 vol.% intermetallic particles was prepared via mechanical alloying starting from elemental powders, followed by hot extrusion. The grain size of 6-45 nm can be achieved after 30-hours of milling. Thermal stability of nanostructured Al93Fe3Ti2Cr 2 alloys was investigated using a variety of analytical techniques including modulated differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, transmission electron microscopy. The MA-processed Al93Fe 3Ti2Cr2 alloy in the as-milled condition was composed of an Al-based supersaturated solid solution with high internal strains. Release of internal strains, intermetallic precipitation and grain growth occurred upon heating of the MA-processed Al alloy. Nevertheless, grain growth in the MA-processed Al alloy was very limited and fcc-Al grains with sizes in the range of 20 nm were still present in the alloys after exposure to 450°C (0.77 Tm). Systematic compressive tests and modulus measurements were performed as a function of temperature and strain rate to investigate the deformation behavior and mechanisms of the nc Al-Fe-Cr-Ti alloys. High strengths and moduli at both ambient and elevated temperatures have been demonstrated. The ductility of the nc Al93Fe3Cr2Ti2 alloy depends strongly on whether the oxide film at the prior powder particle boundary has been broken down or not. The MA-processed Al93Fe3Cr 2Ti2 alloy is brittle when the oxide film is continuous at PPB, and is ductile when the oxide film is broken down into discontinuous particles during extrusion. It is argued that the compressive strength at ambient temperature is controlled by propagation of dislocations into nc fcc-Al grains, whereas the compressive strength at elevated temperature is determined by dislocation propagation as well as dynamic recovery. Since the stress for dislocation propagation into nc fcc-Al grains increases with decreasing the grain size, the smaller the grain size, the higher the compressive strength. This new microstructural design approach could present opportunities for exploiting nc materials in structural applications at both ambient and elevated temperatures. The nanocrystalline Al-Fe-Cr-Ti alloy exhibited significant difference in deformation behavior between tension and compression at 25, 200 and 300°C. However, the strengths obtained in tension and compression were similar at 400°C. Systematic microstructure examinations and deformation mechanism analyses indicate that the asymmetry of this nc Al93Fe3Cr 2Ti2 alloy is related to its dislocation mediated plastic deformation mechanism, its nanoscale grain microstructure, and premature brittle failure in tension tests.

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.

Bulk Nanocrystalline Metals: Review of the Current State of the Art and Future Opportunities for Copper and Copper Alloys

DTIC Science & Technology

2014-05-13

nanocrystalline materials using mechanical alloying, the alloy development and synthesis process for stabilizing these materials at elevated temperatures, and...the physical and mechanical properties of nanocrystalline materials with a focus throughout on nanocrystalline copper and a nanocrystalline Cu-Ta...approaches as well as experimental results for grain growth, grain boundary processes, and deformation mechanisms in nanocrystalline copper are

Synthesis and magnetization studies of nanopowder Fe₇₀Ni₂₀Cr₁₀ alloys prepared by high energy milling

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

Chater, R., E-mail: chatersamy@yahoo.fr; Bououdina, M., E-mail: mboudina@gmail.com; Department of Physics, College of Science, University of Bahrain, PO Box 32038, Kingdom of Bahrain

2013-05-01

Nanocrystalline Fe{sub 1–x–y}Ni xCr y (x=20, y=10% in Wt)) alloy samples were prepared by mechanical alloying process. Fe, Ni and Cr elemental powders have been ball milled in a planetary mill for various periods of time, up to 27 h. XRD analysis allowed the determination of the structure of the mixture, the average crystallite size and the lattice parameter as a function of milling time. The complete formation of FeNiCr is observed after 27 h milling. With increasing milling time from 0 to 27 h, it is observed that the lattice parameter increases from 0.3515 to 0.3593 nm as wellmore » as an increase of microstrain from 0.15 to 0.40%, whereas the grain size decreases from 48 to 13 nm. Grain morphology of the powders at different formation stages was examined using SEM. Saturation magnetization and coercive fields derived from the hysteresis curves are discussed as a function of milling time. - Graphical abstract: Fe₇₀Ni₂₀Cr₁₀ nanopowders were prepared using a planetary ball mill. The structure and microstructure vary with milling time; thereby important modifications of the magnetic properties were observed and discussed. Highlights: • Nanocrystalline Fe₇₀Ni₂₀Cr₁₀ alloy were prepared by the mechanical alloying process. • The complete formation of Fe₇₀Ni₂₀Cr₁₀ is observed after 24 h milling. • With increasing milling time, the grain size decreases, while the strain increases. • The SEM images allowed following the morphology of the materials at different stages. • M s and H C derived from the hysteresis are discussed as a function of milling time.« less

Fabrication and Magnetic Properties of Co₂MnAl Heusler Alloys by Mechanical Alloying.

PubMed

Lee, Chung-Hyo

2018-02-01

We have applied mechanical alloying (MA) to produce nanocrystalline Co2MnAl Heusler alloys using a mixture of elemental Co50Mn25Al25 powders. An optimal milling and heat treatment conditions to obtain a Co2MnAl Heusler phase with fine microstructure were investigated by X-ray diffraction, differential scanning calorimeter and vibrating sample magnetometer measurements. α-(Co, Mn, Al) FCC phases coupled with amorphous phase are obtained after 3 hours of MA without any evidence for the formation of Co2MnAl alloys. On the other hand, a Co2MnAl Heusler alloys can be obtained by the heat treatment of all MA samples up to 650 °C. X-ray diffraction result shows that the average grain size of Co2MnAl Heusler alloys prepared by MA for 5 h and heat treatment is in the range of 95 nm. The saturation magnetization of MA powders decreases with MA time due to the magnetic dilution by alloying with nonmagnetic Mn and Al elements. The magnetic hardening due to the reduction of the grain size with ball milling is also observed. However, the saturation magnetization of MA powders after heat treatment increases with MA time and reaches to a maximum value of 105 emu/g after 5 h of MA. It can be also seen that the coercivity of 5 h MA sample annealed at 650 °C is fairly low value of 25 Oe.

Diffraction, microstructure and thermal stability analysis in a double phase nanocrystalline Al20Mg20Ni20Cr20Ti20 high entropy alloy

NASA Astrophysics Data System (ADS)

Rameshbabu, A. M.; Parameswaran, P.; Vijayan, V.; Panneer, R.

2017-12-01

An effort has been made to develop a new composition of AlMgNiCrTi high entropy alloy (HEA) with a distinct properties includes squat density, intense strength and hardness, superior corrosion resistance, better oxidation resistance, high temperature resistance, fatigue load and crack resistance to congregate the necessity of aircraft applications. The equivalent atomic percentage for the above defined composition is established using analytical correlation for molar and atom renovation by trial and error method. The alloy is synthesized by powder metallurgy technique through mechanical alloying. Succeeding to mechanical alloying it is elucidated that the metal powder is primarily composed of single BCC solid solution with crystallite magnitude <10 nm. It is also observed that the alloy is thermally stable at prominent temperature about 800°C as it is retained its nanostructure which was revealed using differential scanning caloriemetry (DSC). This alloy powder was consolidated and sintered using spark plasma sintering at 800°C with 50 Mpa pressure to a density of 98.83%. Subsequent to sintering, Titanium carbide FCC phase evolved along with the BCC phase. The alloying behavior and phase transformation were studied using X-ray diffraction (XRD) and scanning electron microscope (SEM). The homogeneity of the composition is confirmed by energy dispersive spectroscopy (EDS). The hardness of the alloy is found to be 710±20 HV. The evolutions of the phases and hardness imply that this alloy is apposite for both high strength and high temperature applications.

Development of High-Strength Nanostructured Magnesium Alloys for Light-Weight Weapon Systems and Vehicles

DTIC Science & Technology

2014-01-13

strength nanocrystalline Mg-alloys via cryomilling and spark - plasma - sintering , 2) demonstrate the unveil evidence of nanotwins in nanocrystalline...Christopher Melnyk, Wei H. Kao, Jenn-Ming Yang. Cryomilling and spark plasma sintering of nanocrystalline magnesium-based alloy, Journal of Materials...accomplished several important milestones: 1) manufacture of high strength nanocrystalline Mg-alloys via cryomilling and spark plasma sintering (SPS

Synthesis of Nano-Crystalline Cu-Cr Alloy by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Sheibani, S.; Heshmati-Manesh, S.; Ataie, A.

In this paper, the influence of toluene as the process control agent (PCA) and pre-milling on the extension of solid solubility of 7 wt.% Cr in Cu by mechanical alloying in a high energy ball mill was investigated. The structural evolution and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, respectively. The solid solution formation at different conditions was analyzed by copper lattice parameter change during the milling process. It was found that both the presence of PCA and pre-milling of Cr powder lead to faster dissolution of Cr. The mean crystallite size was also calculated and showed to be about 10 nm after 80 hours of milling.

Hot pressing of nanocrystalline tantalum using high frequency induction heating and pulse plasma sintering

NASA Astrophysics Data System (ADS)

Jakubowicz, J.; Adamek, G.; Sopata, M.; Koper, J. K.; Siwak, P.

2017-12-01

The paper presents the results of nanocrystalline powder tantalum consolidation using hot pressing. The authors used two different heating techniques during hot pressing: high-frequency induction heating (HFIH) and pulse plasma sintering (PPS). A comparison of the structure, microstructure, mechanical properties and corrosion resistance of the bulk nanocrystalline tantalum obtained in both techniques was performed. The nanocrystalline powder was made to start from the microcrystalline one using the high-energy ball milling process. The nanocrystalline powder was hot-pressed at 1000 °C, whereas, for comparison, the microcrystalline powder was hot pressed up to 1500 °C for proper consolidation. The authors found that during hot pressing, the powder partially reacts with the graphite die covered by boron nitride, which facilitated punches and powder displacement in the die during densification. Tantalum carbide and boride in the nanocrystalline material was found, which can improve the mechanical properties. The hardness of the HFIH and PPS nanocrystalline tantalum was as high as 625 and 615 HV, respectively. The microstructure was more uniform in the PPS nanomaterial. The corrosion resistance in both cases deteriorated, in comparison to the microcrystalline material, while the PPS material corrosion resistance was slightly better than that of the HFIH one.

Synthesis and Microstructure Evolution of Nano-Titania Doped Silicon Coatings

NASA Astrophysics Data System (ADS)

Moroz, N. A.; Umapathy, H.; Mohanty, P.

2010-01-01

The Anatase phase of Titania (TiO2) in nanocrystalline form is a well known photocatalyst. Photocatalysts are commercially used to accelerate photoreactions and increase photovoltaic efficiency such as in solar cells. This study investigates the in-flight synthesis of Titania and its doping into a Silicon matrix resulting in a catalyst-dispersed coating. A liquid precursor of Titanium Isopropoxide and ethanol was coaxially fed into the plasma gun to form Titania nanoparticles, while Silicon powder was externally injected downstream. Coatings of 75-150 μm thick were deposited onto flat coupons. Further, Silicon powder was alloyed with aluminum to promote crystallization and reduce the amorphous phase in the Silicon matrix. Dense coatings containing nano-Titania particles were observed under electron microscope. X-ray diffraction showed that both the Rutile and Anatase phases of the Titania exist. The influence of process parameters and aluminum alloying on the microstructure evolution of the doped coatings is analyzed and presented.

Investigations of Nanocrystalline Alloy Electrospark Coating Made of Nanocrystalline Alloy Based on 5БДCP Ferrum

NASA Astrophysics Data System (ADS)

Kolomeichenko, A. V.; Kuznetsov, I. S.; Izmaylov, A. Yu; Solovyev, R. Yu; Sharifullin, S. N.

2017-09-01

The article describes the properties of wear resistant electrospark coating made of nanocrystalline alloy of type 5БДCP (Finemet). It is proved that electrospark coating has nanocrystalline structure which is like amorphous matrix with nanocrystals α - Fe. Coating thickness is 33 μm, micro-hardness is 8461 - 11357 MPa, wear resistance is 0,55×104s/g. Coating ofnanocrystalline alloy of type 5БДCP can be used to increase wear resistance of machinery working surfaces.

Spark plasma sintering synthesis of porous nanocrystalline titanium alloys for biomedical applications.

PubMed

Nicula, R; Lüthen, F; Stir, M; Nebe, B; Burkel, E

2007-11-01

The reason for the extended use of titanium and its alloys as implant biomaterials stems from their lower elastic modulus, their superior biocompatibility and improved corrosion resistance compared to the more conventional stainless steel and cobalt-based alloys [Niinomi, M., Hattori, T., Niwa, S., 2004. Material characteristics and biocompatibility of low rigidity titanium alloys for biomedical applications. In: Jaszemski, M.J., Trantolo, D.J., Lewandrowski, K.U., Hasirci, V., Altobelli, D.E., Wise, D.L. (Eds.), Biomaterials in Orthopedics. Marcel Dekker Inc., New York, pp. 41-62]. Nanostructured titanium-based biomaterials with tailored porosity are important for cell-adhesion, viability, differentiation and growth. Newer technologies like foaming or low-density core processing were recently used for the surface modification of titanium alloy implant bodies to stimulate bone in-growth and improve osseointegration and cell-adhesion, which in turn play a key role in the acceptance of the implants. We here report preliminary results concerning the synthesis of mesoporous titanium alloy bodies by spark plasma sintering. Nanocrystalline cp Ti, Ti-6Al-4V, Ti-Al-V-Cr and Ti-Mn-V-Cr-Al alloy powders were prepared by high-energy wet-milling and sintered to either full-density (cp Ti, Ti-Al-V) or uniform porous (Ti-Al-V-Cr, Ti-Mn-V-Cr-Al) bulk specimens by field-assisted spark plasma sintering (FAST/SPS). Cellular interactions with the porous titanium alloy surfaces were tested with osteoblast-like human MG-63 cells. Cell morphology was investigated by scanning electron microscopy (SEM). The SEM analysis results were correlated with the alloy chemistry and the topographic features of the surface, namely porosity and roughness.

High spatial resolution PEELS characterization of FeAl nanograins prepared by mechanical alloying

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

Valdre, G.; Botton, G.A.; Brown, L.M.

The authors investigate the nanograin ``chemical`` structure in a nanostructured material of possible industrial application (Fe-Al system) prepared by conventional mechanical alloying via ball milling in argon atmosphere. They restrict themselves to the structural and nanochemical behavior of ball-milled nanocrystalline Fe-Al powders with atomic composition Fe{sub 3}Al, corresponding to a well-known intermetallic compound of the Fe-Al system. Scanning transmission electron microscopy (STEM) equipped with a parallel detection electron energy loss spectrometer (PEELS) has provided an insight on the ``chemical`` structure of both nanograins and their surface at a spatial resolution of better than 1 nm. The energy loss near edgemore » structure of the Al L loss reveals that the Al coordination is similar to a B2 compound and the oxidation of the powder during processing may play a significant role in the stabilization of the intermetallic phases. Conventional transmission electron microscopy (TEM) was used for the structural characterization of the material after the ball milling; powder X-ray diffraction (XRD) aided the investigation.« less

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.

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.

Nanophase hydroxyapatite coatings for dental and orthopedic applications

NASA Astrophysics Data System (ADS)

Sato, Michiko

In order to improve dental and orthopedic implant performance, the objective of this study was to synthesize nanocrystalline hydroxyapatite (HA) powders to coat metals (specifically, titanium and tantalum). Precipitated HA powders were either sintered in order to produce UltraCaP HA (or microcrystalline size HA) or were treated hydrothermally to produce nanocrystalline HA. Some of the UltraCaP and nanocrystalline HA powders were doped with yttrium (Y) since previous in vitro studies demonstrated that Y-doped HA in bulk improved osteoblast (or bone-forming cell) function over undoped HA. The nanocrystalline HA powders were also mixed with nanophase titania powders because previous studies demonstrated that titania/HA composite coatings increased coating adhesive strength and HA nucleation. These powders were then deposited onto titanium by a novel room-temperature process, called IonTiteT(TM). The results demonstrated that the chemical properties and crystallite size of the original HA powders were maintained in the coatings. More importantly, in vitro studies showed increased osteoblast (bone-forming cell) adhesion on the single phase nanocrystalline HA and nano-titania/HA coatings compared to traditionally used plasma-sprayed HA coatings and uncoated metals. Results further demonstrated greater amounts of calcium deposition by osteoblasts cultured on nanocrystalline HA coatings compared to UltraCaP coatings and conventionally used plasma-sprayed HA coatings. To elucidate mechanisms that influenced osteoblast functions on the HA coatings, the amount of proteins (fibronectin and vitronectin) onto the HA powders and the adsorbed fibronectin conformation were investigated. Exposure of cell integrin binding domains (in fibronectin III10 segments) was greater in fibronectin adsorbed onto 1.2 mole% Y-doped UltraCaP HA coatings compared to nanocrystalline HA coatings tested. However, 1.2 mole% Y-doped UltraCaP HA coatings did not increase mineralization by osteoblasts compared to the nanocrystalline HA coatings. These results suggested that the availability of integrin binding domains in fibronectin did not correlate to enhanced mineralization by osteoblasts on nanocrystalline HA coatings. Lastly, undoped nanocrystalline HA coatings were studied using a well-established rat calvaria in vivo. Histological analysis showed that nanocrystalline HA coated on tantalum scaffolds increased bone and fibrous tissue infiltration into the scaffolds while uncoated and UltraCaP HA coated scaffolds did not after as early as 6 weeks. In summary, these results encourage further studies on nanocrystalline IonTiteTM HA coatings on various metals for orthopedic and dental applications.

Potential applications of cold sprayed Cu50Ti20Ni30 metallic glassy alloy powders for antibacterial protective coating in medical and food sectors.

PubMed

El-Eskandrany, M Sherif; Al-Azmi, Ahmed

2016-03-01

Mechanical alloying was utilized for synthesizing of metallic glassy Cu50Ti20Ni30 alloy powders, using a low energy ball milling technique. The metallic glassy powders obtained after 100 h of ball milling had an average particle size of 1.7 mm in diameter and possessed excellent thermal stability, indexed by a relatively high glass transition temperature (358.3 °C) with a wide supercooled liquid region (61 °C). This amorphous phase crystallized into Ti2Cu and CuTiNi2 ordered phases through two overlapped crystallization temperatures at 419.3 °C and 447.5 °C, respectively. The total enthalpy change of crystallization was -4.8 kJ/mol. The glassy powders were employed as feedstock materials to double-face coating the surface of SUS 304 substrate, using cold spraying process under helium gas pressure at 400 °C. This coating material had an extraordinary high nanohardness value of 3.1 GPa. Moreover, it showed a high resistance to wear with a low value of the coefficient of friction ranging from 0.45 to 0.45. Biofilms were grown on 20-mm(2) SUS304 sheets coated coupons inoculated with 1.5 × 10(8) CFU ml(-1)E. coli. Significant biofilm inhibition (p The inhibition of biofilm formation by nanocrystalline powders of Cu-based provides a practical approach to achieve the inhibition of biofilms formation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Ferromagnetic nanocomposites

NASA Astrophysics Data System (ADS)

Mazaleyrat, F.; Varga, L. K.

2000-06-01

A survey of magnetic nanocomposites applicable in high-frequency signal and power electronics is given. First, the preparation and properties of ribbon and powder cores from the nanocrystalline "bulk" alloys (Finemet and Nanoperm) is reviewed. A technology is presented to apply continuously a large stress during the annealing and winding of the rapidly quenched ribbons in order to induce uniaxial anisotropy in it. The obtained toroidal cores with flat hysteresis curve are applicable up to 1 MHz with considerable permeability (˜250). The powder cores prepared from ground Finemet with powder size of 30-400 μm are applicable up to 1 MHz and in some cases up to 10 MHz for smaller powder sizes with low permeability (˜10). Finally, the most common methods used for the preparation of metallic nano-particle s are presented. Presently, the compacts prepared from nano-size (40-80 nm) iron powders do not show the expected behavior. It is anticipated that the iron-based ferromagnetic nanocomposites should replace partly the ferrite-type materials in the forthcoming years.

"Bulk" Nanocrystalline Metals: Review of the Current State of the Art and Future Opportunities for Copper and Copper Alloys

NASA Astrophysics Data System (ADS)

Tschopp, M. A.; Murdoch, H. A.; Kecskes, L. J.; Darling, K. A.

2014-06-01

It is a new beginning for innovative fundamental and applied science in nanocrystalline materials. Many of the processing and consolidation challenges that have haunted nanocrystalline materials are now more fully understood, opening the doors for bulk nanocrystalline materials and parts to be produced. While challenges remain, recent advances in experimental, computational, and theoretical capability have allowed for bulk specimens that have heretofore been pursued only on a limited basis. This article discusses the methodology for synthesis and consolidation of bulk nanocrystalline materials using mechanical alloying, the alloy development and synthesis process for stabilizing these materials at elevated temperatures, and the physical and mechanical properties of nanocrystalline materials with a focus throughout on nanocrystalline copper and a nanocrystalline Cu-Ta system, consolidated via equal channel angular extrusion, with properties rivaling that of nanocrystalline pure Ta. Moreover, modeling and simulation approaches as well as experimental results for grain growth, grain boundary processes, and deformation mechanisms in nanocrystalline copper are briefly reviewed and discussed. Integrating experiments and computational materials science for synthesizing bulk nanocrystalline materials can bring about the next generation of ultrahigh strength materials for defense and energy applications.

Production of nanocrystalline metal powders via combustion reaction synthesis

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

Frye, John G.; Weil, Kenneth Scott; Lavender, Curt A.

Nanocrystalline metal powders comprising tungsten, molybdenum, rhenium and/or niobium can be synthesized using a combustion reaction. Methods for synthesizing the nanocrystalline metal powders are characterized by forming a combustion synthesis solution by dissolving in water an oxidizer, a fuel, and a base-soluble, ammonium precursor of tungsten, molybdenum, rhenium, or niobium in amounts that yield a stoichiometric burn when combusted. The combustion synthesis solution is then heated to a temperature sufficient to substantially remove water and to initiate a self-sustaining combustion reaction. The resulting powder can be subsequently reduced to metal form by heating in a reducing gas environment.

Structural and magnetic correlation of Finemet alloys with Ge addition

NASA Astrophysics Data System (ADS)

Muraca, D.; Cremaschi, V.; Moya, J.; Sirkin, H.

The correlation between saturation magnetization and the magnetic moment per Fe atom in the nanocrystalline state is studied for Finemet-type alloys. These studies were performed on nanocrystalline ribbons whose compositions were Fe 73.5Si 13.5-xGe xNb 3B 9Cu 1 ( x=8, 10 and 13.5 at%). We used a simple lineal model, X-ray diffraction and Mössbauer spectroscopy data to calculate the magnetic contribution of the nanocrystals and the results were contrasted with the measured saturation magnetization of the different alloys. The technique presented here provides a very simple and powerful tool to compute the magnetic contribution of the nanocrystalline phase to the alloy. This calculus could be used to determine the volume fraction of nanocrystalline and amorphous phases in the nanocrystallized alloy, without using a very sophisticated microscopy method.

Amorphous and nanocrystalline phase formation in highly-driven Al-based binary alloys

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

Kalay, Yunus Eren

2009-01-01

Remarkable advances have been made since rapid solidification was first introduced to the field of materials science and technology. New types of materials such as amorphous alloys and nanostructure materials have been developed as a result of rapid solidification techniques. While these advances are, in many respects, ground breaking, much remains to be discerned concerning the fundamental relationships that exist between a liquid and a rapidly solidified solid. The scope of the current dissertation involves an extensive set of experimental, analytical, and computational studies designed to increase the overall understanding of morphological selection, phase competition, and structural hierarchy that occursmore » under far-from equilibrium conditions. High pressure gas atomization and Cu-block melt-spinning are the two different rapid solidification techniques applied in this study. The research is mainly focused on Al-Si and Al-Sm alloy systems. Silicon and samarium produce different, yet favorable, systems for exploration when alloyed with aluminum under far-from equilibrium conditions. One of the main differences comes from the positions of their respective T 0 curves, which makes Al-Si a good candidate for solubility extension while the plunging T 0 line in Al-Sm promotes glass formation. The rapidly solidified gas-atomized Al-Si powders within a composition range of 15 to 50 wt% Si are examined using scanning and transmission electron microscopy. The non-equilibrium partitioning and morphological selection observed by examining powders at different size classes are described via a microstructure map. The interface velocities and the amount of undercooling present in the powders are estimated from measured eutectic spacings based on Jackson-Hunt (JH) and Trivedi-Magnin-Kurz (TMK) models, which permit a direct comparison of theoretical predictions. For an average particle size of 10 {micro}m with a Peclet number of ~0.2, JH and TMK deviate from each other. This deviation indicates an adiabatic type solidification path where heat of fusion is reabsorbed. It is interesting that this particle size range is also consistent with the appearance of a microcellular growth. While no glass formation is observed within this system, the smallest size powders appear to consist of a mixture of nanocrystalline Si and Al. Al-Sm alloys have been investigated within a composition range of 34 to 42 wt% Sm. Gas atomized powders of Al-Sm are investigated to explore the morphological and structural hierarchy that correlates with different degrees of departure from full equilibrium conditions. The resultant powders show a variety of structural selection with respect to amount of undercooling, with an amorphous structure appearing at the highest cooling rates. Because of the chaotic nature of gas atomization, Cu-block melt-spinning is used to produce a homogeneous amorphous structure. The as-quenched structure within Al-34 to 42 wt% Sm consists of nanocrystalline fcc-Al (on the order of 5 nm) embedded in an amorphous matrix. The nucleation density of fcc-Al after initial crystallization is on the order of 10 22-10 23m -3, which is 10 5-10 6 orders of magnitude higher than what classical nucleation theory predicts. Detailed analysis of liquid and as-quenched structures using high energy synchrotron X-ray diffraction, high energy transmission electron microscopy, and atom probe tomography techniques revealed an Al-Sm network similar in appearance to a medium range order (MRO) structure. A model whereby these MRO clusters promote the observed high nucleation density of fcc-Al nanocrystals is proposed. The devitrification path was identified using high temperature, in-situ, high energy synchrotron X-ray diffraction techniques and the crystallization kinetics were described using an analytical Johnson-Mehl-Avrami (JMA) approach.« less

Cryomilled Aluminum with Diamantane: Thermal Characterization by DSC and Effects of Magnesium

NASA Astrophysics Data System (ADS)

Arnold, Michael Colin

Many structural applications require a material that is both lightweight and corrosion resistant, for which aluminum and its alloys may be considered for use if not for their relatively low strength. By improving strength of aluminum through the Hall-Petch mechanism, it could become a more suitable choice for many structural applications. Cryomilling is used as a production technique to strengthen aluminum by reduction of grain size to the 20-50 nm range. Although the powders produced by cryomilling are well within the nanocrystalline regime, the powders experience significant grain growth during consolidation to a solid body. Cryomilled powders have been shown to remain nanocrystalline by introducing a nano-diamond, diamantane to the grain boundaries. To better characterize the thermal stability of the cryomilled powder with diamantane, Differential Scanning Calorimetry (DSC) was used to measure the isothermal heat flow in the 0.6Tm to 0.9Tm range. A model was developed to correlate the isothermal DSC signal to a grain growth curve and grain growth parameters were elucidated by assuming variable boundary mobility with a sigmoidal form. The model revealed a tendency for boundary mobility to transition from an athermal grain growth mechanism to standard thermally activated grain growth. Grain growth parameters were compared to shed light on possible mechanisms of aluminum-diamantane involvement during grain growth. Powders and consolidated samples with very low concentrations of diamantane and with magnesium were observed by TEM, SEM and XRD, and compared both separately and together to characterize the how thermal stability is affected by diamantane concentration and the presence of magnesium.

Structural Inheritance and Redox Performance of Nanoporous Electrodes from Nanocrystalline Fe85.2B10-14P0-4Cu0.8 Alloys

PubMed Central

Fu, Chaoqun; Xu, Lijun; Dan, Zhenhua; Makino, Akihiro; Hara, Nobuyoshi; Qin, Fengxiang; Chang, Hui

2017-01-01

Nanoporous electrodes have been fabricated by selectively dissolving the less noble α-Fe crystalline phase from nanocrystalline Fe85.2B14–xPxCu0.8 alloys (x= 0, 2, 4 at.%). The preferential dissolution is triggered by the weaker electrochemical stability of α-Fe nanocrystals than amorphous phase. The final nanoporous structure is mainly composed of amorphous residual phase and minor undissolved α-Fe crystals and can be predicted from initial microstructure of nanocrystalline precursor alloys. The structural inheritance is proved by the similarity of the size and outlines between nanopores formed after dealloying in 0.1 M H2SO4 and α-Fe nanocrystals precipitated after annealing of amorphous Fe85.2B14−xPxCu0.8 (x = 0, 2, 4 at.%) alloys. The Redox peak current density of the nanoporous electrodes obtained from nanocrystalline Fe85.2B10P4Cu0.8 alloys is more than one order higher than those of Fe plate electrode and its counterpart nanocrystalline alloys due to the large surface area and nearly-amorphous nature of ligaments. PMID:28594378

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

Prosviryakov, A.S., E-mail: pro.alex@mail.ru; Shch

Ground chips of as-cast Al-10 wt.% Zr alloy were subjected to mechanical alloying (MA) with 5 vol.% of nanodiamond addition in a high energy planetary ball-mill. The aim of this work was to investigate the microstructure, phase transformation and mechanical properties of the material both after MA and after subsequent annealing. Optical and transmission electron microscopes were used for morphological and microstructural analysis. The effect of milling time on powder microhardness, Al lattice parameter, lattice microstrain and crystallite size was determined. It was shown that mechanical alloying of as-cast Al-10wt.%Zr alloy during 20 h leads to a complete dissolution ofmore » the primary tetragonal Al{sub 3}Zr crystals in aluminum. At the same time, the powder microhardness increases to 370 HV. Metastable cubic Al{sub 3}Zr phase nanoparticles precipitate from the Al solution due to its decomposition after annealing, however, the Al solid solution remains supersaturated and nanocrystalline. Compression tests at room temperature and at 300 °C showed that the strength values of the hot-pressed samples reach 822 MPa and 344 MPa, respectively. - Highlights: •As-cast Al-10 wt.% Zr alloy was mechanically alloyed with 5 vol.% nanodiamond. •The primary tetragonal Al{sub 3}Zr crystals were completely dissolved in Al after 20 h. •Cubic Al{sub 3}Zr phase nanoparticles precipitated from Al solution after aging. •The aged bulk material showed a high strength at room and elevated temperatures.« 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 and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.

Structural and magnetic properties of new uniaxial nanocrystalline Pr5Co19 compound

NASA Astrophysics Data System (ADS)

Bouzidi, W.; Mliki, N.; Bessais, L.

2017-11-01

Highly-coercive nanocrystalline Pr5Co19 powders have been synthesized by mechanical milling for the first time. The structural properties are studied by X-ray diffraction and refined with Rietveld method. This analysis revealed that whatever annealing temperature, samples crystallize in the rhombohedral (3R) of Ce5Co19-type structure (space group R 3 bar m). The magnetization curve as a function of temperature shows a magnetic transition state at the Curie temperature TC = 690 K. The optimum hard magnetic properties have been obtained for Pr5Co19 milled for 5 h and annealed at 1048 K for 30 min. These alloys exhibit a coercivity of 15 kOe at room temperature. This high coercivity is attributed to the high uniaxial magnetocrystalline anisotropy, nanoscale grain size, and to the homogeneous nanostructure developed by mechanical milling process and subsequent annealing.

The Influence of Milling and Spark Plasma Sintering on the Microstructure and Properties of the Al7075 Alloy

PubMed Central

Málek, Přemysl; Minárik, Peter; Novák, Pavel; Průša, Filip

2018-01-01

The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al)2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS) resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm) with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C. PMID:29614046

Surface Properties of a Nanocrystalline Fe-Ni-Nb-B Alloy After Neutron Irradiation

NASA Astrophysics Data System (ADS)

Pavùk, Milan; Sitek, Jozef; Sedlačková, Katarína

2014-09-01

The effect of neutron radiation on the surface properties of the nanocrystalline (Fe0.25Ni0.75)81Nb7B12 alloy was studied. Firstly, amorphous (Fe0.25Ni0.75)81Nb7B12 ribbon was brought by controlled annealing to the nanocrystalline state. After annealing, the samples of the nanocrystalline ribbon were irradiated in a nuclear reactor with neutron fluences of 1×1016cm-2 and 1 × 1017cm-2 . By utilizing the magnetic force microscopy (MFM), topography and a magnetic domain structure were recorded at the surface of the ribbon-shaped samples before and after irradiation with neutrons. The results indicate that in terms of surface the nanocrystalline (Fe0.25Ni0.75)81Nb7B12 alloy is radiation-resistant up to a neutron fluence of 1 × 1017cm-2 . The changes in topography observed for both irradiated samples are discussed

Structural characterization of nanocrystalline cadmium sulphide powder prepared by solvent evaporation technique

NASA Astrophysics Data System (ADS)

Pandya, Samir; Tandel, Digisha; Chodavadiya, Nisarg

2018-05-01

CdS is one of the most important compounds in the II-VI group of semiconductor. There are numerous applications of CdS in the form of nanoparticles and nanocrystalline. Semiconductors nanoparticles (also known as quantum dots), belong to state of matter in the transition region between molecules and solids, have attracted a great deal of attention because of their unique electrical and optical properties, compared to bulk materials. In the field of optoelectronic, nanocrystalline form utilizes mostly in the field of catalysis and fluid technology. Considering these observations, presented work had been carried out, i.e. based on the nanocrystalline material preparation. In the present work CdS nano-crystalline powder was synthesized by a simple and cost effective chemical technique to grow cadmium sulphide (CdS) nanoparticles at 200 °C with different concentrations of cadmium. The synthesis parameters were optimized. The synthesized powder was structurally characterized by X-ray diffraction and particle size analyzer. In the XRD analysis, Micro-structural parameters such as lattice strain, dislocation density and crystallite size were analysed. The broadened diffraction peaks indicated nanocrystalline particles of the film material. In addition to that the size of the prepared particles was analyzed by particle size analyzer. The results show the average size of CdS particles ranging from 80 to 100 nm. The overall conclusion of the work can be very useful in the synthesis of nanocrystalline CdS powder.

Investigating the Thermal and Phase Stability of Nanocrystalline Ni-W Produced by Electrodeposition, Sputtering, and Mechanical Alloying

NASA Astrophysics Data System (ADS)

Marvel, Christopher Jonathan

The development of nanocrystalline materials has been increasingly pursued over the last few decades. They have been shown to exhibit superior properties compared to their coarse-grain counterparts, and thus present a tremendous opportunity to revolutionize the performance of nanoscale devices or bulk structural materials. However, nanocrystalline materials are highly prone to grain growth, and if the nanocrystalline grains coarsen, the beneficial properties are lost. There is a strong effort to determine the most effective thermal stability mechanisms to avoid grain growth, but the physical nature of nanocrystalline grain growth is still unclear due to a lack of detailed understanding of nanocrystalline microstructures. Furthermore, the influence of contamination has scarcely been explored with advanced transmission electron microscopy techniques, nor has there been a direct comparison of alloys fabricated with different bulk processes. Therefore, this research has applied aberration-corrected scanning transmission electron microscopy to characterize nanocrystalline Ni-W on the atomic scale and elucidate the physical grain growth behavior. Three primary objectives were pursued: (1) explore the thermal stability mechanisms of nanocrystalline Ni-W, (2) evaluate the phase stability of Ni-W and link any findings to grain growth behavior, and (3) compare the influences of bulk fabrication processing, including electrodeposition, DC magnetron sputtering, and mechanical alloying, on the thermal stability and phase stability of Ni-W. Several thermal stability mechanisms were identified throughout the course of this research. First and foremost, W-segregation was scarcely observed to grain boundaries, and it is unclear if W-segregation improves thermal stability contrary to most reports in the 2 literature. Long-range Ni4W chemical ordering was observed in alloys with more than 20 at.% W, and it is likely Ni4W domains reduce grain boundary mobility. In addition, lattice diffusivity calculations conceptually suggested that increasing W alloying concentrations can decrease the grain growth rate. The strongest evidence of grain growth stagnation was via nanoscale oxide particle drag in highly contaminated electrodeposited alloys. Interestingly, W-segregation was also detected to the oxide phase boundaries and revealed a potential indirect mechanism of thermal stability. The phase stability of pure and contaminated Ni-W alloys was investigated with density functional theory. Primarily, the calculations suggested that the intermetallic phases NiW and NiW2 are thermodynamically unstable, meaning the binary phase diagram is incorrect, but the ternary carbides Ni 6W6C and Ni2W4C are stable. Several Ni-W binary and Ni-W-C ternary phase diagrams were constructed using a simplified CALPHAD approach to improve the understanding of Ni-W phase stability. Lastly, it was determined that the fabrication process greatly influences the impurity types and concentrations of the alloys, and therefore greatly dictate which thermal stability mechanisms are active. Mechanically alloyed samples were found to be the most resistant to grain growth. The findings of this research will hopefully guide future efforts to design more thermally stable nanocrystalline alloys. The link between phase stability and grain growth behavior of Ni-W was thoroughly discussed, as well as the dependence of bulk fabrication processing on the contamination found in the alloys. Ultimately, this research has greatly expanded the general understanding of nanocrystalline Ni-W microstructures, and it is likely that similar phenomena occur in other nanocrystalline systems.

Behavior and Microstructure in Cryomilled Aluminum alloy Containing Diamondoids Nanoparticles

NASA Astrophysics Data System (ADS)

Hanna, Walid Magdy

Aluminum (Al) alloys have been the materials of choice for both civil and military aircraft structure. Primary among these alloys are 6061 Al and 5083 Al, which have used for several structural applications including those in aerospace and automobile industry. It is desirable to enhance strength in Al alloys beyond that achieved via traditional techniques such as precipitation hardening. Recent developments have indicated strengthening via grain refinement is an effective approach since, according the Hall-Petch relation, as grain size decreases strength significantly increases. The innovate techniques of severe plastic deformation, cryomilling, are successful in reefing grain size. These techniques lead to a minimum grain size that is the result of a dynamic balance between the formation of dislocation structure and its recovery by thermal processes. According to Mohamed's model, each metal is characterized by a minimum grain size that is determined by materials parameters such as the stacking faulty energy and the activation energy for diffusion. In the present dissertation, 6061 Al and 5083 Al were synthesized using cryomilling. Microstructural characterization was extensively carried out to monitor grain size changes. A close examination of the morphology of the 6061 Al powder particles revealed that in the early milling stages, the majority of the particles changed from spheres to thin disk-shaped particles. This change was attributed to the high degree of plastic deformation generated by the impact energy during ball-powder-ball collisions. Both transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to monitor the change in grain size as a function of milling time. The results of both techniques demonstrated a close agreement with respect to two observations: (a) during cryomilling, the grain size of 6061 Al decreased with milling time, and (b) after 15 h of milling, the grain size approached a minimum value of about 22 nm, which is in the range reported for Al (18 nm--24 nm). Despite this agreement, there was a discrepancy: for grain sizes > 40 nm, the grain size measured by TEM was appreciably larger that inferred from XRD. It was suggested that this discrepancy was most likely related to the limitation for accurately measuring grain sizes > 100 nm by the technique of XRD. It was reported that the average grain size of the as-milled powders of 5083 Al alloy was about 20 nm, and that when the as-milled powders were exposed to elevated temperatures or consolidated via hot isostatic pressing and extruded, the average grain size increased to about 250 nm. Very recent results have indicated the success of maintaining the thermal stability of Al by adding diamantane during milling. 5083 Al powders were cryomilled with 0.5 wt. % diamantane for 8 hours producing mechanically alloyed powders with an average grain size of 17 nm. The grain size remained nanocrystalline (less than100 nm) for Al 5083 alloy with 0.5% diamantane, even after 48 h at the highest temperature of 773 K. The Effect of Diamantane on the thermal stability of cryomilled nanocrystalline 5083 Al alloy was investigated by heating the powder in an inert gas atmosphere at temperature range from 473K to 773K for time interval between 0.5 hr. to 48 hr. The average grain size was observed to be in nano scale range less than 100 nm. The thermal stability results were found to be consistent with the grain growth model based on drag forces exerted by dispersed particles against grain boundary migration (Burke model). As observed for other cryomilled Al alloys, two grain growth regimes were identified using this model: one at relatively low temperatures (473--623 K) where the activation energy is about 1.9 kJ/mole and another at higher temperatures where the activation energy is about 18 kJ/mole. The presence of the former region was explained in terms of stress relaxation facilitated by less stable processes such as recovery of dislocation segments or sub-boundary remnants while the latter region was attributed to grain boundary realignment annihilation of grain boundary remnants.

Thermally Stable Nanocrystalline Steel

NASA Astrophysics Data System (ADS)

Hulme-Smith, Christopher Neil; Ooi, Shgh Woei; Bhadeshia, Harshad K. D. H.

2017-10-01

Two novel nanocrystalline steels were designed to withstand elevated temperatures without catastrophic microstructural changes. In the most successful alloy, a large quantity of nickel was added to stabilize austenite and allow a reduction in the carbon content. A 50 kg cast of the novel alloy was produced and used to verify the formation of nanocrystalline bainite. Synchrotron X-ray diffractometry using in situ heating showed that austenite was able to survive more than 1 hour at 773 K (500 °C) and subsequent cooling to ambient temperature. This is the first reported nanocrystalline steel with high-temperature capability.

Study of distribution of Carbon nanotube in Al-CNT nanocomposite synthesized via Spark-Plasma sintering

NASA Astrophysics Data System (ADS)

Maiti, A.; Laha, T.

2018-03-01

In the present study, first ever attempt has been made to develop physically functionalized multiwalled carbon nanotube (MWCNT) reinforced Al-11 5Si alloy nanocomposites synthesized via novel consolidation technique viz spark plasma sintering (SPS). There is a recent trend in employing carbon nanotubes (CNTs), an allotrope of carbon, as reinforcement for high strength structural metallic composite materials, as these cylindrical nano-fibers poses extremely unique mechanical properties such as very high elastic modulus (~ 300 GPa to 1.5 TPa) as well as tensile strength (~150 GPa). However, it has remained as an ever-existing problem to achieve a porosity-free nanocrystalline matrix with homogenously dispersed CNTs, owing to the very high coagulation tendency of CNTs. The gas-atomized, spherical Al-11.5Si alloy powders (1-8 μm) were subjected to high energy ball milling for the purpose of achieving nanocrystallinity in the powders. The improvement in MWCNT dispersion was effort by treating the MWCNTs with a physical surfactant, sodium dodecyl sulfate (SDS). The nano-grained ball-milled Al-Si powders with varying MWCNT content (0.5 and 1 wt%) were consolidated via spark plasma sintering in order to retain the nano-sized grains in the Al-Si matrix, attributed to the faster and highly effective sintering kinetics of the sintering techniques. FESEM study shows problem of MWCNT agglomeration persists by addition of non-SDS treated as pristine MWCNT in the composite. After treated with SDS, MWCNTs are well separated out from each other and as a result of that good morphological and mechanical property such as high hardness value obtained after analysis. Detailed TEM study of the 0.5wt% MWCNT reinforced SPS nanocomposite revealed that the distribution of CNTs in the matrix. Mechanical analysis study of the nanocomposite attributes higher hardness in case of SDS treated CNT reinforced nanocomposite owing to less agglomeration problem of the CNT in the matrix. Nano-tribological data attributed variation of surface roughness after consolidated by SPS.

Oxidation resistant nanocrystalline MCrAl(Y) coatings and methods of forming such coatings

DOEpatents

Cheruvu, Narayana S.; Wei, Ronghua

2014-07-29

The present disclosure relates to an oxidation resistant nanocrystalline coating and a method of forming an oxidation resistant nanocrystalline coating. An oxidation resistant coating comprising an MCrAl(Y) alloy may be deposited on a substrate, wherein M, includes iron, nickel, cobalt, or combinations thereof present greater than 50 wt % of the MCrAl(Y) alloy, chromium is present in the range of 15 wt % to 30 wt % of the MCrAl(Y) alloy, aluminum is present in the range of 6 wt % to 12 wt % of the MCrAl(Y) alloy and yttrium, is optionally present in the range of 0.1 wt % to 0.5 wt % of the MCrAl(Y) alloy. In addition, the coating may exhibit a grain size of 200 nm or less as deposited.

Stability of nanocrystalline Ni-based alloys: coupling Monte Carlo and molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Waseda, O.; Goldenstein, H.; Silva, G. F. B. Lenz e.; Neiva, A.; Chantrenne, P.; Morthomas, J.; Perez, M.; Becquart, C. S.; Veiga, R. G. A.

2017-10-01

The thermal stability of nanocrystalline Ni due to small additions of Mo or W (up to 1 at%) was investigated in computer simulations by means of a combined Monte Carlo (MC)/molecular dynamics (MD) two-steps approach. In the first step, energy-biased on-lattice MC revealed segregation of the alloying elements to grain boundaries. However, the condition for the thermodynamic stability of these nanocrystalline Ni alloys (zero grain boundary energy) was not fulfilled. Subsequently, MD simulations were carried out for up to 0.5 μs at 1000 K. At this temperature, grain growth was hindered for minimum global concentrations of 0.5 at% W and 0.7 at% Mo, thus preserving most of the nanocrystalline structure. This is in clear contrast to a pure Ni model system, for which the transformation into a monocrystal was observed in MD simulations within 0.2 μs at the same temperature. These results suggest that grain boundary segregation of low-soluble alloying elements in low-alloyed systems can produce high-temperature metastable nanocrystalline materials. MD simulations carried out at 1200 K for 1 at% Mo/W showed significant grain boundary migration accompanied by some degree of solute diffusion, thus providing additional evidence that solute drag mostly contributed to the nanostructure stability observed at lower temperature.

Preparation of Nanocrystalline Powders of ZrO2, Stabilized by Y2O3 Dobs for Ceramics

NASA Astrophysics Data System (ADS)

Petrunin, V. F.; Korovin, S. A.

The purpose of this study was to develop a synthesis conditions and produce samples of nanocrystalline zirconia powder in a high-temperature phase state. To increase the stability of this state at room temperature, Y2O3 was used as a dop in the two-stages chemical method including coprecipitation mixture of the corresponding hydroxides and air drying. To reduce agglomeration of nanoparticles during heat treatment of precursors the microwave oven instead of a muffle was used. Different characterisation methods have been used to determine that the obtained powders are nano-scale corresponds to a high-temperature tetragonal phase of ZrO2. It is shown that such nanocrystalline powders may be used to produce highly-dense nanoceramics.

Production of Nanocrystalline Ni-20Cr Coatings for High-Temperature Applications

NASA Astrophysics Data System (ADS)

Kumar, Manoj; Singh, Harpreet; Singh, Narinder

2014-04-01

Presynthesized nanocrystalline Ni-20Cr powder was deposited on SA 516 and T91 boiler steels by a high-velocity oxy-fuel spraying process. Ni-20Cr powder was synthesized by the ball milling approach. The high-temperature oxidation behavior of bare and coated samples was then studied under cyclic isothermal conditions at 900 °C for 50 cycles. The kinetics of oxidation was established using weight change measurements for the bare and coated boiler steels. Uncoated and coated samples of T91 steel were exposed to the superheated zone of a power plant boiler at 750 °C under cyclic conditions for 15 cycles. Each cycle consisted of 100 h of heating followed by 1 h of cooling. Attempts were made to study the kinetics of erosion-corrosion using weight change and thickness loss data for the samples. Different characterization techniques were used to study the oxidized and eroded-corroded samples, including x-ray diffraction, scanning electron microscopy/energy-dispersive spectroscopy, and x-ray mapping analyses. The Ni-20Cr alloy powder coating was found to offer excellent oxidation resistance to the base steels and was successful in reducing the weight gain of SA 516 steel by 98.5 % and that of T91 steel by 65 %. The coating was observed to reduce the erosion-corrosion rate of T91 steel by 86 % in terms of thickness loss. This indicates that the investigated nanostructured coating can be a better choice over conventional coating for erosion-corrosion control of boiler tubes.

Extreme creep resistance in a microstructurally stable nanocrystalline alloy

NASA Astrophysics Data System (ADS)

Darling, K. A.; Rajagopalan, M.; Komarasamy, M.; Bhatia, M. A.; Hornbuckle, B. C.; Mishra, R. S.; Solanki, K. N.

2016-09-01

Nanocrystalline metals, with a mean grain size of less than 100 nanometres, have greater room-temperature strength than their coarse-grained equivalents, in part owing to a large reduction in grain size. However, this high strength generally comes with substantial losses in other mechanical properties, such as creep resistance, which limits their practical utility; for example, creep rates in nanocrystalline copper are about four orders of magnitude higher than those in typical coarse-grained copper. The degradation of creep resistance in nanocrystalline materials is in part due to an increase in the volume fraction of grain boundaries, which lack long-range crystalline order and lead to processes such as diffusional creep, sliding and rotation. Here we show that nanocrystalline copper-tantalum alloys possess an unprecedented combination of properties: high strength combined with extremely high-temperature creep resistance, while maintaining mechanical and thermal stability. Precursory work on this family of immiscible alloys has previously highlighted their thermo-mechanical stability and strength, which has motivated their study under more extreme conditions, such as creep. We find a steady-state creep rate of less than 10-6 per second—six to eight orders of magnitude lower than most nanocrystalline metals—at various temperatures between 0.5 and 0.64 times the melting temperature of the matrix (1,356 kelvin) under an applied stress ranging from 0.85 per cent to 1.2 per cent of the shear modulus. The unusual combination of properties in our nanocrystalline alloy is achieved via a processing route that creates distinct nanoclusters of atoms that pin grain boundaries within the alloy. This pinning improves the kinetic stability of the grains by increasing the energy barrier for grain-boundary sliding and rotation and by inhibiting grain coarsening, under extremely long-term creep conditions. Our processing approach should enable the development of microstructurally stable structural alloys with high strength and creep resistance for various high-temperature applications, including in the aerospace, naval, civilian infrastructure and energy sectors.

A sol-powder coating technique for fabrication of yttria stabilised zirconia

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

Wattanasiriwech, Darunee; Wattanasiriwech, Suthee; Stevens, Ron

Yttria stabilised zirconia has been prepared using a simple sol-powder coating technique. The polymeric yttria sol, which was prepared using 1,3 propanediol as a network modifier, was homogeneously mixed with nanocrystalline zirconia powder and it showed a dual function: as a binder which promoted densification and a phase modifier which stabilised zirconia in the tetragonal and cubic phases. Thermal analysis and X-ray diffraction revealed that the polymeric yttria sol which decomposed at low temperature into yttrium oxide could change the m {sup {yields}} t phase transformation behaviour of the zirconia, possibly due to the small particle size and very highmore » surface area of both yttria and zirconia particles allowing rapid alloying. The sintered samples exhibited three crystalline phases: monoclinic, tetragonal and cubic, in which cubic and tetragonal are the major phases. The weight fractions of the individual phases present in the selected specimens were determined using quantitative Rietveld analysis.« less

Synthesis and mechanical/magnetic properties of nano-grained iron-oxides prepared with an inert gas condensation and pulse electric current sintering process

NASA Astrophysics Data System (ADS)

Choa, Yong-Ho; Nakayama, Tatachika; Sekino, Tohru; Niihara, Koichi

1999-04-01

Nanocrystalline iron-oxide powder was fabricated with an inert gas condensation (IGC) method combined with evaporation, and in-situ oxidation techniques. The particle size of iron-oxide powder was controlled by varying the helium gas pressure between 0.1 and 10 Torr, with the smallest one =10 nm at 0.1 Torr. The nanostructure was characterized by TEM. Nanocrystalline iron-oxide powder was sintered with the pulse electric current sintering (PECS) method to obtain densified γ-Fe2O3 materials, and suitably densified nano-grained γ-Fe2O3 materials (≈ 40 nm) of great hardness were obtained. The correlation between the nanostructure and magnetic properties of nanocrystalline powder and densified γ-Fe2O3 materials was also investigated.

Analysis of Short and Long Range Atomic Order in Nanocrystalline Diamonds with Application of Powder Diffractometry

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Neuefiend, J.; Weber, H.-P.; Proffen, T.; VonDreele, R.; Palosz, W.;

Effects of F-treatment on degradation of Mg 2Ni electrode fabricated by mechanical alloying

NASA Astrophysics Data System (ADS)

Kim, Jun Sung; Lee, Chang Rae; Choi, Jae Woong; Kang, Sung Goon

The effects of surface fluorination on the electrochemical charge-discharge properties of a Mg 2Ni electrode, prepared by mechanical alloying in Ni-MH batteries are investigated. After 20 h milling, Mg and Ni powder form nanocrystalline Mg 2Ni. The discharge capacity of this alloy increases greatly on the initial cycle but, due to the formation of a Mg(OH) 2 passive layer, displays rapid degradation in alkaline solution within 10 cycles. In a 6 M KOH+ x M KF electrolyte ( x=0.5, 1, and 2), a continuous and stable fluorinated layer is formed and the durability of the Mg 2Ni electrode increases marketly and a high rate discharge capability is obtained (90-100 mAh/g). Addition of 2 M KF leads to the highest durability of all the electrodes tested. The improvement is due to a thin MgF 2—flourinated layer, which reduces the charge-transfer resistance and protects the Mg 2Ni electrode from forming a Mg(OH) 2 layer.

On the Formation of Lightweight Nanocrystalline Aluminum Alloys by Electrodeposition

DOE PAGES

Hilty, Robert D.; Masur, Lawrence J.

2017-08-08

New nanocrystalline aluminum alloys have been fabricated by electrodeposition. These are thermodynamically stable alloys of Al-Mn and Al-Zr with grain sizes < 100nm. Al-Mn and Al-Zr alloys are characterized here showing high strength (up to 1350 MPa) and hardness (up to 450 HVN) while maintaining the specific gravity of Al. Smooth and dense deposits plated from ionic liquids, such as EMIM:Cl (1-Ethyl-3-methylimidazolium chloride), can develop to thicknesses of 1mm or more.

X-ray peak broadening analysis of AA 6061{sub 100-x} - x wt.% Al{sub 2}O{sub 3} nanocomposite prepared by mechanical alloying

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

Sivasankaran, S., E-mail: sivasankarangs1979@gmail.com; Sivaprasad, K., E-mail: ksp@nitt.edu; Narayanasamy, R., E-mail: narayan@nitt.edu

2011-07-15

Nanocrystalline AA 6061 alloy reinforced with alumina (0, 4, 8, and 12 wt.%) in amorphized state composite powder was synthesized by mechanical alloying and consolidated by conventional powder metallurgy route. The as-milled and as-sintered (573 K and 673 K) nanocomposites were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The peaks corresponding to fine alumina was not observed by XRD patterns due to amorphization. Using high-resolution transmission electron microscope, it is confirmed that the presence of amorphized alumina observed in Al lattice fringes. The crystallite size, lattice strain, deformation stress, and strain energy density of AA 6061 matrixmore » were determined precisely from the first five most intensive reflection of XRD using simple Williamson-Hall models; uniform deformation model, uniform stress deformation model, and uniform energy density deformation model. Among the developed models, uniform energy density deformation model was observed to be the best fit and realistic model for mechanically alloyed powders. This model evidenced the more anisotropic nature of the ball milled powders. The XRD peaks of as-milled powder samples demonstrated a considerable broadening with percentage of reinforcement due to grain refinement and lattice distortions during same milling time (40 h). The as-sintered (673 K) unreinforced AA 6061 matrix crystallite size from well fitted uniform energy density deformation model was 98 nm. The as-milled and as-sintered (673 K) nanocrystallite matrix sizes for 12 wt.% Al{sub 2}O{sub 3} well fitted by uniform energy density deformation model were 38 nm and 77 nm respectively, which indicate that the fine Al{sub 2}O{sub 3} pinned the matrix grain boundary and prevented the grain growth during sintering. Finally, the lattice parameter of Al matrix in as-milled and as-sintered conditions was also investigated in this paper. Research highlights: {yields} Integral breadth methods using various Williamson-Hall models were investigated for line profile analysis. {yields} Uniform energy density deformation model is observed to the best realistic model. {yields} The present analysis is used for understanding the stress and the strain present in the nanocomposites.« less

Synthesis, characterization and magnetic properties of nanocrystalline FexNi80-xCo20 ternary alloys

NASA Astrophysics Data System (ADS)

Dalavi, Shankar B.; Theerthagiri, J.; Raja, M. Manivel; Panda, R. N.

2013-10-01

Fe-Ni-Co alloys of various compositions (FexNi80-xCo20,x=20-50) were synthesized by using a sodium borohydride reduction route. The phase purity and crystallite size was ascertained by using powder X-ray diffraction (XRD). The alloys crystallize in the face centered cubic (fcc) structure with lattice parameters, a=3.546-3.558 Å. The XRD line broadening indicates the fine particle nature of the materials. The estimated crystallite sizes were found to be 27.5, 27, 24, and 22.8 nm for x=20, 30, 40, and 50; alloys respectively. Scanning electron micrograph studies indicates particle sizes to be in the range of 83-60 nm for Fe-Ni-Co alloys. The values of saturation magnetization for FexNi80-xCo20 are found to be in the range of 54.3-41.2 emu/g and are significantly lower than the bulk values (175-180 emu/g). The coercivity decreases from 170 to 122 Oe with decrease in Fe content. The observed magnetic behavior has been explained on the basis of size, surface effects, spin canting and the presence of superparamagnetic fractions in the ultrafine materials.

Nanocrystalline Aluminum Truss Cores for Lightweight Sandwich Structures

NASA Astrophysics Data System (ADS)

Schaedler, Tobias A.; Chan, Lisa J.; Clough, Eric C.; Stilke, Morgan A.; Hundley, Jacob M.; Masur, Lawrence J.

2017-12-01

Substitution of conventional honeycomb composite sandwich structures with lighter alternatives has the potential to reduce the mass of future vehicles. Here we demonstrate nanocrystalline aluminum-manganese truss cores that achieve 2-4 times higher strength than aluminum alloy 5056 honeycombs of the same density. The scalable fabrication approach starts with additive manufacturing of polymer templates, followed by electrodeposition of nanocrystalline Al-Mn alloy, removal of the polymer, and facesheet integration. This facilitates curved and net-shaped sandwich structures, as well as co-curing of the facesheets, which eliminates the need for extra adhesive. The nanocrystalline Al-Mn alloy thin-film material exhibits high strength and ductility and can be converted into a three-dimensional hollow truss structure with this approach. Ultra-lightweight sandwich structures are of interest for a range of applications in aerospace, such as fairings, wings, and flaps, as well as for the automotive and sports industries.

Gigacycle fatigue behavior by ultrasonic nanocrystalline surface modification.

PubMed

Ahn, D G; Amanov, A; Cho, I S; Shin, K S; Pyoun, Y S; Lee, C S; Park, I G

2012-07-01

Nanocrystalline surface layer up to 84 microm in thick is produced on a specimen made of Al6061-T6 alloy by means of surface treatment called ultrasonic nanocrystalline surface modification (UNSM) technique. The refined grain size is produced in the top-layer and it is increased with increasing depth from the top surface. Vickers microhardness measurement for each nanocrystalline surface layer is performed and measurement results showed that the microhardness is increased from 116 HV up to 150 HV, respectively. In this study, fatigue behavior of Al6061-T6 alloy was studied up to 10(7)-10(9) cycles by using a newly developed ultrasonic fatigue testing (UFT) rig. The fatigue results of the UNSM-treated Al6061-T6 alloy specimens were compared with those of the untreated specimens. The microstructure of the untreated and UNSM-treated specimens was characterized by means of scanning electron microscopey (SEM) and transmission electron microscopey (TEM).

Microstructural studies of nanocrystalline α-alumina powder produced from Al13-cluster

NASA Astrophysics Data System (ADS)

Harun Al Rashid Megat Ahmad, Megat; Aziz Mohamed, Abdul; Ibrahim, Azmi; Seman Mahmood, Che; Giri Rachman Putra, Edy; Jamro, Rafhayudi; Kasim, Razali; Rawi Muhammad Zin, Muhammad

2007-12-01

Nanocrystalline alumina powder was produced from calcinations of Al13-oxalate precipitates at 1100 °C. A nearly normal distribution of agglomerated alumina powder was obtained with an average particle size of about 1 μm. XRD measurement confirmed that the alumina produced was of high purity and crystalline α-phase. Microstructural features of both the precipitates and alumina obtained were studied using the small angle neutron scattering (SANS) technique. SANS examinations show the formation of microstructures in the alumina powder of mass fractals type with dimension of ˜2.8 indicative of low intra-granular porosity.

Iron-rich (Fe1-x-yNixCoy)88Zr7B4Cu1 nanocrystalline magnetic materials for high temperature applications with minimal magnetostriction

NASA Astrophysics Data System (ADS)

Martone, Anthony; Dong, Bowen; Lan, Song; Willard, Matthew A.

2018-05-01

As inductor technology advances, greater efficiency and smaller components demand new core materials. With recent developments of nanocrystalline magnetic materials, soft magnetic properties of these cores can be greatly improved. FeCo-based nanocrystalline magnetic alloys have resulted in good soft magnetic properties and high Curie temperatures; however, magnetoelastic anisotropies persist as a main source of losses. This investigation focuses on the design of a new Fe-based (Fe,Ni,Co)88Zr7B4Cu1 alloy with reduced magnetostriction and potential for operation at elevated temperatures. The alloys have been processed by arc melting, melt spinning, and annealing in a protective atmosphere to produce nanocrystalline ribbons. These ribbons have been analyzed for structure, hysteresis, and magnetostriction using X-Ray diffraction, vibrating sample magnetometry (VSM), and a home-built magnetostriction system, respectively. In addition, Curie temperatures of the amorphous phase were analyzed to determine the best performing, high-temperature material. Our best result was found for a Fe77Ni8.25Co2.75Zr7B4Cu1 alloy with a 12 nm average crystallite size (determined from Scherrer broadening) and a 2.873 Å lattice parameter determined from the Nelson-Riley function. This nanocrystalline alloy possesses a coercivity of 10 A/m, magnetostrictive coefficient of 4.8 ppm, and amorphous phase Curie temperature of 218°C.

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

PubMed Central

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

2017-01-01

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

Determination of Microstructural Parameters of Nanocrystalline Hydroxyapatite Prepared by Mechanical Alloying Method

NASA Astrophysics Data System (ADS)

Joughehdoust, Sedigheh; Manafi, Sahebali

2011-12-01

Hydroxyapatite [HA, Ca10(PO4)6(OH)2] is chemically similar to the mineral component of bones and hard tissues. HA can support bone ingrowth and osseointegration when used in orthopaedic, dental and maxillofacial applications. In this research, HA nanostructure was synthesized by mechanical alloying method. Phase development, particle size and morphology of HA were investigated by X-ray diffraction (XRD) pattern, zetasizer instrument, scanning electron microscopy (SEM), respectively. XRD pattern has been used to determination of the microstructural parameters (crystallite size, lattice parameters and crystallinity percent) by Williamson-Hall equation, Nelson-Riley method and calculating the areas under the peaks, respectively. The crystallite size and particle size of HA powders were in nanometric scales. SEM images showed that some parts of HA particles have agglomerates. The ratio of lattice parameters of synthetic hydroxyapatite (c/a = 0.73) was determined in this study is the same as natural hydroxyapatite structure.

Nanocrystalline (U0.5Ce0.5)O2±x solid solutions through citrate gel-combustion

NASA Astrophysics Data System (ADS)

Maji, D.; Ananthasivan, K.; Venkata Krishnan, R.; Balakrishnan, S.; Amirthapandian, S.; Joseph, Kitheri; Dasgupta, Arup

2018-04-01

Nanocrystalline powders of (U0.5Ce0.5)O2±x solid solutions were synthesized in bulk (100-200 g) through the citrate gel combustion. The fuel (citric acid) to oxidant (nitrate) mole ratio (R) was varied from 0.1 to 1.0. Two independent lots of the products obtained through the gel-combustion were calcined at 973 K in air and in a mixture of argon containing 8% H2 respectively. All these powders were characterized for their bulk density, X-ray crystallite size, specific surface area, size distribution of the particles, porosity as well as residual carbon. The morphology and microstructures of these powders were studied by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. Nanocrystalline single phase fluorite solid solutions having a typical crystallite size of about (7-15 nm) were obtained. These powders were highly porous comprising cuboidal flaky agglomerates. The combustion mixture with an 'R' value of 0.25 was found to undergo volume combustion and was found to yield a product that was distinctly different. The systematic investigation on synthesis and characterization of nanocrystalline UCeO2 is reported for the first time.

Effects of grain size on the properties of bulk nanocrystalline Co-Ni alloys

NASA Astrophysics Data System (ADS)

Qiao, Gui-Ying; Xiao, Fu-Ren

2017-08-01

Bulk nanocrystalline Co78Ni22 alloys with grain size ranging from 5 nm to 35 nm were prepared by high-speed jet electrodeposition (HSJED) and annealing. Microhardness and magnetic properties of these alloys were investigated by microhardness tester and vibrating sample magnetometer. Effects of grain size on these characteristics were also discussed. Results show that the microhardness of nanocrystalline Co78Ni22 alloys increases following a d -1/2-power law with decreasing grain size d. This phenomenon fits the Hall-Petch law when the grain size ranges from 5 nm to 35 nm. However, coercivity H c increases following a 1/d-power law with increasing grain size when the grain size ranges from 5 nm to 15.9 nm. Coercivity H c decreases again for grain sizes above 16.6 nm according to the d 6-power law.

Influence of Weak External Magnetic Field on Amorphous and Nanocrystalline Fe-based Alloys

NASA Astrophysics Data System (ADS)

Degmová, J.; Sitek, J.

2010-07-01

Nanoperm, Hitperm and Finamet amorphous and nanocrystalline alloys were measured by Mössbauer spectrometry in a weak external magnetic field of 0.5 T. It was shown that the most sensitive parameters of Mössbauer spectra are the intensities of the 2nd and the 5th lines. Rather small changes were observed also in the case of internal magnetic field values. The spectrum of nanocrystalline Nanoperm showed the increase in A23 parameter (ratio of line intensities) from 2.4 to 3.7 and decrease of internal magnetic field from 20 to 19 T for amorphous subspectrum under the influence of magnetic field. Spectrum of nanocrystalline Finemet shown decrease in A23 parameter from 3.5 to 2.6 almost without a change in the internal magnetic field value. In the case of amorphous Nanoperm and Finemet samples, the changes are almost negligible. Hitperm alloy showed the highest sensitivity to the weak magnetic field, when the A23 parameter increased from 0.4 to 2.5 in the external magnetic fields. The A23 parameter of crystalline subspectrum increased from 2.7 to 3.8 and the value of internal magnetic field corresponding to amorphous subspectrum increased from 22 to 24 T. The behavior of nanocrystalline alloys under weak external magnetic field was analyzed within the three-level relaxation model of magnetic dynamics in an assembly of single-domain particles.

On the AC-conductivity mechanism in nano-crystalline Se79-xTe15In6Pbx (x = 0, 1, 2, 4, 6, 8 and 10) alloys

NASA Astrophysics Data System (ADS)

Anjali; Patial, Balbir Singh; Bhardwaj, Suresh; Awasthi, A. M.; Thakur, Nagesh

2017-10-01

In-depth analysis of complex AC-conductivity for nano-crystalline Se79-xTe15In6Pbx (x = 0, 1, 2, 4, 6, 8 and 10 at wt%) alloys is made in the temperature range 308-423 K and over the frequency range 10-1-107 Hz, to understand the conduction mechanism. The investigated nano-crystalline alloys were prepared by melt-quench technique. Sharp structural peaks in X-ray diffraction pattern indicate the nano-crystalline nature, which is also confirmed by FESEM. The AC conductivity shows universal characteristics and at higher frequency a transition from dc to dispersive behavior occurs. Moreover, it is confirmed that ac conductivity (σac) obeys the Jonscher power law as ωs (s< 1). The obtained results are analyzed in the light of various theoretical models. The correlated barrier hopping (CBH) model associated with non-intimate valence alternation pairs (NVAP's) is found most appropriate to describe the conduction mechanisms in these alloys. In addition, the CBH model description reveals that the bipolaron (single polaron) transport dominates at lower (higher) temperature. The density of localized states has also been deduced.

Microstructures and mechanical properties of nanocrystalline NiTi intermetallics formed by mechanosynthesis

NASA Astrophysics Data System (ADS)

Arunkumar, S.; Kumaravel, P.; Velmurugan, C.; Senthilkumar, V.

2018-01-01

The formulation of nanocrystalline NiTi shape memory alloys has potential effects in mechanical stimulation and medical implantology. The present work elucidates the effect of milling time on the product's structural characteristics, chemical composition, and microhardness for NiTi synthesized by mechanical alloying for different milling durations. Increasing the milling duration led to the formation of a nanocrystalline NiTi intermetallic at a higher level. The formation of nanocrystalline materials was directed through cold fusion, fracturing, and the development of a steady state, which were influenced by the accumulation of strain energy. In the morphological study, uninterrupted cold diffusion and fracturing were visualized using transmission electron microscopy. Particle size analysis revealed that the mean particle size was reduced to 93 μm after 20 h of milling. The mechanical strength was enhanced by the formation of a nanocrystalline intermetallic phase at longer milling time, which was confirmed by the results of Vickers hardness analyses.

Microstructures evolution and physical properties of laser induced NbC modified nanocrystalline composites

NASA Astrophysics Data System (ADS)

Li, Jianing; Liu, Kegao; Yuan, Xingdong; Shan, Feihu; Zhang, Bolun; Wang, Zhe; Xu, Wenzhuo; Zhang, Zheng; An, Xiangchen

2017-10-01

The nanoscale quasicrystals (NQs), amorphous and ultrafine nanocrystals (UNs) modified hard composites are produced by laser cladding (LC) of the Ni60A-TiC-NbC-Sb mixed powders on the additive manufacturing (AM) TA1 titanium alloy. The LC technique is favorable to formations of icosahedral quasicrystals (I-phase) with five-fold symmetry due to its rapid cooling and solidification characteristics. The formation mechanism of this I-phase is explained here. Under the actions of NQs, amorphous and UNs, such LC composites exhibited an extremely high micro-hardness. UNs may also intertwin with amorphous, forming yarn-shape materials. This research provides essential theoretical basis to improve the quality of laser-treated composites.

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

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less

Structure and soft magnetic properties of Fe-Si-B-P-Cu nanocrystalline alloys with minor Mn addition

NASA Astrophysics Data System (ADS)

Jia, Xingjie; Li, Yanhui; Wu, Licheng; Zhang, Wei

2018-05-01

Addition of minor Mn effectively improves the amorphous-forming ability and thermal stability of the Fe85Si2B8P4Cu1 alloy. With increasing the Mn content from 0 to 3 at.%, the critical thickness for amorphous formation and onset temperature of the primary crystallization increase from 14 μm and 659 K to 27 μm and 668 K, respectively. The fine nanocrystalline structure with α-Fe grains in size (D) of < 20 nm was obtained for the annealed amorphous alloys, which show excellent soft magnetic properties. The alloying of Mn reduces the coercivity (Hc) by decreasing the D value and widens the optimum annealing temperature range for obtaining low Hc, although the saturation magnetic flux density (Bs) is decreased slightly. The Fe83Mn2Si2B8P4Cu1 nanocrystalline alloy possesses fine structure with a D of ˜17.5 nm, and exhibits a high Bs of ˜1.75 T and a low Hc of ˜5.9 A/m. The mechanism related to the alloying effects on the structure and magnetic properties was discussed in term of the crystallization activation energy.

Transport and magnetic properties of HITPERM alloys

NASA Astrophysics Data System (ADS)

Pekala, K.; Latuch, J.; Pekala, M.; Skorvanek, I.; Jaskiewicz, P.

2003-02-01

Nanocrystalline HITPERM alloys Fe44.6Co43.3X7.4B3.7Cu1 (X = Nb, Zr, Hf) prepared by crystallization of amorphous precursors are studied by magnetization and electrical resistivity measurements for the first time. Structural and magnetic components of the electrical resistivity are separated. The electrical resistivity of the nanocrystalline α' (FeCo) phase calculated using the Maxwell Garnett relation proves strong electron scattering on the grain boundaries. The temperature variation of the crystalline fraction during the first crystallization stage is calculated for the Hf based alloy.

Method to produce nanocrystalline powders of oxide-based phosphors for lighting applications

DOEpatents

Loureiro, Sergio Paulo Martins; Setlur, Anant Achyut; Williams, Darryl Stephen; Manoharan, Mohan; Srivastava, Alok Mani

2007-12-25

Some embodiments of the present invention are directed toward nanocrystalline oxide-based phosphor materials, and methods for making same. Typically, such methods comprise a steric entrapment route for converting precursors into such phosphor material. In some embodiments, the nanocrystalline oxide-based phosphor materials are quantum splitting phosphors. In some or other embodiments, such nanocrystalline oxide based phosphor materials provide reduced scattering, leading to greater efficiency, when used in lighting applications.

Debye–Waller coefficient of heavily deformed nanocrystalline iron1

PubMed Central

Abdellatief, M.

2017-01-01

Synchrotron radiation X-ray diffraction (XRD) patterns from an extensively ball-milled iron alloy powder were collected at 100, 200 and 300 K. The results were analysed together with those using extended X-ray absorption fine structure, measured on the same sample at liquid nitrogen temperature (77 K) and at room temperature (300 K), to assess the contribution of static disorder to the Debye–Waller coefficient (B iso). Both techniques give an increase of ∼20% with respect to bulk reference iron, a noticeably smaller difference than reported by most of the literature for similar systems. Besides good quality XRD patterns, proper consideration of the temperature diffuse scattering seems to be the key to accurate values of the Debye–Waller coefficient. Molecular dynamics simulations of nanocrystalline iron aggregates, mapped on the evidence provided by XRD in terms of domain size distribution, shed light on the origin of the observed B iso increase. The main contribution to the static disorder is given by the grain boundary, while line and point defects have a much smaller effect. PMID:28381974

Debye–Waller coefficient of heavily deformed nanocrystalline iron

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

Scardi, P.; Rebuffi, L.; Abdellatief, M.

2017-02-17

Synchrotron radiation X-ray diffraction (XRD) patterns from an extensively ball-milled iron alloy powder were collected at 100, 200 and 300 K. The results were analysed together with those using extended X-ray absorption fine structure, measured on the same sample at liquid nitrogen temperature (77 K) and at room temperature (300 K), to assess the contribution of static disorder to the Debye–Waller coefficient (B iso). Both techniques give an increase of ~20% with respect to bulk reference iron, a noticeably smaller difference than reported by most of the literature for similar systems. Besides good quality XRD patterns, proper consideration of themore » temperature diffuse scattering seems to be the key to accurate values of the Debye–Waller coefficient. Molecular dynamics simulations of nanocrystalline iron aggregates, mapped on the evidence provided by XRD in terms of domain size distribution, shed light on the origin of the observedB isoincrease. The main contribution to the static disorder is given by the grain boundary, while line and point defects have a much smaller effect.« less

Efficient and Convenient Synthesis of 1,8-Dioxodecahydroacridine Derivatives Using Cu-Doped ZnO Nanocrystalline Powder as a Catalyst under Solvent-Free Conditions

PubMed Central

Alinezhad, Heshmatollah; Mohseni Tavakkoli, Sahar

2013-01-01

A simple and convenient one-step method for synthesis of acridines and their derivatives from condensation of aromatic aldehydes, cyclic diketones, and aryl amines using Cu-doped ZnO nanocrystalline powder as a catalyst is reported. The present protocol provides several advantages such as good yields, short reaction time, easy workup, and simplicity in operation. PMID:24294130

Novel Fe-based nanocrystalline powder cores with excellent magnetic properties produced using gas-atomized powder

NASA Astrophysics Data System (ADS)

Chang, Liang; Xie, Lei; Liu, Min; Li, Qiang; Dong, Yaqiang; Chang, Chuntao; Wang, Xin-Min; Inoue, Akihisa

2018-04-01

FeSiBPNbCu nanocrystalline powder cores (NPCs) with excellent magnetic properties were fabricated by cold-compaction of the gas-atomized amorphous powder. Upon annealing at the optimum temperature, the NPCs showed excellent magnetic properties, including high initial permeability of 88, high frequency stability up to 1 MHz with a constant value of 85, low core loss of 265 mW/cm3 at 100 kHz for Bm = 0.05 T, and superior DC-bias permeability of 60% at a bias field of 100 Oe. The excellent magnetic properties of the present NPCs could be attributed to the ultrafine α-Fe(Si) phase precipitated in the amorphous matrix and the use of gas-atomized powder coated with a uniform insulation layer.

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

NASA Astrophysics Data System (ADS)

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

2013-08-01

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

Improvement of the functional properties of nanostructured Ti-Ni shape memory alloys by means of thermomechanical processing

NASA Astrophysics Data System (ADS)

Kreitcberg, Alena

Severe plastic deformation (SPD) is commonly used for nanostructure formation in Ti-Ni shape memory alloys (SMAs), but it increases the risk of damage during processing and, consequently, negatively affects functional fatigue resistance of these materials. The principal objective of this project is, therefore, to study the interrelations between the processing conditions, damageability during processing, microstructure and the functional properties of Ti-Ni SMAs with the aim of improving long-term functional performances of these materials by optimizing their processing conditions. First, microstructure and fatigue properties of Ti-Ni SMAs were studied after thermomechanical treatment (TMT) with different combinations of severe cold and warm rolling (CR and WR), as well as intermediate and post-deformation annealing (IA and PDA) technological steps. It was shown that either when WR and IA were introduced into the TMT schedule, or CR intensity was decreased, the fatigue life was improved as a consequence of less processing-induced damage and higher density of the favorable B2-austenite texture. This improvement was reached, however, at a price of a lower multi-cycle functional stability of these materials, the latter being a direct consequence of the microstructure coarsening after higher-temperature lower-intensity processing. At the end of this study, however, it was not possible to distinguish between contributions to the functional performances of Ti-Ni SMAs from different processing-related features: a) grain/subgrain size; b) texture; and c) level of rolling-induced defects. To be capable of separating contributions to the functional properties of Ti-Ni alloys from grain/subgrain size and from texture, the theoretical crystallographic resource of recovery strain after different TMTs and, therefore, different textures, were calculated and compared with the experiment. The comparative analysis showed that the structural factors (grain/subgrain size) strongly dominate the texture contributions, and therefore, there is no real alternative to having nanocrystalline Ti-Ni alloys, if one needs to maximize the Ti-Ni alloys functional properties. Since the creation of such a microstructure requires the use of severe cold deformation techniques and neither of these techniques can be completely exempt from defects, it was deemed necessary to compare the damage tolerance of nanocrystalline Ti-Ni alloys to that of their nanosubgrained and mixed nanocrystalline/nanosubgrained counterparts. With this objective in mind, a detailed analysis of interrelations between the level of the CR/WR-induced damage (edge microcrack size and concentration) and the fatigue life of Ti- Ni SMAs was carried out. It was shown that nanocrystalline structure provides higher tolerance to small-crack propagation than nanosubgrained or mixed nanocrystalline/ nanosubgrained structures, and that low-temperature deformability of these alloys has to be improved to benefit from the property-enhancement potential of nanocrystalline structure. To broaden our knowledge in the field of Ti-Ni alloy deformability, the strain-rate sensitivity of these alloys was studied. Different microstructures, varying from the coarse- to ultrafinegrained, were created by means of equal-channel angular pressing (ECAP) and subjected to strain-rate sensitivity testing. As a result, the material with ultrafine-grained microstructure demonstrated an improved deformability as compared to the coarse-grained structure, at any deformation temperature. Moreover, it was determined that the smaller the grain size, the lower the temperature and the higher the strain-rate at which superplasticity occurs. Based on the results obtained, combined thermomechanical processing (ECAP at elevated temperatures followed by CR) was proposed and validated in terms of structural refinement with reduced level of processing-induced defects. Scientific contributions. This thesis contributes to the advancement of knowledge in the field of Ti-Ni SMAs' processing-structure-properties interactions, and the main conclusions of this study can be summed-up as follows: • Nanocrystalline Ti-Ni alloys significantly outperform nanosubgrain Ti-Ni alloys in terms of the absolute values and stability of their single- and multiple-cycle functional properties (superelasticity and shape memory characteristics). The main factor limiting the number of cycles to failure of the nanocrystalline alloys is the processingrelated damage. • The structure of Ti-Ni alloys plays significantly higher role in the realization of their functional potential that does their texture. • In terms of fatigue life, the nanocrystalline structure has lower small-crack sensitivity than does the nanosubgrained structure. • Grain refinement makes it possible to improve deformability of Ti-Ni alloys at any temperature. • To produce nanocrystalline Ti-Ni SMAs free of processing-induced-defects, a novel three-step processing is proposed (ECAP+CR+PDA): grain-refining severe plastic deformation at elevated temperatures (ECAP), followed-up by amorphizing SPD at low temperatures (CR), and ended-up by nanocrystallizing post-deformation heat treatment (PDA).

Enhanced Hydrogen Storage Kinetics of Nanocrystalline and Amorphous Mg₂Ni-type Alloy by Melt Spinning.

PubMed

Zhang, Yang-Huan; Li, Bao-Wei; Ren, Hui-Ping; Li, Xia; Qi, Yan; Zhao, Dong-Liang

2011-01-18

Mg₂Ni-type Mg₂Ni 1-x Co x (x = 0, 0.1, 0.2, 0.3, 0.4) alloys were fabricated by melt spinning technique. The structures of the as-spun alloys were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The hydrogen absorption and desorption kinetics of the alloys were measured by an automatically controlled Sieverts apparatus. The electrochemical hydrogen storage kinetics of the as-spun alloys was tested by an automatic galvanostatic system. The results show that the as-spun (x = 0.1) alloy exhibits a typical nanocrystalline structure, while the as-spun (x = 0.4) alloy displays a nanocrystalline and amorphous structure, confirming that the substitution of Co for Ni notably intensifies the glass forming ability of the Mg₂Ni-type alloy. The melt spinning treatment notably improves the hydriding and dehydriding kinetics as well as the high rate discharge ability (HRD) of the alloys. With an increase in the spinning rate from 0 (as-cast is defined as spinning rate of 0 m/s) to 30 m/s, the hydrogen absorption saturation ratio () of the (x = 0.4) alloy increases from 77.1 to 93.5%, the hydrogen desorption ratio () from 54.5 to 70.2%, the hydrogen diffusion coefficient (D) from 0.75 × 10 - 11 to 3.88 × 10 - 11 cm²/s and the limiting current density I L from 150.9 to 887.4 mA/g.

Synthesis and properties of nanocrystalline Bi-Te based thermoelectric materials for energy application

NASA Astrophysics Data System (ADS)

Almohaimeed, Sulaiman

Thermoelectric phenomenon is the science associated with converting thermal energy into electricity based on the Seebeck effect. Bismuth telluride Bi 2Te3 is currently considered to be the state-of-the art thermoelectric material with high efficiency for low temperature applications and is therefore attractive for energy harvesting processes. Nanostructures thermoelectric materials provide a novel way to enhance thermoelectric properties and are considered to be the efficient building blocks for thermoelectric devices. In this work, n- and p-type bulk nanocrystalline Bismuth telluride thermoelectric materials were prepared by mechanical alloying / ball milling technique. The produced nano-crystalline powder were then consolidated using hot compaction under inert atmosphere. The novel processing of these materials maintained the nanostructure in both n- and p-type. Structural properties of the n- and p-types were characterized using X ray diffraction, scanning electron microscopy and transmission electron microscope. These techniques proved that the average grian size of the milled thermoelectric materials was about 20 nm. Accordingly, a Significant improvement in the figure of merit (ZT) is achieved through significant lattice thermal conductivity reduction and Seebeck coefficient improvement. The maximum ZT value for the n-type nanocrystalline thermoelectric was 1.67 at 373 K while the maximum ZT value for the p-type was 1.78 at the same temperature. These values are considered to be the highest values reported for similar materials. Evaluation of the mechanical properties was also performed through microhardness measurement using Vickers micro-hardness test, which shows an enhancement in mechanical properties for the produced materials.

Aqueous Combustion Synthesis and Characterization of Nanosized Tetragonal Zirconia Single Crystals

NASA Astrophysics Data System (ADS)

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

2007-08-01

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

Thermal Stability of Nanocrystalline Alloys by Solute Additions and A Thermodynamic Modeling

NASA Astrophysics Data System (ADS)

Saber, Mostafa

Nanocrystalline alloys show superior properties due to their exceptional microstructure. Thermal stability of these materials is a critical aspect. It is well known that grain boundaries in nanocrystalline microstructures cause a significant increase in the total free energy of the system. A driving force provided to reduce this excess free energy can cause grain growth. The presence of a solute addition within a nanocrystalline alloy can lead to the thermal stability. Kinetic and thermodynamic stabilization are the two basic mechanisms with which stability of a nanoscale grain size can be achieved at high temperatures. The basis of this thesis is to study the effect of solute addition on thermal stability of nanocrystalline alloys. The objective is to determine the effect of Zr addition on the thermal stability of mechanically alloyed nanocrysatillne Fe-Cr and Fe-Ni alloys. In Fe-Cr-Zr alloy system, nanoscale grain size stabilization was maintained up to 900 °C by adding 2 at% Zr. Kinetic pinning by intermetallic particles in the nanoscale range was identified as a primary mechanism of thermal stabilization. In addition to the grain size strengthening, intermetallic particles also contribute to strengthening mechanisms. The analysis of microhardness, XRD data, and measured grain sizes from TEM micrographs suggested that both thermodynamic and kinetic mechanisms are possible mechanisms. It was found that alpha → gamma phase transformation in Fe-Cr-Zr system does not influence the grain size stabilization. In the Fe-Ni-Zr alloy system, it was shown that the grain growth in Fe-8Ni-1Zr alloy is much less than that of pure Fe and Fe-8Ni alloy at elevated temperatures. The microstructure of the ternary Fe-8Ni-1Zr alloy remains in the nanoscale range up to 700 °C. Using an in-situ TEM study, it was determined that drastic grain growth occurs when the alpha → gamma phase transformation occurs. Accordingly, there can be a synergistic relationship between grain growth and alpha → gamma phase transformation in Fe-Ni-Zr alloys. In addition to the experimental study of thermal stabilization of nanocrystalline Fe-Cr-Zr or Fe-Ni-Zr alloys, the thesis presented here developed a new predictive model, applicable to strongly segregating solutes, for thermodynamic stabilization of binary alloys. This model can serve as a benchmark for selecting solute and evaluating the possible contribution of stabilization. Following a regular solution model, both the chemical and elastic strain energy contributions are combined to obtain the mixing enthalpy. The total Gibbs free energy of mixing is then minimized with respect to simultaneous variations in the grain boundary volume fraction and the solute concentration in the grain boundary and the grain interior. The Lagrange multiplier method was used to obtained numerical solutions. Application are given for the temperature dependence of the grain size and the grain boundary solute excess for selected binary system where experimental results imply that thermodynamic stabilization could be operative. This thesis also extends the binary model to a new model for thermodynamic stabilization of ternary nanocrystalline alloys. It is applicable to strongly segregating size-misfit solutes and uses input data available in the literature. In a same manner as the binary model, this model is based on a regular solution approach such that the chemical and elastic strain energy contributions are incorporated into the mixing enthalpy DeltaHmix, and the mixing entropy DeltaSmix is obtained using the ideal solution approximation. The Gibbs mixing free energy Delta Gmix is then minimized with respect to simultaneous variations in grain growth and solute segregation parameters. The Lagrange multiplier method is similarly used to obtain numerical solutions for the minimum Delta Gmix. The temperature dependence of the nanocrystalline grain size and interfacial solute excess can be obtained for selected ternary systems. As an example, model predictions are compared to experimental results for Fe-Cr-Zr and Fe-Ni-Zr alloy systems. Consistency between the experimental results and the present model predictions provide a more rigorous criterion for investigating thermal stabilization. However, other possible contributions for grain growth stabilization should still be considered.

Nanocrystalline High-Entropy Alloys: A New Paradigm in High-Temperature Strength and Stability.

PubMed

Zou, Yu; Wheeler, Jeffrey M; Ma, Huan; Okle, Philipp; Spolenak, Ralph

2017-03-08

Metals with nanometer-scale grains or nanocrystalline metals exhibit high strengths at ambient conditions, yet their strengths substantially decrease with increasing temperature, rendering them unsuitable for usage at high temperatures. Here, we show that a nanocrystalline high-entropy alloy (HEA) retains an extraordinarily high yield strength over 5 GPa up to 600 °C, 1 order of magnitude higher than that of its coarse-grained form and 5 times higher than that of its single-crystalline equivalent. As a result, such nanostructured HEAs reveal strengthening figures of merit-normalized strength by the shear modulus above 1/50 and strength-to-density ratios above 0.4 MJ/kg, which are substantially higher than any previously reported values for nanocrystalline metals in the same homologous temperature range, as well as low strain-rate sensitivity of ∼0.005. Nanocrystalline HEAs with these properties represent a new class of nanomaterials for high-stress and high-temperature applications in aerospace, civilian infrastructure, and energy sectors.

Nanocrystalline Nb-Al-Ge mixtures fabricated using wet mechanical milling

NASA Astrophysics Data System (ADS)

Pusceddu, E.; Charlton, S.; Hampshire, D. P.

2008-02-01

An investigation into Nb-Al-Ge mixtures is presented with special attention to the superconducting compounds Nb3(Al1-xGex) with x = 0, 0.3 and 1, which are reported to provide the highest upper critical field values for Nb-based compounds. Wet mechanical milling using copper milling media and distilled water as a process control agent (PCA) was used with the intention of improving the yield, properties and the performance of these materials. Very high yields of nanocrystalline material were achieved but significant copper contamination occurred - confirmed using inductively-coupled-plasma atomic-emission-spectroscopy. Simultaneous thermogravimetric measurements and differential scanning calorimetry were performed on powders milled for up to 20 h with different PCA content, to quantify the work done on the powders. A typical grain size of a few nm was obtained for the Nb-Al-Ge mixtures after several hours milling. Powder ground for 20 h with 5% PCA was processed using a hot isostatic press (HIP) operating at 2000 atm and temperatures up to 750 °C. The room temperature resistivity decreased as the temperature of the HIPing increased. Unfortunately, despite the nanocrystalline microstructure of the powders and the high HIP temperatures, if superconducting material was formed it was below the detection level of resistivity, Ac. susceptibility and SQUID measurements. We conclude that during milling there was widespread contamination of the powders by the PCA so that milling with distilled water as a PCA is not to be recommended for fabricating nanocrystalline Nb3(Al1-xGex) A15 superconducting compounds.

Ultrahigh hardness and high electrical resistivity in nano-twinned, nanocrystalline high-entropy alloy films

NASA Astrophysics Data System (ADS)

Huo, Wenyi; Liu, Xiaodong; Tan, Shuyong; Fang, Feng; Xie, Zonghan; Shang, Jianku; Jiang, Jianqing

2018-05-01

Nano-twinned, nanocrystalline CoCrFeNi high-entropy alloy films were produced by magnetron sputtering. The films exhibit a high hardness of 8.5 GPa, the elastic modulus of 161.9 GPa and the resistivity as high as 135.1 μΩ·cm. The outstanding mechanical properties were found to result from the resistance of deformation created by nanocrystalline grains and nano-twins, while the electrical resistivity was attributed to the strong blockage effect induced by grain boundaries and lattice distortions. The results lay a solid foundation for the development of advanced films with structural and functional properties combined in micro-/nano-electronic devices.

Effect of SMAT on microstructural and mechanical properties of AA2024

NASA Astrophysics Data System (ADS)

Tadge, Prashant; Sasikumar, C.

2016-05-01

In recent days surface mechanical attrition treatment (SMAT) had attracted the attention of researchers as it produces a nano-crystalline surface with improved mechanical properties. In the present study Al-4%Cu alloy used in automobile and aerospace application is subjected to surface mechanical attrition treatment using steel shots. The microstructural changes introduced on the surface of the Al alloy was investigated using Scanning Electron Microscopy (SEM). The secondary phases formed during the SMAT process is been investigated using EDX and XRD analysis. The effects of SMAT on the mechanical properties were analyzed using a tensile testing. The SMA treatment had resulted in severe plastic deformation of the surface, thereby yielded a nanocrystalline surface with a grain size of 30 to 50 nm. Further, it is also found that the SMAT produced ultra nanocrystalline particles of Cu2Al dispersed uniformly into α-Al matrix. These microstructural changes had resulted in considerable change in the mechanical properties of these alloys. The tensile strength of these alloys had increased from ˜212 MPa to 303 MPa while the fracture toughness increased up to 28% in 10 minutes of SMAT.

Resistivity changes of some amorphous alloys undergoing nanocrystallization

NASA Astrophysics Data System (ADS)

Barandiarán, J. M.; Fernández Barquín, L.; Sal, J. C. Gómez; Gorría, P.; Hernando, A.

1993-10-01

The electrical resistivity of amorphous alloys with compositions: Fe 73.5Nb 3Cu 1Si 13.5B 9, Fe 86Zr 7Cu 1B 6 and Co 80Nb 8B 12 has been studied in the temperature range from 300 to 1100 K, where crystallization occurs. The products of crystallization and the grain size have been studied by X-ray diffraction. In a first step, all the alloys crystallize with small grains of a few nanometers in diameter (nanocrystalline state), and the resistivity behavior at this process accounts for the difference between the amorphous and nanocrystalline phases. The nanocrystalline phases are: α-Fe-Si, α-Fe and fcc Co for the three compounds studied respectively. A second process, at which grain growth and precipitation of intermetallic compounds and borides takes place, has been found for all the alloys. The resistivity is sensitive, not only to the total transformed sample amount, but to the topological distribution of the crystalline phases, and therefore shows a more complex behavior than other well established techniques, as differential scanning calorimetry. This supplementary information given by the resistivity is also discussed.

Rietveld analysis of the effect of annealing atmosphere on phase evolution of nanocrystalline TiO2 powders.

PubMed

Salari, M; Rezaee, M; Chidembo, A T; Konstantinov, K; Liu, H K

2012-06-01

The structural evolution of nanocrystalline TiO2 was studied by X-ray diffraction (XRD) and the Rietveld refinement method (RRM). TiO2 powders were prepared by the sol-gel technique. Post annealing of as-synthesized powders in the temperature range from 500 degrees C to 800 degrees C under air and argon atmospheres led to the formation of TiO2 nanoparticles with mean crystallite size in the range of 37-165 nm, based on the Rietveld refinement results. It was found that the phase structure, composition, and crystallite size of the resulting particles were dependent on not only the annealing temperature, but also the annealing atmosphere. Rietveld refinement of the XRD data showed that annealing the powders under argon atmosphere promoted the polymorphic phase transformation from anatase to rutile. Field emission scanning electron microscopy (FESEM) was employed to investigate the morphology and size of the annealed powders.

Soft magnetic properties of nanocrystalline FeRuGaSi-Hf alloy films and head characteristics for the embedded thin film tape head

NASA Astrophysics Data System (ADS)

Ohmori, H.; Shoji, M.; Kobayashi, T.; Yamamoto, T.; Sugiyama, Y.; Hayashi, K.; Hono, K.

1996-04-01

The Hf-added FeRuGaSi alloy film has an amorphous structure in the as-deposited state and becomes nanocrystalline after annealing. Due to this structure change from crystalline to amorphous by the addition of Hf, soft magnetic degradation of the film deposited on the slant grooved substrate, which is necessary for the sophisticated embedded thin film (ETF) head structure, is greatly suppressed and the undesirable film stress is relieved. The FeRuGaSi-Hf alloy film has higher resistivity and permeability at high frequencies than those of sendust film, and the read/write characteristics of this alloy film show better performance than sendust film.

Mechanical properties of nanocrystalline cobalt

NASA Astrophysics Data System (ADS)

Karimpoor, Amir A.; Erb, Uwe

2006-05-01

Due to their excellent wear and corrosion properties, nanocrystalline cobalt and several cobalt alloys made by electrodeposition are currently being developed as environmentally benign replacement coatings for hard chromium electrodeposits. The focus of this study is on the mechanical properties of nanocrystalline cobalt, which are currently not well understood. A comparison is presented for hardness, tensile properties, Charpy impact properties and fracture surface analysis of both nanocrystalline (grain size: 12 nm) and conventional polycrystalline (grain size: 4.8 m) cobalt. It is shown that the hardness and tensile strength of nanocrystalline cobalt is 2-3 times higher than for polycrystalline cobalt. However, in contrast to other nanocrystalline materials tested previously, nanocrystalline cobalt retains considerable ductility with elongation to fracture values up to 7%.

Diamond-silicon carbide composite

DOEpatents

Qian, Jiang; Zhao, Yusheng

2006-06-13

Fully dense, diamond-silicon carbide composites are prepared from ball-milled microcrystalline diamond/amorphous silicon powder mixture. The ball-milled powder is sintered (P=5–8 GPa, T=1400K–2300K) to form composites having high fracture toughness. A composite made at 5 GPa/1673K had a measured fracture toughness of 12 MPa.dot.m^1/2. By contrast, liquid infiltration of silicon into diamond powder at 5 GPa/1673K produces a composite with higher hardness but lower fracture toughness. X-ray diffraction patterns and Raman spectra indicate that amorphous silicon is partially transformed into nanocrystalline silicon at 5 GPa/873K, and nanocrystalline silicon carbide forms at higher temperatures.

Diamond-Silicon Carbide Composite And Method For Preparation Thereof

DOEpatents

Qian, Jiang; Zhao, Yusheng

2005-09-06

Fully dense, diamond-silicon carbide composites are prepared from ball-milled microcrystalline diamond/amorphous silicon powder mixture. The ball-milled powder is sintered (P=5-8 GPa, T=1400K-2300K) to form composites having high fracture toughness. A composite made at 5 GPa/1673K had a measured fracture toughness of 12 MPa.multidot.m.sup.1/2. By contrast, liquid infiltration of silicon into diamond powder at 5 GPa/1673K produces a composite with higher hardness but lower fracture toughness. X-ray diffraction patterns and Raman spectra indicate that amorphous silicon is partially transformed into nanocrystalline silicon at 5 GPa/873K, and nanocrystalline silicon carbide forms at higher temperatures.

Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

PubMed

Vogt, Frederick G; Williams, Glenn R

2012-07-01

Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

Preparation of (Fe, N)-doped TiO2 powders and their antibacterial activities under visible light irradiation.

PubMed

He, Rong-Liang; Wei, Yi; Cao, Wen-Bin

2009-02-01

Yellowish (Fe, N)-doped nanocrystalline TiO2 powders have been prepared using TiOSO4, CO(NH2)2, Fe(NO3)3.9H2O and CN3H5.HCl as precursors by hydrothermal method. The as-synthesized powders were anatase in phase and the grain size was about 10 nm according to the TEM photos. The ratio of Fe/Ti is 2.2 at% and N/O is 0.8 at% respectively. TiO2 powders were mixed with organic silicon and acrylic syrup to test their antibacterial performance by the colony counting method. The results show that the sterilization ratio of E. coli by the heat-treated (Fe, N)-doped nanocrystalline TiO2 powders is reached up to 94.5% while that of the powders without any heat treatment is 91.1% by 8 hours-400 lux-Visible-light irradiation with humidity of 55% RH.

Studies on the sensing behaviour of nanocrystalline CuGa(2)O(4) towards hydrogen, liquefied petroleum gas and ammonia.

PubMed

Biswas, Soumya Kanti; Sarkar, Arpita; Pathak, Amita; Pramanik, Panchanan

2010-06-15

In the present article, the gas sensing behaviour of nanocrystalline CuGa(2)O(4) towards H(2), liquefied petroleum gas (LPG) and NH(3) has been reported for the first time. Nanocrystalline powders of CuGa(2)O(4) having average particle sizes in the range of 30-60nm have been prepared through thermal decomposition of an aqueous precursor solution comprising copper nitrate, gallium nitrate and triethanol amine (TEA), followed by calcination at 750 degrees C for 2h. The synthesized nanocrystalline CuGa(2)O(4) powders have been characterised through X-ray diffraction (XRD), transmission electron microscopy (TEM), field-emission scanning electron microscopy (FESEM) study, energy dispersive X-ray (EDX) analysis and BET (Brunauer-Emmett-Teller) surface area measurement. The synthesized CuGa(2)O(4) having spinel structure with specific surface area of 40m(2)/g exhibits maximum sensitivity towards H(2), LPG, and NH(3) at 350 degrees C.

Thermohydrogen processing (THP) of titanium alloy and titanium-aluminum alloys

NASA Astrophysics Data System (ADS)

Qazi, Javaid Iqbal

The microstructures, phases and phase transformations occurring in cast and Hot Isostatic Pressed (HIP'd) Ti-6Al-4V-H and the blended elemental (BE) TiAl-H systems were investigated. In this work, the existing Ti-6Al-4V-H phase diagram was revised and the time-temperature-transformation (TTT) diagrams for beta-phase (isothermal) and martensite (quench plus aging) decomposition were determined at different hydrogen concentrations. Alloying with hydrogen decreases the nose temperatures for the start of both the beta/martensite decompositions in a linear fashion and increases the nose times for both of these in a non-linear fashion. During aging at temperatures below the beta transus temperature, the martensite decomposes into alpha+betaM (metastable beta) and on quenching, from the aging temperature, the betaM transforms to martensite + beta R (residual beta) with the amount of latter increasing with increasing hydrogen content. Microstructures varying from alpha-lamellar laths to fine equiaxed alpha-grains were produced in the Ti-6Al-4V alloy, by using different thermohydrogen processing (THP) treatments. A microstructure consisting of mixed equiaxed and elongated alpha-grains were only produced in samples containing 30at.%H after the complete decomposition of the beta/martensite below a critical temperature (Tc), followed by dehydrogenation. A mixture consisting of partially equiaxed alpha-grains thus produced by THP, increased the tensile strength from 841MPa (starting Ti-6Al-4V) to 965MPa after THP and also increased the % elongation from 7.5% to 10.5%. In addition to other THP parameters, the final microstructure also depends on the starting microstructure and recommendations are made for future work in this regard. Initial results of temperature cycling treatments, which involved heat treating of Ti-6Al-4V samples containing 30at.%H at 680°C for 5 minutes followed by water quenching and repetition of the same treatment for 10 cycles, did not show a decrease in the average prior beta grain size; recommendations have been made for future work in this area. Fully dense hydrogenated nano-crystalline TiAl compacts were produced from BE powders. HIP'ing of the mechanically alloyed hydrogenated powders at 850°C resulted in a homogenous microstructure, whereas prior powder particle boundaries were visible in the samples produced from non-hydrogenated powders. The hydrogen was removed by vacuum annealing resulting in nano-size gamma-TiAl.

Effect of amorphous Mg{sub 50}Ni{sub 50} on hydriding and dehydriding behavior of Mg{sub 2}Ni alloy

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

Guzman, D., E-mail: danny.guzman@uda.cl; Ordonez, S.; Fernandez, J.F.

Composite Mg{sub 2}Ni (25 wt.%) amorphous Mg{sub 50}Ni{sub 50} was prepared by mechanical milling starting with nanocrystalline Mg{sub 2}Ni and amorphous Mg{sub 50}Ni{sub 50} powders, by using a SPEX 8000 D mill. The morphological and microstructural characterization of the powders was performed via scanning electron microscopy and X-ray diffraction. The hydriding characterization of the composite was performed via a solid gas reaction method in a Sievert's-type apparatus at 363 K under an initial hydrogen pressure of 2 MPa. The dehydriding behavior was studied by differential thermogravimetry. On the basis of the results, it is possible to conclude that amorphous Mg{submore » 50}Ni{sub 50} improved the hydriding and dehydriding kinetics of Mg{sub 2}Ni alloy upon cycling. A tentative rationalization of experimental observations is proposed. - Research Highlights: {yields} First study of the hydriding behavior of composite Mg{sub 2}Ni (25 wt.%) amorphous Mg{sub 50}Ni{sub 50}. {yields} Microstructural characterization of composite material using XRD and SEM was obtained. {yields} An improved effect of Mg{sub 50}Ni{sub 50} on the Mg{sub 2}Ni hydriding behavior was verified. {yields} The apparent activation energy for the hydrogen desorption of composite was obtained.« less

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.

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.

Thermal stability comparison of nanocrystalline Fe-based binary alloy pairs

DOE PAGES

Clark, Blythe G.; Hattar, Khalid Mikhiel; Marshall, Michael Thomas; ...

2016-03-24

Here, the widely recognized property improvements of nanocrystalline (NC) materials have generated significant interest, yet have been difficult to realize in engineering applications due to the propensity for grain growth in these interface-dense systems. While traditional pathways to thermal stabilization can slow the mobility of grain boundaries, recent theories suggest that solute segregation in NC alloy can reduce the grain boundary energy such that thermodynamic stabilization is achieved. Following the predictions of Murdock et al., here we compare for the first time the thermal stability of a predicted NC stable alloy (Fe-10at.% Mg) with a predicted non-NC stable alloy (Fe-10at.%more » Cu) using the same processing and characterization methodologies. Results indicate improved thermal stability of the Fe-Mg alloy in comparison to the Fe-Cu, and observed microstructures are consistent with those predicted by Monte Carlo simulations.« less

Effect of SMAT on microstructural and mechanical properties of AA2024

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

Tadge, Prashant, E-mail: prashant-tadge@rediffmail.com; Sasikumar, C., E-mail: csasimv@gmail.com

In recent days surface mechanical attrition treatment (SMAT) had attracted the attention of researchers as it produces a nano-crystalline surface with improved mechanical properties. In the present study Al-4%Cu alloy used in automobile and aerospace application is subjected to surface mechanical attrition treatment using steel shots. The microstructural changes introduced on the surface of the Al alloy was investigated using Scanning Electron Microscopy (SEM). The secondary phases formed during the SMAT process is been investigated using EDX and XRD analysis. The effects of SMAT on the mechanical properties were analyzed using a tensile testing. The SMA treatment had resulted inmore » severe plastic deformation of the surface, thereby yielded a nanocrystalline surface with a grain size of 30 to 50 nm. Further, it is also found that the SMAT produced ultra nanocrystalline particles of Cu{sub 2}Al dispersed uniformly into α-Al matrix. These microstructural changes had resulted in considerable change in the mechanical properties of these alloys. The tensile strength of these alloys had increased from ∼212 MPa to 303 MPa while the fracture toughness increased up to 28% in 10 minutes of SMAT.« less

Preferential magnetic orientation in amorphous alloys determined by NFS and Mössbauer spectroscopy

NASA Astrophysics Data System (ADS)

Procházka, Vít; Vrba, Vlastimil; Šretrová, Pavla; Smrčka, David; Miglierini, Marcel

2016-10-01

Amorphous and nanocrystalline alloys frequently exhibit anisotropic behavior, which is a consequence of magnetic moments preferential orientation. This study reports the results obtained from a set of nuclear forward scattering experiments and transmission Mössbauer spectroscopy experiments that we have run in order to determine the degree of crystallization and the preferential orientation of magnetic moments in the material. The nuclear forward scattering of synchrotron radiation and the transmission Mössbauer spectroscopy were performed on the nanocrystalline alloy of the composition Fe79Mo8Cu1B12. The experimental data were evaluated and magnetic texture was determined. Relevance of the results was confronted with transmission Mössbauer experiments.

Nanocrystalline CuNi alloys: improvement of mechanical properties and thermal stability

NASA Astrophysics Data System (ADS)

Nogues, Josep; Varea, A.; Pellicer, E.; Sivaraman, K. M.; Pane, S.; Nelson, B. J.; Surinach, S.; Baro, M. D.; Sort, J.

2014-03-01

Nanocrystalline metallic films are known to benefit from novel and enhanced physical and chemical properties. In spite of these outstanding properties, nanocrystalline metals typically show relatively poor thermal stability which leads to deterioration of the properties due to grain coarsening. We have studied nanocrystalline Cu1-xNix (0.56 < x < 1) thin films (3 μm-thick) electrodeposited galvanostatically onto Cu/Ti/Si (100) substrates. CuNi thin films exhibit large values of hardness (6.15 < H < 7.21 GPa), which can be tailored by varying the composition. However, pure Ni films (x = 1) suffer deterioration of their mechanical and magnetic properties after annealing during 3 h at relatively low temperatures (TANN > 475 K) due to significant grain growth. Interestingly, alloying Ni with Cu clearly improves the thermal stability of the material because grain coarsening is delayed due to segregation of a Cu-rich phase at grain boundaries, thus preserving both the mechanical and magnetic properties up to higher TANN.

Insights into the deformation behavior of the CrMnFeCoNi high-entropy alloy revealed by elevated temperature nanoindentation

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

Maier-Kiener, Verena; Schuh, Benjamin; George, Easo P.

A CrMnFeCoNi high-entropy alloy was investigated by nanoindentation from room temperature to 400 °C in the nanocrystalline state and cast plus homogenized coarse-grained state. In the latter case a < 100 >-orientated grain was selected by electron back scatter diffraction for nanoindentation. It was found that hardness decreases more strongly with increasing temperature than Young’s modulus, especially for the coarse-grained state. The modulus of the nanocrystalline state was slightly higher than that of the coarse-grained one. For the coarse-grained sample a strong thermally activated deformation behavior was found up to 100–150 °C, followed by a diminishing thermally activated contribution atmore » higher testing temperatures. For the nanocrystalline state, different temperature dependent deformation mechanisms are proposed. At low temperatures, the governing processes appear to be similar to those in the coarse-grained sample, but with increasing temperature, dislocation-grain boundary interactions likely become more dominant. Finally, at 400 °C, decomposition of the nanocrystalline alloy causes a further reduction in thermal activation. Furthermore, this is rationalized by a reduction of the deformation controlling internal length scale by precipitate formation in conjunction with a diffusional contribution.« less

Change of magnetic properties of nanocrystalline alloys under influence of external factors

NASA Astrophysics Data System (ADS)

Sitek, Jozef; Holková, Dominika; Dekan, Julius; Novák, Patrik

2016-10-01

Nanocrystalline (Fe3Ni1)81Nb7B12 alloys were irradiated using different types of radiation and subsequently studied by Mössbauer spectroscopy. External magnetic field of 0.5 T, electron-beam irradiation up to 4 MGy, neutron irradiation up to 1017 neutrons/cm2 and irradiation with Cu ions were applied on the samples. All types of external factors had an influence on the magnetic microstructure manifested as a change in the direction of the net magnetic moment, intensity of the internal magnetic field and volumetric fraction of the constituent phases. The direction of the net magnetic moment was the most sensitive parameter. Changes of the microscopic magnetic parameters were compared after different external influence and results of nanocrystalline samples were compared with their amorphous precursors.

Effect of interstitial and substitution alloying elements on the intrinsic stacking fault energy of nanocrystalline fcc-iron by atomistic simulation study

NASA Astrophysics Data System (ADS)

Mohammadzadeh, Mina; Mohammadzadeh, Roghayeh

2017-11-01

The stacking fault energy (SFE) is an important parameter in the deformation mechanism of face centered cubic (fcc) iron-based alloy. In this study, the effect of interstitial (C and N) and substitution (Nb and Ti) alloying elements on the intrinsic SFE (ISFE) of nanocrystalline iron were investigated via molecular dynamics (MD) simulation. The modified embedded atom method (MEAM) inter-atomic potential was used in the MD simulations. The results demonstrate a strong dependence of ISFE with addition of interstitial alloying elements but only a mild increase in ISFE with addition of substitution alloying elements in the composition range of 0 < {CNb, CTi} < 3 (at%). Moreover, it is shown that alloying of fcc iron with N decreases ISFE, whereas it increases significantly by addition of carbon element [0 < {CC, CN} < 3.5 (at%)]. The simulation method employed in this work shows reasonable agreement with some published experimental/calculated data.

Fabrication of an Fe80.5Si7.5B6Nb5Cu Amorphous-Nanocrystalline Powder Core with Outstanding Soft Magnetic Properties

NASA Astrophysics Data System (ADS)

Zhang, Zongyang; Liu, Xiansong; Feng, Shuangjiu; Rehman, Khalid Mehmood Ur

2018-03-01

In this study, the melt spinning method was used to develop Fe80.5Si7.5B6Nb5Cu amorphous ribbons in the first step. Then, the Fe80.5Si7.5B6Nb5Cu amorphous-nanocrystalline core with a compact microstructure was obtained by multiple processes. The main properties of the magnetic powder core, such as micromorphology, thermal behavior, permeability, power loss and quality factor, have been analyzed. The obtained results show that an Fe80.5Si7.5B6Nb5Cu amorphous-nanocrystalline duplex core has high permeability (54.8-57), is relatively stable at different frequencies and magnetic fields, and the maximum power loss is only 313 W/kg; furthermore, it has a good quality factor.

Nanocrystalline ordered vanadium carbide: Superlattice and nanostructure

NASA Astrophysics Data System (ADS)

Kurlov, A. S.; Gusev, A. I.; Gerasimov, E. Yu.; Bobrikov, I. A.; Balagurov, A. M.; Rempel, A. A.

2016-02-01

The crystal structure, micro- and nanostructure of coarse- and nanocrystalline powders of ordered vanadium carbide V8C7 have been examined by X-ray and neutron diffraction and electron microscopy methods. The synthesized coarse-crystalline powder of ordered vanadium carbide has flower-like morphology. It was established that the real ordered phase has the composition V8C7-δ (δ ≅ 0.03) deviating from perfect stoichiometric composition V8C7. The vanadium atoms forming the octahedral environment □V6 of vacant sites in V8C7-δ are displaced towards the vacancy □. The presence of carbon onion-like structures was found in the vanadium carbide powders with a small content of free (uncombined) carbon. The nanopowders of V8C7-δ carbide with average particle size of 20-30 nm produced by high-energy milling of coarse-crystalline powder retain the crystal structure of the initial powder, but differ in the lattice deformation distortion anisotropy.

Green synthesis of nanocrystalline α-Al2O3 powders by both wet-chemical and mechanochemical methods

NASA Astrophysics Data System (ADS)

Gao, Huiying; Li, Zhiyong; Zhao, Peng

2018-03-01

Nanosized α-Al2O3 powders were prepared with AlCl3ṡ6H2O and NH4HCO3 as raw materials by both wet-chemical and mechanochemical methods, through the synthesis of the ammonium aluminum carbonate hydroxide (AACH) precursor followed by calcination. The environmentally benign starch was used as an effective dispersant during the preparation of nanocrystalline α-Al2O3 powders. X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were employed to characterize the precursor AACH and products. The results show that nanosized spherical α-Al2O3 powders without hard agglomeration and with particle size in the range of 20-40 nm can be obtained by the two methods. Comparing the two “green” processes, the mechanochemical method has better prospects for commercial production.

Structural, thermal, optical, and photoacoustic study of nanocrystalline Bi{sub 2}Te{sub 3} produced by mechanical alloying

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

Souza, S. M.; Triches, D. M.; Poffo, C. M.

2011-01-01

Nanocrystalline Bi{sub 2}Te{sub 3} was produced by mechanical alloying and its properties were investigated by differential scanning calorimetry (DSC) x-ray diffraction (XRD), Raman spectroscopy (RS), and photoacoustic spectroscopy (PAS). Combining the XRD and RS results, the volume fraction of the interfacial component in as-milled and annealed samples was estimated. The PAS results suggest that the contribution of the interfacial component to the thermal diffusivity of nanostructured Bi{sub 2}Te{sub 3} is very significant.

Recoil-free Fraction in Amorphous and Nanocrystalline Aluminium Based Alloys

NASA Astrophysics Data System (ADS)

Sitek, Jozef

2008-10-01

Aluminium based rapidly quenched alloys of nominal composition Al90Fe7Nb3 and Al94Fe2V4 were studied by Mössbauer spectroscopy. We have measured the recoil-free fraction and thermal shift at room and liquid nitrogen temperature. The frequency modes of atomic vibrations were determined and consequently the characteristic Debye temperature was derived. Characteristic temperature calculated from f-factor was lower than those fitted from second order Doppler shift. This indicates the presence of different frequency modes for amorphous and nanocrystalline states.

Nanotwins in Nanocrystalline Mg-Al Alloys: An Insight from High-Resolution TEM and Molecular Dynamics Simulation

DTIC Science & Technology

2013-09-25

Mathaudhu, C.Y.A. Tsao and E.J. Lavernia, Mater. Sci. Eng. A528 (2011) p. 2180. [21] S . Plimpton , J. Comput. Phys. 117 (1995) p. 1. [22] X.-Y. Liu, J.B...grained Mg are identi ? ed and supported with atomistic The views, opinions and/or findings contained in this report are those of the author( s ) and should...MONITORING AGENCY NAME( S ) AND ADDRESS (ES) U.S. Army Research Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 nanocrystalline Mg – Al alloys

The strengthening mechanism of a nickel-based alloy after laser shock processing at high temperatures

PubMed Central

Li, Yinghong; Zhou, Liucheng; He, Weifeng; He, Guangyu; Wang, Xuede; Nie, Xiangfan; Wang, Bo; Luo, Sihai; Li, Yuqin

2013-01-01

We investigated the strengthening mechanism of laser shock processing (LSP) at high temperatures in the K417 nickel-based alloy. Using a laser-induced shock wave, residual compressive stresses and nanocrystals with a length of 30–200 nm and a thickness of 1 μm are produced on the surface of the nickel-based alloy K417. When the K417 alloy is subjected to heat treatment at 900 °C after LSP, most of the residual compressive stress relaxes while the microhardness retains good thermal stability; the nanocrystalline surface has not obviously grown after the 900 °C per 10 h heat treatment, which shows a comparatively good thermal stability. There are several reasons for the good thermal stability of the nanocrystalline surface, such as the low value of cold hardening of LSP, extreme high-density defects and the grain boundary pinning of an impure element. The results of the vibration fatigue experiments show that the fatigue strength of K417 alloy is enhanced and improved from 110 to 285 MPa after LSP. After the 900 °C per 10 h heat treatment, the fatigue strength is 225 MPa; the heat treatment has not significantly reduced the reinforcement effect. The feature of the LSP strengthening mechanism of nickel-based alloy at a high temperature is the co-working effect of the nanocrystalline surface and the residual compressive stress after thermal relaxation. PMID:27877617

Corrosion Screening of EV31A Magnesium and Other Magnesium Alloys using Laboratory-Based Accelerated Corrosion and Electro-Chemical Methods

DTIC Science & Technology

2014-07-01

corrosion studies (16). A schematic of the SWAP process and example of the powder produced is included in figure 4. This alloy contains amounts of Al ...advanced powder -based alloy and ZAXE1711 (both from Japan) were produced using a Spinning Water Atomization Process (SWAP) to yield powder particles with...and ZAXE1711 Mg alloy powders and (b) morphology of coarse Mg alloy powder prepared by SWAP

X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

NASA Astrophysics Data System (ADS)

Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

2009-06-01

Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

Characterization of an aluminum alloy hemispherical shell fabricated via direct metal laser melting

DOE PAGES

Holesinger, T. G.; Carpenter, J. S.; Lienert, T. J.; ...

2016-01-11

The ability of additive manufacturing to directly fabricate complex shapes provides characterization challenges for part qualification. The orientation of the microstructures produced by these processes will change relative to the surface normal of a complex part. In this work, the microscopy and x-ray tomography of an AlSi10Mg alloy hemispherical shell fabricated using powder bed metal additive manufacturing are used to illustrate some of these challenges. The shell was manufactured using an EOS M280 system in combination with EOS-specified powder and process parameters. The layer-by-layer process of building the shell with the powder bed additive manufacturing approach results in a position-dependentmore » microstructure that continuously changes its orientation relative to the shell surface normal. X-ray tomography was utilized to examine the position-dependent size and distribution of porosity and surface roughness in the 98.6% dense part. Optical and electron microscopy were used to identify global and local position-dependent structures, grain morphologies, chemistry, and precipitate sizes and distributions. The rapid solidification processes within the fusion zone (FZ) after the laser transit results in a small dendrite size. Cell spacings taken from the structure in the middle of the FZ were used with published relationships to estimate a cooling rate of ~9 × 10 5 K/s. Uniformly-distributed, nanoscale Si precipitates were found within the primary α-Al grains. A thin, distinct boundary layer containing larger α-Al grains and extended regions of the nanocrystalline divorced eutectic material surrounds the FZ. Moreover, subtle differences in the composition between the latter layer and the interior of the FZ were noted with scanning transmission electron microscopy (STEM) spectral imaging.« less

Characterization of an Aluminum Alloy Hemispherical Shell Fabricated via Direct Metal Laser Melting

NASA Astrophysics Data System (ADS)

Holesinger, T. G.; Carpenter, J. S.; Lienert, T. J.; Patterson, B. M.; Papin, P. A.; Swenson, H.; Cordes, N. L.

2016-03-01

The ability of additive manufacturing to directly fabricate complex shapes provides characterization challenges for part qualification. The orientation of the microstructures produced by these processes will change relative to the surface normal of a complex part. In this work, the microscopy and x-ray tomography of an AlSi10Mg alloy hemispherical shell fabricated using powder bed metal additive manufacturing are used to illustrate some of these challenges. The shell was manufactured using an EOS M280 system in combination with EOS-specified powder and process parameters. The layer-by-layer process of building the shell with the powder bed additive manufacturing approach results in a position-dependent microstructure that continuously changes its orientation relative to the shell surface normal. X-ray tomography was utilized to examine the position-dependent size and distribution of porosity and surface roughness in the 98.6% dense part. Optical and electron microscopy were used to identify global and local position-dependent structures, grain morphologies, chemistry, and precipitate sizes and distributions. The rapid solidification processes within the fusion zone (FZ) after the laser transit results in a small dendrite size. Cell spacings taken from the structure in the middle of the FZ were used with published relationships to estimate a cooling rate of ~9 × 105 K/s. Uniformly-distributed, nanoscale Si precipitates were found within the primary α-Al grains. A thin, distinct boundary layer containing larger α-Al grains and extended regions of the nanocrystalline divorced eutectic material surrounds the FZ. Subtle differences in the composition between the latter layer and the interior of the FZ were noted with scanning transmission electron microscopy (STEM) spectral imaging.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

The Bulk Nanocrystalline zn Produced by Mechanical Attrition

NASA Astrophysics Data System (ADS)

Zhu, X. K.; Zhao, K. Y.; Li, C. J.; Tao, J. M.; Chan, T. L.; Koch, C. C.

The purpose of experiment was to produce bulk nanocrystalline Zn by mechanical attrition. The bulk nanocrystalline Zn produced by mechanical attrition was studied. The microstructural evolution during cryomilling and subsequent room temperature milling was characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD). In this paper, Nanocrystalline Zn was produced by insitu consolidation of Zn elemental powder using mechanical attrition at liquid nitrogen and room temperature. For the samples studied, the longest elongation of 65% and highest stress of 200 MPa is obtained in nanocrystalline Zn during tensile testing at the condition of strain rate (10-3 sec-1) and 20°C which is equal to 0.43 Tm (Tm is the melting temperature of pure Zn).

Bandgap engineering through nanocrystalline magnetic alloy grafting on reduced graphene oxide.

PubMed

De, D; Chakraborty, M; Majumdar, S; Giri, S

2014-09-28

High conductivity and the absence of ferromagnetism in pristine graphene fail to satisfy primary criteria for possible technological application in spintronics. Opening of the bandgap in graphene is primarily desirable for such applications. We report a simplified and novel approach of controlled grafting of a magnetic alloy on reduced graphene oxide. This eventually leads to ferromagnetism of the stable hybrid material at room temperature, with a large moment (∼1.2 μB) and a remarkable decrease in conductivity (∼10 times) compared to highly ordered pyrolytic graphite. Our model band-structure calculation indicates that the combined effect of controlled vacancies and impurities attributed to the nanocrystalline alloy grafting leads to a promising step toward band gap engineering.

Corrosion Behavior of Ultra-fine Grained 1050 Aluminum Alloy Fabricated by ARB Process in a Buffer Borate Solution

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, A.; Gashti, S. O.

2015-09-01

Accumulative roll bonding (ARB) has been used as a severe plastic deformation process for the industrial production of ultra-fine grained (UFG) and nano-crystalline sheets with excellent mechanical properties. In the present study, the effect of the ARB process on the corrosion behavior of UFG and nano-crystalline 1050 aluminum alloy in a buffer borate solution (pH 5.5) has been investigated. The result of microhardness tests revealed that microhardness values increase with an increasing number of ARB cycles. A sharp increase in microhardness is seen after three ARB cycles, whereas moderate additional increases are observed afterward for up to nine cycles. Also, the XRD results showed that the mean crystallite size decreased to about 91 nm after nine cycles. The potentiodynamic plots show that as a result of ARB, the corrosion behavior of the UFG and nano-crystalline specimens improves, compared to the annealed 1050 aluminum alloy. Moreover, electrochemical impedance spectroscopy measurements showed that the polarization resistance increases with an increasing number of ARB cycles.

Combining Hard with Soft Materials in Nanoscale Under High-Pressure High-Temperature Conditions

NASA Technical Reports Server (NTRS)

Palosz, B.; Gierlotka, S.; Swiderska-Sroda, A.; Fietkiewicz, K.; Kalisz, G.; Grzanka, E.; Stel'makh, S.; Palosz, W.

2004-01-01

Nano-composites with a primary nanocrystalline ceramic matrix and a secondary nanocrystalline material (metal or semiconductor) were synthesized by infiltration of an appropriate liquid into ceramic compacts under pressures of up to 8 GPa and temperatures of up to 2000 K. The purpose of our work is to obtain nanocomposites which constitute homoger?ous mixtures of two phases, both forming nano- grains of about 10 nm in size. The high pressure is used to bring the porosity of the compacted powders down to the nano-scale and force a given liquid into the nano-sized pores. The advantage of the infiltration technique is that, in a single, continuous process, we start with a nanocrystalline powder, compress it to form the matrix of the composite, and crystallize and/or synthesize a second nanomaterial in the matrix pores. The key limitation of this technology is, that the pores in the matrix need to stay open during the entire process of infiltration. Thus the initial powder should form a rigid skeleton, otherwise the so-called self-stop process can limit cr block a further flow of the liquid phase and hinder the process of the composite formation. Therefore powders of only very hard ceramic materials like diamond, Sic, or Alz03, which can withstand a substantial external load without undesired deformation, can be used as the primary phase. With this technique, using diamond and S i c ceramic powders infiltrated by liquid metals (AI, Zn, Sn, Ag, Au) and semiconductors (Si, Ge, GaAs, CdTe), we obtained nano-composites with the grain size in the range of 10 - 30 nm. Our work addresses the key problem in manufacturing bulk nanocrystalline materials, i.e. preservation of nano-scale during the fabrication process. In this paper we discuss basic technical and methodological problems associated with nano-infiltration based on the results obtained for Zn-Sic composites.

Formation of high electrical-resistivity thin surface layer on carbonyl-iron powder (CIP) and thermal stability of nanocrystalline structure and vortex magnetic structure of CIP

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

Sugimura, K.; Miyajima, Y.; Sonehara, M.

2016-05-15

This study focuses on the carbonyl-iron powder (CIP) used in the metal composite bulk magnetic core for high-efficient/light-weight SiC/GaN power device MHz switching dc-dc converter, where the fine CIP with a mean diameter of 1.1 μm is used to suppress the MHz band eddy current inside the CIP body. When applying the CIP to composite core together with the resin matrix, high electrical resistivity layer must be formed on the CIP-surface in order to suppress the overlapped eddy current between adjacent CIPs. In this study, tens nm thick silica (SiO{sub 2}) was successfully deposited on the CIP-surface by using hydrolysismore » of TEOS (Si(OC{sub 2}H{sub 5}){sub 4}). Also tens nm thick oxidized layer of the CIP-surface was successfully formed by using CIP annealing in dry air. The SiC/GaN power device can operate at ambient temperature over 200 degree-C, and the composite magnetic core is required to operate at such ambient temperature. The as-made CIP had small coercivity below 800 A/m (10 Oe) due to its nanocrystalline-structure and had a single vortex magnetic structure. From the experimental results, both nanocrystalline and single vortex magnetic structure were maintained after heat-exposure of 250 degree-C, and the powder coercivity after same heat-exposure was nearly same as that of the as-made CIP. Therefore, the CIP with thermally stable nanocrystalline-structure and vortex magnetic state was considered to be heat-resistant magnetic powder used in the iron-based composite core for SiC/GaN power electronics.« less

Formation of high electrical-resistivity thin surface layer on carbonyl-iron powder (CIP) and thermal stability of nanocrystalline structure and vortex magnetic structure of CIP

NASA Astrophysics Data System (ADS)

Sugimura, K.; Miyajima, Y.; Sonehara, M.; Sato, T.; Hayashi, F.; Zettsu, N.; Teshima, K.; Mizusaki, H.

2016-05-01

This study focuses on the carbonyl-iron powder (CIP) used in the metal composite bulk magnetic core for high-efficient/light-weight SiC/GaN power device MHz switching dc-dc converter, where the fine CIP with a mean diameter of 1.1 μm is used to suppress the MHz band eddy current inside the CIP body. When applying the CIP to composite core together with the resin matrix, high electrical resistivity layer must be formed on the CIP-surface in order to suppress the overlapped eddy current between adjacent CIPs. In this study, tens nm thick silica (SiO2) was successfully deposited on the CIP-surface by using hydrolysis of TEOS (Si(OC2H5)4). Also tens nm thick oxidized layer of the CIP-surface was successfully formed by using CIP annealing in dry air. The SiC/GaN power device can operate at ambient temperature over 200 degree-C, and the composite magnetic core is required to operate at such ambient temperature. The as-made CIP had small coercivity below 800 A/m (10 Oe) due to its nanocrystalline-structure and had a single vortex magnetic structure. From the experimental results, both nanocrystalline and single vortex magnetic structure were maintained after heat-exposure of 250 degree-C, and the powder coercivity after same heat-exposure was nearly same as that of the as-made CIP. Therefore, the CIP with thermally stable nanocrystalline-structure and vortex magnetic state was considered to be heat-resistant magnetic powder used in the iron-based composite core for SiC/GaN power electronics.

Structure and magnetic properties of amorphous and nanocrystalline Fe 40Co 40Cu 0.5Zr 9Al 2Si 4B 4.5 alloys

NASA Astrophysics Data System (ADS)

Mitra, A.; Kim, H.-Y.; Louzguine, D. V.; Nishiyama, N.; Shen, B.; Inoue, A.

2004-07-01

Crystallisation behaviour and magnetic properties of as-spun and annealed Fe 40Co 40Cu 0.5Zr 9Al 2Si 4B 4.5 alloy have been studied. The annealing was performed at 873 K for 15 min. XRD and TEM studies shows the formation of nanocrystalline α-(Fe,Co)(SiAl) particles with 7.5±2 nm in diameter dispersed in an amorphous matrix. The Curie temperature of the as-spun amorphous ribbon is 736 K. Saturation magnetisation of the annealed sample decreases at a rate of 0.5 emu/g/K in the measured temperature range of 300-1000 K. Excellent room temperature AC magnetic properties are achieved for the nanocrystalline sample. The low value of the imaginary part of the permeability and the high cut-off frequency (20 kHz) suggest that the eddy current contribution in the annealed materials is low. The coercivity of the annealed sample remains almost constant at 95 A/m up to the frequency of 20 kHz. High saturation magnetisation, high Curie temperature and excellent soft magnetic properties in the nanocrystalline state suggests that Fe 40Co 40Cu 0.5Zr 9Al 2Si 4B 4.5 alloy is a strong candidate for high temperature magnetic application.

Biocompatibility and Corrosion Protection Behaviour of Hydroxyapatite Sol-Gel-Derived Coatings on Ti6Al4V Alloy

PubMed Central

El Hadad, Amir A.; Peón, Eduardo; García-Galván, Federico R.; Barranco, Violeta; Parra, Juan; Jiménez-Morales, Antonia; Galván, Juan Carlos

2017-01-01

The aim of this work was to prepare hydroxyapatite coatings (HAp) by a sol-gel method on Ti6Al4V alloy and to study the bioactivity, biocompatibility and corrosion protection behaviour of these coatings in presence of simulated body fluids (SBFs). Thermogravimetric/Differential Thermal Analyses (TG/DTA) and X-ray Diffraction (XRD) have been applied to obtain information about the phase transformations, mass loss, identification of the phases developed, crystallite size and degree of crystallinity of the obtained HAp powders. Fourier Transformer Infrared Spectroscopy (FTIR) has been utilized for studying the functional groups of the prepared structures. The surface morphology of the resulting HAp coatings was studied by Scanning Electron Microscopy (SEM). The bioactivity was evaluated by soaking the HAp-coatings/Ti6Al4V system in Kokubo’s Simulated Body Fluid (SBF) applying Inductively Coupled Plasma (ICP) spectrometry. 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide (MTT) and Alamar blue cell viability assays were used to study the biocompatibility. Finally, the corrosion behaviour of HAp-coatings/Ti6Al4V system was researched by means of Electrochemical Impedance Spectroscopy (EIS). The obtained results showed that the prepared powders were nanocrystalline HAp with little deviations from that present in the human bone. All the prepared HAp coatings deposited on Ti6Al4V showed well-behaved biocompatibility, good bioactivity and corrosion protection properties. PMID:28772455

Biocompatibility and Corrosion Protection Behaviour of Hydroxyapatite Sol-Gel-Derived Coatings on Ti6Al4V Alloy.

PubMed

El Hadad, Amir A; Peón, Eduardo; García-Galván, Federico R; Barranco, Violeta; Parra, Juan; Jiménez-Morales, Antonia; Galván, Juan Carlos

2017-01-24

The aim of this work was to prepare hydroxyapatite coatings (HAp) by a sol-gel method on Ti6Al4V alloy and to study the bioactivity, biocompatibility and corrosion protection behaviour of these coatings in presence of simulated body fluids (SBFs). Thermogravimetric/Differential Thermal Analyses (TG/DTA) and X-ray Diffraction (XRD) have been applied to obtain information about the phase transformations, mass loss, identification of the phases developed, crystallite size and degree of crystallinity of the obtained HAp powders. Fourier Transformer Infrared Spectroscopy (FTIR) has been utilized for studying the functional groups of the prepared structures. The surface morphology of the resulting HAp coatings was studied by Scanning Electron Microscopy (SEM). The bioactivity was evaluated by soaking the HAp-coatings/Ti6Al4V system in Kokubo's Simulated Body Fluid (SBF) applying Inductively Coupled Plasma (ICP) spectrometry. 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl tetrazolium bromide (MTT) and Alamar blue cell viability assays were used to study the biocompatibility. Finally, the corrosion behaviour of HAp-coatings/Ti6Al4V system was researched by means of Electrochemical Impedance Spectroscopy (EIS). The obtained results showed that the prepared powders were nanocrystalline HAp with little deviations from that present in the human bone. All the prepared HAp coatings deposited on Ti6Al4V showed well-behaved biocompatibility, good bioactivity and corrosion protection properties.

Soft magnetic characteristics of laminated magnetic block cores assembled with a high Bs nanocrystalline alloy

NASA Astrophysics Data System (ADS)

Yao, Atsushi; Inoue, Masaki; Tsukada, Kouhei; Fujisaki, Keisuke

2018-05-01

This paper focuses on an evaluation of core losses in laminated magnetic block cores assembled with a high Bs nanocrystalline alloy in high magnetic flux density region. To discuss the soft magnetic properties of the high Bs block cores, the comparison with amorphous (SA1) block cores is also performed. In the high Bs block core, both low core losses and high saturation flux densities Bs are satisfied in the low frequency region. Furthermore, in the laminated block core made of the high Bs alloy, the rate of increase of iron losses as a function of the magnetic flux density remains small up to around 1.6 T, which cannot be realized in conventional laminated block cores based on amorphous alloy. The block core made of the high Bs alloy exhibits comparable core loss with that of amorphous alloy core in the high-frequency region. Thus, it is expected that this laminated high Bs block core can achieve low core losses and high saturation flux densities in the high-frequency region.

Stress-induced solid-state amorphization of nanocrystalline Ni and NiZr investigated by atomistic simulations

NASA Astrophysics Data System (ADS)

Meraj, Md.; Deng, Chuang; Pal, Snehanshu

2018-01-01

In this study, the feasibility of stress induced solid-state amorphization (SSA) of nanocrystalline (NC) Ni and NiZr alloys having ˜10 nm grain size has been investigated under constant tensile load (uniaxial and triaxial) via molecular dynamics simulations. In order to track the structural evaluation in both NC Ni and NiZr alloys during the SSA process, various types of analysis have been used, including simulated X-ray diffraction, centro-symmetry parameter, Voronoi cluster, common neighbor analysis, and radial distribution function. It is found that SSA in both NC Ni and NiZr alloys can only be achieved under triaxial loading conditions, and the hydrostatic tensile stress required for SSA is significantly lower when at. % Zr is increased in the NC NiZr alloy. Specifically, SSA in NC Ni and Ni-5 at. % Zr alloy was observed only when the temperature and hydrostatic tensile stress reached 800 K and 6 GPa, while SSA could occur in NC Ni-10 at. % Zr alloy under just 2 GPa of hydrostatic tensile stress at 300 K.

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.

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

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

Balagurov, Anatoly M.; Bobrikov, Ivan A.; Bokuchava, Gizo D.

2015-11-15

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of themore » material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.« less

Removal of cadmium(II) ions from aqueous solution using Ni (15 wt.%)-doped α-Fe2O3 nanocrystals: equilibrium, thermodynamic, and kinetic studies.

PubMed

OuldM'hamed, Mohamed; Khezami, L; Alshammari, Abdulrahman G; Ould-Mame, S M; Ghiloufi, I; Lemine, O M

2015-01-01

The present publication investigates the performance of nanocrystalline Ni (15 wt.%)-doped α-Fe2O3 as an effective nanomaterial for the removal of Cd(II) ions from aqueous solutions. The nanocrystalline Ni-doped α-Fe2O3 powders were prepared by mechanical alloying, and characterized by X-ray diffraction and a vibrating sample magnetometer. Batch-mode experiments were realized to determine the adsorption equilibrium, kinetics, and thermodynamic parameters of toxic heavy metal ions by Ni (15 wt.%)-doped α-Fe2O3. The adsorption isotherms data were found to be in good agreement with the Langmuir model. The adsorption capacity of Cd(II) ion reached a maximum value of about 90.91 mg g(-1) at 328 K and pH 7. The adsorption process kinetics was found to comply with pseudo-second-order rate law. Thermodynamic parameters related to the adsorption reaction, free energy change, enthalpy change and entropy change, were evaluated. The found values of free energy and enthalpy revealed a spontaneous endothermic adsorption-process. Moreover, the positive entropy suggests an increase of randomness during the process of heavy metal removal at the adsorbent-solution interface.

Methods of forming steel

DOEpatents

Branagan, Daniel J.; Burch, Joseph V.

2001-01-01

In one aspect, the invention encompasses a method of forming a steel. A metallic glass is formed and at least a portion of the glass is converted to a crystalline steel material having a nanocrystalline scale grain size. In another aspect, the invention encompasses another method of forming a steel. A molten alloy is formed and cooled the alloy at a rate which forms a metallic glass. The metallic glass is devitrified to convert the glass to a crystalline steel material having a nanocrystalline scale grain size. In yet another aspect, the invention encompasses another method of forming a steel. A first metallic glass steel substrate is provided, and a molten alloy is formed over the first metallic glass steel substrate to heat and devitrify at least some of the underlying metallic glass of the substrate.

Infiltration sintering properties of Ni-4B-4Si(wt.%) alloy powders

NASA Astrophysics Data System (ADS)

Yang, Q.; Zhang, X. C.; Wang, F. L.; Zou, J. T.

2018-01-01

The Ni-4B-4Si(wt.%) alloy powders were infiltrated into the nickel skeletons, the effects of sintering temperatures (1050-1150 °C) and skeletons (loose and compact nickel powders) on the microstructures and hardness of the sintered alloys were investigated. The Ni-B-Si alloy sintered at 1100 °C consisted of γ-Ni and Ni3B, and Si mainly solid soluted in the γ-Ni. The loose nickel powders favored to the infiltration of Ni-B-Si liquid alloy into the nickel skeletons, the sintered alloys exhibited dense microstructures and good interfacial bonding with Ni substrates. The interfacial hardness was equal to that of the sintered alloys and Ni substrates. Loose nickel powders ensured the density and interfacial bonding of the sintered alloys, the infiltration sintering process can be simplified and easily applied to practice.

Structural analysis of nanocrystalline ZnTe alloys synthesized by melt quenching technique

NASA Astrophysics Data System (ADS)

Singh, Harinder; Singh, Tejbir; Thakur, Anup; Sharma, Jeewan

2018-05-01

Nanocrystalline ZnxTe100-x (x=0, 5, 20, 30, 40, 50) alloys have been synthesized using melt quenching technique. Energy-dispersive X-Ray spectroscopy (EDS) has been used to verify the elemental composition of samples. Various absorption modes are recorded from Fourier transform infrared spectroscopy (FTIR) confirming the formation of ZnTe. The structural study has been performed using X-Ray Diffraction (XRD) method. All synthesized samples have been found to be nanocrystalline in nature with average crystallite size in the range from 49.3 nm to 77.1 nm. Results have shown that Zn0Te100 exhibits hexagonal phase that transforms into a cubic ZnTe phase as the amount of zinc is increased. Pure ZnTe phase has been obtained for x = 50. The texture coefficient (Tc) has been calculated to find the prominent orientations of different planes.

Thermal Stability of Milled Nanocrystalline Tungsten Powders

DTIC Science & Technology

2011-05-01

v Acknowledgments This research is supported by mission funding from the Depleted Uranium Replacement Program and is the result of collaborative...L.; Reddy, R. G. Synthesis of Titanium Carbide Nano-powders by Thermal Plasma. Scripta Materialia 2005, 52 (12), 1253–1258. 4. Karagedov, G. R

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.

Reactive Ball Milling to Fabricate Nanocrystalline Titanium Nitride Powders and Their Subsequent Consolidation Using SPS

NASA Astrophysics Data System (ADS)

El-Eskandarany, M. Sherif

2017-05-01

The room-temperature reactive ball milling (RBM) approach was employed to synthesize nanostructured fcc-titanium nitride (TiN) powders, starting from milling hcp-titanium (Ti) powders under 10 bar of a nitrogen gas atmosphere, using a roller mill. During the first and intermediate stage of milling, the agglomerated Ti powders were continuously disintegrated into smaller particles with fresh surfaces. Increasing the RBM time led to an increase in the active-fresh surfaces of Ti, resulting increasing of the mole fraction of TiN against unreacted hcp-Ti. Toward the end of the RBM time (20 h), ultrafine spherical powder (with particles 0.5 μm in diameter) of the fcc-TiN phase was obtained, composed of nanocrystalline grains with an average diameter of 8 nm. The samples obtained after different stages of RBM time were consolidated under vacuum at 1600 °C into cylindrical bulk compacts of 20 mm diameter, using spark plasma sintering technique. These compacts that maintained their nanocrystalline characteristics with an average grain size of 56 nm in diameter, possessed high relative density (above 99% of the theoretical density). The Vickers hardness of the as-consolidated TiN was measured and found to be 22.9 GPa. The modulus of elasticity and shear modulus of bulk TiN were measured by a nondestructive test and found to be 384 and 189 GPa, respectively. In addition, the coefficient of friction of the end-product TiN bulk sample was measured and found to be 0.35.

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.

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

Article and method for making an article

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

Lacy, Benjamin Paul; Schick, David Edward; Kottilingam, Srikanth Chandrudu

An article and a method for making shaped cooling holes in an article are provided. The method includes the steps of depositing a metal alloy powder to form an initial layer including at least one aperture, melting the metal alloy powder with a focused energy source to transform the powder layer to a sheet of metal alloy, sequentially depositing an additional layer of the metal alloy powder to form a layer including at least one aperture corresponding to the at least one aperture in the initial layer, melting the additional layer of the metal alloy powder with the focused energymore » source to increase the sheet thickness, and repeating the steps of sequentially depositing and melting the additional layers of metal alloy powder until a structure including at least one aperture having a predetermined profile is obtained. The structure is attached to a substrate to make the article.« less

Formation of nanocrystalline diamond in polymer like carbon films deposited by plasma CVD.

PubMed

Bhaduri, A; Chaudhuri, P

2009-09-01

Conventional plasma enhanced chemical vapour deposition (PECVD) method is generally not suitable for the growth of nanocrystalline diamond (NCD) films. However, our study shows that conditions favourable for powder formation help to grow large amount of nanocrystallites in conventional PECVD. With CH4 as the carbon source gas, dilution with Ar and moderate (50 W) rf power enhances formations of powders (nanoparticles) and C2 dimers within the plasma. On the other hand, with pure CH4 or with hydrogen diluted CH4, powder formation as also NCD growth is hindered. It is proposed that the nanoparticles formed in the plasma act as the "islands" while the C2 dimers are the "seeds" for the NCD growth. The structure of the films deposited on the grounded anode under different conditions of dilution has been studied. It is observed that with high Ar dilution the films contain NCD embedded in polymer like carbon (PLC) matrix.

Fuel additives and heat treatment effects on nanocrystalline zinc ferrite phase composition

NASA Astrophysics Data System (ADS)

Hu, Ping; Pan, De-an; Wang, Xin-feng; Tian, Jian-jun; Wang, Jian; Zhang, Shen-gen; Volinsky, Alex A.

2011-03-01

Nanocrystalline ZnFe 2O 4 powder was prepared by the auto-combustion method using citric acid, acetic acid, carbamide and acrylic acid as fuel additives. Pure spinel zinc ferrite with the crystallite size of about 15 nm can be obtained by using acrylic acid as fuel additive. Samples prepared using other fuel additives contain ZnO impurities. In order to eliminate ZnO impurities, the sample prepared with citric acid as fuel additive was annealed at different temperatures up to 1000 °C in air and in argon. Annealed powders have pure ZnFe 2O 4 phase when annealing temperature is higher than 650 °C in air. Sample annealed at 650 °C in air is paramagnetic. However, annealed powders become a mixture of Fe 3O 4 and FeO after annealing at 1000 °C in argon atmosphere due to Zn volatility and the reduction reaction.

Microstructure of rapidly solidified Nb-based pre-alloyed powders for additive manufacturing

NASA Astrophysics Data System (ADS)

Guo, Yueling; Jia, Lina; Kong, Bin; Zhang, Shengnan; Zhang, Fengxiang; Zhang, Hu

2017-07-01

For powder-based additive manufacturing, sphere-shaped Nb-37Ti-13Cr-2Al-1Si pre-alloyed powders were prepared by plasma rotating electrode processing (PREP). The microstructure, surface oxidation and microhardness of the pre-alloyed powders were systematically investigated. Results showed that the main phases were Nb solid solution (Nbss) and Cr2Nb. The Cr2Nb phases were further determined using transmission electron microscopy (TEM). Fine dendrite structures were observed in the as-fabricated pre-alloyed powders, which transformed to large grains after heat treatment (HT) at 1450 °C for 3 h. With the increase of powder size, the secondary dendrite arm spacing (SDAS) increased and the microhardness (HV) decreased. A clean powder surface free of oxide particles was obtained by PREP and an oxide layer with 9.39 nm in thickness was generated on the powder surface. Compared with Cr- and Nb-oxides, more Ti-oxides were formed on outmost powder surface with a higher content of Ti (up to 47.86 at.%). The differences upon the microstructure and microhardness of the pre-alloyed powders with different sizes were discussed.

Synthesis of nanocrystalline TiO 2 in toluene by a solvothermal route

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Tae Chung, Su; Son, Se-Mo

2003-07-01

A solvothermal synthetic method to TiO 2 nanoparticles has been investigated in toluene solutions with titanium isopropoxide (TIP) as precursor. Weight ratios of precursor to solvent prepared in the mixture are 5/100, 10/100, 20/100, 30/100 and 40/100. At the weight ratio of 10/100, 20/100 and 30/100, TiO 2 nanocrystalline particles were obtained after synthesis at 250°C for 3 h in an autoclave. X-ray diffraction and tranmission electron microscopy shows that the product has uniform anatase structure with average particle size below 20 nm. As the composition of TIP in the solution increases, the particle size of TiO 2 powder tends to increase. At 5/100 and 40/100, however, pale yellow colloidal solution is obtained after synthesis and crystalline phase of TiO 2 is not produced. The specific surface area of the TiO 2 nanocrystalline powder was also investigated using BET surface area analyzer.

Nanocrystalline cellulose as an eco-friendly reinforcing additive to polyurethane coating for augmented anticorrosive behavior.

PubMed

Abd El-Fattah, M; Hasan, Abdulraheim M A; Keshawy, Mohamed; El Saeed, Ashraf M; Aboelenien, Ossama M

2018-03-01

Nanocrystalline cellulose (NCC) and micro-powdered cellulose (MPC) were extracted from rice straw by mechanical and alkali treatment methods, then characterized via infrared spectroscopy and dynamic light scattering. A series of polyurethane nanocrystalline cellulose composite (PNCCC) and polyurethane micro-powdered cellulose composite (PMPCC) coatings were prepared with various loading levels of NCC and MPC from 0.5 to 2.0 wt.%, and the coatings were applied onto the pretreated mild steel substrate at room temperature. The results showed that the NCC and MPC influenced positively the studied properties of the polyurethane coating; furthermore the most pronounced anticorrosive properties were obtained at 1 wt.% NCC and MPC, as confirmed by open circuit potential (OCP) study, electrochemical impedance spectroscopy (EIS) study and salt spray test. However, the optimum enhancement of mechanical properties was found at 1.5 wt.% loading level, after which further loading of NCC and MPC led to the reduction in the mechanical properties. Copyright © 2018 Elsevier Ltd. All rights reserved.

Phase composition and magnetic properties in hot deformed magnets based on Misch-metal

NASA Astrophysics Data System (ADS)

Ma, Q.; Zhang, Z. Y.; Zhang, X. F.; Hu, Z. F.; Liu, Y. L.; Liu, F.; Jv, X. M.; Wang, J.; Li, Y. F.; Zhang, J. X.

2018-04-01

In this paper, the Rare-earth Iron Boron (RE-Fe-B) magnets were fabricated successfully by using the double main phase method through mixing the Neodymium Iron Boron (Nd-Fe-B) powders and Misch-metal Iron Boron (MM-Fe-B) powders with different ratio. Aiming at the nanocrystalline RE2Fe14B magnets prepared by using spark plasma sintering technology, phase structure and magnetic properties were investigated. It is found that the Misch-metal (MM) alloys promote the domain nucleation during the the process of magnetization reversal and then damage the coercivity (Hcj) of isotropic RE2Fe14B magnets, while the Hcj could still remain more than 1114.08 kA/m when the mass proportion of MM (simplified as: "a") is 30%. Curie temperature and phase structure were also researched. Two kinds of mixed-solid-solution (MSS) main phases with different Lanthanum (La) and Cerium (Ce) content were believed to be responsible for the two curie temperature of the RE2Fe14B magnets with "a" ≥20%. This is resulted from the inhomogeneous elemental distribution of RE2Fe14B phase.

Electrodeposition of Nanocrystalline Ni–Fe Alloy Coatings Based on 1-Butyl-3-Methylimidazolium-Hydrogen Sulfate Ionic Liquid.

PubMed

He, Xinkuai; Zhang, Chuang; Zhu, Qingyun; Lu, Haozi; Cai, Youxing; Wu, Luye

2017-02-01

The electrodeposition of nanocrystalline Ni–Fe alloy coatings and associated nucleation/growth processes are investigated on the glassy carbon (GC) electrode in 1-butyl-3-methylimidazolium-hydrogen sulfate ([BMIM]HSO4) ionic liquid (IL). Cyclic voltammetric data suggest that the co-electrodeposition of Ni–Fe alloys is quasi-reversible. Moreover, chronoamperometry results indicate that the electrodeposition proceeds via a simultaneous nucleation and three-dimensional growth mechanism. In addition, the effects of electrodeposition potential and electrolyte temperature on the coating thickness and Fe content are also studied. The microstructure and composition of the Ni–Fe alloy coatings on Cu substrate are investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy-dispersive spectroscopy (EDS). SEM observations show that these electrodeposits present a dense and compact structure, EDS analysis indicates that the coatings are composed of Ni and Fe, XRD pattern shows the coatings are crystalline with a face-centred cubic (fcc) structure. Tafel plots reveal that the Ni–Fe alloy prepared from [BMIM]HSO4 IL presents better corrosion resistance than that of pure Ni.

Structural and magnetic properties on the Fe-B-P-Cu-W nano-crystalline alloy system

NASA Astrophysics Data System (ADS)

Zhang, Yan; Wang, Yaocen; Makino, Akihiro

2018-04-01

In the present article, the structural and soft magnetic properties of Fe-B-P-Cu alloy system with W addition have been studied as well as the annealing configurations required for magnetic softness. It is found that the substitution of B by W deteriorates the soft magnetic properties after annealing. The reason of such impact with W addition may lie in the insufficient bonding strength between W and B so that the addition of W is not effective enough to suppress grain growth against the high concentration and high crystallization tendency of Fe during annealing. The addition of 4 at.% W is also found to reduce the saturation magnetization of the nano-crystalline alloy by 14%. It is also found that the addition of P in the Fe-based alloys could help reduce the coercivity upon annealing with high heating rate. The existence of P could also help slightly increase the overall saturation magnetization by enhancing the electron transfer away from Fe in the residual amorphous structure.

Thermal conductivity of nanocrystalline SiGe alloys using molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Abs da Cruz, Carolina; Katcho, Nebil A.; Mingo, Natalio; Veiga, Roberto G. A.

2013-10-01

We have studied the effect of nanocrystalline microstructure on the thermal conductivity of SiGe alloys using molecular dynamics simulations. Nanograins are modeled using both the coincidence site lattice and the Voronoi tessellation methods, and the thermal conductivity is computed using the Green-Kubo formalism. We analyze the dependence of the thermal conductivity with temperature, grain size L, and misorientation angle. We find a power dependence of L1/4 of the thermal conductivity with the grain size, instead of the linear dependence shown by non-alloyed nanograined systems. This dependence can be derived analytically underlines the important role that disorder scattering plays even when the grains are of the order of a few nm. This is in contrast to non-alloyed systems, where phonon transport is governed mainly by the boundary scattering. The temperature dependence is weak, in agreement with experimental measurements. The effect of angle misorientation is also small, which stresses the main role played by the disorder scattering.

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.

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

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

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

Citrate gel-combustion synthesis and sintering of nanocrystalline ThO2 powders

NASA Astrophysics Data System (ADS)

Sanjay Kumar, D.; Ananthasivan, K.; Amirthapandian, S.; Dasgupta, Arup; Jogeswara Rao, G.

2017-12-01

A systematic study of the influence of citric acid to nitrate mole (R) ratio (R = 0 to 0.50) on the citrate gel-combustion synthesis of nanocrystalline (nc) ThO2 in bulk quantities (30 g) by using citrate gel-combustion was carried out. The nc-ThO2 powders were characterized for their bulk density, size distribution of particles, specific surface area, carbon residue and X-ray crystallite size. All these powders were compacted at pressures varying from 60 to 353 MPa and sintered by using the "two-step sintering" method. Powders prepared from a mixture with an "R" value of 0.125 compacted at 243 MPa yielded a maximum sintered density of 98.8 ± 0.3% T.D. For nc-ThO2, this is the highest sintered density reported so far. The microstructural investigations on nc-ThO2 powders were carried out by using both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM images of the sintered thoria monoliths revealed faceted grains with well defined grain boundaries. Shrinkage anisotropy factor (α) revealed that the compacts prepared from the powders obtained from starting mixtures with R values of 0.125-0.50 had undergone uniform sintering (near isotropic shrinkage).

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

NASA Astrophysics Data System (ADS)

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

2017-05-01

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

New atom probe approaches to studying segregation in nanocrystalline materials.

PubMed

Samudrala, S K; Felfer, P J; Araullo-Peters, V J; Cao, Y; Liao, X Z; Cairney, J M

2013-09-01

Atom probe is a technique that is highly suited to the study of nanocrystalline materials. It can provide accurate atomic-scale information about the composition of grain boundaries in three dimensions. In this paper we have analysed the microstructure of a nanocrystalline super-duplex stainless steel prepared by high pressure torsion (HPT). Not all of the grain boundaries in this alloy display obvious segregation, making visualisation of the microstructure challenging. In addition, the grain boundaries present in the atom probe data acquired from this alloy have complex shapes that are curved at the scale of the dataset and the interfacial excess varies considerably over the boundaries, making the accurate characterisation of the distribution of solute challenging using existing analysis techniques. In this paper we present two new data treatment methods that allow the visualisation of boundaries with little or no segregation, the delineation of boundaries for further analysis and the quantitative analysis of Gibbsian interfacial excess at boundaries, including the capability of excess mapping. Copyright © 2013 Elsevier B.V. All rights reserved.

Visualizing decoupling in nanocrystalline alloys: A FORC-temperature analysis

NASA Astrophysics Data System (ADS)

Rivas, M.; Martínez-García, J. C.; Gorria, P.

2016-02-01

Devitrifying ferromagnetic amorphous precursors in the adequate conditions may give rise to disordered assemblies of densely packed nanocrystals with extraordinary magnetic softness well explained by the exchange coupling among multiple crystallites. Whether the magnetic exchange interaction is produced by direct contact or mediated by the intergranular amorphous matrix has a strong influence on the behaviour of the system above room temperature. Multi-phase amorphous-nanocrystalline systems dramatically harden when approaching the amorphous Curie temperature (TC) due to the hard grains decoupling. The study of the thermally induced decoupling of nanosized crystallites embedded in an amorphous matrix has been performed in this work by the first-order reversal curves (FORCs) analysis. We selected a Fe-rich amorphous alloy with TC = 330 K, in order to follow the evolution of the FORC diagrams obtained below and above such temperature in samples with different percentages of nanocrystalline phase. The existence of up to four regions exhibiting unlike magnetic behaviours is unambiguously determined from the temperature evolution of the FORC.

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

Revealing Grain Boundary Sliding from Textures of a Deformed Nanocrystalline Pd–Au Alloy

PubMed Central

Skrotzki, Werner; Zhao, Yajun; Pukenas, Aurimas; Birringer, Rainer

2018-01-01

Employing a recent modeling scheme for grain boundary sliding [Zhao et al. Adv. Eng. Mater. 2017, doi:10.1002/adem.201700212], crystallographic textures were simulated for nanocrystalline fcc metals deformed in shear compression. It is shown that, as grain boundary sliding increases, the texture strength decreases while the signature of the texture type remains the same. Grain boundary sliding affects the texture components differently with respect to intensity and angular position. A comparison of a simulation and an experiment on a Pd–10 atom % Au alloy with a 15 nm grain size reveals that, at room temperature, the predominant deformation mode is grain boundary sliding contributing to strain by about 60%. PMID:29370130

Advanced powder metallurgy aluminum alloys via rapid solidification technology

NASA Technical Reports Server (NTRS)

Ray, R.

1984-01-01

Aluminum alloys containing 10 to 11.5 wt. pct. of iron and 1.5 to 3 wt. pct. of chromium using the technique of rapid solidification powder metallurgy were studied. Alloys were prepared as thin ribbons (.002 inch thick) rapidly solidified at uniform rate of 10(6) C/second by the melt spinning process. The melt spun ribbons were pulverized into powders (-60 to 400 mesh) by a rotating hammer mill. The powders were consolidated by hot extrusion at a high reduction ratio of 50:1. The powder extrusion temperature was varied to determine the range of desirable processing conditions necessary to yield useful properties. Powders and consolidated alloys were characterized by SEM and optical metallography. The consolidated alloys were evaluated for (1) thermal stability, (2) tensile properties in the range, room temperature to 450 F, and (3) notch toughness in the range, room temperature to 450 F.

Nanocrystalline hydroxyapatite doped with selenium oxyanions: a new material for potential biomedical applications.

PubMed

Kolmas, Joanna; Oledzka, Ewa; Sobczak, Marcin; Nałęcz-Jawecki, Grzegorz

2014-06-01

Selenium-substituted hydroxyapatites containing selenate SeO4(2-) or selenite SeO3(2-) ions were synthesized using a wet precipitation method. The selenium content was determined by atomic absorbance spectrometry. The raw, unsintered powders were also characterized using powder X-ray diffraction, middle-range FT-IR spectroscopy and transmission electron microscopy with energy-dispersive X-ray spectroscopic microanalysis. The synthesized apatites were found to be pure and nanocrystalline with a crystal size similar to that in bone mineral. The incorporation of selenium oxyanions into the crystal lattice was confirmed. The toxicity of hydroxyapatites containing selenite or selenate ions was evaluated with a protozoan assay and bacterial luminescence test. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of TbCu7-type Sm-Fe powders by low-temperature HDDR treatment

NASA Astrophysics Data System (ADS)

Takagi, Kenta; Jinno, Miho; Ozaki, Kimihiro

2018-05-01

Low-temperature hydrogen-disproportionation-desorption-recombination (HDDR) treatment of Sm-Fe alloy powder was conducted to prepare a metastable TbCu7 type Sm-Fe alloy powder with a grain size of more than a few hundreds of nanometers. While a treatment temperature above 700 °C produced the familiar Th2Zn17 type alloy, one below 600 °C resulted in successful synthesis of the TbCu7 type Sm-Fe alloy with submicron-size grains. This TbCu7 type alloy powder, however, showed no significant improvement in magnetic properties compared to the Th2Zn17 type, as its composition was estimated to be near SmFe8.5 and thus did not achieve the expected Fe-rich composition. Therefore, cross-sectional transmission electron microscope observation of the unfinished TbCu7 type alloy powder was conducted in order to explore means of forming the Fe-rich phase.

Hydrogen Storage Characteristics of Nanocrystalline and Amorphous Nd-Mg-Ni-Based NdMg12-Type Alloys Synthesized via Mechanical Milling

NASA Astrophysics Data System (ADS)

Zhang, Yanghuan; Shang, Hongwei; Hou, Zhonghui; Yuan, Zeming; Yang, Tai; Qi, Yan

2016-12-01

In this study, Mg was partially substituted by Ni with the intent of improving the hydrogen storage kinetics performance of NdMg12-type alloy. Mechanical milling technology was adopted to fabricate the nanocrystalline and amorphous NdMg11Ni + x wt pct Ni ( x = 100, 200) alloys. The effects of Ni content and milling duration on the microstructures and hydrogen storage kinetics of as-milled alloys have been systematically investigated. The structures were characterized by XRD and HRTEM. The electrochemical hydrogen storage properties were tested by an automatic galvanostatic system. Moreover, the gaseous hydrogen storage properties were investigated by Sievert apparatus and a differential scanning calorimeter connected with a H2 detector. Hydrogen desorption activation energy of alloy hydrides was estimated by using Arrhenius and Kissinger methods. The results reveal that the increase of Ni content dramatically ameliorates the gaseous and electrochemical hydrogen storage kinetics performance of the as-milled alloys. Furthermore, high rate discharge ability (HRD) reach the maximum value with the variation of milling time. The maximum HRDs of the NdMg11Ni + x wt pct Ni ( x = 100, 200) alloys are 80.24 and 85.17 pct. The improved gaseous hydrogen storage kinetics of alloys via increasing Ni content and milling time can be attributed to a decrease in the hydrogen desorption activation energy.

Oxidized nanocrystalline Fe-Cu pseudoalloy subjected to high pressure and electrodischarge pulses: Mössbauer and x-ray investigations

NASA Astrophysics Data System (ADS)

Gavriliuk, A. G.; Voitkovsky, V. S.; Sidorov, V. A.; Filonenko, V. P.; Tsiok, O. B.; Khvostantsev, L. G.

1998-05-01

Nanocrystalline Fe15Cu85 pseudoalloy has been subjected to pulsed heating up to 1500 K at high pressure (8 GPa). Two regimes were studied: the direct heating using electrodischarge through the sample and indirect heating with the use of cylindrical heater around the sample. The temperature and time conditions in both types of experiments were adjusted to be equivalent. The discharge parameters (stored energy, discharge time, and magnitude of current pulse) were sufficient to move defects by conduction electrons, but insufficient to melt the sample. The properties of treated samples were studied using Mössbauer absorption spectra and x-ray diffraction for three types of samples: (a) primary powder treated by high pressure up to 8 GPa, (b) powder subjected to indirect pulsed heating at 8 GPa, (c) powder treated by electrical pulses at 8 GPa. The x-ray diffraction pattern of primary powder exhibits peaks of copper, iron, and copper oxide (CuO). The Mössbauer spectrum of primary powder exhibits six peaks of alpha iron and some peaks near zero velocity due to the small iron clusters in the copper matrix and ultrafine clusters of paramagnetic phase x-Fe2O3. The transformation of CuO to Cu2O takes place in the course of indirect heating, the Mössbauer spectrum being almost unchanged. The direct electrodischarge heating causes the appearance of new magnetic phase with the magnetic field on iron nucleus 505 kOe, which corresponds to α-Fe2O3. The formation of α-Fe2O3 was confirmed by x-ray diffraction. At the same time the transformation of CuO to Cu2O is incomplete. These experiments demonstrate that high density current pulses, causing the electron wind, can be a useful tool to influence the structure of nanocrystalline powder.

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.

Size effects of nano-spaced basal stacking faults on the strength and deformation mechanisms of nanocrystalline pure hcp metals

NASA Astrophysics Data System (ADS)

Wang, Wen; Jiang, Ping; Yuan, Fuping; Wu, Xiaolei

2018-05-01

The size effects of nano-spaced basal stacking faults (SFs) on the tensile strength and deformation mechanisms of nanocrystalline pure cobalt and magnesium have been investigated by a series of large-scale 2D columnar and 3D molecular dynamics simulations. Unlike the strengthening effect of basal SFs on Mg alloys, the nano-spaced basal SFs are observed to have no strengthening effect on the nanocrystalline pure cobalt and magnesium from MD simulations. These observations could be attributed to the following two reasons: (i) Lots of new basal SFs are formed before (for cobalt) or simultaneously with (for magnesium) the other deformation mechanisms (i.e. the formation of twins and the < c + a > edge dislocations) during the tensile deformation; (ii) In hcp alloys, the segregation of alloy elements and impurities at typical interfaces, such as SFs, can stablilise them for enhancing the interactions with dislocation and thus elevating the strength. Without such segregation in pure hcp metals, the < c + a > edge dislocations can cut through the basal SFs although the interactions between the < c + a > dislocations and the pre-existing SFs/newly formed SFs are observed. The nano-spaced basal SFs are also found to have no restriction effect on the formation of deformation twins.

Magnetoelectric coupling characteristics in multiferroic heterostructures with different thickness of nanocrystalline soft magnetic alloy

NASA Astrophysics Data System (ADS)

Chen, Lei; Wang, Yao

2016-05-01

Magnetoelectric(ME) coupling characteristics in multiferroic heterostructures with different thickness of nanocrystalline soft magnetic alloy has been investigated at low frequency. The ME response with obvious hysteresis, self-biased and dual-peak phenomenon is observed for multiferroic heterostructures, which results from strong magnetic interactions between two ferromagnetic materials with different magnetic properties, magnetostrictions and optimum bias magnetic fields Hdc,opti. The proposed multiferroic heterostructures not only enhance ME coupling significantly, but also broaden dc magnetic bias operating range and overcomes the limitations of narrow bias range. By optimizing the thickness of nanocrystalline soft magnetic alloy Tf, a significantly zero-biased ME voltage coefficient(MEVC) of 14.8mV/Oe (185 mV/cmṡ Oe) at Tf = 0.09 mm can be obtained, which is about 10.8 times as large as that of traditional PZT/Terfenol-D composite with a weak ME coupling at zero bias Hdc,zero. Furthermore, when Tf increases from 0.03 mm to 0.18 mm, the maximum MEVC increases nearly linearly with the increased Tf at Hdc,opti. Additionally, the experimental results demonstrate the ME response for multiferroic heterostructures spreads over a wide magnetic dc bias operating range. The excellent ME performance provides a promising and practicable application for both highly sensitive magnetic field sensors without bias and ME energy harvesters.

Extremely hard amorphous-crystalline hybrid steel surface produced by deformation induced cementite amorphization

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

Guo, Wei; Meng, Yifei; Zhang, Xie

Amorphous and nanograined (NG) steels are two categories of strong steels. However, over the past decade, their application has been hindered by their limited plasticity, the addition of expensive alloying elements, and processing challenges associated with producing bulk materials. Here in this work, we report that the surface of a carburized Fe-Mn-Si martensitic steel with extremely low elemental alloying additions can be economically fabricated into an amorphous-nanocrystalline hybrid structure. Atom probe tomography and nanobeam diffraction of a hard turned steel surface together with molecular dynamics (MD) simulations reveal that the original cementite surface structure experiences a size-dependent amorphization and phasemore » transformation during heavy plastic deformation. MD simulations further show that the martensite-cementite interface serves as a nucleation site for cementite amorphization, and that cementite can become disordered if further strained when the cementite particles are relatively small. These graded structures exhibit a surface hardness of ~16.2 GPa, which exceeds the value of ~8.8 GPa for the original nanocrystalline martensitic steel and most nanocrystalline steels reported before. Finally, this practical and cost-efficient approach for producing a hard surface with retained bulk ductility and toughness can provide expanded opportunities for producing an amorphous-crystalline hybrid structure in steels and other alloy systems.« less

Extremely hard amorphous-crystalline hybrid steel surface produced by deformation induced cementite amorphization

DOE PAGES

Guo, Wei; Meng, Yifei; Zhang, Xie; ...

2018-04-11

Amorphous and nanograined (NG) steels are two categories of strong steels. However, over the past decade, their application has been hindered by their limited plasticity, the addition of expensive alloying elements, and processing challenges associated with producing bulk materials. Here in this work, we report that the surface of a carburized Fe-Mn-Si martensitic steel with extremely low elemental alloying additions can be economically fabricated into an amorphous-nanocrystalline hybrid structure. Atom probe tomography and nanobeam diffraction of a hard turned steel surface together with molecular dynamics (MD) simulations reveal that the original cementite surface structure experiences a size-dependent amorphization and phasemore » transformation during heavy plastic deformation. MD simulations further show that the martensite-cementite interface serves as a nucleation site for cementite amorphization, and that cementite can become disordered if further strained when the cementite particles are relatively small. These graded structures exhibit a surface hardness of ~16.2 GPa, which exceeds the value of ~8.8 GPa for the original nanocrystalline martensitic steel and most nanocrystalline steels reported before. Finally, this practical and cost-efficient approach for producing a hard surface with retained bulk ductility and toughness can provide expanded opportunities for producing an amorphous-crystalline hybrid structure in steels and other alloy systems.« less

Influence of Annealing on Microstructure and Mechanical Properties of a Nanocrystalline CrCoNi Medium-Entropy Alloy

PubMed Central

Schuh, Benjamin; Völker, Bernhard; Todt, Juraj; Kormout, Karoline S.; Schell, Norbert; Hohenwarter, Anton

2018-01-01

An equiatomic CrCoNi medium-entropy alloy was subjected to high-pressure torsion. This process led to a refinement of the microstructure to a grain size of about 50 nm, combined with a strong increase in the materials hardness. Subsequently, the thermodynamic stability of the medium entropy alloy was evaluated by isothermal and isochronal heat treatments. Annealed samples were investigated by scanning and transmission electron microscopy as well as X-ray diffraction, and were subjected to tensile tests to establish microstructure-property relationships. Furthermore, a comparison of mechanical properties with a grade 316L stainless steel was performed in order to evaluate if the CrCoNi alloy is competitive with commercially available structural materials in the nanocrystalline state. A minority phase embedded in the face-centered cubic matrix of the CrCoNi alloy could be observed in multiple annealed states, as well as the as-received and high-pressure torsion processed material. For 200 h of annealing at 500 °C, it was determined that the minority phase has a hexagonal-closed-packed crystal structure. A possible explanation for the formation of the phase is a preferential segregation of Co to stacking faults. PMID:29695142

Characterization of Nanocrystalline Nickel-Cobalt Alloys Synthesized by Direct and Pulse Electrodeposition

NASA Astrophysics Data System (ADS)

Salehi, M.; Saidi, A.; Ahmadian, M.; Raeissi, K.

2014-01-01

Nanocrystalline Ni-Co alloys are electrodeposited by direct (DC) and pulse current (PC) in an electrolyte solution which consisted of nickel sulfate, cobalt sulfate and boric acid. Electrodeposition parameters including current density, electrolyte pH and pulse times in a single electrolyte bath were changed. XRD pattern showed that the structure of the alloys depends on Co content and the synthesis parameter and changed from single phase structure (fcc) to dual phase structure (fcc + hcp). The Co content in the deposited alloys declined from 70 at.% to 50 at.% by increasing in direct current from 70 mA/cm2 to 115 mA/cm2 and also decreased from 75 at.% to 33 at.% with decrease in pH values from 4 to 2. By applying PC the Co content changed from 76 at.% to 41 at.%. Magnetic properties measurements showed the saturation magnetization (Ms) increased with increasing the Co content. There was no significant effect on coercivity values (Hc) with change in Co content and about 40 Oe was obtained for all samples. The grain size of deposited alloys obtained between 24-58 nm and 15-21 nm by applying DC and PC, respectively.

Superplastic Deformation Mechanisms of Superfine/Nanocrystalline Duplex PM-TiAl-Based Alloy

PubMed Central

Gong, Xuebo; Duan, Zhenxin; Pei, Wen; Chen, Hua

2017-01-01

In this paper, the equiaxed superfine/nanocrystalline duplex PM-TiAl-based alloy with (γ + α2) microstructure, Ti-45Al-5Nb (at %), has been synthesized by high-energy ball milling and vacuum hot pressing sintering. Superplastic deformation behavior has been investigated at 1000 °C and 1050 °C with strain rates from 5 × 10−5 s−1 to 1 × 10−3 s−1. The effects of deformation on the microstructure and mechanical behaviors of high Nb containing TiAl alloy have been characterized and analyzed. The results showed that, the ultimate tensile strength of the alloy was 58.7 MPa at 1000 °C and 10.5 MPa at 1050 °C with a strain rate of 5 × 10−5 s−1, while the elongation was 121% and 233%, respectively. The alloy exhibited superplastic elongation at 1000 and 1050 °C with an exponent (m) of 0.48 and 0.45. The main softening mechanism was dynamic recrystallization of γ grains; the dislocation slip and γ/γ interface twinning were responsible for superplastic deformation. The orientation relationship of γ/γ interface twinning obeyed the classical one: (001)γ//(110)γ. PMID:28925971

EFFECT OF ANNEALING TEMPERATURE ON THE STRUCTURE AND AC MAGNETIC PROPERTIES OF Fe73Cu1Nb3.5-xVxSi13.5B9 (x = 1.0, 1.5, 2.0) NANOCRYSTALLINE SOFT MAGNETIC ALLOYS

NASA Astrophysics Data System (ADS)

Lu, Wei; Huang, Ping; Wang, Yuxin; Yan, Biao

2013-07-01

In this paper, Nb element was partially replaced by V element in Finemet-type Fe73Cu1Nb3.5-xVxSi13.5B9 (x = 1, 1.5, 2) alloys and the effect of annealing temperatures on the microstructure and AC magnetic properties of the samples are studied. The annealing temperatures affect the grain sizes of the bcc α-Fe phase greatly. When the annealing temperature is between 540-560°C, the samples have better AC magnetic properties than the samples annealed at other temperatures. The optimized annealing temperature of the studied samples is around 560°C. The coercivity and iron loss of the V2 sample is a little bit higher than that of V1 and V1.5 alloys while the amplitude permeability of V2 alloy is larger than that of V1 and V1.5, which indicate that the content of V element has strong influence on the magnetic properties of nanocrystalline soft magnetic alloys.

Superplastic Deformation Mechanisms of Superfine/Nanocrystalline Duplex PM-TiAl-Based Alloy.

PubMed

Gong, Xuebo; Duan, Zhenxin; Pei, Wen; Chen, Hua

2017-09-19

In this paper, the equiaxed superfine/nanocrystalline duplex PM-TiAl-based alloy with (γ + α₂) microstructure, Ti-45Al-5Nb (at %), has been synthesized by high-energy ball milling and vacuum hot pressing sintering. Superplastic deformation behavior has been investigated at 1000 °C and 1050 °C with strain rates from 5 × 10 -5 s -1 to 1 × 10 -3 s -1 . The effects of deformation on the microstructure and mechanical behaviors of high Nb containing TiAl alloy have been characterized and analyzed. The results showed that, the ultimate tensile strength of the alloy was 58.7 MPa at 1000 °C and 10.5 MPa at 1050 °C with a strain rate of 5 × 10 -5 s -1 , while the elongation was 121% and 233%, respectively. The alloy exhibited superplastic elongation at 1000 and 1050 °C with an exponent (m) of 0.48 and 0.45. The main softening mechanism was dynamic recrystallization of γ grains; the dislocation slip and γ/γ interface twinning were responsible for superplastic deformation. The orientation relationship of γ/γ interface twinning obeyed the classical one: (001) γ //(110) γ .

Porous Nb-Ti based alloy produced from plasma spheroidized powder

NASA Astrophysics Data System (ADS)

Li, Qijun; Zhang, Lin; Wei, Dongbin; Ren, Shubin; Qu, Xuanhui

Spherical Nb-Ti based alloy powder was prepared by the combination of plasma spheroidization and mechanical alloying. Phase constituents, microstructure and surface state of the powder, and pore characteristics of the resulting porous alloy were investigated. The results show that the undissolved W and V in the mechanically alloyed powder is fully alloyed after spheroidization, and single β phase is achieved. Particle size of the spheroidized powder is in the range of 20-110 μm. With the decrease of particle size, a transformation from typical dendrite solidification structure to fine cell microstructure occurs. The surface of the spheroidized powder is coated by a layer of oxides consisting mainly of TiO2 and Nb2O5. Probabilities of sinter-neck formation and particle coalescence increases with increasing sintering temperature. Porous skeleton with relatively homogeneous pore distribution and open pore channel is formed after vacuum sintering at 1700 °C, and the porosity is 32%. The sintering kinetic analysis indicates that grain boundary diffusion is the primary mass transport mechanism during sintering process.

Preparation of nanocrystalline TiN coated cubic boron nitride powders by a sol-gel process.

PubMed

Park, Hee S; Umer, M Adeel; Ryu, Ho J; Hong, Soon H

2011-01-01

Cubic boron nitride (cBN) particles coated with 20 wt% nanocrystalline TiN were prepared by coating the surface of cBN particles with TiO2, followed by nitridation with NH3 gas at 900 degrees C. Coating of TiO2 on cBN powders was accomplished by a sol-gel process from a solution of titanium (IV) isopropoxide and anhydrous ethanol. An amorphous TiO(x) layer of 50 nm thickness was homogenously formed on the surface of the cBN particles by the sol-gel process. The amorphous layer was then crystallized to an anatase TiO2 phase through calcination in air at 400 degrees C. The crystallized TiO2 layer was 50 nm in thickness, and the size of TiO2 particles comprising the layer was nearly 10 nm. The TiO2 on cBN surfaces was completely converted into nanocrystalline TiN of uniform particles 20 nm in size on cBN particles by nitridation under flowing NH3 gas.

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

NASA Astrophysics Data System (ADS)

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

2015-11-01

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

Ternary and coupled binary zinc tin oxide nanopowders: Synthesis, characterization, and potential application in photocatalytic processes

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

Ivetić, T.B., E-mail: tamara.ivetic@df.uns.ac.rs; Finčur, N.L.; Đačanin, Lj. R.

2015-02-15

Highlights: • Mechanochemically synthesized nanocrystalline zinc tin oxide (ZTO) powders. • Photocatalytic degradation of alprazolam in the presence of ZTO water suspensions. • Coupled binary ZTO exhibits enhanced photocatalytic activity compared to ternary ZTO. - Abstract: In this paper, ternary and coupled binary zinc tin oxide nanocrystalline powders were prepared via simple solid-state mechanochemical method. X-ray diffraction, scanning electron microscopy, Raman and reflectance spectroscopy were used to study the structure and optical properties of the obtained powder samples. The thermal behavior of zinc tin oxide system was examined through simultaneous thermogravimetric-differential scanning calorimetric analysis. The efficiencies of ternary (Zn{sub 2}SnO{submore » 4} and ZnSnO{sub 3}) and coupled binary (ZnO/SnO{sub 2}) zinc tin oxide water suspensions in the photocatalytic degradation of alprazolam, short-acting anxiolytic of the benzodiazepine class of psychoactive drugs, under UV irradiation were determined and compared with the efficiency of pure ZnO and SnO{sub 2}.« less

Weakly-agglomerated nanocrystalline (ZrO 2) 0.9(Yb 2O 3) 0.1 powders hydrothermally synthesized at low temperature

NASA Astrophysics Data System (ADS)

Dell'Agli, Gianfranco; Mascolo, Giuseppe; Mascolo, Maria Cristina; Pagliuca, Concetta

2006-09-01

Nanocrystalline ytterbia (10 mol%)-doped cubic zirconia powders were synthesized by hydrothermal treatment of either an amorphous co-precipitate of hydrated ytterbia-zirconia or of zirconia xerogel in mixture with crystalline Yb 2O 3. The treatments were performed at 110 °C in the presence of diluted (0.2 M) or concentrated (2.0 M) solution of (K 2CO 3 + KOH) mineralizer and for different reaction times. The reaction times for the full crystallization of cubic-YbSZ-based products were determined for both the employed precursors and for each mineralizer solution. The various fully crystallized products were characterized in their degree of agglomeration and sintered at 1500 °C for 2 h. The best performance on sintering was achieved with the less agglomerated powder synthesized from the mechanical mixture and in the presence of the diluted solution of the mineralizer. The resulting density was the highest achieved with materials having the same composition.

Advanced powder metallurgy aluminum alloys and composites

NASA Technical Reports Server (NTRS)

Lisagor, W. B.; Stein, B. A.

1982-01-01

The differences between powder and ingot metallurgy processing of aluminum alloys are outlined. The potential payoff in the use of advanced powder metallurgy (PM) aluminum alloys in future transport aircraft is indicated. The national program to bring this technology to commercial fruition and the NASA Langley Research Center role in this program are briefly outlined. Some initial results of research in 2000-series PM alloys and composites that highlight the property improvements possible are given.

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.

77 FR 32942 - Application(s) for Duty-Free Entry of Scientific Instruments

Federal Register 2010, 2011, 2012, 2013, 2014

2012-06-04

.... Intended Use: The instrument will be used to fabricate bulk nanostructured metals and metallic glasses, in particular Mg based alloys, CuNb, NiAl, Nb based alloys and metal matrix composites with oxide nanoparticles... oxide nanoparticles during the melting of metals. Suction casting is required to achieve nanocrystalline...

Mechanically induced self-propagating reaction and consequent consolidation for the production of fully dense nanocrystalline Ti{sub 55}C{sub 45} bulk material

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

Sherif El-Eskandarany, M., E-mail: msherif@kisr.edu.kw; Al-Hazza, Abdulsalam

2014-11-15

We employed a high-energy ball mill for the synthesis of nanograined Ti{sub 55}C{sub 45} powders starting from elemental Ti and C powders. The mechanically induced self-propagating reaction that occurred between the reactant materials was monitored via a gas atmosphere gas-temperature-monitoring system. A single phase of NaCl-type TiC was obtained after 5 h of ball milling. To decrease the powder and grain sizes, the material was subjected to further ball milling time. The powders obtained after 200 h of milling possessed spherical-like morphology with average particle and grain sizes of 45 μm and 4.2 nm, respectively. The end-products obtained after 200more » h of ball milling time, were then consolidated into full dense compacts, using hot pressing and spark plasma sintering at 1500 and 34.5 MPa, with heating rates of 20 °C/min and 500 °C/min, respectively. Whereas hot pressing of the powders led to severe grain growth (∼ 436 nm in diameter), the as-spark plasma sintered powders maintained their nanograined characteristics (∼ 28 nm in diameter). The as-synthesized and as-consolidated powders were characterized, using X-ray diffraction, high-resolution electron microscopy, and scanning electron microscopy. The mechanical properties of the consolidated samples obtained via the hot pressing and spark plasma sintering techniques were characterized, using Vickers microhardness and non-destructive testing techniques. The Vickers hardness, Young's modulus, shear modulus and fracture toughness of as-spark plasma sintered samples were 32 GPa, 358 GPa, 151 GPa and 6.4 MPa·m{sup 1/2}, respectively. The effects of the consolidation approach on the grain size and mechanical properties were investigated and are discussed. - Highlights: • Room-temperature synthesizing of NaCl-type TiC • Dependence on the grain size on the ball milling time • Fabrication of equiaxed nanocrystalline grains with a diameter of 4.2 nm • Fabrication of nanocrystalline bulk TiC material by SPS with minimal grain growth • Dependence of improved mechanical properties on the consolidation techniques.« less

Application of sintered titanium alloys to metal denture bases: a study of titanium powder sheets for complete denture base.

PubMed

Doi, H; Harrori, M; Hasegawa, K; Yoshinari, M; Kawada, E; Oda, Y

2001-02-01

The purpose of this study was the fabrication of titanium powder sheets to enable the application of sintered titanium alloys as metal denture bases. The effects of titanium particle shape and size, binder content, and plasticizer content on the surface smoothness, tensile strength and elongation of titanium powder sheets was investigated. To select a suitable ratio of powdered metal contents for application as a metal denture base, the effects of aluminum content in Ti sheets and various other powder metal contents in Ti-Al sheets on the density, sintering shrinkage, and bending strength were evaluated. Based on the results of the above experiments, we developed a mixed powder sheet composed of 83Ti-7Al-10Cr with TA45 titanium powder (atomized, -45 microm), and 8 mass% binder content. This titanium alloy sheet had good formability and ductility. Its sintered titanium alloy had a density of 3.2 g/cm3, sintering shrinkage of 3.8%, and bending strength of 403 MPa. The titanium alloy sheet is clinically acceptable for fabricating denture bases.

Research activities of biomedical magnesium alloys in China

NASA Astrophysics Data System (ADS)

Zheng, Yufeng; Gu, Xuenan

2011-04-01

The potential application of Mg alloys as bioabsorable/biodegradable implants have attracted much recent attention in China. Advances in the design and biocompatibility evaluation of bio-Mg alloys in China are reviewed in this paper. Bio-Mg alloys have been developed by alloying with the trace elements existing in human body, such as Mg-Ca, Mg-Zn and Mg-Si based systems. Additionally, novel structured Mg alloys such as porous, composited, nanocrystalline and bulk metallic glass alloys were tried. To control the biocorrosion rate of bio-Mg implant to match the self-healing/regeneration rate of the surrounding tissue in vivo, surface modification layers were coated with physical and chemical methods.

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

NASA Astrophysics Data System (ADS)

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

2013-03-01

This paper describes a new method for making Fe-Si magnetic powders using a pack-cementation process. It was found that Fe-Si alloy powders were formed by a reaction of the pack mixture of Fe, Si, NaF, and Al2O3 powders at 900 °C for 24 h under a hydrogen atmosphere. Separation of the Fe-Si alloy powders was dependent on the particle size of the Fe powders in the pack. For small Fe powders, magnetic separation in a medium of strong alkali solution was recommended. But, for relatively larger Fe powders, the Fe-Si alloy powders were easily separated from Al2O3 powders using a magnet in air atmosphere. The Si content in the Fe-Si magnetic powders were easily controlled by changing the weight ratio of Si to (Si+Fe) in the pack.

Calcium hydride synthesis of Ti-Nb-based alloy powders

NASA Astrophysics Data System (ADS)

Kasimtsev, A. V.; Shuitsev, A. V.; Yudin, S. N.; Levinskii, Yu. V.; Sviridova, T. A.; Alpatov, A. V.; Novosvetlova, E. E.

2017-09-01

The metallothermic (calcium hydride) synthesis of Ti-Nb alloy powders alloyed with tantalum and zirconium is experimentally studied under various conditions. Chemical, X-ray diffraction, and metallographic analyses of the synthesized products show that initial oxides are completely reduced and a homogeneous β-Ti-based alloy powder forms under the optimum synthesis conditions at a temperature of 1200°C. At a lower synthesis temperature, the end products have a high oxygen content. The experimental results are used to plot the thermokinetic dependences o formation of a bcc solid solution at various times of isothermal holding of Ti-22Nb-6Ta and Ti-22Nb-6Zr (at %) alloys. The physicochemical and technological properties of the Ti-22Nb-6Ta and Ti-22Nb-6Zr alloy powders synthesized by calcium hydride reduction under the optimum conditions are determined.

Microanalytical characterization of multi-rare earth nanocrystalline magnets by TEM and APT

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

Wu, Y. Q.; Tang, W.; Miller, Michael K

2006-01-01

The partitioning behavior of various rare-earth (RE) elements during solidification and their segregation behavior at the grain boundaries were investigated in nanocrystalline (Y{sub 0.5}Dy{sub 0.5}{sub 2.2}Fe{sub 14}B and (Nd{sub 0.5}Y{sub 0.25}Dy{sub 0.25}){sub 1.8}Zr{sub 0.4}Co{sub 1.5}Fe{sub 12.5}B alloys by transmission electron microscopy and atom probe tomography. The best hard magnetic properties obtained are H{sub cj} = 22 kOe, B{sub r}=5.10 kG, and (BH){sub max} = 5.97 MG Oe for the Y-Dy-based alloy and H{sub cj}=10.6 kOe, B{sub r}=6.64 kG, and (BH){sub max}=9.56 MG Oe for the Y-Nd-Dy based alloy. The grain size of the Y-Dy based alloy was {approx} 50 nm.more » The Y-Nd-Dy based alloy had an overall finer, bimodal grain size. An intergranular (Y{sub 0.36}Dy{sub 0.64}){sub 6}Fe{sub 23} phase was detected in the Y-Dy based alloy. A uniform distribution of RE elements was found within the 2-14-1 grains in both alloys. The Y:(Dy+Nd) ratio in the Y-Nd-Dy alloy was lower than its nominal composition, indicating that the Y is segregating to grain boundaries or forming a second phase.« less

Development of Bulk Nanocrystalline Tungsten Alloys for Fusion Reactor Structures

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

Fang, Zhigang Zak

This project developed a technology for manufacturing bulk ultrafine tungsten materials that are at or near full density for fusion reactor structural applications, aiming to improve ductility and toughness of tungsten before and after irradiation. The project involved the development of fabrication processes for making bulk ultrafine grained W, the development of new alloys of ultrafine grained W and evaluations of properties of these specific materials. The goal of this fabrication process is to produce fully dense bulk W with ultrafine grain sizes, with uniform distributions of grain size and additives. To date there is no known process that couldmore » be used to make ultrafine grained tungsten in a fully dense state and in a cost-acceptable fashion. The specific technology described in this proposal for making ultrafine grained tungsten involves a suite of nano-particle processing and sintering techniques. The program also developed new alloys of ultrafine grained W, e.g. W-(Ta,V,Ti)-TiC alloys to improve ductility and toughness before and after irradiation. By completing this project, we achieved the following objectives: • Demonstrated experimentally the feasibility of producing bulk ultrafine grained tungsten alloys (at or near 100% dense, <1000 nm grain size) using the proposed process • Demonstrated the proposed ultrafine grained W alloys, namely, W-(Ta, V, Ti)-TiC, can indeed be made using the proposed process • Demonstrated that the properties of nano tungsten alloys meet the requirements for fusion reactor applications. The overall goal was to harness the potential of ultrafine grained W produced using the proposed processes as the core structural materials for future fusion reactors. The project was very successful overall, meeting all milestones and surpassing project goals in terms of process development and material’s blistering resistance properties. A novel process similar to the conventional press-and-sinter powder metallurgy method was developed for producing ultrafine grain tungsten from nanosize tungsten powders. Grain growth was significantly controlled during sintering by certain alloy compositions, particularly Ti, and most compositions sintered to maximum densification. To optimize this process, the effect of processing parameters on the densification and grain growth of nano-W powders was investigated. Near-fully densified tungsten was obtained at sintering temperatures between 1100 and 1300 °C, and both Ar and H2 sintering atmospheres were investigated. The Ar sintering atmosphere was determined to more favorably promote densification and minimize grain growth. The nanosized tungsten powder compacts were subjected to reduction in H2 as a part of the sintering cycle. The reduction temperature was found to have significant effects on the sintering of nano-W powder, primarily as a result of grain coarsening, which was seen at temperatures as low as 700 °C. In an effort to inhibit grain growth, the effect of Ti-based additives on the densification and grain growth of nano-W powders was investigated in this project. The addition of 1 wt.% Ti into tungsten led to more than a 63% decrease in average grain size of sintered samples at comparable density levels. Compared to conventional high temperature sintering, a lower temperature sintering cycle for a longer hold time resulted in both near-full density and fine grain size. The roles of the Ti additives include not only the inhibition of grain growth, but also the potential absorption of oxygen from W particles. The project has resulted in the publication; thus far, of six peer reviewed journal articles and seven conference presentations, as well as a master’s thesis. Two additional journal articles are currently in preparation. Presentations and articles were a particular focus of the second half of the project, once significant experimentation had been performed and analyzed. As part of our efforts to disseminate information of our results, the W research teams with Prof. Fang had a strong presence at multiple international conferences during 2015 and 2016. Several research groups in the US are now performing experiments using the ultrafine grained W materials.« less

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

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

Ting, Jason

1999-02-12

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

The Mechanical Properties and In Vitro Biocompatibility of PM-Fabricated Ti-28Nb-35.4Zr Alloy for Orthopedic Implant Applications.

PubMed

Xu, Wei; Li, Ming; Wen, Cuie; Lv, Shaomin; Liu, Chengcheng; Lu, Xin; Qu, Xuanhui

2018-03-30

A biocompatible Ti-28Nb-35.4Zr alloy used as bone implant was fabricated through the powder metallurgy process. The effects of mechanical milling and sintering temperatures on the microstructure and mechanical properties were investigated systematically, before in vitro biocompatibility of full dense Ti-28Nb-35.4Zr alloy was evaluated by cytotoxicity tests. The results show that the mechanical milling and sintering temperatures have significantly effects on the density and mechanical properties of the alloys. The relative density of the alloy fabricated by the atomized powders at 1500 °C is only 83 ± 1.8%, while the relative density of the alloy fabricated by the ball-milled powders can rapidly reach at 96.4 ± 1.3% at 1500 °C. When the temperature was increased to 1550 °C, the alloy fabricated by ball-milled powders achieve full density (relative density is 98.1 ± 1.2%). The PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C can achieve a wide range of mechanical properties, with a compressive yield strength of 1058 ± 35.1 MPa, elastic modulus of 50.8 ± 3.9 GPa, and hardness of 65.8 ± 1.5 HRA. The in vitro cytotoxicity test suggests that the PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C has no adverse effects on MC3T3-E1 cells with cytotoxicity ranking of 0 grade, which is nearly close to ELI Ti-6Al-4V or CP Ti. These properties and the net-shape manufacturability makes PM-fabricated Ti-28Nb-35.4Zr alloy a low-cost, highly-biocompatible, Ti-based biomedical alloy.

Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders.

PubMed

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong; Zheng, Feng

2017-09-21

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH₄)₂C₂O₄·H₂O and Na₂CO₃) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7-10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na₂CO₃ precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed.

Phase fields of nickel silicides obtained by mechanical alloying in the nanocrystalline state

NASA Astrophysics Data System (ADS)

Datta, M. K.; Pabi, S. K.; Murty, B. S.

2000-06-01

Solid state reactions induced by mechanical alloying (MA) of elemental blends of Ni and Si have been studied over the entire composition range of the Ni-Si system. A monotonous increase of the lattice parameter of the Ni rich solid solution, Ni(Si), is observed with refinement of crystallite size. Nanocrystalline phase/phase mixtures of Ni(Si), Ni(Si)+Ni31Si12, Ni31Si12+Ni2Si, Ni2Si+NiSi and NiSi+Si, have been obtained during MA, over the composition ranges of 0-10, 10-28, 28-33, 33-50, and >50 at. % Si, respectively. The results clearly suggest that only congruent melting phases, Ni31Si12, Ni2Si, and NiSi form, while the formation of noncongruent melting phases, Ni3Si, Ni3Si2, and NiSi2, is bypassed in the nanocrystalline state. The phase formation during MA has been discussed based on thermodynamic arguments. The predicted phase fields obtained from effective free energy calculations are quite consistent with those obtained during MA.

Influence of Nb addition on vacancy defects and magnetic properties of the nanocrystalline Nd-Fe-B permanent magnets

NASA Astrophysics Data System (ADS)

Szwaja, Małgorzata; Gębara, Piotr; Filipecki, Jacek; Pawlik, Katarzyna; Przybył, Anna; Pawlik, Piotr; Wysłocki, Jerzy J.; Filipecka, Katarzyna

2015-05-01

In present work, influence of Nb addition on vacancy defects and magnetic properties of nanocrystalline Nd-Fe-B permanent magnets, was investigated. Samples with composition (Nd,Fe,B)100-xNbx (where x=6,7,8) were studied in as-cast state and after annealing. Samples were prepared by arc-melting with high purity of constituent elements under Ar atmosphere. Ribbons were obtained by melt-spinning technique under low pressure of Ar. Ribbon samples in as-cast state had amorphous structure and soft magnetic properties. Positron annihilation lifetime spectroscopy PALS has been applied to detection of positron - trapping voids (vacancy defects). With increase of Nb in alloy increasing of vacancy defects concentration was observed. Heat treatment of the samples was carried out at various temperatures (from 923 K to 1023 K) for 5 min, in order to obtain nanocrystalline structure. The aim of present work was to determine the influence of Nb addition and annealing conditions on the vacancy defects and magnetic properties of the Nd-Fe-B- type alloys in as-cast state and after heat treatment.

Atomic level structural modulation during the structural relaxation and its effect on magnetic properties of Fe81Si4B10P4Cu1 nanocrystalline alloy

NASA Astrophysics Data System (ADS)

Cao, C. C.; Zhu, L.; Meng, Y.; Zhai, X. B.; Wang, Y. G.

2018-06-01

The evolution of local structure and defects in the Fe81Si4B10P4Cu1 amorphous alloy during the structural relaxation has been investigated by Mössbauer spectroscopy, positron annihilation lifetime spectroscopy and transmission electron microscopy to explore their effects on magnetic properties of the nanocrystalline. The atomic rearrangements at the early stage of the structural relaxation cause the density increase of the amorphous matrix, but the subsequent atomic rearrangements contribute to the transformation of Fe3B-like atomic arrangements to FeB-like ones with the temperature increasing. As the structural relaxation processes, the released Fe atoms both from Fe3B- and Fe3P-like atomic arrangements result in the formation of new Fe clusters and the increase of Fe-Fe coordination number in the existing Fe clusters and the nucleation sites for α-Fe gradually increase, both of which promote the crystallization. However, the homogeneity of amorphous matrix will be finally destroyed under excessive relaxation temperature, which coarsens nanograins during the crystallization instead. Therefore, soft magnetic properties of the Fe81Si4B10P4Cu1 nanocrystalline alloy can be improved by pre-annealing the amorphous precursor at an appropriate temperature due to the atomic level structural optimization.

The formation mechanisms of surface nanocrystallites in β-type biomedical TiNbZrFe alloy by surface mechanical attrition treatment

NASA Astrophysics Data System (ADS)

Jin, Lei; Cui, Wenfang; Song, Xiu; Zhou, Lian

2015-08-01

A nanostructured surface layer was successfully performed on a biomedical β-type TiNbZrFe alloy by surface mechanical attrition treatment (SMAT). The results reveal that the surface layer along the depth from treated surface to strain-free matrix could be divided into an outer nanocrystalline layer (0-30 μm), a high-density dislocation region (30-200 μm) and an inner region with low-density dislocations and twins (200-700 μm) when the surface was treated for 60 min. The microhardness of the surface layer is enhanced and increases with increasing treatment time. Although the {1 1 2} <1 1 1> twin coordinates the deformations with dislocations, this coordination only occurs in the low strain area and cannot affect the nanocrystalline formation. The self-nanocrystallization of TiNbZrFe alloy is mainly attributed to dislocation movements. First, the dislocations start to move and easily form dislocation bands along certain crystal directions; then, multiple slips of dislocations gradually form dislocation tangles; after that, high-density dislocation tangles increases, which divides primary grains into many small domain areas. As high strain energies accumulate on the interfaces among these areas, the lattice rotation can be driven between the adjacent small domain areas, finally resulting in a large number of nanocrystalline regions with low or large angle grain boundaries.

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

NASA Astrophysics Data System (ADS)

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

2017-10-01

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

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

Zhang, Lehao

A nanocrystalline surface layer was produced on Mg-3 wt.% Li-6 wt.% Al alloy by means of surface mechanical attrition treatment (SMAT). Microstructure features of various sections were systematically characterized by transmission electron microscopy. The results indicate that grain refinement induced by SMAT is dominated mainly by dislocation slip. Twinning is active at the early stage of grain refinement process when the grain size is large. The dislocation-dominated deformation mechanism is attributed to the change of c/a ratio due to the alloying of Li in Mg matrix and the suppression of twinning due to grain refinement. Nanoindentation results show that themore » hardness of the surface is enhanced by SMAT. - Highlights: •Nanocrystalline surface layer was produced on Mg-3 wt.%Li-6 wt.%Al alloy by SMAT. •Grain refinement induced by SMAT is dominated mainly by dislocation slip. •Twinning is active at the early stage of grain refinement process. •The hardness of the surface was enhanced by SMAT.« less

An Evaluation of a Borided Layer Formed on Ti-6Al-4V Alloy by Means of SMAT and Low-Temperature Boriding

PubMed Central

Yao, Quantong; Sun, Jian; Fu, Yuzhu; Tong, Weiping; Zhang, Hui

2016-01-01

In this paper, a nanocrystalline surface layer without impurities was fabricated on Ti-6Al-4V alloy by means of surface mechanical attrition treatment (SMAT). The grain size in the nanocrystalline layer is about 10 nm and grain morphology displays a random crystallographic orientation distribution. Subsequently, the low-temperature boriding behaviors (at 600 °C) of the SMAT sample, including the phase composition, microstructure, micro-hardness, and brittleness, were investigated in comparison with those of coarse-grained sample borided at 1100 °C. The results showed that the boriding kinetics could be significantly enhanced by SMAT, resulting in the formation of a nano-structured boride layers on Ti-6Al-4V alloy at lower temperature. Compared to the coarse-grained boriding sample, the SMAT boriding sample exhibits a similar hardness value, but improved surface toughness. The satisfactory surface toughness may be attributed to the boriding treatment that was carried out at lower temperature. PMID:28774115

Evaluation of the amalgamation reaction of experimental Ag-Sn-Cu alloys containing Pd using a mercury plating technique.

PubMed

Koike, Marie; Ferracane, Jack L; Fujii, Hiroyuki; Okabe, Toru

2003-09-01

A mercury plating technique was used to determine the phases forming on experimental Ag-Sn-Cu alloy powders (with and without Pd) exposed to electrolytically deposited mercury. Four series of alloy powders were made: a) 1.5% Pd with 10-14% Cu (CU series); b) 1.0% Pd with 10-14% Cu (1PD series); c) 1.5% Pd with different ratios of Ag3Sn (gamma) to Ag4Sn (beta) with 12% Cu (AGSN series); and d) 9-13% Cu with no Pd (NOPD series). Each powder was pressed on a freshly prepared amalgam specimen made from the same powder and metallographically polished until cross sections appeared; mercury was electroplated on the alloy particles. Alloy powders, amalgams and electroplated specimens were examined using XRD and SEM/EDS. XRD confirmed the presence of gamma2 in amalgams made from alloys with Cu < 13% or with Ag3Sn/Ag4Sn > 0.8. Specimens with moderately plated Hg showed gamma1 (Ag2Hg3) polyhedra and eta' Cu6Sn5, but not gamma2. This method effectively identifies alloys prone to forming gamma2.

The structure-property relationships of powder processed Fe-Al-Si alloys

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

Prichard, Paul D.

1998-02-23

Iron-aluminum alloys have been extensively evaluated as semi-continuous product such as sheet and bar, but have not been evaluated by net shape P/M processing techniques such as metal injection molding. The alloy compositions of iron-aluminum alloys have been optimized for room temperature ductility, but have limited high temperature strength. Hot extruded powder alloys in the Fe-Al-Si system have developed impressive mechanical properties, but the effects of sintering on mechanical properties have not been explored. This investigation evaluated three powder processed Fe-Al-Si alloys: Fe-15Al, Fe-15Al-2.8Si, Fe-15Al-5Si (atomic %). The powder alloys were produced with a high pressure gas atomization (HPGA) processmore » to obtain a high fraction of metal injection molding (MIM) quality powder (D 84 < 32 μm). The powders were consolidated either by P/M hot extrusion or by vacuum sintering. The extruded materials were near full density with grain sizes ranging from 30 to 50 μm. The vacuum sintering conditions produced samples with density ranging from 87% to 99% of theoretical density, with an average grain size ranging from 26 μm to 104 μm. Mechanical property testing was conducted on both extruded and sintered material using a small punch test. Tensile tests were conducted on extruded bar for comparison with the punch test data. Punch tests were conducted from 25 to 550 C to determine the yield strength, and fracture energy for each alloy as a function of processing condition. The ductile to brittle transition temperature (DBTT) was observed to increase with an increasing silicon content. The Fe-15Al-2.8Si alloy was selected for more extensive testing due to the combination of high temperature strength and low temperature toughness due to the two phase α + DO 3 structure. This investigation provided a framework for understanding the effects of silicon in powder processing and mechanical property behavior of Fe-Al-Si alloys.« less

Nano-Scale Characterization of Al-Mg Nanocrystalline Alloys

NASA Astrophysics Data System (ADS)

Harvey, Evan; Ladani, Leila

Materials with nano-scale microstructure have become increasingly popular due to their benefit of substantially increased strengths. The increase in strength as a result of decreasing grain size is defined by the Hall-Petch equation. With increased interest in miniaturization of components, methods of mechanical characterization of small volumes of material are necessary because traditional means such as tensile testing becomes increasingly difficult with such small test specimens. This study seeks to characterize elastic-plastic properties of nanocrystalline Al-5083 through nanoindentation and related data analysis techniques. By using nanoindentation, accurate predictions of the elastic modulus and hardness of the alloy were attained. Also, the employed data analysis model provided reasonable estimates of the plastic properties (strain-hardening exponent and yield stress) lending credibility to this procedure as an accurate, full mechanical characterization method.

Synthesis and magnetostrictive properties of Pr(Fe1.95B0.05)1.93 bulk nanocrystalline alloy

NASA Astrophysics Data System (ADS)

Shi, Y. G.; Hu, C. C.; Fan, J. Y.; Shi, D. N.; Lv, L. Y.; Tang, S. L.

2012-11-01

The structure, magnetic properties, and magnetostriction of Pr(Fe1.95B0.05)1.93 alloys prepared by annealing its precursor amorphous ribbons under high pressure were investigated. It was found that Pr(Fe1.95B0.05)1.93 single cubic Laves phase could be obtained only when the pressure is up to 3 GPa. The average grain size about 20 nm is found in the sample synthesized under 6 GPa. A large linear magnetostriction of 541 ppm at 3 kOe is observed in the Pr(Fe1.95B0.05)1.93 compound synthesized under 6 GPa, which is 25% larger than that under 3 GPa. The present work offers an effective method to obtain bulk nanocrystalline magnetostrictive compounds.

Hyperfine Fields in Nanocrystalline Fe0.48Al0.52

NASA Astrophysics Data System (ADS)

Szymański, K.; Satuła, D.; Dobrzyński, L.; Voronina, E.; Yelsukov, E. P.

2004-12-01

Mössbauer measurements with circularly polarized radiation were performed on a nanocrystalline, disordered Fe48Al52 alloy. The analysis of the data for various polarization states resulted in the characterization of the hyperfine magnetic field distribution and the dependence of the average z-component of hyperfine field on the chemical environment. An increasing number of Al in the first coordination shell causes not only a decrease of magnetic moments but also introduces noncollinearity.

Wear behavior of Cu-Zn alloy by ultrasonic nanocrystalline surface modification.

PubMed

Cho, In Shik; Amanov, Auezhan; Ahn, Deok Gi; Shin, Keesam; Lee, Chang Soon; Pyoun, Young-Shik; Park, In-Gyu

2011-07-01

The ultrasonic nanocrystalline surface modification (UNSM) was applied to disk specimens made of Cu-Zn alloy in order to investigate the UNSM effects under five various conditions on wear of deformation twinning. In this paper, ball-on-disk test was conducted, and the results of UNSM-treated specimens showed that surface layer dislocation density and multi-directional twins were abruptly increased, and the grain size was altered into nano scale. UNSM delivers force onto the workpiece surface 20,000 times per second with 1,000 to 4,000 contact counts per square millimeter. The UNSM technology creates nanocrystalline and deformation twinning on the workpiece surface. One of the main concepts of this study is that defined phenomena of the UNSM technology, and the results revealed that nanocrystalline and deformation twinning depth might be controlled by means of impact energy of UNSM technology. EBSD and TEM analyses showed that deformation layer was increased up to 268 microm, and initial twin density was 0.001 x 10(6) cm(-2) and increased up to 0.343 x 10(6) cm(-2). Wear volume loss was also decreased from 703 x 10(3) mm3 to 387 x 10(3) mm3. Wear behavior according to deformation depth was observed under three different combinations. This is related to deformation depth which was created by UNSM technology.

Reduction mechanism of surface oxide films and characterization of formations on pulse electric-current sintered Al Mg alloy powders

NASA Astrophysics Data System (ADS)

Xie, Guoqiang; Ohashi, Osamu; Song, Minghui; Mitsuishi, Kazutaka; Furuya, Kazuo

2005-02-01

The microstructure of interfaces between powder particles in Al-Mg alloy specimens sintered by pulse electric-current sintering (PECS) process was characterized using high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (EDS). The crystalline precipitates with nano-size in the interface were observed in all of Al-Mg alloy specimens. The composition was determined to be MgAl 2O 4 or MgO, or both of them, which depended on Mg content in alloy powder and sintering temperature. The precipitates were suggested to contribute to reduction reaction of Mg with oxide films originally covered at powder particles surface.

Method and article of manufacture corresponding to a composite comprised of ultra nonacrystalline diamond, metal, and other nanocarbons useful for thermoelectric and other applications

DOEpatents

Gruen, Dieter M.

2010-05-18

One provides (101) disperse ultra-nanocrystalline diamond powder material that comprises a plurality of substantially ordered crystallites that are each sized no larger than about 10 nanometers. One then reacts (102) these crystallites with a metallic component. The resultant nanowire is then able to exhibit a desired increase with respect to its ability to conduct electricity while also substantially preserving the thermal conductivity behavior of the disperse ultra-nanocrystalline diamond powder material. The reaction process can comprise combining (201) the crystallites with one or more metal salts in an aqueous solution and then heating (203) that aqueous solution to remove the water. This heating can occur in a reducing atmosphere (comprising, for example, hydrogen and/or methane) to also reduce the salt to metal.

Application of Powder Diffraction Methods to the Analysis of Short- and Long-Range Atomic Order in Nanocrystalline Diamond and SiC: The Concept of the Apparent Lattice Parameter (alp)

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Gierlotka, S.; Stelmakh, S.; Pielaszek, R.; Bismayer, U.; Weber, H.-P.; Palosz, W.

2003-01-01

Two methods of the analysis of powder diffraction patterns of diamond and SiC nanocrystals are presented: (a) examination of changes of the lattice parameters with diffraction vector Q ('apparent lattice parameter', alp) which refers to Bragg scattering, and (b), examination of changes of inter-atomic distances based on the analysis of the atomic Pair Distribution Function, PDF. Application of these methods was studied based on the theoretical diffraction patterns computed for models of nanocrystals having (i) a perfect crystal lattice, and (ii), a core-shell structure, i.e. constituting a two-phase system. The models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the shell. X-ray and neutron experimental diffraction data of nanocrystalline SiC and diamond powders of the grain diameter from 4 nm up to micrometers were used. The effects of the internal pressure and strain at the grain surface on the structure are discussed based on the experimentally determined dependence of the alp values on the Q-vector, and changes of the interatomic distances with the grain size determined experimentally by the atomic Pair Distribution Function (PDF) analysis. The experimental results lend a strong support to the concept of a two-phase, core and the surface shell structure of nanocrystalline diamond and SiC.

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Oxide strengthened molybdenum-rhenium alloy

DOEpatents

Bianco, Robert; Buckman, Jr., R. William

2000-01-01

Provided is a method of making an ODS molybdenum-rhenium alloy which includes the steps of: (a) forming a slurry containing molybdenum oxide and a metal salt dispersed in an aqueous medium, the metal salt being selected from nitrates or acetates of lanthanum, cerium or thorium; (b) heating the slurry in the presence of hydrogen to form a molybdenum powder comprising molybdenum and an oxide of the metal salt; (c) mixing rhenium powder with the molybdenum powder to form a molybdenum-rhenium powder; (d) pressing the molybdenum-rhenium powder to form a molybdenum-rhenium compact; (e) sintering the molybdenum-rhenium compact in hydrogen or under a vacuum to form a molybdenum-rhenium ingot; and (f) compacting the molybdenum-rhenium ingot to reduce the cross-sectional area of the molybdenum-rhenium ingot and form a molybdenum-rhenium alloy containing said metal oxide. The present invention also provides an ODS molybdenum-rhenium alloy made by the method. A preferred Mo--Re-ODS alloy contains 7-14 weight % rhenium and 2-4 volume % lanthanum oxide.

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.

Structural, optical, and magnetic properties of Cu- and Ni-codoped CdO dilute magnetic nanocrystalline semiconductor: effect of hydrogen post-treatment

NASA Astrophysics Data System (ADS)

Dakhel, A. A.; Bououdina, M.

2015-06-01

Cadmium oxide codoped with Cu and Ni ions powders was synthesised by thermal co-decomposition of a mixture of cadmium, copper, and nickel acetylacetonates. The mass ratio of Cu/Cd was fixed, while the Ni/Cd mass ratio was varied systematically. The purpose of the present study is to prepare powders having room-temperature ferromagnetic (RT-FM) properties. X-ray fluorescence (XRF) and X-ray diffraction (XRD) confirm the purity and the formation of single nanocrystalline structure of the as-prepared powders. The energy bandgap of the as-prepared powders was found to vary slightly and then increases by 3.96-38.02 % after post-H2-treatment. Magnetic measurements reveal that all as-prepared doped CdO powders gained partial (RT-FM) properties. Furthermore, the created RT-FM is dependent on the Ni% doping level. After annealing under H2 gas, a strong enhancement of RT-FM was observed, especially for 1.2 % Ni-doping-level powder where the whole powder became ferromagnetic with coercivity, remanence, and saturation magnetisation of 249.2 Oe, 4.52 memu/g, and 14.57 memu/g, respectively, representing an increase by ~241.3, 1062, and 1700 %, respectively, in comparison with the as-prepared sample. Thus, it was proved, for the first time, the possibility of producing of codoped CdO with RT-FM, where the magnetic characteristics can be tailored by doping and post-treatment under H2 atmosphere, thus a new potential candidate for dilute magnetic semiconductor (DMS).

Properties of WZ21 (%wt) alloy processed by a powder metallurgy route.

PubMed

Cabeza, Sandra; Garcés, Gerardo; Pérez, Pablo; Adeva, Paloma

2015-06-01

Microstructure, mechanical properties and corrosion behaviour of WZ21 (%wt) alloy prepared by a powder metallurgy route from rapidly solidified powders have been studied. Results were compared to those of the same alloy prepared through a conventional route of casting and extrusion. The microstructure of the extruded ingot consisted of α-Mg grains and Mg3Zn3Y2 (W-phase) and LPSO-phase particles located at grain boundaries. Moreover, stacking faults were also observed within α-Mg grains. The alloy processed by the powder metallurgy route exhibited a more homogeneous and finer microstructure, with a grain size of 2 μm. In this case W-phase and Mg24Y5 phase were identified, but not the LPSO-phase. The microstructural refinement induced by the use of rapidly solidified powders strengthened the alloy at room temperature and promoted superplasticity at higher strain rates. Corrosion behaviour in PBS medium evidenced certain physical barrier effect of the almost continuous arrangements of second phases aligned along the extrusion direction in conventionally processed WZ21 alloy, with a stable tendency around 7 mm/year. On the other hand, powder metallurgy processing promoted significant pitting corrosion, inducing accelerated corrosion rate during prolonged immersion times. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effects of Precipitant and pH on Coprecipitation of Nanosized Co-Cr-V Alloy Powders

PubMed Central

Chen, Xiaoyu; Li, Yongxia; Huang, Lan; Zou, Dan; Wu, Enxi; Liu, Yanjun; Xie, Yuanyan; Yao, Rui; Liao, Songyi; Wang, Guangrong

2017-01-01

Nanosized Co-Cr-V alloy powders were synthesized via coprecipitation method. Effects of precipitants ((NH4)2C2O4·H2O and Na2CO3) and pH were investigated by X-ray diffraction (XRD), Zeta potential analyzer, thermogravimetry-differential scanning calorimetry (TG-DSC), inductively coupled plasma-atomic emission spectrometry (ICP-AES) and scanning electron microscopy (SEM). Co-Cr-V alloy powders were consisted of major face-centered cubic Co (fcc Co) and minor hexagonal close-packed Co (hcp Co). Grain sizes of precursors and Co-Cr-V alloy powders were increased with pH value (7–10) within the ranges of 3~39 and 39~66 nm, respectively. Rod-like or granular Co-Cr-V alloy particles were assembled by interconnected nanograins. At pH = 7, Na2CO3 precipitant was found to be beneficial to maintain the desirable composition of Co-Cr-V powders. It was also found that lower pH favors the maintenance of pre-designed composition, while grain coarsens at higher pH. Effects of variation for precipitant and pH on the morphology and composition of Co-Cr-V alloy powder were discussed in detail and relevant mechanism was further proposed. PMID:28934147

Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.

Characterization of corrosion products of AB{sub 5}-type hydrogen storage alloys for nickel-metal hydride batteries

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

Maurel, F.; Knosp, B.; Backhaus-Ricoult, M.

2000-01-01

To better understand the decrease in storage capacity of AB{sub 5}-type alloys in rechargeable Ni/MH batteries undergoing repeated charge/discharge cycles, the corrosion of a MnNi{sub 3.55}Co{sub 0.75}Mn{sub 0.4}Al{sub 0.3} alloy in aqueous KOH electrolyte was studied. The crystal structure, chemical composition, and distribution of corrosion products were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Hollow and filed needles of a mixed rare earth hydroxide Mn(OH){sub 3} were found to cover a continuous nanocrystalline corrosion scale composed of metal (Ni, Co) solid solution, oxide (Ni,Co)O solid solution and rare earth hydroxide, and a Mn-depleted alloy subscale. Corrosionmore » kinetics were measured for three different temperatures. Growth kinetics of the continuous corrosion scale and of the Mm(OH){sub 3} needles obeyed linear and parabolic rate laws, respectively. Models for the corrosion mechanism were developed on the basis of diffusional transport of Mn and OH through the hydroxide needles and subsequent diffusion along grain boundaries through the nanocrystalline scale.« less

[Use of powder metallurgy for development of implants of Co-Cr-Mo alloy powder].

PubMed

Dabrowski, J R

2001-04-01

This paper discusses the application of powder metallurgy for the development of porous implantation materials. Powders obtained from Co-Cr-Mo alloy with different carbon content by water spraying and grinding, have been investigated. Cold pressing and rotary re-pressing methods were used for compressing the powder. It was found that the sintered materials obtained from water spraying have the most advantageous properties.

Microstructure and Shape Memory Characteristics of Powder-Metallurgical-Processed Ti-Ni-Cu Alloys

NASA Astrophysics Data System (ADS)

Kim, Yeon-Wook; Chung, Young-Soo; Choi, Eunsoo; Nam, Tae-Hyun

2012-08-01

Even though Ti-Ni-Cu alloys have attracted a lot of attention because of their high performance in shape memory effect and decrease in thermal and stress hysteresis compared with Ti-Ni binary alloys, their poor workability restrains the practical applications of Ti-Ni-Cu shape memory alloys. Consolidation of Ti-Ni-Cu alloy powders is useful for the fabrication of bulk near-net-shape shape memory alloy. Ti50Ni30Cu20 shape memory alloy powders were prepared by gas atomization, and the sieved powders with the specific size range of 25 to 150 μm were chosen for this study. The evaluation of powder microstructures was based on a scanning electron microscope (SEM) examination of the surface and the polished and etched powder cross sections. The typical images showed cellular/dendrite morphology and high population of small shrinkage cavities at intercellular regions. Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) analysis showed that a B2-B19 one-step martensitic transformation occurred in the as-atomized powders. The martensitic transformation start temperature (Ms) of powders ranging between 25 and 50 μm was 304.5 K (31.5 °C). The Ms increased with increasing powder size. However, the difference of Ms in the as-atomized powders ranging between 25 and 150 μm was only 274 K (1 °C). A dense cylindrical specimen of 10 mm diameter and 15 mm length were fabricated by spark plasma sintering (SPS) at 1073 K (800 °C) and 10 MPa for 20 minutes. Then, this bulk specimen was heat treated for 60 minutes at 1123 K (850 °C) and quenched in ice water. The Ms of the SPS specimen was 310.5 K (37.5 °C) whereas the Ms of conventionally cast ingot is found to be as high as 352.7 K (79.7 °C). It is considered that the depression of the Ms in rapidly solidified powders is ascribed to the density of dislocations and the stored energy produced by rapid solidification.

Producing High-Quality Titanium Alloy by a Cost-Effective Route Combining Fast Heating and Hot Processing

NASA Astrophysics Data System (ADS)

Yang, Fei; Raynova, Stella; Singh, Ajit; Zhao, Qinyang; Romero, Carlos; Bolzoni, Leandro

2018-02-01

Powder metallurgy is a very attractive method for producing titanium alloys, which can be near-net-shape formed and have freedom in composition selection. However, applications are still limited due to product affordability. In this paper, we will discuss a possible cost-effective route, combining fast heating and hot processing, to produce titanium alloys with similar or even better mechanical properties than that of ingot metallurgy titanium alloys. Two titanium alloys, Ti-5Al-5V-5Mo-3Cr (Ti-5553) and Ti-5Fe, were successfully produced from HDH titanium powder and other master alloy powders using the proposed processing route. The effect of the processing route on microstructural variation and mechanical properties have been discussed.

Laboratory Powder Metallurgy Makes Tough Aluminum Sheet

NASA Technical Reports Server (NTRS)

Royster, D. M.; Thomas, J. R.; Singleton, O. R.

1993-01-01

Aluminum alloy sheet exhibits high tensile and Kahn tear strengths. Rapid solidification of aluminum alloys in powder form and subsequent consolidation and fabrication processes used to tailor parts made of these alloys to satisfy such specific aerospace design requirements as high strength and toughness.

Reverse micelle synthesis of oxide nanopowders: mechanisms of precipitate formation and agglomeration effects.

PubMed

Graeve, Olivia A; Fathi, Hoorshad; Kelly, James P; Saterlie, Michael S; Sinha, Kaustav; Rojas-George, Gabriel; Kanakala, Raghunath; Brown, David R; Lopez, Enrique A

2013-10-01

We present an analysis of reverse micelle stability in four model systems. The first two systems, composed of unstable microemulsions of isooctane, water, and Na-AOT with additions of either iron sulfate or yttrium nitrate, were used for the synthesis of iron oxide or yttrium oxide powders. These oxide powders were of nanocrystalline character, but with some level of agglomeration that was dependent on calcination temperature and cleaning procedures. Results show that even though the reverse micellar solutions were unstable, nanocrystalline powders with very low levels of agglomeration could be obtained. This effect can be attributed to the protective action of the surfactant on the surfaces of the powders that prevents neck formation until after all the surfactant has volatilized. A striking feature of the IR spectra collected on the iron oxide powders is the absence of peaks in the ~1715 cm(-1) to 1750 cm(-1) region, where absorption due to the symmetric C=O (carbonyl) stretching occurs. The lack of such peaks strongly suggests the carbonyl group is no longer free, but is actively participating in the surfactant-precipitate interaction. The final two microemulsion systems, containing CTAB as the surfactant, showed that loss of control of the reverse micelle synthesis process can easily occur when the amount of salt in the water domains exceeds a critical concentration. Both model systems eventually resulted in agglomerated powders of broad size distributions or particles that were large compared to the sizes of the reverse micelles, consistent with the notion that the microemulsions were not stable and the powders were precipitated in an uncontrolled fashion. This has implications for the synthesis of nanopowders by reverse micelle synthesis and provides a benchmark for process control if powders of the highest quality are desired. Copyright © 2013 Elsevier Inc. All rights reserved.

Characterisation of Suspension Precipitated Nanocrystalline Hydroxyapatite Powders

NASA Astrophysics Data System (ADS)

Mallik, P. K.; Swain, P. K.; Patnaik, S. C.

2016-02-01

Hydroxyapatite (HA) is a well-known biomaterial for coating on femoral implants, filling of dental cavity and scaffold for tissue replacement. Hydroxyapatite possess limited load bearing capacity due to their brittleness. In this paper, the synthesis of nanocrystalline hydroxyapatite powders was prepared by dissolving calcium oxide in phosphoric acid, followed by addition of ammonia liquor in a beaker. The prepared solution was stirred by using magnetic stirrer operated at temperature of 80°C for an hour. This leads to the formation of hydroxyapatite precipitate. The precipitate was dried in oven for overnight at 100°C. The dried agglomerated precipitate was calcined at 800°C in conventional furnace for an hour. The influence of calcium oxide concentration and pH on the resulting precipitates was studied using BET, XRD and SEM. As result, a well-defined sub-rounded morphology of powders size of ∼41 nm was obtained with a salt concentration of 0.02 M. Finally, it can be concluded that small changes in the reaction conditions led to large changes in final size, shape and degree of aggregation of the hydroxyapatite particles.

Mechanical properties and rapid low-temperature consolidation of nanocrystalline Cu-ZrO2 composites by pulsed current activated heating

NASA Astrophysics Data System (ADS)

Kang, Bo-Ram; Yoon, Jin-kook; Hong, Kyung-Tae; Shon, In-Jin

2015-07-01

Metal-ceramic compositr can be obtained with an optimum combination of low density, high oxidation resistance, and high hardness of the ceramic and toughness of the metal. Therefore, metal matrix composites are recognized as candidates for aerospace, automotive, biomaterials, and defense applications. Despite its many attractive properties, the low fracture toughness of ZrO2 limits its wide application. One of the most obvious tactics to improve the mechanical properties has been to fabricate a nanostructured material and composite material. Nano-powders of Cu and ZrO2 were synthesized from 2CuO and Zr powders by high-energy ball milling. Nanocrystalline 2Cu-ZrO2 composite was consolidated within 5 minutes from mechanically synthesized powders of ZrO2 and 2Cu at low temperature, by a pulsed current activated sintering method. The relative density of the composite was 98.5%. The fracture toughness of 2Cu-ZrO2 composite in this study is higher than that of monolithic ZrO2, without great decrease of hardness.

Mechanical Alloying of W-Mo-V-Cr-Ta High Entropy Alloys

NASA Astrophysics Data System (ADS)

Das, Sujit; Robi, P. S.

2018-04-01

Recent years have seen the emergence of high-entropy alloys (HEAs) consisting of five or more elements in equi-atomic or near equi-atomic ratios. These alloys in single phase solid solution exhibit exceptional mechanical properties viz., high strength at room and elevated temperatures, reasonable ductility and stable microstructure over a wide range of temperatures making it suitable for high temperature structural materials. In spite of the attractive properties, processing of these materials remains a challenge. Reports regarding fabrication and characterisation of a few refractory HEA systems are available. The processing of these alloys have been carried out by arc melting of small button sized materials. The present paper discusses the development of a novel refractory W-Mo-V-Cr-Ta HEA powder based on a new alloy design concept. The powder mixture was milled for time periods up to 64 hours. Single phase alloy powder having body centred cubic structure was processed by mechanical alloying. The milling characteristics and extent of alloying during the ball milling were characterized using X-ray diffractiometre (XRD), field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM). A single phase solid solution alloy powder having body-centred cubic (BCC) structure with a lattice parameter of 3.15486 Å was obtained after milling for 32 hours.

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

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

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

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

The Mechanical Properties and In Vitro Biocompatibility of PM-Fabricated Ti-28Nb-35.4Zr Alloy for Orthopedic Implant Applications

PubMed Central

Xu, Wei; Li, Ming; Wen, Cuie; Lv, Shaomin; Liu, Chengcheng; Lu, Xin

2018-01-01

A biocompatible Ti-28Nb-35.4Zr alloy used as bone implant was fabricated through the powder metallurgy process. The effects of mechanical milling and sintering temperatures on the microstructure and mechanical properties were investigated systematically, before in vitro biocompatibility of full dense Ti-28Nb-35.4Zr alloy was evaluated by cytotoxicity tests. The results show that the mechanical milling and sintering temperatures have significantly effects on the density and mechanical properties of the alloys. The relative density of the alloy fabricated by the atomized powders at 1500 °C is only 83 ± 1.8%, while the relative density of the alloy fabricated by the ball-milled powders can rapidly reach at 96.4 ± 1.3% at 1500 °C. When the temperature was increased to 1550 °C, the alloy fabricated by ball-milled powders achieve full density (relative density is 98.1 ± 1.2%). The PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C can achieve a wide range of mechanical properties, with a compressive yield strength of 1058 ± 35.1 MPa, elastic modulus of 50.8 ± 3.9 GPa, and hardness of 65.8 ± 1.5 HRA. The in vitro cytotoxicity test suggests that the PM-fabricated Ti-28Nb-35.4Zr alloy by ball-milled powders at 1550 °C has no adverse effects on MC3T3-E1 cells with cytotoxicity ranking of 0 grade, which is nearly close to ELI Ti-6Al-4V or CP Ti. These properties and the net-shape manufacturability makes PM-fabricated Ti-28Nb-35.4Zr alloy a low-cost, highly-biocompatible, Ti-based biomedical alloy. PMID:29601517

Heat Treatment of Gas-Atomized Powders for Cold Spray Deposition

NASA Astrophysics Data System (ADS)

Story, William A.; Brewer, Luke N.

2018-02-01

This communication demonstrates the efficacy of heat treatment on the improved deposition characteristics of aluminum alloy powders. A novel furnace was constructed for solutionizing of feedstock powders in an inert atmosphere while avoiding sintering. This furnace design achieved sufficiently high cooling rates to limit re-precipitation during powder cooling. Microscopy showed homogenization of the powder particle microstructures after heat treatment. Cold spray deposition efficiency with heat-treated powders substantially increased for the alloys AA2024, AA6061, and AA7075.

Nanocrystalline Cobalt-Phosphorous Electroplating as an Alternative to Hard Chromium Electroplating

DTIC Science & Technology

2012-08-01

Validate pulsed electrodeposition of Nanocrystalline Cobalt-Phosphorous (nCoP) alloy coatings as a Hard Chrome electroplating alternative for DoD...limits Cr+6  Cathode Efficiency Cr Plating *Co PEL is 20 µg/m3  ≈5X faster than Chrome plating  Increased throughput  One nCo-P tank can...replace several hard chrome tanks  Bath is Stable nCoP Plating Approaches 100% Efficiency  Process Comparison CoP Technical Approach

Particle Characteristics and Densification of W6Mo5Cr4V2Co5Nb Overspray Powder

NASA Astrophysics Data System (ADS)

Pi, Ziqiang; Lu, Xin; Yang, Fei; Liu, Bowen; Jia, Chengchang; Qu, Xuanhui; Zheng, Wei; Wu, Lizhi; Shao, Qingli

2018-05-01

W6Mo5Cr4V2Co5Nb (825 K) alloy was prepared by a two-step sintering process from overspray 825 K alloy powder. The overspray powder characteristics and the microstructure and mechanical properties of the as-sintered 825 K alloy were investigated. Results showed that two types of carbides formed a network structure in the overspray powder, which had spherical or quasispherical shape: one was MC carbide that was rich in vanadium (V), and the other was M2C carbide enriched with vanadium (V) and tungsten (W). The sintered 825 K alloy contained M6C and MC carbides, of which M6C was rich in tungsten (W) and molybdenum (Mo), and both of these two carbides were uniformly distributed in the alloy matrix. The alloy had relative density of 98.43%, hardness of HRC 51.8, and superior bending strength of 2042 MPa. These mechanical properties can meet the requirements of most engineering applications.

Method to grow pure nanocrystalline diamond films at low temperatures and high deposition rates

DOEpatents

Carlisle, John A [Plainfield, IL; Gruen, Dieter M [Downers Grove, IL; Auciello, Orlando [Bolingbrook, IL; Xiao, Xingcheng [Woodridge, IL

2009-07-07

A method of depositing nanocrystalline diamond film on a substrate at a rate of not less than about 0.2 microns/hour at a substrate temperature less than about 500.degree. C. The method includes seeding the substrate surface with nanocrystalline diamond powder to an areal density of not less than about 10.sup.10sites/cm.sup.2, and contacting the seeded substrate surface with a gas of about 99% by volume of an inert gas other than helium and about 1% by volume of methane or hydrogen and one or more of acetylene, fullerene and anthracene in the presence of a microwave induced plasma while maintaining the substrate temperature less than about 500.degree. C. to deposit nanocrystalline diamond on the seeded substrate surface at a rate not less than about 0.2 microns/hour. Coatings of nanocrystalline diamond with average particle diameters of less than about 20 nanometers can be deposited with thermal budgets of 500.degree. C.-4 hours or less onto a variety of substrates such as MEMS devices.

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

PubMed

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

2013-04-01

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

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

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.

An application of powder metallurgy to dentistry.

PubMed

Oda, Y; Ueno, S; Kudoh, Y

1995-11-01

Generally, the dental casting method is used to fabricate dental prostheses made with metal. The method of fabricating dental prostheses from sintered titanium alloy has certain advantages: the elimination of casting defects, a sintering temperature that is lower than the melting point, and a shorter processing time. By examining (1) the properties of green, sintered compacts of titanium powder, (2) the effects of adding aluminum powder on the properties of green, sintered compacts of Ti-Al compound, and (3) the effects of adding copper powder on the properties of green, sintered compacts of Ti-Al-Cu compound, the authors developed a sintered titanium alloy on a trial basis. Because the properties satisfied the requirements of dental restorations, a powder metallurgical method of making dental restorations from this sintered titanium alloy was devised. Applications of such sintered titanium alloys for the metal coping of metal-ceramic crowns and denture base plates were discussed.

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

PubMed

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

2016-11-01

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

Effects of carbon and hafnium concentrations in wrought powder-metallurgy superalloys based on NASA 2B-11 alloy

NASA Technical Reports Server (NTRS)

Miner, R. V., Jr.

1976-01-01

A candidate alloy for advanced-temperature turbine engine disks, and four modifications of that alloy with various C and Hf concentrations were produced as cross-rolled disks from prealloyed powder that was hot isostatically compacted. The mechanical properties, microstructures, and phase relations of the alloys are discussed in terms of their C and Hf concentrations. A low-C and high-Hf modification of IIB-11 had the best balance of mechanical properties for service below about 750 C. Because of their finer grain sizes, none of the powder-metallurgy alloys produced had the high-temperature rupture strength of conventionally cast and wrought IIB-11.

Structure of dental gallium alloys.

PubMed

Herø, H; Simensen, C J; Jørgensen, R B

1996-07-01

The interest in gallium alloys as a replacement for amalgam has increased in recent years due to the risk of environmental pollution from amalgam. Alloy powders with compositions close to those for alloys of amalgam are mixed with a liquid gallium alloy. The mix is condensed into a prepared cavity in much the same way as for amalgam. The aim of the present work was to study the structure of: (1) two commercial alloy powders containing mainly silver, tin and copper, and (2) the phases formed by mixing these powders with a liquid alloy of gallium, indium and tin. One of the alloy powders contained 9 wt% palladium. Cross-sections of cylindrical specimens made by these gallium mixes were investigated by scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction. Discrete grains of the following phases were found to be present in both gallium alloys: hexagonal Ag2Ga, tetragonal Cu(Pd)Ga2, cubic Ag9In4 and tetragonal beta-Sn. Indications of hexagonal or orthorhombic Ag2Sn were found in the remaining, unreacted alloy particles. In the palladium-containing alloy the X-ray reflections indicate a minor fraction of cubic Cu9Ga4 in addition to the Cu(Pd)Ga2 phase. Particles of beta-Sn are probably precipitated because Sn-Ga phases cannot be formed according to the binary phase diagram.

The role of nanocrystalline binder metallic coating into WC after additive manufacturing

NASA Astrophysics Data System (ADS)

Cavaleiro, A. J.; Fernandes, C. M.; Farinha, A. R.; Gestel, C. V.; Jhabvala, J.; Boillat, E.; Senos, A. M. R.; Vieira, M. T.

2018-01-01

Tungsten carbide with microsized particle powders are commonly used embedded in a tough binder metal. The application of these composites is not limited to cutting tools, WC based material has been increasingly used in gaskets and other mechanical parts with complex geometries. Consequently, additive manufacturing processes as Selective Laser Sintering (SLS) might be the solution to overcome some of the manufacturing problems. However, the use of SLS leads to resolve the problems resulting from difference of physical properties between tungsten carbide and the metallic binder, such as laser absorbance and thermal conductivity. In this work, an original approach of powder surface modification was considered to prepare WC-metal composite powders and overcome these constraints, consisting on the sputter-coating of the WC particle surfaces with a nanocrystalline thin film of metallic binder material (stainless steel). The coating improves the thermal behavior and rheology of the WC particles and, at the same time, ensures a binder homogenous distribution. The feasibility of the SLS technology as manufacturing process for WC powder sputter-coated with 13 wt% stainless steel AISI 304L was explored with different laser power and scanning speed parameters. The SLS layers were characterized regarding elemental distribution, phase composition and morphology, and the results are discussed emphasizing the role of the coating on the consolidation process.

Argon-shielded hot pressing of titanium alloy (Ti6Al4V) powders.

PubMed

Gronostajski, Zbigniew; Bandoła, P; Skubiszewski, T

2010-01-01

The paper presents the method of the argon - shielded hot pressing of titanium alloy (Ti6A14V) powder (used in medical industry). The powders produced in the GA (gas atomization) process and in the HDH (hydride - dehydride) process were used in the experiments. A pressing process was conducted at a temperature of 800-850 degrees C for different lengths of time. An unoxidized sintered material, nearly as dense as a solid material and having a lamellar structure (alpha+beta), was obtained from the titanium alloy powder produced in the HDH process.

Enhanced Magnetic Properties of Nd15Fe77B8 Alloy Powders Produced by Melt-Spinning Technique

NASA Astrophysics Data System (ADS)

Öztürk, Sultan; İcin, Kürşat; Öztürk, Bülent; Topal, Uğur; Odabaşı, Hülya Kaftelen; Göbülük, Metin; Cora, Ömer Necati

2017-10-01

Rapidly solidified Nd15Fe77B8 alloy powders were produced by means of melt-spinning method in high-vacuum atmosphere to achieve improved magnetic and thermal properties. To this goal, a vacuum milling apparatus was designed and constructed to ball-mill the melt-spun powders in a surfactant active atmosphere. Various milling times were experimented to reveal the effect of the milling time on the mean particle size and other size-dependent properties such as magnetism and Curie temperature. Grain structure, cooling rate, and phase structure of the produced powders were also investigated. The Curie points shifted to higher temperatures from the ingot condition to surfactant active ball-milling and the values for Nd15Fe77B8 ingot alloy, melt-spun powders, and surfactant active ball-milled powders were 552 K, 595 K, and 604 K (279 °C, 322 °C, and 331 °C), respectively. It was noted that the surfactant active ball-milling process improved the magnetic and thermal properties of melt-spun Nd15Fe77B8 alloy powders. Compared to relevant literature, the coercivity of powders increased significantly with increasing milling time and decreasing in powder size. The coercivity value as high as 3427 kA m-1 was obtained.

Nanoindentation testing as a powerful screening tool for assessing phase stability of nanocrystalline high-entropy alloys

DOE PAGES

Maier-Kiener, Verena; Schuh, Benjamin; George, Easo P.; ...

2016-11-19

The equiatomic high-entropy alloy (HEA), CrMnFeCoNi, has recently been shown to be microstructurally unstable, resulting in a multi-phase microstructure after intermediate-temperature annealing treatments. The decomposition occurs rapidly in the nanocrystalline (NC) state and after longer annealing times in coarse-grained states. To characterize the mechanical properties of differently annealed NC states containing multiple phases, nanoindentation was used in this paper. The results revealed besides drastic changes in hardness, also for the first time significant changes in the Young's modulus and strain rate sensitivity. Finally, nanoindentation of NC HEAs is, therefore, a useful complementary screening tool with high potential as a highmore » throughput approach to detect phase decomposition, which can also be used to qualitatively predict the long-term stability of single-phase HEAs.« less

Contamination Effects on Improving the Hydrogenation/Dehydrogenation Kinetics of Binary Magnesium Hydride/Titanium Carbide Systems Prepared by Reactive Ball Milling

PubMed Central

El-Eskandarany, M. Sherif; Shaban, Ehab

2015-01-01

Ultrafine MgH2 nanocrystalline powders were prepared by reactive ball milling of elemental Mg powders after 200 h of high-energy ball milling under a hydrogen gas pressure of 50 bar. The as-prepared metal hydride powders were contaminated with 2.2 wt. % of FeCr-stainless steel that was introduced to the powders upon using stainless steel milling tools made of the same alloy. The as-synthesized MgH2 was doped with previously prepared TiC nanopowders, which were contaminated with 2.4 wt. % FeCr (materials of the milling media), and then ball milled under hydrogen gas atmosphere for 50 h. The results related to the morphological examinations of the fabricated nanocomposite powders beyond the micro-and nano-levels showed excellent distributions of 5.2 wt. % TiC/4.6 wt. % FeCr dispersoids embedded into the fine host matrix of MgH2 powders. The as-fabricated nanocomposite MgH2/5.2 wt. % TiC/4.6 wt. % FeCr powders possessed superior hydrogenation/dehydrogenation characteristics, suggested by the low value of the activation energy (97.74 kJ/mol), and the short time required for achieving a complete absorption (6.6 min) and desorption (8.4 min) of 5.51 wt. % H2 at a moderate temperature of 275 °C under a hydrogen gas pressure ranging from 100 mbar to 8 bar. van’t Hoff approach was used to calculate the enthalpy (∆H) and entropy (∆S) of hydrogenation for MgH2, which was found to be −72.74 kJ/mol and 112.79 J/mol H2/K, respectively. Moreover, van’t Hoff method was employed to calculate the ΔH and ΔS of dehydrogenation, which was found to be 76.76 kJ/mol and 119.15 J/mol H2/K, respectively. This new nanocomposite system possessed excellent absorption/desorption cyclability of 696 complete cycles, achieved in a cyclic-life-time of 682 h. PMID:28793606

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.

Method for Production of Powders

NASA Technical Reports Server (NTRS)

Stoltzfus, Joel M. (Inventor); Sircar, Subhasish (Inventor)

1997-01-01

Apparatus and method are disclosed for producing oxides of metals and of metal alloys. The metal or alloy is placed in an oxygen atmosphere in a combustion chamber and ignited. Products of the combustion include one or more oxides of the metal or alloy in powdered form. In one embodiment of the invention a feeder is provided whereby material to be oxidized by combustion can be achieved into a combustion chamber continuously. A product remover receives the powder product of the combustion.

Examination of Short- and Long-Range Atomic Order Nanocrystalline SiC and Diamond by Powder Diffraction Methods

NASA Technical Reports Server (NTRS)

Palosz, B.; Grzanka, E.; Stelmakh, S.; Gierlotka, S.; Weber, H.-P.; Proffen, T.; Palosz, W.

2002-01-01

The real atomic structure of nanocrystals determines unique, key properties of the materials. Determination of the structure presents a challenge due to inherent limitations of standard powder diffraction techniques when applied to nanocrystals. Alternate methodology of the structural analysis of nanocrystals (several nanometers in size) based on Bragg-like scattering and called the "apparent lattice parameter" (alp) is proposed. Application of the alp methodology to examination of the core-shell model of nanocrystals will be presented. The results of application of the alp method to structural analysis of several nanopowders were complemented by those obtained by determination of the Atomic Pair Distribution Function, PDF. Based on synchrotron and neutron diffraction data measured in a large diffraction vector of up to Q = 25 Angstroms(exp -1), the surface stresses in nanocrystalline diamond and SiC were evaluated.

Atomic simulation of mechanical behavior of Mg in a super-lattice of nanocrystalline Mg and amorphous Mg-Al alloy

NASA Astrophysics Data System (ADS)

Song, H. Y.; An, M. R.; Li, Y. L.; Deng, Q.

2014-12-01

The mechanical properties of a super-lattice architecture composed of nanocrystalline Mg and Mg-Al amorphous alloy are investigated using molecular dynamics simulation. The results indicate that deformation mechanism of nanocrystalline Mg is obviously affected by the amorphous boundary spacing and temperature. The strength of the material increases with the decrease of amorphous boundary spacing, presenting a Hall-Petch effect at both 10 K and 300 K. A stress platform and following stiffness softening, as well as a linear strengthening in the plastic stage, are observed when the amorphous boundary spacing below 8.792 nm at 10 K. The implying reason may be that the amorphous boundary acts as the dislocations emission and absorption source. However, the second stress peak is not observed for the models at 300 K. Instead, the flow stress in plastic stage is a nearly constant value. The simulation demonstrates the emergence of the new grain, accompanied by the deformation twins and stacking faults associated with the plastic behaviors at 300 K. The general conclusions derived from this work may provide a guideline for the design of high-performance hexagonal close-packed metals.

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

Processing-Microstructure-Property Relationships for Cold Spray Powder Deposition of Al-Cu Alloys

DTIC Science & Technology

2015-06-01

MICROSTRUCTURE - PROPERTY RELATIONSHIPS FOR COLD SPRAY POWDER DEPOSITION OF Al - Cu ALLOYS by Jeremy D. Leazer June 2015 Thesis Advisor: Sarath K...basic microstructure -mechanical property relationships for cold spray deposited Al - Cu alloy coatings The microstructure of the deposited materials will...the dynamic mechanical

48 CFR 252.225-7008 - Restriction on Acquisition of Specialty Metals.

Code of Federal Regulations, 2012 CFR

2012-10-01

... atomization or sputtering of titanium, or final consolidation of non-melt derived titanium powder or titanium alloy powder. (3) Specialty metal means— (i) Steel— (A) With a maximum alloy content exceeding one or..., molybdenum, nickel, niobium (columbium), titanium, tungsten, or vanadium; (ii) Metal alloys consisting of— (A...

48 CFR 252.225-7008 - Restriction on Acquisition of Specialty Metals.

Code of Federal Regulations, 2010 CFR

2010-10-01

... atomization or sputtering of titanium, or final consolidation of non-melt derived titanium powder or titanium alloy powder. (3) Specialty metal means— (i) Steel— (A) With a maximum alloy content exceeding one or..., molybdenum, nickel, niobium (columbium), titanium, tungsten, or vanadium; (ii) Metal alloys consisting of— (A...

48 CFR 252.225-7008 - Restriction on Acquisition of Specialty Metals.

Code of Federal Regulations, 2011 CFR

2011-10-01

... atomization or sputtering of titanium, or final consolidation of non-melt derived titanium powder or titanium alloy powder. (3) Specialty metal means— (i) Steel— (A) With a maximum alloy content exceeding one or..., molybdenum, nickel, niobium (columbium), titanium, tungsten, or vanadium; (ii) Metal alloys consisting of— (A...

Synthesis of a single phase of high-entropy Laves intermetallics in the Ti-Zr-V-Cr-Ni equiatomic alloy

NASA Astrophysics Data System (ADS)

Yadav, T. P.; Mukhopadhyay, Semanti; Mishra, S. S.; Mukhopadhyay, N. K.; Srivastava, O. N.

2017-12-01

The high-entropy Ti-Zr-V-Cr-Ni (20 at% each) alloy consisting of all five hydride-forming elements was successfully synthesised by the conventional melting and casting as well as by the melt-spinning technique. The as-cast alloy consists entirely of the micron size hexagonal Laves Phase of C14 type; whereas, the melt-spun ribbon exhibits the evolution of nanocrystalline Laves phase. There was no evidence of any amorphous or any other metastable phases in the present processing condition. This is the first report of synthesising a single phase of high-entropy complex intermetallic compound in the equiatomic quinary alloy system. The detailed characterisation by X-ray diffraction, scanning and transmission electron microscopy and energy-dispersive X-ray spectroscopy confirmed the existence of a single-phase multi-component hexagonal C14-type Laves phase in all the as-cast, melt-spun and annealed alloys. The lattice parameter a = 5.08 Å and c = 8.41 Å was determined from the annealed material (annealing at 1173 K). The thermodynamic calculations following the Miedema's approach support the stability of the high-entropy multi-component Laves phase compared to that of the solid solution or glassy phases. The high hardness value (8.92 GPa at 25 g load) has been observed in nanocrystalline high-entropy alloy ribbon without any cracking. It implies that high-yield strength ( 3.00 GPa) and the reasonable fracture toughness can be achieved in this high-entropy material.

Magnetic ageing study of high and medium permeability nanocrystalline FeSiCuNbB alloys

NASA Astrophysics Data System (ADS)

Lekdim, Atef; Morel, Laurent; Raulet, Marie-Ange

2017-04-01

increasing the energy efficiency is one of the most important issues in modern power electronic systems. In aircraft applications, the energy efficiency must be associated with a maximum reduction of mass and volume, so a high components compactness. A consequence from this compactness is the increase of operating temperature. Thus, the magnetic materials used in these applications, have to work at high temperature. It raises the question of the thermal ageing problem. The reliability of these components operating at this condition becomes a real problem which deserves serious interest. Our work takes part in this context by studying the magnetic material thermal ageing. The nanocrystalline materials are getting more and more used in power electronic applications. Main advantages of nanocrystalline materials compared to ferrite are: high saturation flux density of almost 1.25 T and low dynamic losses for low and medium frequencies. The nanocrystalline Fe73.5Cu1Nb3Si15.5B7 alloys have been chosen in our aging study. This study is based on monitoring the magnetic characteristics for several continuous thermal ageing (100, 150, 200 and 240 °C). An important experimental work of magnetic characterization is being done following a specific monitoring protocol. Elsewhere, X-Ray Diffraction and magnetostriction measurements were carried out to support the study of the anisotropy energies evolution with ageing. This latter is discussed in this paper to explain and give hypothesis about the ageing phenomena.

Microstructure and Aging of Powder-Metallurgy Al Alloys

NASA Technical Reports Server (NTRS)

Blackburn, L. B.

1987-01-01

Report describes experimental study of thermal responses and aging behaviors of three new aluminum alloys. Alloys produced from rapidly solidified powders and contain 3.20 to 5.15 percent copper, 0.24 to 1.73 percent magnesium, 0.08 to 0.92 percent iron, and smaller amounts of manganese, nickel, titanium, silicon, and zinc. Peak hardness achieved at lower aging temperatures than with standard ingot-metallurgy alloys. Alloys of interest for automobile, aircraft, and aerospace applications.

X-ray absorption fine structure and x-ray diffraction studies of crystallographic grains in nanocrystalline FePd:Cu thin films

NASA Astrophysics Data System (ADS)

Krupinski, M.; Perzanowski, M.; Polit, A.; Zabila, Y.; Zarzycki, A.; Dobrowolska, A.; Marszalek, M.

2011-03-01

FePd alloys have recently attracted considerable attention as candidates for ultrahigh density magnetic storage media. In this paper we investigate FePd thin alloy film with a copper admixture composed of nanometer-sized grains. [Fe(0.9 nm)/Pd(1.1 nm)/Cu(d nm)]×5 multilayers were prepared by thermal deposition at room temperature in UHV conditions on Si(100) substrates covered by 100 nm SiO2. The thickness of the copper layer has been changed from 0 to 0.4 nm. After deposition, the multilayers were rapidly annealed at 600 °C in a nitrogen atmosphere, which resulted in the creation of the FePd:Cu alloy. The structure of alloy films obtained this way was determined by x-ray diffraction (XRD), glancing angle x-ray diffraction, and x-ray absorption fine structure (EXAFS). The measurements clearly showed that the L10 FePd:Cu nanocrystalline phase has been formed during the annealing process for all investigated copper compositions. This paper concentrates on the crystallographic grain features of FePd:Cu alloys and illustrates that the EXAFS technique, supported by XRD measurements, can help to extend the information about grain size and grain shape of poorly crystallized materials. We show that, using an appropriate model of the FePd:Cu grains, the comparison of EXAFS and XRD results gives a reasonable agreement.

Stability of an Electrodeposited Nanocrystalline Ni-Based Alloy Coating in Oil and Gas Wells with the Coexistence of H₂S and CO₂.

PubMed

Sui, Yiyong; Sun, Chong; Sun, Jianbo; Pu, Baolin; Ren, Wei; Zhao, Weimin

2017-06-09

The stability of an electrodeposited nanocrystalline Ni-based alloy coating in a H₂S/CO₂ environment was investigated by electrochemical measurements, weight loss method, and surface characterization. The results showed that both the cathodic and anodic processes of the Ni-based alloy coating were simultaneously suppressed, displaying a dramatic decrease of the corrosion current density. The corrosion of the Ni-based alloy coating was controlled by H₂S corrosion and showed general corrosion morphology under the test temperatures. The corrosion products, mainly consisting of Ni₃S₂, NiS, or Ni₃S₄, had excellent stability in acid solution. The corrosion rate decreased with the rise of temperature, while the adhesive force of the corrosion scale increased. With the rise of temperature, the deposited morphology and composition of corrosion products changed, the NiS content in the corrosion scale increased, and the stability and adhesive strength of the corrosion scale improved. The corrosion scale of the Ni-based alloy coating was stable, compact, had strong adhesion, and caused low weight loss, so the corrosion rates calculated by the weight loss method cannot reveal the actual oxidation rate of the coating. As the corrosion time was prolonged, the Ni-based coating was thinned while the corrosion scale thickened. The corrosion scale was closely combined with the coating, but cannot fully prevent the corrosive reactants from reaching the substrate.

Nanostructured Mg 2Ni materials prepared by cold rolling and used as negative electrode for Ni-MH batteries

NASA Astrophysics Data System (ADS)

Pedneault, Sylvain; Huot, Jacques; Roué, Lionel

In the present work, cold rolling has been investigated as a new means of producing Mg-based metal hydrides for nickel-metal hydride (Ni-MH) batteries. Structure and electrochemical evolution of 2Mg-Ni cold-rolled samples were investigated as a function of the number of rolling passes as well as heat treatment. It was found that nanocrystalline Mg 2Ni alloy can be obtained by an appropriate three step process involving rolling, heat treatment and rolling again. It was shown that the number of primary and secondary rolling passes must be carefully optimized in order to favour the complete formation of Mg 2Ni alloy having a nanocrystalline structure (∼10 nm in crystallite size) without excessive sample oxidation. Actually, the best result was obtained by first rolling 90 times, followed by a heat treatment at 400 °C for 4 h and roll again 20 times. The resulting material displayed an initial discharge capacity of 205 mAh g -1, which is quite similar to that obtained with ball-milled Mg 2Ni alloy.

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.

Method and apparatus for production of powders

NASA Technical Reports Server (NTRS)

Stolzfus, Joel M. (Inventor); Sircar, Subhasish (Inventor)

1995-01-01

Apparatus and method are disclosed for producing oxides of metals and of metal alloys. The metal or alloy is placed in an oxygen atmosphere in a combustion chamber and ignited. Products of the combustion include one or more oxides of the metal or alloy in powdered form. In one embodiment of the invention a feeder is provided whereby material to be oxidized by combustion can be advanced into a combustion chamber continuously. A product remover receives the powder product of the combustion.

Structure and properties of electrodeposited nanocrystalline Ni and Ni-Fe alloy continuous foils

NASA Astrophysics Data System (ADS)

Giallonardo, Jason Derek

This research work presents the first comprehensive study on nanocrystalline materials produced in bulk quantities using a novel continuous electrodeposition process. A series of nanocrystalline Ni and Ni-Fe alloy continuous foils were produced and an intensive investigation into their structure and various properties was carried out. High-resolution transmission electron microscopy (HR-TEM) revealed the presence of local strain at high and low angle, and twin boundaries. The cause for these local strains was explained based on the interpretation of non-equilibrium grain boundary structures that result when conditions of compatibility are not satisfied. HR-TEM also revealed the presence of twin faults of the growth type, or "growth faults", which increased in density with the addition of Fe. This observation was found to be consistent with a corresponding increase in the growth fault probabilities determined quantitatively using X-ray diffraction (XRD) pattern analysis. Hardness and Young's modulus were measured by nanoindentation. Hardness followed the regular Hall-Petch behaviour down to a grain size of 20 nm after which an inverse trend was observed. Young's modulus was slightly reduced at grain sizes less than 20 nm and found to be affected by texture. Microstrain based on XRD line broadening was measured for these materials and found to increase primarily with a decrease in grain size or an increase in intercrystal defect density (i.e., grain boundaries and triple junctions). This microstrain is associated with the local strains observed at grain boundaries in the HR-TEM image analysis. A contribution to microstrain from the presence of growth faults in the nanocrystalline Ni-Fe alloys was also noted. The macrostresses for these materials were determined from strain measurements using a two-dimensional XRD technique. At grain sizes less than 20 nm, there was a sharp increase in compressive macrostresses which was also owed to the corresponding increase in intercrystal defects or interfaces in the solid.

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

Phumying, Santi; Labuayai, Sarawuth; Swatsitang, Ekaphan

Graphical abstract: This figure shows the specific magnetization curves of the as-prepared MFe{sub 2}O{sub 4} (M = Ni, Co, Mn, Mg, Zn) powders obtained from room temperature VSM measurement. These curves are typical for a soft magnetic material and indicate hysteresis ferromagnetism in the field ranges of ±500 Oe, ±1000 Oe, and ±2000 Oe for the CoFe{sub 2}O{sub 4}, MgFe{sub 2}O{sub 4} and MnFe{sub 2}O{sub 4} respectively, whereas the samples of NiFe{sub 2}O{sub 4} and ZnFe{sub 2}O{sub 4} show a superparamagnetic behavior. Highlights: ► Nanocrystalline MFe{sub 2}O{sub 4} powders were synthesized by a novel hydrothermal method. ► Metal acetylacetonates andmore » aloe vera plant-extracted solution are used. ► This biosynthetic route is very simple and provides high-yield oxide nanomaterials. ► XRD and TEM results indicate that the prepared samples have only spinel structure. ► The maximum M{sub s} of 68.9 emu/g at 10 kOe were observed for the samples of MnFe{sub 2}O{sub 4}. - Abstract: Nanocrystalline spinel ferrite MFe{sub 2}O{sub 4} (M = Ni, Co, Mn, Mg, Zn) powders were synthesized by a novel hydrothermal method using Fe(acac){sub 3}, M(acac){sub 3} (M = Ni, Co, Mn, Mg, Zn) and aloe vera plant extracted solution. The X-ray diffraction and selected-area electron diffraction results indicate that the synthesized nanocrystalline have only spinel structure without the presence of other phase impurities. The crystal structure and morphology of the spinel ferrite powders, as revealed by TEM, show that the NiFe{sub 2}O{sub 4} and CoFe{sub 2}O{sub 4} samples contain nanoparticles, whereas the MnFe{sub 2}O{sub 4} and MgFe{sub 2}O{sub 4} samples consist of many nanoplatelets and nanoparticles. Interestingly, the ZnFe{sub 2}O{sub 4} sample contains plate-like structure of networked nanocrystalline particles. Room temperature magnetization results show a ferromagnetic behavior of the CoFe{sub 2}O{sub 4}, MnFe{sub 2}O{sub 4} and MgFe{sub 2}O{sub 4} samples, whereas the samples of NiFe{sub 2}O{sub 4} and ZnFe{sub 2}O{sub 4} exhibit a superparamagnetic behavior.« less

Fabrication of high-alloy powders consisting of spherical particles from ultradispersed components

NASA Astrophysics Data System (ADS)

Samokhin, A. V.; Fadeev, A. A.; Sinayskiy, M. A.; Alekseev, N. V.; Tsvetkov, Yu. V.; Arzhatkina, O. A.

2017-07-01

It is shown that powders of a model high alloy consisting of spherical particles 25-50 μm in size can be synthesized from a starting ultradispersed powder, which is made of a mixture of the alloy components and is fabricated by the magnesiothermal reduction of metal chlorides in the potassium chloride melt. The synthesis includes the stages of microgranulation of an ultradispersed powder, heat treatment of microgranules, classification of the microgranules with the separation of microgranule fraction of 25-50 μm, spheroidization of the separated fraction in a thermal plasma flow, and classification with the separation of a fraction of micro- and submicrometer-sized particles.

A Novel Process for Joining Ti Alloy and Al Alloy using Two-Stage Sintering Powder Metallurgy

NASA Astrophysics Data System (ADS)

Long, Luping; Liu, Wensheng; Ma, Yunzhu; Wu, Lei; Liu, Chao

2018-04-01

The major challenges for conventional diffusion bonding of joining Ti alloy and Al alloy are the undesirable interfacial reaction, low matrixes and joint strength. To avoid the problem in diffusion bonding, a novel two-stage sintering powder metallurgy process is developed. In the present work, the interface characterization and joint performance of the bonds obtained by powder metallurgy bonding are investigated and are compared with the diffusion bonded Ti/Al joints obtained with the same and the optimized process parameters. The results show that no intermetallic compound is visible in the Ti/Al joint obtained by powder metallurgy bonding, while a new layer formed at the joint diffusion bonded with the same parameters. The maximum tensile strength of joint obtained by diffusion bonding is 58 MPa, while a higher tensile strength reaching 111 MPa for a bond made by powder metallurgy bonding. Brittle fractures occur at all the bonds. It is shown that the powder metallurgy bonding of Ti/Al is better than diffusion bonding. The results of this study should benefit the bonding quality.

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.

Investigation of the Surface Stress in SiC and Diamond Nanocrystals by In-situ High Pressure Powder Diffraction Technique

NASA Technical Reports Server (NTRS)

Palosz, B.; Stelmakh, S.; Grzanka, E.; Gierlotka, S.; Zhao, Y.; Palosz, W.

2003-01-01

The real atomic structure of nanocrystals determines key properties of the materials. For such materials the serious experimental problem lies in obtaining sufficiently accurate measurements of the structural parameters of the crystals, since very small crystals constitute rather a two-phase than a uniform crystallographic phase system. As a result, elastic properties of nanograins may be expected to reflect a dual nature of their structure, with a corresponding set of different elastic property parameters. We studied those properties by in-situ high-pressure powder diffraction technique. For nanocrystalline, even one-phase materials such measurements are particularly difficult to make since determination of the lattice parameters of very small crystals presents a challenge due to inherent limitations of standard elaboration of powder diffractograms. In this investigation we used our methodology of the structural analysis, the 'apparent lattice parameter' (alp) concept. The methodology allowed us to avoid the traps (if applied to nanocrystals) of standard powder diffraction evaluation techniques. The experiments were performed for nanocrystalline Sic and GaN powders using synchrotron sources. We applied both hydrostatic and isostatic pressures in the range of up to 40 GPa. Elastic properties of the samples were examined based on the measurements of a change of the lattice parameters with pressure. The results show a dual nature of the mechanical properties (compressibilities) of the materials, indicating a complex, core-shell structure of the grains.

Thermal Stabilization and Mechanical Properties of Nanocrystalline Iron-Nickel-Zirconium Alloys

NASA Astrophysics Data System (ADS)

Kotan, Hasan

Ultrafine grained and nanostructured materials are promising for structural applications because of the high strength compared to coarse grained counterparts. However, their widespread application is limited by an inherently high driving force for thermally induced grain growth, even at low temperatures. Accordingly, the understanding of and control over grain growth in nanoscale materials is of great technological and scientific importance as many physical properties (i.e. mechanical properties) are functions of the average grain size and the grain size distribution within the microstructure. Here, we investigate the microstructural evolution and grain growth in Fe-Ni alloys with Zr addition and differentiate the stabilization mechanisms acting on grain boundaries. Fe-Ni alloys are chosen for stability investigations since they are important for understanding the behavior of many steels and other ferrous alloys. Zirconium is proven to be an effective grain size stabilizer in pure Fe and Fe-base systems. In this study, nanocrystalline alloys were prepared by high energy ball milling. In situ and ex situ experiments were utilized to directly follow grain growth and microstructural evolution as a function of temperature and composition. The information obtained from these experiments enables the real time observation of microstructural evolution and phase transformation and provides a unique view of dynamic reactions as they occur. The knowledge of the thermal stability will exploit the potential high temperature applications and the consolidation conditions (i.e. temperature and pressure) to obtain high dense materials for advanced mechanical tests. Our investigations reveal that the grain growth of Fe-Ni alloys is not affected by Ni content but strongly inhibited by the addition of 1 at% Zr up to about 700 °C. The microstructural stability is lost due to the bcc-to-fcc transformation (occurring at 700°C) by the sudden appearance of abnormally grown fcc grains. However it was determined grain growth can be suppressed kinetically at higher temperatures for high Zr containing alloys by precipitation of intermetallic compounds. Eventually at high enough temperatures the retention of nanocrystallinity was lost, leaving behind fine micron grains filled with nanoscale intermetallic precipitates. Despite the loss of stability the in-situ formed precipitates were found to induce an Orowan hardening affect. The results from the mechanical tests show that Orowan particle strengthening can be as significant as Hall Petch hardening is at the smallest grain sizes.

K3Na(SO4)2 : Eu nanoparticles for high dose of ionizing radiation

NASA Astrophysics Data System (ADS)

Sahare, P. D.; Ranjan, Ranju; Salah, Numan; Lochab, S. P.

2007-02-01

K3Na(SO4)2 : Eu nanocrystalline powder was synthesized by the chemical co-precipitation method. The x-ray diffraction pattern of the nanomaterials shows a hexagonal structure for its crystals having grain size of ~28 nm. Transmission electron microscopy revealed that the K3Na(SO4)2 : Eu nanoparticles are single crystals with almost a uniform shape and size. Thermoluminescence (TL) was taken after irradiating the samples at various exposures of γ-rays from a 60Co source. A prominent TL glow peak is observed at 423 K along with three small peaks/shoulders at around 382, 460 and 509 K. The observed TL sensitivity of the prepared nanocrystalline powder is around 4 times more than that of LiF : Mg,Ti (TLD-100) phosphor. The 423 K peak of the nanomaterial phosphor eventually shows a near linear response with exposures increasing up to very high values (as high as 70 kGy), where all the other TLD phosphors saturate. This property along with its other desired properties such as high sensitivity, relatively simple glow curve structure and low fading makes the nanocrystalline phosphor a suitable dosimeter to estimate low as well as high exposures of γ-rays. TL analysis using the glow curve deconvolution technique was also done for determining different trapping parameters.

Optical Properties of ZnO-Alloyed Nanocrystalline Films

DOE PAGES

Che, Hui; Huso, Jesse; Morrison, John L.; ...

2012-01-01

ZnO is emore » merging as one of the materials of choice for UV applications. It has a deep excitonic energy level and a direct bandgap of ~3.4 eV. Alloying ZnO with certain atomic constituents adds new optical and electronic functionalities to ZnO. This paper presents research on M g x Z n 1 − x O and Z n S 1 − x O x nanocrystalline flexible films, which enable tunable optical properties in the deep-UV and in the visible range. The ZnO and Mg 0 .3 Zn 0 .7 O films were found to have bandgaps at 3.35 and 4.02 eV, respectively. The photoluminescence of the Mg 0 .3 Zn 0 .7 O exhibited a bandedge emission at 3.95 eV, and at lower energy 3.38 eV due to the limited solubility inherent to these alloys. ZnS 0 .76 O 0 .24 and ZnS 0 .16 O 0 .84 were found to have bandgaps at 3.21 and 2.65 eV, respectively. The effect of nitrogen doping on ZnS 0 .16 O 0 .84 is discussed in terms of the highly lattice mismatched nature of these alloys and the resulting valence-band modification.« less

Growth Structure and Properties of Gradient Nanocrystalline Coatings of the Ti-Al-Si-Cu-N System

NASA Astrophysics Data System (ADS)

Ovchinnikov, S. V.; Pinzhin, Yu. P.

2016-10-01

Methods of electron microprobe analysis, X-ray structure analysis and electron microscopy were used to study the element composition and features of the structure-phase, elastic stress state of nanocrystalline coatings of the Ti- Al- Si- Cu- N system with gradient of copper concentration across their thickness. The authors established the effects of element composition modification, non-monotonous behavior of the lattice constant of alloyed nitride and rise in the bending-torsion value of the crystalline lattice in individual nanocrystals to values of around 400 degrees/μm with increase in copper concentration, whereas the sizes of alloyed nitride crystals remained practically unchanged. Mechanical (hardness), adhesion and tribological properties of coatings were examined. Comparative analysis demonstrates higher values of adhesion characteristics in the case of gradient coatings of the Ti- Al- Si- Cu- N system than in the case of single-layer (with constant element concentration) analogues.

Shear-Coupled Grain Growth and Texture Development in a Nanocrystalline Ni-Fe Alloy during Cold Rolling

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

Li, Li; Ungár, Tamás; Toth, Laszlo S.

The evolution of texture, grain size, grain shape, dislocation and twin density has been determined by synchrotron X-ray diffraction and line profile analysis in a nanocrystalline Ni- Fe alloy after cold rolling along different directions related to the initial fiber and the long axis of grains. The texture evolution has been simulated by the Taylor-type relaxed constraints viscoplastic polycrystal model. The simulations were based on the activity of partial dislocations in correlation with the experimental results of dislocation density determination. The concept of stress-induced shear-coupling is supported and strengthened by both the texture simulations and the experimentally determined evolution ofmore » the microstructure parameters. Grain-growth and texture evolution are shown to proceed by the shear-coupling mechanism supported by dislocation activity as long as the grain size is not smaller than about 20 nm.« less

Optical and electrical properties of mechanochemically synthesized nanocrystalline delafossite CuAlO2.

PubMed

Prakash, T; Prasad, K Padma; Ramasamy, S; Murty, B S

2008-08-01

Nanocrystalline p-type semiconductor copper aluminum oxide (CuAlO2) has been synthesized by mechanical alloying using freshly prepared Cu2O and alpha-AlO2O3 nanocrystals in toluene medium. A study on structural property performed with different alloying and post annealing durations, by X-ray diffraction (XRD) reveals the formation of single phase with average crystallite size approximately 45 nm. Optical absorbance onset at 364.5 nm confirms its wide band gap nature (E(g) = 3.4 eV) and the fluorescence emission behaviour (390 nm) confirms its direct band type transition. The activation energy for electrical conduction has been calculated by Arrhenius plots using impedance measurement. Both grain and grain boundary conductivity takes place with almost equal activation energies of approximately 0.45 eV. The paper discusses synthesis, structural, optical and electrical properties of delafossite CuAlO2 in detail.

Nanoscale phase transition behavior of shape memory alloys — closed form solution of 1D effective modelling

NASA Astrophysics Data System (ADS)

Li, M. P.; Sun, Q. P.

2018-01-01

We investigate the roles of grain size (lg) and grain boundary thickness (lb) on the stress-induced phase transition (PT) behaviors of nanocrystalline shape memory alloys (SMAs) by using a Core-shell type "crystallite-amorphous composite" model. A non-dimensionalized length scale lbarg(=lg /lb) is identified as the governing parameter which is indicative of the energy competition between the crystallite and the grain boundary. Closed form analytical solutions of a reduced effective 1D model with embedded microstructure length scales of lg and lb are presented in this paper. It is shown that, with lbarg reduction, the energy of the elastic non-transformable grain boundary will gradually become dominant in the phase transition process, and eventually bring fundamental changes of the deformation behaviors: breakdown of two-phase coexistence and vanishing of superelastic hysteresis. The predictions are supported by experimental data of nanocrystalline NiTi SMAs.

Semisolid Microstructural Evolution during Partial Remelting of a Bulk Alloy Prepared by Cold Pressing of the Ti-Al-2024Al Powder Mixture

PubMed Central

Qin, Yahong; Chen, Tijun; Wang, Yingjun; Zhang, Xuezheng; Li, Pubo

2016-01-01

A new method, powder thixoforming, has been proposed to fabricate an in situ Al3Tip/2024Al composite. During partial remelting, the microstructural evolution of the bulk alloy prepared by cold pressing of the Ti, Al, 2024Al powder mixture was investigated, and the formation mechanism of the Al3Ti particles produced by the reaction between the Ti powder and the Al alloy melt is also discussed in detail. The results indicate that the microstructural evolution of the 2024 alloy matrix can be divided into three stages: a rapid coarsening of the powder grains; a formation of primary α-Al particles surrounded with a continuous liquid film; and a slight coarsening of the primary α-Al particles. Simultaneously, a reaction layer of Al3Ti can be formed on the Ti powder surface when the bulk is heated for 10 min at 640 °C The thickness (X) of the reaction layer increases with the time according to the parabolic law of X=−0.43t2+4.21t+0.17. The stress generated in the reaction layer due to the volume dilatation can be calculated by using the equation σAl3Ti=−EAl3Ti6(1−υAl3Ti)t2Al3TitTi(1R−1R0). Comparing the obtained data with the results of the drip experiment, the reaction rate for the Ti powder and Al powder mixture is greater than that for the Ti plate and Al alloy mixture, respectively.

Powder Metallurgy Processing of a WxTaTiVCr High-Entropy Alloy and Its Derivative Alloys for Fusion Material Applications.

PubMed

Waseem, Owais Ahmed; Ryu, Ho Jin

2017-05-16

The W x TaTiVCr high-entropy alloy with 32at.% of tungsten (W) and its derivative alloys with 42 to 90at.% of W with in-situ TiC were prepared via the mixing of elemental W, Ta, Ti, V and Cr powders followed by spark plasma sintering for the development of reduced-activation alloys for fusion plasma-facing materials. Characterization of the sintered samples revealed a BCC lattice and a multi-phase structure. The selected-area diffraction patterns confirmed the formation of TiC in the high-entropy alloy and its derivative alloys. It revealed the development of C15 (cubic) Laves phases as well in alloys with 71 to 90at.% W. A mechanical examination of the samples revealed a more than twofold improvement in the hardness and strength due to solid-solution strengthening and dispersion strengthening. This study explored the potential of powder metallurgy processing for the fabrication of a high-entropy alloy and other derived compositions with enhanced hardness and strength.

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.

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.

Synthesis and in vitro bioactivity of bredigite powders.

PubMed

Wu, Chengtie; Chang, Jiang

2007-01-01

Pure bredigite (Ca7MgSi4O16) powders are synthesized by the sol-gel method. The bredigite powders are composed of polycrystalline particles with dimensions of 1-10 micro m. The in vitro bioactivity of the bredigite powders are examined by evaluation of hydroxyapatite (HAp) formation ability in simulated body fluid (SBF) and the effect of ionic products from bredigite dissolution on osteoblast proliferation. The results showed that bredigite induced the formation of nanocrystalline HAp after soaking in SBF for 10 days. The Ca, Si, and Mg ions from bredigite dissolution at a certain concentration range stimulates osteoblast proliferation. Our study indicates that bredigite is bioactive and might be used for preparation of new biomaterials.

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.

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).

Quality by Design approach to spray drying processing of crystalline nanosuspensions.

PubMed

Kumar, Sumit; Gokhale, Rajeev; Burgess, Diane J

2014-04-10

Quality by Design (QbD) principles were explored to understand spray drying process for the conversion of liquid nanosuspensions into solid nano-crystalline dry powders using indomethacin as a model drug. The effects of critical process variables: inlet temperature, flow and aspiration rates on critical quality attributes (CQAs): particle size, moisture content, percent yield and crystallinity were investigated employing a full factorial design. A central cubic design was employed to generate the response surface for particle size and percent yield. Multiple linear regression analysis and ANOVA were employed to identify and estimate the effect of critical parameters, establish their relationship with CQAs, create design space and model the spray drying process. Inlet temperature was identified as the only significant factor (p value <0.05) to affect dry powder particle size. Higher inlet temperatures caused drug surface melting and hence aggregation of the dried nano-crystalline powders. Aspiration and flow rates were identified as significant factors affecting yield (p value <0.05). Higher yields were obtained at higher aspiration and lower flow rates. All formulations had less than 3% (w/w) moisture content. Formulations dried at higher inlet temperatures had lower moisture compared to those dried at lower inlet temperatures. Published by Elsevier B.V.

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.

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

PubMed

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

2012-01-01

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

Deformation-induced localized solid-state amorphization in nanocrystalline nickel

PubMed Central

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

2012-01-01

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

Strength-Ductility Property Maps of Powder Metallurgy (PM) Ti-6Al-4V Alloy: A Critical Review of Processing-Structure-Property Relationships

NASA Astrophysics Data System (ADS)

Kumar, P.; Chandran, K. S. Ravi

2017-05-01

A comprehensive assessment of tensile properties of powder metallurgical (PM) processed Ti-6Al-4V alloy, through the mapping of strength-ductility property domains, is performed in this review. Tensile property data of PM Ti-6Al-4V alloys made from blended element (BE) and pre-alloyed powders including that additive manufactured (AM) from powders, as well as that made using titanium hydride powders, have been mapped in the form of strength-ductility domains. Based on this, porosity and microstructure have been identified as the dominant variables controlling both the strength and the tensile ductility of the final consolidated materials. The major finding is that tensile ductility of the PM titanium is most sensitive to the presence of pores. The significance of extreme-sized pores or defects in inducing large variations in ductility is emphasized. The tensile strength, however, has been found to depend only weakly on the porosity. The effect of microstructure on properties is masked by the variations in porosity and to some extent by the oxygen level. It is shown that any meaningful comparison of the microstructure can only be made under a constant porosity or density level. The beneficial effect of a refined microstructure is also brought out by logically organizing the data in terms of microstructure groups. The advantages of new processes, using titanium hydride powder to produce PM titanium alloys, in simultaneously increasing strength and ductility, are also highlighted. The tensile properties of AM Ti-6Al-4V alloys are also brought to light, in comparison with the other PM and wrought alloys, through the strength-ductility maps.

Application of powder metallurgy to an advanced-temperature nickel-base alloy, NASA-TRW 6-A

NASA Technical Reports Server (NTRS)

Freche, J. C.; Ashbrook, R. L.; Waters, W. J.

1971-01-01

Bar stock of the NASA-TRW 6-A alloy was made by prealloyed powder techniques and its properties evaluated over a range of temperatures. Room temperature ultimate tensile strength was 1894 MN/sq m (274 500 psi). The as-extruded powder product showed substantial improvements in strength over the cast alloy up to 649 C (1200 F) and superplasticity at 1093 C (2000 F). Both conventional and autoclave heat treatments were applied to the extruded powder product. The conventional heat treatment was effective in increasing rupture life at 649 and 704 C (1200 and 1300 F); the autoclave heat treatment, at 760 and 816 C (1400 and 1500 F).

Stability of gas atomized reactive powders through multiple step in-situ passivation

DOEpatents

Anderson, Iver E.; Steinmetz, Andrew D.; Byrd, David J.

2017-05-16

A method for gas atomization of oxygen-reactive reactive metals and alloys wherein the atomized particles are exposed as they solidify and cool in a very short time to multiple gaseous reactive agents for the in-situ formation of a protective reaction film on the atomized particles. The present invention is especially useful for making highly pyrophoric reactive metal or alloy atomized powders, such as atomized magnesium and magnesium alloy powders. The gaseous reactive species (agents) are introduced into the atomization spray chamber at locations downstream of a gas atomizing nozzle as determined by the desired powder or particle temperature for the reactions and the desired thickness of the reaction film.

Improve oxidation resistance at high temperature by nanocrystalline surface layer

NASA Astrophysics Data System (ADS)

Xia, Z. X.; Zhang, C.; Huang, X. F.; Liu, W. B.; Yang, Z. G.

2015-08-01

An interesting change of scale sequence occurred during oxidation of nanocrystalline surface layer by means of a surface mechanical attrition treatment. The three-layer oxide structure from the surface towards the matrix is Fe3O4, spinel FeCr2O4 and corundum (Fe,Cr)2O3, which is different from the typical two-layer scale consisted of an Fe3O4 outer layer and an FeCr2O4 inner layer in conventional P91 steel. The diffusivity of Cr, Fe and O is enhanced concurrently in the nanocrystalline surface layer, which causes the fast oxidation in the initial oxidation stage. The formation of (Fe,Cr)2O3 inner layer would inhabit fast diffusion of alloy elements in the nanocrystalline surface layer of P91 steel in the later oxidation stage, and it causes a decrease in the parabolic oxidation rate compared with conventional specimens. This study provides a novel approach to improve the oxidation resistance of heat resistant steel without changing its Cr content.

Preparation and characterization of Fe50Co50 nanostructured alloy

NASA Astrophysics Data System (ADS)

Yepes, N.; Orozco, J.; Caamaño, Z.; Mass, J.; Pérez, G.

2014-04-01

Nanostructured Fe50Co50 alloy was prepared by mechanical alloying of Fe and Co powders in a planetary high energy ball milling. The microstructure and structural evolution of the alloy have been investigated as a function of milling time (0 h, 8 h, 20 h and 35 h) by scanning electron microscopy (SEM) and X-Ray diffraction (XRD) characterization techniques. SEM micrographs showed different powder particles morphologies during the mechanical alloying stages. By XRD analysis it could be identified the structural phases of the alloy and the crystallite size was calculated as a function of the milling time.

Dispersion strengthening of precipitation hardened Al-Cu-Mg alloys prepared by rapid solidification and mechanical alloying

NASA Technical Reports Server (NTRS)

Gilman, P. S.; Sankaran, K. K.

1988-01-01

Several Al-4Cu-1Mg-1.5Fe-0.75Ce alloys have been processed from either rapidly solidified or mechanically alloyed powder using various vacuum degassing parameters and consolidation techniques. Strengthening by the fine subgrains, grains, and the dispersoids individually or in combination is more effective when the alloys contain shearable precipitates; consequently, the strength of the alloys is higher in the naturally aged rather than the artificially aged condition. The strengths of the mechanically alloyed variants are greater than those produced from prealloyed powder. Properties and microstructural features of these dispersion strengthened alloys are discussed in regards to their processing histories.

High pressure FAST of nanocrystalline barium titanate

DOE PAGES

Fraga, Martin B.; Delplanque, Jean -Pierre; Yang, Nancy; ...

2016-06-01

Here, this work studies the microstructural evolution of nanocrystalline (<1 µm) barium titanate (BaTiO 3), and presents high pressure in field-assisted sintering (FAST) as a robust methodology to obtain >100 nm BaTiO 3 compacts. Using FAST, two commercial ~50 nm powders were consolidated into compacts of varying densities and grain sizes. Microstructural inhomogeneities were investigated for each case, and an interpretation is developed using a modified Monte Carlo Potts (MCP) simulation. Two recurrent microstructural inhomogeneities are highlighted, heterogeneous grain growth and low-density regions, both ubiqutously present in all samples to varying degrees. In the worst cases, HGG presents an areamore » coverage of 52%. Because HGG is sporadic but homogenous throughout a sample, the catalyst (e.g., the local segregation of species) must be, correspondingly, distributed in a homogenous manner. MCP demonstrates that in such a case, a large distance between nucleating abnormal grains is required—otherwise abnormal grains prematurely impinge on each other, and their size is not distinguishable from that of normal grains. Compacts sintered with a pressure of 300 MPa and temperatures of 900 °C, were 99.5% dense and had a grain size of 90±24 nm. These are unprecedented results for commercial BaTiO 3 powders or any starting powder of 50 nm particle size—other authors have used 16 nm lab-produced powder to obtain similar results.« less

The gas-sensing potential of nanocrystalline SnO2 produced by a mechanochemical milling via centrifugal action

NASA Astrophysics Data System (ADS)

Kersen, Ü.

In this work, the synthesis of undoped nanocrystalline tin dioxide powders and the subsequent preparation of SnO2 thick-films were studied. An initial mixture of SnCl2 and Ca(OH)2 was sealed in a vial for milling in an air atmosphere. Heat treatment of the milled powder resulted in the formation of tetragonal and orthorhombic SnO2 phases, which was confirmed by X-ray diffraction (XRD) analysis. It was found that crystallite size could be controlled by varying the milling time, the rotation speed and the temperature used for the heat treatment. Crystallite sizes in the range 20 to 30 nm (determined by XRD measurements) were obtained. The total pore volume was 0.22 ml/g for a measured particle size of 37 m2/g. No contamination of the powder during milling was found. The response of the prepared thick-films to H2S gas in the concentration range 0.5 to 10 ppm in air was investigated as a function of the preparation conditions. The advantage of mechanochemical synthesis of powder is its relative simplicity, low cost and possibility of obtaining isolated, unagglomerated nanosized grains. It is shown that chemical reactions, which usually occur in the vibratory mill to produce the SnO phase, can also be initiated during a short processing time in the centrifugal mill.

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.

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.

Magnetic properties of mechanically alloyed Mn-Al-C powders

NASA Astrophysics Data System (ADS)

Kohmoto, O.; Kageyama, N.; Kageyama, Y.; Haji, H.; Uchida, M.; Matsushima, Y.

2011-01-01

We have prepared supersaturated-solution Mn-Al-C alloy powders by mechanical alloying using a planetary high-energy mill. The starting materials were pure Mn, Al and C powers. The mechanically-alloyed powders were subjected to a two-step heating. Although starting particles are Al and Mn with additive C, the Al peak disappears with MA time. With increasing MA time, transition from α-Mn to β-Mn does not occur; the α-Mn structure maintains. At 100 h, a single phase of supersaturated-solution α-Mn is obtained. The lattice constant of α-Mn decreases with increasing MA time. From the Scherrer formula, the crystallite size at 500 h is obtained as 200Å, which does not mean amorphous state. By two-step heating, high magnetization (66 emu/g) was obtained from short-time-milled powders (t=10 h). The precursor of the as-milled powder is not a single phase α-Mn but contains small amount of fcc Al. After two-step heating, the powder changes to τ-phase. Although the saturation magnetization increases, the value is less than that by conventional bulk MnAl (88 emu/g). Meanwhile, long-time-milled powder of single α-Mn phase results in low magnetization (5.2 emu/g) after two-step heating.

Method for low temperature preparation of a noble metal alloy

DOEpatents

Even, Jr., William R.

2002-01-01

A method for producing fine, essentially contamination free, noble metal alloys is disclosed. The alloys comprise particles in a size range of 5 to 500 nm. The method comprises 1. A method for preparing a noble metal alloy at low temperature, the method comprising the steps of forming solution of organometallic compounds by dissolving the compounds into a quantity of a compatible solvent medium capable of solvating the organometallic, mixing a portion of each solution to provide a desired molarity ratio of ions in the mixed solution, adding a support material, rapidly quenching droplets of the mixed solution to initiate a solute-solvent phase separation as the solvent freezes, removing said liquid cryogen, collecting and freezing drying the frozen droplets to produce a dry powder, and finally reducing the powder to a metal by flowing dry hydrogen over the powder while warming the powder to a temperature of about 150.degree. C.

Synthesis of porous nanocrystalline NiO with hexagonal sheet-like morphology by homogeneous precipitation method

NASA Astrophysics Data System (ADS)

Sharma, Ravi Kant; Ghose, Ranjana

2015-04-01

Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.

Nanocrystalline CuInS2 And CuInSe2 via Low-Temperature Pyrolysis Of Single-Source Molecular Precursors

NASA Technical Reports Server (NTRS)

Castro, Stephanie L.; Bailey, Sheila G.; Raffaelle, Ryne P.; Banger, Kulbinder K.; Hepp, Aloysius F.

2002-01-01

Single-source precursors are molecules which contain all the necessary elements for synthesis of a desired material. Thermal decomposition of the precursor results in the formation of the material with the correct stoichiometry, as a nanocrystalline powder or a thin film. Nanocrystalline materials hold potential as components of next-generation Photovoltaic (PV) devices. Presented here are the syntheses of CuInS2 and CuInSe2 nanocrystals from the precursors (PPh3)2CuIn(SEt)4 and (PPh3)2CuIn(SePh)4, respectively. The size of the nanocrystals varies with the reaction temperature; a minimum of 200 C is required for the formation of the smallest CuInS2 crystals (approximately 1.6 nm diameter); at 300 C, crystals are approximately 7 nm.

Evaluation of powder metallurgy superalloy disk materials

NASA Technical Reports Server (NTRS)

Evans, D. J.

1975-01-01

A program was conducted to develop nickel-base superalloy disk material using prealloyed powder metallurgy techniques. The program included fabrication of test specimens and subscale turbine disks from four different prealloyed powders (NASA-TRW-VIA, AF2-1DA, Mar-M-432 and MERL 80). Based on evaluation of these specimens and disks, two alloys (AF2-1DA and Mar-M-432) were selected for scale-up evaluation. Using fabricating experience gained in the subscale turbine disk effort, test specimens and full scale turbine disks were formed from the selected alloys. These specimens and disks were then subjected to a rigorous test program to evaluate their physical properties and determine their suitability for use in advanced performance turbine engines. A major objective of the program was to develop processes which would yield alloy properties that would be repeatable in producing jet engine disks from the same powder metallurgy alloys. The feasibility of manufacturing full scale gas turbine engine disks by thermomechanical processing of pre-alloyed metal powders was demonstrated. AF2-1DA was shown to possess tensile and creep-rupture properties in excess of those of Astroloy, one of the highest temperature capability disk alloys now in production. It was determined that metallographic evaluation after post-HIP elevated temperature exposure should be used to verify the effectiveness of consolidation of hot isostatically pressed billets.

Mechanical alloying, characterization and consolidation of Ti-Al-Ni alloys

NASA Technical Reports Server (NTRS)

Nash, P.; Higgins, G. T.; Dillinger, N.; Hwang, S. J.; Kim, H.

1989-01-01

Mechanical alloying is being investigated as a processing route for the production of aluminide intermetallics. This program involves powder production and characterization, consolidation and thermal treatments and determination of microstructure-property relationships. An attritor mill is being used to produce powder in lots up to 1000 grams and the processing parameters are being systematically varied to establish the optimum milling conditions. The mill is being instrumented to generate data related to the processing to provide a basis for theoretical modeling. Powder is being characterized using thermal analysis, optical and electron microscopy and X-ray diffraction. Particle size distributions and powder density are being determined. Consolidation of the powder is being approached in several different ways including, cold isostatic pressing, sintering, extrusion and hot pressing. The results of the program so far will be presented and future directions discussed.

Effect of Electropulsing-Assisted Ultrasonic Nanocrystalline Surface Modification on the Surface Mechanical Properties and Microstructure of Ti-6Al-4V Alloy

NASA Astrophysics Data System (ADS)

Ye, Yongda; Wang, Haibo; Tang, Guoyi; Song, Guolin

2018-05-01

The effect of electropulsing-assisted ultrasonic nanocrystalline surface modification (EP-UNSM) on surface mechanical properties and microstructure of Ti-6Al-4V alloy is investigated. Compared to conventional ultrasonic nanocrystalline surface modification (UNSM), EP-UNSM can effectively facilitate surface roughness and morphology, leading to excellent surface roughness (reduced from Ra 0.918 to Ra 0.028 μm by UNSM and Ra 0.019 μm by EP-UNSM) and smoother morphology with less cracks and defects. Surface friction coefficients are enhanced, resulting in lower and smoother friction coefficients. In addition, the surface-strengthened layer and ultra-refined grains are significantly enhanced with more severe plastic deformation and a greater surface hardness (a maximum hardness value of 407 HV and an effective depth of 550 μm, in comparison with the maximum hardness value of 364 HV and effective depth of 300 μm obtained by conventional UNSM). Remarkable enhancement of surface mechanical properties can be attributed to the refined gradient microstructure and the enhanced severe plastic deformation layer induced by coupling the effects of UNSM and electropulsing. The accelerated dislocation mobility and atom diffusion caused by the thermal and athermal effects of electropulsing treatment may be the primary intrinsic reasons for these improvements.

Powder metallurgy preparation of Mg-Ca alloy for biodegradable implant application

NASA Astrophysics Data System (ADS)

Annur, D.; Suhardi, A.; Amal, M. I.; Anwar, M. S.; Kartika, I.

2017-04-01

Magnesium and its alloys is a promising candidate for implant application especially due to its biodegradability. In this study, Mg-7Ca alloys (in weight %) were processed by powder metallurgy from pure magnesium powder and calcium granule. Milling process was done in a shaker mill using stainless steel balls in various milling time (3, 5, and 8 hours) followed by compaction and sintering process. Different sintering temperatures were used (450°C and 550°C) to examine the effect of sintering temperature on mechanical properties and corrosion resistance. Microstructure evaluation was characterized by X-ray diffraction, scanning electron microscope and energy dispersive X-ray spectroscopy. Mechanical properties and corrosion behavior were examined through hardness testing and electrochemical testing in Hank’s solution (simulation body fluid). In this report, a prolonged milling time reduced particle size and later affected mechanical properties of Mg alloy. Meanwhile, the phase analysis showed that α Mg, Mg2Ca, MgO phases were formed after the sintering process. Further, this study showed that Mg-Ca alloy with different powder metallurgy process would have different corrosion rate although there were no difference of Ca content in the alloy.

Microstructure and magnetic behavior of Cu-Co-Si ternary alloy synthesized by mechanical alloying and isothermal annealing

NASA Astrophysics Data System (ADS)

Chabri, Sumit; Bera, S.; Mondal, B. N.; Basumallick, A.; Chattopadhyay, P. P.

2017-03-01

Microstructure and magnetic behavior of nanocrystalline 50Cu-40Co-10Si (at%) alloy prepared by mechanical alloying and subsequent isothermal annealing in the temperature range of 450-650 °C have been studied. Phase evolution during mechanical alloying and isothermal annealing is characterized by X-ray diffraction (XRD), differential thermal analyzer (DTA), high resolution transmission electron microscopy (HRTEM) and magnetic measurement. Addition of Si has been found to facilitate the metastable alloying of Co in Cu resulting into the formation of single phase solid solution having average grain size of 9 nm after ball milling for 50 h duration. Annealing of the ball milled alloy improves the magnetic properties significantly and best combination of magnetic properties has been obtained after annealing at 550 °C for 1 h duration.

Laminated composite of magnetic alloy powder and ceramic powder and process for making same

DOEpatents

Moorhead, Arthur J.; Kim, Hyoun-Ee

1999-01-01

A laminated composite structure of alternating metal powder layers, and layers formed of an inorganic bonding media powder, and a method for manufacturing same are discosed. The method includes the steps of assembling in a cavity alternating layers of a metal powder and an inorganic bonding media of a ceramic, glass, and glass-ceramic. Heat, with or without pressure, is applied to the alternating layers until the particles of the metal powder are sintered together and bonded into the laminated composite structure by the layers of sintered inorganic bonding media to form a strong composite structure. The method finds particular application in the manufacture of high performance magnets wherein the metal powder is a magnetic alloy powder.

Laminated composite of magnetic alloy powder and ceramic powder and process for making same

DOEpatents

Moorhead, A.J.; Kim, H.

1999-08-10

A laminated composite structure of alternating metal powder layers, and layers formed of an inorganic bonding media powder, and a method for manufacturing same are disclosed. The method includes the steps of assembling in a cavity alternating layers of a metal powder and an inorganic bonding media of a ceramic, glass, and glass-ceramic. Heat, with or without pressure, is applied to the alternating layers until the particles of the metal powder are sintered together and bonded into the laminated composite structure by the layers of sintered inorganic bonding media to form a strong composite structure. The method finds particular application in the manufacture of high performance magnets wherein the metal powder is a magnetic alloy powder. 9 figs.

The Back Scattering Micro-Raman Spectroscopy of Different Crystalline Phases of TiO2 Nanoparticles Produced by Sol-Gel Technique

NASA Astrophysics Data System (ADS)

Malekfar, R.; Mihanyar, S.; Mozaffari, M.

2007-09-01

TiO2 is known to be one of the best photocatalysts among the semiconductors. In order to improve its photocatalytic features, it is necessary to be able to control factors such as the mean particle size, nanocrystalline system, grain shapes and diffraction. Nanocrystalline TiO2 sample powders were produced using H2O2 and Ti(OBu)4 as precursor materials and their above features were then characterized by using XRD, Raman spectroscopy and SEM. The grain size was calculated using the Debye Scherrer formula for anatase phase, 15 nm, which is in agreement with the value obtained by SEM imaging. Ti(OBu)4 was added dropwise to a very ice-cold solution of H2O2 under intensive stirring. This immediately yielded a red solution which was shortly followed by a strong exothermic reaction due to the unstable nature of the reaction at this stage. This process also involved rigorous giving off of H2O2, O2, and butyl alcohol. A yellow transparent peroxo-polytitanic (PPT) acid gel was thus prepared. This gel was then heated at 150 °C for 5 hours and was transformed into amorphous TiO2. The produced yellow powder was heated at 250 °C, 350 °C and 450 °C for one hour with a ramping up speed of 5 °C/min heating rate. It was later calcined at 550 °C, 750 °C and 950 °C for 30 minutes. By investigating the Raman spectra typically shown in figure 1 and also XRD patterns, it was confirmed that the anatase phase nanocrystalline powder, which is well known for its application as photocatalysts, was produced at the first three lower treatment temperatures mentioned above.

Stability of an Electrodeposited Nanocrystalline Ni-Based Alloy Coating in Oil and Gas Wells with the Coexistence of H2S and CO2

PubMed Central

Sui, Yiyong; Sun, Chong; Sun, Jianbo; Pu, Baolin; Ren, Wei; Zhao, Weimin

2017-01-01

The stability of an electrodeposited nanocrystalline Ni-based alloy coating in a H2S/CO2 environment was investigated by electrochemical measurements, weight loss method, and surface characterization. The results showed that both the cathodic and anodic processes of the Ni-based alloy coating were simultaneously suppressed, displaying a dramatic decrease of the corrosion current density. The corrosion of the Ni-based alloy coating was controlled by H2S corrosion and showed general corrosion morphology under the test temperatures. The corrosion products, mainly consisting of Ni3S2, NiS, or Ni3S4, had excellent stability in acid solution. The corrosion rate decreased with the rise of temperature, while the adhesive force of the corrosion scale increased. With the rise of temperature, the deposited morphology and composition of corrosion products changed, the NiS content in the corrosion scale increased, and the stability and adhesive strength of the corrosion scale improved. The corrosion scale of the Ni-based alloy coating was stable, compact, had strong adhesion, and caused low weight loss, so the corrosion rates calculated by the weight loss method cannot reveal the actual oxidation rate of the coating. As the corrosion time was prolonged, the Ni-based coating was thinned while the corrosion scale thickened. The corrosion scale was closely combined with the coating, but cannot fully prevent the corrosive reactants from reaching the substrate. PMID:28772995

Data on processing of Ti-25Nb-25Zr β-titanium alloys via powder metallurgy route: Methodology, microstructure and mechanical properties.

PubMed

Ueda, D; Dirras, G; Hocini, A; Tingaud, D; Ameyama, K; Langlois, P; Vrel, D; Trzaska, Z

2018-04-01

The data presented in this article are related to the research article entitled "Cyclic Shear behavior of conventional and harmonic structure-designed Ti-25Nb-25Zr β-titanium alloy: Back-stress hardening and twinning inhibition" (Dirras et al., 2017) [1]. The datasheet describes the methods used to fabricate two β-titanium alloys having conventional microstructure and so-called harmonic structure (HS) design via a powder metallurgy route, namely the spark plasma sintering (SPS) route. The data show the as-processed unconsolidated powder microstructures as well as the post-SPS ones. The data illustrate the mechanical response under cyclic shear loading of consolidated alloy specimens. The data show how electron back scattering diffraction(EBSD) method is used to clearly identify induced deformation features in the case of the conventional alloy.

Thermal transport in nanocrystalline Si and SiGe by ab initio based Monte Carlo simulation.

PubMed

Yang, Lina; Minnich, Austin J

2017-03-14

Nanocrystalline thermoelectric materials based on Si have long been of interest because Si is earth-abundant, inexpensive, and non-toxic. However, a poor understanding of phonon grain boundary scattering and its effect on thermal conductivity has impeded efforts to improve the thermoelectric figure of merit. Here, we report an ab-initio based computational study of thermal transport in nanocrystalline Si-based materials using a variance-reduced Monte Carlo method with the full phonon dispersion and intrinsic lifetimes from first-principles as input. By fitting the transmission profile of grain boundaries, we obtain excellent agreement with experimental thermal conductivity of nanocrystalline Si [Wang et al. Nano Letters 11, 2206 (2011)]. Based on these calculations, we examine phonon transport in nanocrystalline SiGe alloys with ab-initio electron-phonon scattering rates. Our calculations show that low energy phonons still transport substantial amounts of heat in these materials, despite scattering by electron-phonon interactions, due to the high transmission of phonons at grain boundaries, and thus improvements in ZT are still possible by disrupting these modes. This work demonstrates the important insights into phonon transport that can be obtained using ab-initio based Monte Carlo simulations in complex nanostructured materials.

Thermal transport in nanocrystalline Si and SiGe by ab initio based Monte Carlo simulation

PubMed Central

Yang, Lina; Minnich, Austin J.

2017-01-01

Nanocrystalline thermoelectric materials based on Si have long been of interest because Si is earth-abundant, inexpensive, and non-toxic. However, a poor understanding of phonon grain boundary scattering and its effect on thermal conductivity has impeded efforts to improve the thermoelectric figure of merit. Here, we report an ab-initio based computational study of thermal transport in nanocrystalline Si-based materials using a variance-reduced Monte Carlo method with the full phonon dispersion and intrinsic lifetimes from first-principles as input. By fitting the transmission profile of grain boundaries, we obtain excellent agreement with experimental thermal conductivity of nanocrystalline Si [Wang et al. Nano Letters 11, 2206 (2011)]. Based on these calculations, we examine phonon transport in nanocrystalline SiGe alloys with ab-initio electron-phonon scattering rates. Our calculations show that low energy phonons still transport substantial amounts of heat in these materials, despite scattering by electron-phonon interactions, due to the high transmission of phonons at grain boundaries, and thus improvements in ZT are still possible by disrupting these modes. This work demonstrates the important insights into phonon transport that can be obtained using ab-initio based Monte Carlo simulations in complex nanostructured materials. PMID:28290484

Microstructure, mechanical properties, bio-corrosion properties and antibacterial properties of Ti-Ag sintered alloys.

PubMed

Chen, Mian; Zhang, Erlin; Zhang, Lan

2016-05-01

In this research, Ag element was selected as an antibacterial agent to develop an antibacterial Ti-Ag alloy by a powder metallurgy. The microstructure, phase constitution, mechanical properties, corrosion resistance and antibacterial properties of the Ti-Ag sintered alloys have been systematically studied by X-ray diffraction (XRD), scanning electron microscope (SEM), compressive test, electrochemical measurements and antibacterial test. The effects of the Ag powder size and the Ag content on the antibacterial property and mechanical property as well as the anticorrosion property have been investigated. The microstructure results have shown that Ti-Ag phase, residual pure Ag and Ti were the mainly phases in Ti-Ag(S75) sintered alloy while Ti2Ag was synthesized in Ti-Ag(S10) sintered alloy. The mechanical test indicated that Ti-Ag sintered alloy showed a much higher hardness and the compressive yield strength than cp-Ti but the mechanical properties were slightly reduced with the increase of Ag content. Electrochemical results showed that Ag powder size had a significant effect on the corrosion resistance of Ti-Ag sintered alloy. Ag content increased the corrosion resistance in a dose dependent way under a homogeneous microstructure. Antibacterial tests have demonstrated that antibacterial Ti-Ag alloy was successfully prepared. It was also shown that the Ag powder particle size and the Ag content influenced the antibacterial activity seriously. The reduction in the Ag powder size was benefit to the improvement in the antibacterial property and the Ag content has to be at least 3wt.% in order to obtain a strong and stable antibacterial activity against Staphylococcus aureus bacteria. The bacterial mechanism was thought to be related to the Ti2Ag and its distribution. Copyright © 2016 Elsevier B.V. All rights reserved.

Temperature dependence of the radiation tolerance of nanocrystalline pyrochlores A 2Ti 2O 7 (A = Gd, Ho and Lu)

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

Wen, J.; Sun, C.; Dholabhai, P. P.

A potentially enhanced radiation resistance of nanocrystalline materials, as a consequence of the high density of interfaces and surfaces, has attracted much attention both to understand the fundamental role of these defect sinks and to develop them for high-radiation environments. Here, irradiation response of nanocrystalline A 2Ti 2O 7 (A = Gd, Ho and Lu) pyrochlore powders with grain sizes of 20–30 nm was investigated by 1-MeV Kr 2+ ion bombardment. In situ transmission electron microscopy (TEM) revealed that the critical amorphization fluence for each nanocrystalline compound at room temperature was greater than that for their coarse-grained counterparts, indicating anmore » enhanced amorphization resistance. The effect of temperature on the irradiation response of one of these compounds, nanocrystalline Lu 2Ti 2O 7, was further examined by performing ion irradiation at an elevated temperature range of 480–600 K. The critical amorphization temperature (T c) was found to be noticeably higher in nanocrystalline Lu 2Ti 2O 7 (610 K) than its coarse-grained counterpart (480 K), revealing that nanocrystalline Lu 2Ti 2O 7 is less resistant to amorphization compared to its coarse-grained phase under high temperatures. We interpret these results with the aid of atomistic simulations. Molecular statics calculations find that cation antisite defects are less energetically costly to form near surfaces than in the bulk, suggesting that the nanocrystalline form of these materials is generally less susceptible to amorphization than coarse-grained counterparts at low temperatures where defect kinetics are negligible. In contrast, at high temperatures, the annealing efficiency of antisite defects by cation interstitials is significantly reduced due to the sink properties of the surfaces in the nanocrystalline pyrochlore, which contributes to the observed higher amorphization temperature in the nano-grained phase than in coarse-grained counterpart. Altogether, these results provide new insight into the behavior of nanocrystalline materials under irradiation.« less

Temperature dependence of the radiation tolerance of nanocrystalline pyrochlores A 2Ti 2O 7 (A = Gd, Ho and Lu)

DOE PAGES

Wen, J.; Sun, C.; Dholabhai, P. P.; ...

2016-03-21

A potentially enhanced radiation resistance of nanocrystalline materials, as a consequence of the high density of interfaces and surfaces, has attracted much attention both to understand the fundamental role of these defect sinks and to develop them for high-radiation environments. Here, irradiation response of nanocrystalline A 2Ti 2O 7 (A = Gd, Ho and Lu) pyrochlore powders with grain sizes of 20–30 nm was investigated by 1-MeV Kr 2+ ion bombardment. In situ transmission electron microscopy (TEM) revealed that the critical amorphization fluence for each nanocrystalline compound at room temperature was greater than that for their coarse-grained counterparts, indicating anmore » enhanced amorphization resistance. The effect of temperature on the irradiation response of one of these compounds, nanocrystalline Lu 2Ti 2O 7, was further examined by performing ion irradiation at an elevated temperature range of 480–600 K. The critical amorphization temperature (T c) was found to be noticeably higher in nanocrystalline Lu 2Ti 2O 7 (610 K) than its coarse-grained counterpart (480 K), revealing that nanocrystalline Lu 2Ti 2O 7 is less resistant to amorphization compared to its coarse-grained phase under high temperatures. We interpret these results with the aid of atomistic simulations. Molecular statics calculations find that cation antisite defects are less energetically costly to form near surfaces than in the bulk, suggesting that the nanocrystalline form of these materials is generally less susceptible to amorphization than coarse-grained counterparts at low temperatures where defect kinetics are negligible. In contrast, at high temperatures, the annealing efficiency of antisite defects by cation interstitials is significantly reduced due to the sink properties of the surfaces in the nanocrystalline pyrochlore, which contributes to the observed higher amorphization temperature in the nano-grained phase than in coarse-grained counterpart. Altogether, these results provide new insight into the behavior of nanocrystalline materials under irradiation.« less

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.

Al xGa 1-xN (0⩽ x⩽1) nanocrystalline powder by pyrolysis route

NASA Astrophysics Data System (ADS)

Garcia, R.; Srinivasan, S.; Contreras, O. E.; Thomas, A. C.; Ponce, F. A.

2007-10-01

A novel method to synthesize nanocrystalline Al xGa 1-xN (0⩽ x⩽1) powders is presented in this work. AlGaN nanocrystallites with the wurtzite structure were produced by thermal decomposition of a gallium-aluminum complex compound at 1000 °C in a three-zone horizontal quartz tube reactor under high-purity ammonia atmosphere. The crystallites showed a hexagonal structure, high homogeneity, and a narrow particle-size distribution at around 50 nm. A continuous composition range from 0 to 1 mol fraction can be reached by this method, allowing high control on the gallium and aluminum composition by monitoring the stoichiometry of the reaction between the metal nitrates and carbohydrazide. Low-temperature photoluminescence and cathodoluminescence studies showed that some impurities, such as carbon and oxygen, are unintentionally present in the final product and affect the optical properties. Subsequent thermal treatments between 900 and 1100 °C under an ammonia atmosphere significantly improved the quality of these materials.

Research to Conduct an Exploratory Experimental and Analytical Investigation of Alloys

DTIC Science & Technology

1978-03-01

d« (f n«r««a«rv on« 149*111* hv *l«c* f*u0«««> Titanium Aluminides , Alloy Development, Mechemical Properties, Powder Metallurgy, Forging, Joining...Ccmpcsition of Titanium 79 Aluminida Alloy 9 Nuclear Metals Reported REP Titanium 80 Aluminide Powder Size Distribution 10 Phase I, Task I...137 141 24 Chemical Composition of Titanium Aluminide Alloy TMCA Heat 75301 Ti-13.5Al-21.4Nb 25 Isothermal Forging Results 26 Tensile Results

Plasma Spray for Difficult-To-Braze Alloys

NASA Technical Reports Server (NTRS)

Brennan, A.

1982-01-01

Nickel plating on surfaces makes brazing easier for some alloys. Sometimes nickel plating may not be feasible because of manufacturing sequence, size of hardware, or lack of suitable source for nickel plating. Alternative surface preparation in such cases is to grit-blast surface lightly and then plasma-spray 1 1/2 to 2 mils of fine nickel powder or braze-alloy material directly on surface. Powder is sprayed from plasma gun, using argon as carrier gas to prevent oxidation of nickel or braze alloy.

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

Holesinger, T. G.; Carpenter, J. S.; Lienert, T. J.

The ability of additive manufacturing to directly fabricate complex shapes provides characterization challenges for part qualification. The orientation of the microstructures produced by these processes will change relative to the surface normal of a complex part. In this work, the microscopy and x-ray tomography of an AlSi10Mg alloy hemispherical shell fabricated using powder bed metal additive manufacturing are used to illustrate some of these challenges. The shell was manufactured using an EOS M280 system in combination with EOS-specified powder and process parameters. The layer-by-layer process of building the shell with the powder bed additive manufacturing approach results in a position-dependentmore » microstructure that continuously changes its orientation relative to the shell surface normal. X-ray tomography was utilized to examine the position-dependent size and distribution of porosity and surface roughness in the 98.6% dense part. Optical and electron microscopy were used to identify global and local position-dependent structures, grain morphologies, chemistry, and precipitate sizes and distributions. The rapid solidification processes within the fusion zone (FZ) after the laser transit results in a small dendrite size. Cell spacings taken from the structure in the middle of the FZ were used with published relationships to estimate a cooling rate of ~9 × 10 5 K/s. Uniformly-distributed, nanoscale Si precipitates were found within the primary α-Al grains. A thin, distinct boundary layer containing larger α-Al grains and extended regions of the nanocrystalline divorced eutectic material surrounds the FZ. Moreover, subtle differences in the composition between the latter layer and the interior of the FZ were noted with scanning transmission electron microscopy (STEM) spectral imaging.« less

Chemical and Phase Composition of Powders Obtained by Electroerosion Dispersion from WC - Co Alloys

NASA Astrophysics Data System (ADS)

Putintseva, M. N.

2004-03-01

The dependence of the chemical and phase composition of dispersed powders on the mode and medium of electroerosion dispersion and the content of cobalt in the initial alloy is considered. It is shown that the dissociation of carbon from tungsten carbide occurs even in dispersion in liquid hydrocarbon-bearing media (kerosene and industrial oils). The phase composition is primarily determined by the dispersion medium and the content of cobalt in the initial alloy. Compound tungsten-cobalt carbides and even a Co7W6 intermetallic are determined in all the powders.

Rietveld analysis of the cubic crystal structure of Na-stabilized zirconia

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

Fagherazzi, G.; Canton, P.; Benedetti, A.

Using x-ray Rietveld analysis the fcc (fluorite-type) structure of a Na-containing nanocrystalline zirconia powder (9.5 nm estimated of crystallite size) obtained by precipitation and subsequent calcination has been confirmed. The result shows that using conventional x-ray diffraction techniques the cubic crystallographic form of ZrO{sub 2} from the tetragonal one in nanosized powders. These conclusions are supported by the findings of independent Raman scattering experiments. {copyright} {ital 1997 Materials Research Society.}

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.

Influence of preliminary deformation on the hardening effect upon aging of Al-Cu-Li alloys

NASA Astrophysics Data System (ADS)

Betsofen, S. Ya.; Ashmarin, A. A.; Knyazev, M. I.; Dolgova, M. I.

2016-09-01

The influence of preliminary deformation upon rolling of wedge specimens on the mechanical properties and the structural phase state of Al-Cu-Li alloys are studied by X-ray diffraction and hardness measurements. Strong dependence of the hardening effect upon aging on the reduction upon rolling has been revealed. Deformation weakly influences the hardness and significantly increases the hardening upon aging. Herewith, the hardening effect is nearly absent at the minimum deformation ratio of 1% and increases with its increase. It is demonstrated that the content of T1 phase increases from 2 to 4% in the range of a preliminary deformation ratio of 6-10% and the content of δ' phase is 17% at a deformation ratio in the range 1‒6% and increases to 18-19% at a deformation ratio of 6-10%. The δ' phase in an alloy contains <20% nanocrystalline particles with 6-20 nm in size, and the remaining part consists of amorphous particles (as detected by X-ray diffraction) <5 nm in size, which precipitate coherently from the matrix and have the same orientation as the nanocrystalline particles and the solid solution.

Thermal Stability of Microstructure and Microhardness of Heterophase BCC-Alloys After Torsional Deformation on Bridgman Anvils

NASA Astrophysics Data System (ADS)

Ditenberg, I. A.; Tyumentsev, A. N.

2018-03-01

The results of investigations of thermal stability of microstructure and microhardness of alloys of the V-4Ti-4Cr and Mo-47Re systems, subjected to torsional deformation by high quasi-hydrostatic pressure at room temperature, are reported. It is shown that submicrocrystalline and nanocrystalline states, and the respective high values of microhardness, persist up to the upper bound ( 0.4 Tmelt) of the temperature interval of their recovery and polygonization in a single-phase state. The main factors ensuring thermal stability of highlydefective states in heterophase alloys are discussed.

On the existence of declared 9R phase in Fe–Ni invar alloy

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

Kabanova, I. G.; Sagaradze, V. V., E-mail: vsagaradze@imp.uran.ru; Kataeva, N. V.

2016-07-15

An analysis of recently reported electron diffraction patterns suggests that metastable austenitic Fe–32Ni alloy subjected to α → γ transformation upon slow heating does not exhibit any signs of formation of the 9R phase; the conventional nanocrystalline γ phase with an fcc lattice is formed instead. Extended lamellae with a layered structure, erroneously identified as a new phase of the (3R + 9R) type in Fe–32Ni alloy, are conventional twinning (midrib) regions of each initial α crystal, in which γ-phase twin nanolamellae are formed upon heating.

Densification behavior, nanocrystallization, and mechanical properties of spark plasma sintered Fe-based bulk amorphous alloys

NASA Astrophysics Data System (ADS)

Singh, Ashish Kumar

Fe-based amorphous alloys are gaining increasing attention due to their exceptional wear and corrosion resistance for potential structural applications. Two major challenges that are hindering the commercialization of these amorphous alloys are difficulty in processing of bulk shapes (diameter > 10 mm) and lack of ductility. Spark plasma sintering (SPS) is evolving as a promising technique for processing bulk shapes of amorphous and nanocrystalline materials. The objective of this work is to investigate densification behavior, nanocrystallization, and mechanical properties of SPS sintered Fe-based amorphous alloys of composition Fe48Cr15Mo14Y2C15B6. SPS processing was performed in three distinct temperature ranges of amorphous alloys: (a) below glass transition temperature (Tg), (b) between Tg and crystallization temperature (Tx), and (c) above Tx. Punch displacement data obtained during SPS sintering was correlated with the SPS processing parameters such as temperature, pressure, and sintering time. Powder rearrangement, plastic deformation below T g, and viscous flow of the material between Tg and Tx were observed as the main densification stages during SPS sintering. Micro-scale temperature distributions at the point of contact and macro-scale temperature distribution throughout the sample during SPS of amorphous alloys were modeled. The bulk amorphous alloys are expected to undergo structural relaxation and nanocrystallization during SPS sintering. X-ray diffraction (XRD), small angle neutron scattering (SANS), and transmission electron microscopy (TEM) was performed to investigate the evolution of nanocrystallites in SPS sintered Fe-based bulk amorphous alloys. The SANS analysis showed significant scattering for the samples sintered in the supercooled region indicating local structural and compositional changes with the profuse nucleation of nano-clusters (~4 nm). Compression tests and microhardness were performed on the samples sintered at different temperatures ranging from 570 °C to 800 °C. Maximum compression strength (1.1+/-0.2 MPa) was obtained for the samples sintered in the supercooled region. Effects of crystallization on tribological behavior of sintered samples were also investigated where crystallization resulted in increase in wear resistance. Laser surface hardening of SPS sintered amorphous samples were performed. Depending on the processing parameters, the laser surface irradiation causes structural relaxation and nanocrystallization, resulting in surface hardening.

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

PubMed Central

Zherebtsov, Dmitry; Radionova, Ludmila

2018-01-01

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

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

PubMed

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

2018-05-07

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

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

Yu, Cun; Aoun, Bachir; Cui, Lishan

Microstructure evolution of a cold-drawn NiTi shape memory alloy wire was investigated by means of in-situ synchrotron high-energy X-ray diffraction during continuous heating. The cold-drawn wire contained amorphous regions and nano-crystalline domains in its microstructure. Pair distribution function analysis revealed that the amorphous regions underwent structural relaxation via atomic rearrangement when heated above 100 °C. The nano-crystalline domains were found to exhibit a strong cold work induced lattice strain anisotropy having a preferential <111> fiber orientation along the wire axial direction. The lattice strain anisotropy systematically decreased upon heating above 200 °C, implying a structural recovery. A broad conical texturemore » was formed in the wire specimen after crystallization similar in detail to the initial <111> texture axial orientation of the nano-crystalline domains produced by the severe cold wire drawing deformation.« less

Luminescence of mesoporous silicon powders treated by high-pressure water vapor annealing

NASA Astrophysics Data System (ADS)

Gelloz, Bernard; Loni, Armando; Canham, Leigh; Koshida, Nobuyoshi

2012-07-01

We have studied the photoluminescence of nanocrystalline silicon microparticle powders fabricated by fragmentation of PSi membranes. Several porosities were studied. Some powders have been subjected to further chemical etching in HF in order to reduce the size of the silicon skeleton and reach quantum sizes. High-pressure water vapor annealing was then used to enhance both the luminescence efficiency and stability. Two visible emission bands were observed. A red band characteristic of the emission of Si nanocrystals and a blue band related to localized centers in oxidized powders. The blue band included a long-lived component, with a lifetime exceeding 1 sec. Both emission bands depended strongly on the PSi initial porosity. The colors of the processed powders were tunable from brown to off-white, depending on the level of oxidation. The surface area and pore volume of some powders were also measured and discussed. The targeted applications are in cosmetics and medicine.

Formation of 4H-closely packed structure in thin films of metastable nanocrystalline Co 13Cu 87 alloy

NASA Astrophysics Data System (ADS)

Khalyapin, D. L.; Kim, J.; Stolyar, S. V.; Turpanov, I. A.; Kim, P. D.; Kim, I.

2003-11-01

The crystal structure of the thin films of metastable Co 13Cu 87 alloy prepared by magnetron sputtering was investigated by transmission electron microscope. As-deposited films have a nanocrystal structure with an fcc lattice. As a result of the prolonged ion polishing with a beam of Ar ions with the energy of 4.7 keV, the four-layer 4H dhcp structure was formed.

Powder metallurgy technology of NiTi shape memory alloy

NASA Astrophysics Data System (ADS)

Dutkiewicz, J. M.; Maziarz, W.; Czeppe, T.; Lityńska, L.; Nowacki, W. K.; Gadaj, S. P.; Luckner, J.; Pieczyska, E. A.

2008-05-01

Powder metallurgy technology was elaborated for consolidation of shape memory NiTi powders. The shape memory alloy was compacted from the prealloyed powder delivered by Memry SA. The powder shows Ms = 10°C and As = -34°C as results from DSC measurements. The samples were hot pressed in the as delivered spherical particle's state. The hot compaction was performed in a specially constructed vacuum press, at temperature of 680°C and pressure of 400 MPa. The alloy powder was encapsulated in copper capsules prior to hot pressing to avoid oxidation or carbides formation. The alloy after hot vacuum compaction at 680°C (i.e. within the B2 NiTi stability range) has shown similar transformation range as the powder. The porosity of samples compacted in the as delivered state was only 1%. The samples tested in compression up to ɛ = 0.06 have shown partial superelastic effect due to martensitic reversible transform- ation which started at the stress above 300 MPa and returned back to ɛ = 0.015 after unloading. They have shown also a high ultimate compression strength of 1600 MPa. Measurements of the samples temperature changes during the process allowed to detect the temperature increase above 12°C for the strain rate 10-2 s-1 accompanied the exothermic martensite transformation during loading and the temperature decrease related to the reverse endothermic transformation during unloading.

Effect of Fe3O4 addition on dielectric properties of LaFeO3 nano-crystalline materials synthesized by sol-gel method

NASA Astrophysics Data System (ADS)

Laysandra, H.; Triyono, D.

2017-04-01

Dielectric properties of nano-crystalline material LaFeO3.xFe3O4 with x = 0, 0.1, 0.2, 0.3, and 0.4 at.% have been studied by impedance spectroscopy method. LaFeO3 was synthesized by sol-gel method resulting nano-particle. Then, it was mixed with Fe3O4 powder. The mixture powder was pressed to form pellet and then sintered at 1300°C for 1 h to form nano-crystalline of LaFeO3.xFe3O4. X-ray diffraction characterization at room temperature for all samples show two phases i.e. perovskite LaFeO3 (orthorhombic) as a main phase and Fe3O4 (cubic) as second phase. It is found that the crystallite size of main phase increases with addition of Fe3O4 until 0.3 at.%. The electrical properties as a function of temperature (300-500 K) and frequency (100 Hz - 1 MHz) are presented in Nyquist and Bode plots. It is observed that from equivalent circuit and their parameters, dielectrical properties are contributed by grain and grain boundary. The dielectric constant, ε‧ were calculated by parallel plate method and their values reach up to 107 exhibiting typical colossal dielectric constant (CDC) material like behavior.

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.

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.

Study the effect of mechanical alloying parameters on synthesis of Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite

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

Shayesteh, Payam, E-mail: shayesteh.payam@gmail.com; Mirdamadi, Shamseddin; Razavi, Hossein

2014-01-01

Graphical abstract: - Highlights: • Cr{sub 2}Nb–Al{sub 2}O{sub 3} nanocomposite synthesized through MA. • Effect of BPR, rotating speed, milling time and PCA concentration investigated. • After annealing at 1100 °C crystalline phase were appeared. • Williamson–Hall analysis was used in order to study the grain size of nano composite. - Abstract: In this study, Cr{sub 2}Nb–20 vol.% Al{sub 2}O{sub 3} nanocomposite was prepared successfully by mechanochemical reaction between Al, Nb and Cr{sub 2}O{sub 3} powders. Amorphization of powder occurred during mechanical alloying because of high energy collisions between powders and steel balls in milling container which transfer high degreemore » of energy to powders. Therefore, annealing was needed to form crystalline phases. The influence of different mechanical alloying parameters such as BPR, rotating speed, milling time and PCA concentration on synthesis of composite material were investigated. After mechanical alloying, the powder was encapsulated in quartz and then annealed at 1100 °C for 3 h. After annealing, 3 different phases were appeared (Cr{sub 2}Nb (cubic), Cr{sub 2}Nb (hexagonal) and α-Al{sub 2}O{sub 3}). The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometry (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM)« less

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.

Improved Mo-Re VPS Alloys for High-Temperature Uses

NASA Technical Reports Server (NTRS)

Hickman, Robert; Martin, James; McKechnie, Timothy; O'Dell, John Scott

2011-01-01

Dispersion-strengthened molybdenum- rhenium alloys for vacuum plasma spraying (VPS) fabrication of high-temperature-resistant components are undergoing development. In comparison with otherwise equivalent non-dispersion-strengthened Mo-Re alloys, these alloys have improved high-temperature properties. Examples of VPS-fabricated high-temperature-resistant components for which these alloys are expected to be suitable include parts of aircraft and spacecraft engines, furnaces, and nuclear power plants; wear coatings; sputtering targets; x-ray targets; heat pipes in which liquid metals are used as working fluids; and heat exchangers in general. These alloys could also be useful as coating materials in some biomedical applications. The alloys consist of 60 weight percent Mo with 40 weight percent Re made from (1) blends of elemental Mo and Re powders or (2) Re-coated Mo particles that have been subjected to a proprietary powder-alloying-and-spheroidization process. For most of the dispersion- strengthening experiments performed thus far in this development effort, 0.4 volume percent of transition-metal ceramic dispersoids were mixed into the feedstock powders. For one experiment, the proportion of dispersoid was 1 volume percent. In each case, the dispersoid consisted of either ZrN particles having sizes <45 m, ZrO2 particles having sizes of about 1 m, HfO2 particles having sizes <45 m, or HfN particles having sizes <1 m. These materials were chosen for evaluation on the basis of previously published thermodynamic stability data. For comparison, Mo-Re feedstock powders without dispersoids were also prepared.

Effect of initial microstructure on the compactability of rapidly solidified Ti-rich TiAl powder

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

Nishida, M.; Chiba, A.; Morizono, Y.

1997-12-31

Initial microstructure dependence of compactability at elevated temperature in rapidly solidified Ti-rich TiAl alloy powders produced by plasma rotating electrode process (PREP) has been investigated. There were two kinds of powders with respect to the microstructure. The first one had a surface relief of a martensitic phase, which was referred as M powder. The second one had a dendritic structure, which was referred as D powder. {alpha}{sub 2}+{gamma} microduplex and {alpha}{sub 2}/{gamma} lamellar structures were formed in M and D powders of the Ti-40 at%Al alloy by heat treatment at 1,273 K, respectively. The microduplex structure consisted of {gamma} precipitatemore » in the twin related {alpha}{sub 2} matrix with the usual orientation relationship. It was difficult to compact the D powder by hot pressing at 1,273 K under 50 MPa for 14.4 ks. On the other hand, the M powder was compacted easily by hot pressing with the same condition. The twin related {alpha}{sub 2} and {alpha}{sub 2} boundary changed to random ones and the {alpha}{sub 2} and {gamma} phases lost the usual orientation relationship in the duplex structure during the hot pressing. In other words, the low energy boundaries were changed to the high energy ones suitable for grain boundary sliding. Dislocations were scarcely observed inside of both the {alpha}{sub 2} and {gamma} crystal grains. It was concluded that the grain boundary sliding was a predominant deformation mode in the M powder during the hot pressing. D and M powders in Ti-45 and 47 at%Al alloys showed the same tendency as those in Ti-40 at%Al alloy during hot pressing.« less

Experience of high-nitrogenous steel powder application in repairs and surface hardening of responsible parts for power equipment by plasma spraying

NASA Astrophysics Data System (ADS)

Kolpakov, A. S.; Kardonina, N. I.

2016-02-01

The questions of the application of novel diffusion-alloying high-nitrogenous steel powders for repair and surface hardening of responsible parts of power equipment by plasma spraying are considered. The appropriateness of the method for operative repair of equipment and increasing its service life is justified. General data on the structure, properties, and manufacture of nitrogen-, aluminum-, and chromium-containing steel powders that are economically alloyed using diffusion are described. It is noted that the nitrogen release during the decomposition of iron nitrides, when heating, protects the powder particles from oxidation in the plasma jet. It is shown that the coating retains 50% of nitrogen that is contained in the powder. Plasma spraying modes for diffusion-alloying high-nitrogenous steel powders are given. The service properties of plasma coatings based on these powders are analyzed. It is shown that the high-nitrogenous steel powders to a nitrogen content of 8.9 wt % provide the necessary wear resistance and hardness of the coating and the strength of its adhesion to the substrate and corrosion resistance to typical aggressive media. It is noted that increasing the coating porosity promotes stress relaxation and increases its thickness being limited with respect to delamination conditions in comparison with dense coatings on retention of the low defectiveness of the interface and high adhesion to the substrate. The examples of the application of high-nitrogenous steel powders in power engineering during equipment repairs by service companies and overhaul subdivisions of heat power plants are given. It is noted that the plasma spraying of diffusion-alloyed high-nitrogenous steel powders is a unique opportunity to restore nitrided steel products.

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.

Self-Lubricating Coatings for Elevated Temperature Applications Using A High-Velocity-Particle-Consolidation (HVPC) Process

DTIC Science & Technology

2008-12-01

Deposition of copper by cold gas dynamic spraying : An investigation of dependence of microstructure and properties of the deposits on the...the deposition of metals, alloys , polymers, and composite powder -materials onto various substrates without significant heating of the spray powders or... Spray method is a relatively new coating method for deposition of metal, alloy , polymer, and/or composite powder material onto

Magnesium Nanocomposites: Current Status and Prospects for Army Applications

DTIC Science & Technology

2011-09-01

and reinforcement that cannot be produced through melt-based processing . In mechanical alloying , the powder and milling media are placed into...mixing vessels that are agitated in a high-energy milling machine. During the mixing process , the powder particles undergo repeated cycles of cold ...welding and fracturing of interparticle bonds. At the end of the process , the powder has been alloyed to the desired composition. Although typically used

Properties of boride-added powder metallurgy magnesium alloys

NASA Astrophysics Data System (ADS)

Tanaka, Atsushi; Yoshimura, Syota; Fujima, Takuya; Takagi, Ken-ichi

2009-06-01

Magnesium alloys with metallic borides, magnesium diboride (MgB2) or aluminum diboride (AlB2), were investigated regarding their mechanical properties, transverse rupture strength (TRS) and micro Vickers hardness (HV). The alloys were made from pure Mg, Al and B powders by mechanical alloying and hot pressing to have boride content of between 2.0 and 20 vol%. The alloy with AlB2 exhibited an obvious improvement of HV around a boride content of 6 vol% though the other alloy, with MgB2, did not. TRS showed moderate maxima around the same boride content region for the both alloys. X-ray diffraction measurements indicated an intermetallic compound, Mg17Al12, formed in the alloy with AlB2, which was consistent with its higher hardness.

Microstructural Examination of Oxidized Fe_(14-x) Nb5_x Alloy Produced from Powders Prepared by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Demirkıran, A. Şükran; Sen, Saduman; Ozdemir, Ozkan; Sen, Ugur

In the present study, ferrous niobium, ferrous boron and iron were used as starting powders. The mixture of the powders which were calculated to give the designed compositions was prepared by using planetary high energy ball mill. Mechanically alloyed powders were pressed and sintered at 1350°C for 120 min in Ar atmosphere. The cyclic oxidation experiments were carried out in an electrical furnace at 650, 750 and 850 °C in open atmosphere for 96 h. The specimens were periodically weighed for the determination of weight change. Before and after oxidation, the present phases of the samples were determined by X-ray diffraction analysis (XRD). The microstructural characterizations were realized using scanning electron microscopy (SEM) with EDS attachment.

JPRS Report, Science & Technology, USSR: Materials Science

DTIC Science & Technology

1988-10-25

POROSHKOVAYA METALLURGIYA No 4, Apr 88] 17 Influence of Sintering Conditions on Structure and Mechanical Properties of Aluminum-Based Powder Alloys [A.B... Mechanics Institute, UkSSR Academy of Sci- ences] [Abstract] An experimental study of the ZhS3DK cast heat-resistant Ni alloy was made concerning the two...References 2: both Russian. 2415/12232 Influence of Sintering Conditions on Structure and Mechanical Properties of Aluminum-Based Powder Alloys

Laser Powder Cladding of Ti-6Al-4V α/β Alloy

PubMed Central

Al-Sayed Ali, Samar Reda; Hussein, Abdel Hamid Ahmed; Nofal, Adel Abdel Menam Saleh; Elgazzar, Haytham Abdelrafea; Sabour, Hassan Abdel

2017-01-01

Laser cladding process was performed on a commercial Ti-6Al-4V (α + β) titanium alloy by means of tungsten carbide-nickel based alloy powder blend. Nd:YAG laser with a 2.2-KW continuous wave was used with coaxial jet nozzle coupled with a standard powder feeding system. Four-track deposition of a blended powder consisting of 60 wt % tungsten carbide (WC) and 40 wt % NiCrBSi was successfully made on the alloy. The high content of the hard WC particles is intended to enhance the abrasion resistance of the titanium alloy. The goal was to create a uniform distribution of hard WC particles that is crack-free and nonporous to enhance the wear resistance of such alloy. This was achieved by changing the laser cladding parameters to reach the optimum conditions for favorable mechanical properties. The laser cladding samples were subjected to thorough microstructure examinations, microhardness and abrasion tests. Phase identification was obtained by X-ray diffraction (XRD). The obtained results revealed that the best clad layers were achieved at a specific heat input value of 59.5 J·mm−2. An increase by more than three folds in the microhardness values of the clad layers was achieved and the wear resistance was improved by values reaching 400 times. PMID:29036935

New Powder Metallurgical Approach to Achieve High Fatigue Strength in Ti-6Al-4V Alloy

NASA Astrophysics Data System (ADS)

Cao, Fei; Ravi Chandran, K. S.; Kumar, Pankaj; Sun, Pei; Zak Fang, Z.; Koopman, Mark

2016-05-01

Recently, manufacturing of titanium by sintering and dehydrogenation of hydride powders has generated a great deal of interest. An overarching concern regarding powder metallurgy (PM) titanium is that critical mechanical properties, especially the high-cycle fatigue strength, are lower than those of wrought titanium alloys. It is demonstrated here that PM Ti-6Al-4V alloy with mechanical properties comparable (in fatigue strength) and exceeding (in tensile properties) those of wrought Ti-6Al-4V can be produced from titanium hydride powder, through the hydrogen sintering and phase transformation process. Tensile and fatigue behavior, as well as fatigue fracture mechanisms, have been investigated under three processing conditions. It is shown that a reduction in the size of extreme-sized pores by changing the hydride particle size distribution can lead to improved fatigue strength. Further densification by pneumatic isostatic forging leads to a fatigue strength of ~550 MPa, comparable to the best of PM Ti-6Al-4V alloys prepared by other methods and approaching the fatigue strengths of wrought Ti-6Al-4V alloys. The microstructural factors that limit fatigue strength in PM titanium have been investigated, and pathways to achieve greater fatigue strengths in PM Ti-6Al-4V alloys have been identified.

Laser Powder Cladding of Ti-6Al-4V α/β Alloy.

PubMed

Al-Sayed Ali, Samar Reda; Hussein, Abdel Hamid Ahmed; Nofal, Adel Abdel Menam Saleh; Hasseb Elnaby, Salah Elden Ibrahim; Elgazzar, Haytham Abdelrafea; Sabour, Hassan Abdel

2017-10-15

Laser cladding process was performed on a commercial Ti-6Al-4V (α + β) titanium alloy by means of tungsten carbide-nickel based alloy powder blend. Nd:YAG laser with a 2.2-KW continuous wave was used with coaxial jet nozzle coupled with a standard powder feeding system. Four-track deposition of a blended powder consisting of 60 wt % tungsten carbide (WC) and 40 wt % NiCrBSi was successfully made on the alloy. The high content of the hard WC particles is intended to enhance the abrasion resistance of the titanium alloy. The goal was to create a uniform distribution of hard WC particles that is crack-free and nonporous to enhance the wear resistance of such alloy. This was achieved by changing the laser cladding parameters to reach the optimum conditions for favorable mechanical properties. The laser cladding samples were subjected to thorough microstructure examinations, microhardness and abrasion tests. Phase identification was obtained by X-ray diffraction (XRD). The obtained results revealed that the best clad layers were achieved at a specific heat input value of 59.5 J·mm -2 . An increase by more than three folds in the microhardness values of the clad layers was achieved and the wear resistance was improved by values reaching 400 times.

Development of low-Cr ODS FeCrAl alloys for accident-tolerant fuel cladding

NASA Astrophysics Data System (ADS)

Dryepondt, Sebastien; Unocic, Kinga A.; Hoelzer, David T.; Massey, Caleb P.; Pint, Bruce A.

2018-04-01

Low-Cr oxide dispersion strengthened (ODS) FeCrAl alloys were developed as accident tolerant fuel cladding because of their excellent oxidation resistance at very high temperature, high strength and improved radiation tolerance. Fe-12Cr-5Al wt.% gas atomized powder was ball milled with Y2O3+FeO, Y2O3+ZrO2 or Y2O3+TiO2, and the resulting powders were extruded at 950 °C. The resulting fine grain structure, particularly for the Ti and Zr containing alloys, led to very high strength but limited ductility. Comparison with variants of commercial PM2000 (Fe-20Cr-5Al) highlighted the significant impact of the powder consolidation step on the alloy grain size and, therefore, on the alloy mechanical properties at T < 500 °C. These low-Cr compositions exhibited good oxidation resistance at 1400 °C in air and steam for 4 h but could not form a protective alumina scale at 1450 °C, similar to observations for fine grained PM2000 alloys. The effect of alloy grain size, Zr and Ti additions, and impurities on the alloy mechanical and oxidation behaviors are discussed.

Dendritic Ag-Fe nanocrystalline alloy synthesized by pulsed electrodeposition and its characterization

NASA Astrophysics Data System (ADS)

Santhi, Kalavathy; Revathy, T. A.; Narayanan, V.; Stephen, A.

2014-10-01

Synthesis of dendrite shaped Ag-Fe alloy nanomaterial by pulsed electrodeposition route was investigated. The alloy samples were deposited at different current densities from electrolytes of different compositions to study the influence of current density and bath composition on metal contents in the alloy, which was determined by ICP-OES analysis. The XRD studies were carried out to determine the structure of these samples. Magnetic characterization at room temperature and during heating was carried out to understand their magnetic behaviour and to confirm the inferences drawn from the XRD results. The XPS spectra proved the presence of Fe and Ag in the metallic form in the alloy samples. The FESEM and TEM micrographs were taken to view the surface morphology of the nanosized particles.

Microwave assisted combustion synthesis of nanocrystalline CoFe2O4 for LPG sensing

NASA Astrophysics Data System (ADS)

Chaudhari, Prashant; Acharya, S. A.; Darunkar, S. S.; Gaikwad, V. M.

2015-08-01

A microwave-assisted citrate precursor method has been utilized for synthesis of nanocrystalline powders of CoFe2O4. The process takes only a few minutes to obtain as-synthesized CoFe2O4. Structural properties of the synthesized material were investigated by X-ray diffraction; scanning electron microscopy, Thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy. The gas sensing properties of thick film of CoFe2O4 prepared by screen printing towards Liquid Petroleum Gas (LPG) revealed that CoFe2O4 thick films are sensitive and shows maximum sensitivity at 350°C for 2500 ppm of LPG.

Alloying Behavior and Properties of FeSiBAlNiCo x High Entropy Alloys Fabricated by Mechanical Alloying and Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Wang, Wen; Li, Boyu; Zhai, Sicheng; Xu, Juan; Niu, Zuozhe; Xu, Jing; Wang, Yan

2018-02-01

In this paper, FeSiBAlNiCo x (x = 0.2, 0.8) high-entropy alloy (HEA) powders were fabricated by mechanical alloying process, and the powders milled for 140 h were sintered by spark plasma sintering (SPS) technique. The microstructures and properties of as-milled powders and as-sintered samples were investigated. The results reveal that the final milling products (140 h) of both sample powders present the fully amorphous structure. The increased Co contents obviously enhance the glass forming ability and thermal stability of amorphous HEA powders, which are reflected by the shorter formation time of fully amorphous phase and the higher onset crystallization temperature, respectively. According to coercivity, the as-milled FeSiBAlNiCo x (x = 0.2, 0.8) powders (140 h) are the semi-hard magnetic materials. FeSiBAlNiCo0.8 HEA powders possess the highest saturation magnetization and largest remanence ratio. The SPS-ed products of both bulk HEAs are composed of body-centered cubic solid solution, and FeSi and FeB intermetallic phases. They possess the high relative density above 97% and excellent microhardness exceeding 1150 HV. The as-sintered bulks undergo the remarkable increase in saturation magnetization compared with the as-milled state. The SPS-ed FeSiBAlNiCo0.8 HEA exhibits the soft magnetic properties. The electrochemical corrosion test is carried out in 3.5% NaCl solution. The SPS-ed FeSiBAlNiCo0.2 HEA reveals the better passivity with low passive current density, and the higher pitting resistance with wide passive region.

From Powders to Dense Metal Parts: Characterization of a Commercial AlSiMg Alloy Processed through Direct Metal Laser Sintering

PubMed Central

Manfredi, Diego; Calignano, Flaviana; Krishnan, Manickavasagam; Canali, Riccardo; Ambrosio, Elisa Paola; Atzeni, Eleonora

2013-01-01

In this paper, a characterization of an AlSiMg alloy processed by direct metal laser sintering (DMLS) is presented, from the analysis of the starting powders, in terms of size, morphology and chemical composition, through to the evaluation of mechanical and microstructural properties of specimens built along different orientations parallel and perpendicular to the powder deposition plane. With respect to a similar aluminum alloy as-fabricated, a higher yield strength of about 40% due to the very fine microstructure, closely related to the mechanisms involved in this additive process is observed. PMID:28809344

From Powders to Dense Metal Parts: Characterization of a Commercial AlSiMg Alloy Processed through Direct Metal Laser Sintering.

PubMed

Manfredi, Diego; Calignano, Flaviana; Krishnan, Manickavasagam; Canali, Riccardo; Ambrosio, Elisa Paola; Atzeni, Eleonora

2013-03-06

In this paper, a characterization of an AlSiMg alloy processed by direct metal laser sintering (DMLS) is presented, from the analysis of the starting powders, in terms of size, morphology and chemical composition, through to the evaluation of mechanical and microstructural properties of specimens built along different orientations parallel and perpendicular to the powder deposition plane. With respect to a similar aluminum alloy as-fabricated, a higher yield strength of about 40% due to the very fine microstructure, closely related to the mechanisms involved in this additive process is observed.

Dendritic microstructure in argon atomized superalloy powders

NASA Technical Reports Server (NTRS)

Tewari, S. N.; Kumar, Mahundra

1986-01-01

The dendritic microstructure of atomized nickel base superalloy powders (Ni-20 pct Cr, NIMONIC-80A, ASTROALOY, and ZHS6-K) was studied. Prealloyed vacuum induction melted ingots were argon-atomized, the powders were cooled to room temperature, and various powder-size fractions were examined by optical metallography. Linear correlations were obtained for the powder size dependence of the secondary dendrite arm spacing, following the expected d-alpha (R) to the m power dependence on the particle size for all four superalloy compositions. However, the Ni-20 pct Cr alloy, which had much coarser arm spacing as compared to the other three alloys, had a much larger value of m.

Method of fabricating thin-walled articles of tungsten-nickel-iron alloy

DOEpatents

Hovis, Jr., Victor M.; Northcutt, Jr., Walter G.

1982-01-01

The present invention relates to a method for fabricating thin-walled high-density structures oftungsten-nickel-iron alloys. A powdered blend of the selected alloy constituents is plasma sprayed onto a mandrel having the desired article configuration. The sprayed deposit is removed from the mandrel and subjected to liquid phase sintering to provide the alloyed structure. The formation of the thin-walled structure by plasma spraying significantly reduces shrinkage, and cracking while increasing physical properties of the structure over that obtainable by employing previously known powder metallurgical procedures.

Method of fabricating thin-walled articles of tungsten-nickel-iron alloy

DOEpatents

Hovis, V.M. Jr.; Northcutt, W.G. Jr.

The present invention relates to a method for fabricating thin-walled high-density structures of tungsten-nickel-iron alloys. A powdered blend of the selected alloy constituents is plasma sprayed onto a mandrel having the desired article configuration. The sprayed deposit is removed from the mandrel and subjected to liquid phase sintering to provide the alloyed structure. The formation of the thin-walled structure by plasma spraying significantly reduces shrinkage, and cracking while increasing physical properties of the structure over that obtainable by employing previously known powder metallurgical procedures.

Nanocrystalline Iron-Cobalt Alloys for High Saturation Indutance

DTIC Science & Technology

2016-02-24

toroid. Before fully embarking on the problem of creating the toroid’s from particles sintered by a process known as sparked plasma sintering which...allows the particles to be rapidly sintered without compromising the nano crystalline particle size, it was deemed necessary to anticipate the

Mechanical properties of in situ consolidated nanocrystalline multi-phase Al-Pb-W alloy studied by nanoindentation

NASA Astrophysics Data System (ADS)

Varam, Sreedevi; Prasad, Muvva D.; Rao, K. Bhanu Sankara; Rajulapati, Koteswararao V.

2016-12-01

Formation of chunks of various sizes ranging between 2 and 6 mm was achieved using high-energy ball milling in Al-1at.%Pb-1at.%W alloy system at room temperature during milling itself, aiding in in situ consolidation. X-ray diffraction and transmission electron microscopy (TEM) studies indicate the formation of multi-phase structure with nanocrystalline structural features. From TEM data, an average grain size of 23 nm was obtained for Al matrix and the second-phase particles were around 5 nm. A high strain rate sensitivity (SRS) of 0.071 ± 0.004 and an activation volume of 4.71b3 were measured using nanoindentation. Modulus mapping studies were carried out using Berkovich tip in dynamic mechanical analysis mode coupled with in situ scanning probe microscopy imaging. The salient feature of this investigation is highlighting the role of different phases, their crystal structures and the resultant interfaces on the overall SRS and activation volume of a multi-phase nc material.

Structural Transformation in Fe73.5Nb3Cu1Si15.5B7 Amorphous Alloy Induced by Laser Heating

NASA Astrophysics Data System (ADS)

Nykyruy, Yu. S.; Mudry, S. I.; Kulyk, Yu. O.; Zhovneruk, S. V.

2018-03-01

The effect of continuous laser irradiation (λ = 1.06 μm) with laser power of 45 W on the structure of Fe73.5Nb3Cu1Si15.5B7 amorphous alloy has been studied using X-ray diffraction and SEM methods. The sample of the ribbon has been placed at a distance from the focal plane of the lens, so a laser beam has been defocused and the diameter of laser spot on the ribbon surface has been about 10 mm. An exposure time τ varied within interval 0.25-0.70 s. Under such conditions structural transformation processes, which depend on the exposure time, have occurred in an irradiated zone. Crystallization process has started at τ = 0.35 s with the formation of α-Fe(Si) nanocrystalline phase, while complete crystallization has occurred at τ = 0.55 s with formation of two nanocrystalline phases: α-Fe(Si) and a hexagonal H-phase.

Dendrite-Free Nanocrystalline Zinc Electrodeposition from an Ionic Liquid Containing Nickel Triflate for Rechargeable Zn-Based Batteries.

PubMed

Liu, Zhen; Cui, Tong; Pulletikurthi, Giridhar; Lahiri, Abhishek; Carstens, Timo; Olschewski, Mark; Endres, Frank

2016-02-18

Metallic zinc is a promising anode material for rechargeable Zn-based batteries. However, the dendritic growth of zinc has prevented practical applications. Herein it is demonstrated that dendrite-free zinc deposits with a nanocrystalline structure can be obtained by using nickel triflate as an additive in a zinc triflate containing ionic liquid. The formation of a thin layer of Zn-Ni alloy (η- and γ-phases) on the surface and in the initial stages of deposition along with the formation of an interfacial layer on the electrode strongly affect the nucleation and growth of zinc. A well-defined and uniform nanocrystalline zinc deposit with particle sizes of about 25 nm was obtained in the presence of Ni(II) . Further, it is shown that the nanocrystalline Zn exhibits a high cycling stability even after 50 deposition/stripping cycles. This strategy of introducing an inorganic metal salt in ionic liquid electrolytes can be considered as an efficient way to obtain dendrite-free zinc. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Grain boundary character distribution in nanocrystalline metals produced by different processing routes

DOE PAGES

Bober, David B.; Kumar, Mukal; Rupert, Timothy J.; ...

2015-12-28

Nanocrystalline materials are defined by their fine grain size, but details of the grain boundary character distribution should also be important. Grain boundary character distributions are reported for ball-milled, sputter-deposited, and electrodeposited Ni and Ni-based alloys, all with average grain sizes of ~20 nm, to study the influence of processing route. The two deposited materials had nearly identical grain boundary character distributions, both marked by a Σ3 length percentage of 23 to 25 pct. In contrast, the ball-milled material had only 3 pct Σ3-type grain boundaries and a large fraction of low-angle boundaries (16 pct), with the remainder being predominantlymore » random high angle (73 pct). Furthermore, these grain boundary character measurements are connected to the physical events that control their respective processing routes. Consequences for material properties are also discussed with a focus on nanocrystalline corrosion. As a whole, the results presented here show that grain boundary character distribution, which has often been overlooked in nanocrystalline metals, can vary significantly and influence material properties in profound ways.« less

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

Odette, G Robert; Cunningham, Nicholas J., Wu, Yuan; Etienne, Auriane

The broad objective of this NEUP was to further develop a class of 12-15Cr ferritic alloys that are dispersion strengthened and made radiation tolerant by an ultrahigh density of Y-Ti-O nanofeatures (NFs) in the size range of less than 5 nm. We call these potentially transformable materials nanostructured ferritic alloys (NFAs). NFAs are typically processed by ball milling pre-alloyed rapidly solidified powders and yttria (Y2O3) powders. Proper milling effectively dissolves the Ti, Y and O solutes that precipitate as NFs during hot consolidation. The tasks in the present study included examining alternative processing paths, characterizing and optimizing the NFs andmore » investigating solid state joining. Alternative processing paths involved rapid solidification by gas atomization of Fe, 14% Cr, 3% W, and 0.4% Ti powders that are also pre-alloyed with 0.2% Y (14YWT), where the compositions are in wt.%. The focus is on exploring the possibility of minimizing, or even eliminating, the milling time, as well as producing alloys with more homogeneous distributions of NFs and a more uniform, fine grain size. Three atomization environments were explored: Ar, Ar plus O (Ar/O) and He. The characterization of powders and alloys occurred through each processing step: powder production by gas atomization; powder milling; and powder annealing or hot consolidation by hot isostatic pressing (HIPing) or hot extrusion. The characterization studies of the materials described here include various combinations of: a) bulk chemistry; b) electron probe microanalysis (EPMA); c) atom probe tomography (APT); d) small angle neutron scattering (SANS); e) various types of scanning and transmission electron microscopy (SEM and TEM); and f) microhardness testing. The bulk chemistry measurements show that preliminary batches of gas-atomized powders could be produced within specified composition ranges. However, EPMA and TEM showed that the Y is heterogeneously distributed and phase separated, but TEM, SANS and APT show that attritor milling for 20 to 40 h sufficiently mixes the Y. TEM, SANS and APT showed that subsequent powder annealing treatments result in the precipitation of a high density of NFs. All the annealed powder variants and HIP consolidated alloys had a bimodal distribution of grain sizes; however, APT and TEM show the presence of NFs in both large and small grains. Alloys extruded at 850°C contain a unimodal distribution of fine grains. The initial milling procedures in this study added a significant quantity of O as well as contaminant N to the powders. An improved milling procedure effectively eliminated the contamination resulting in lower O content that was insufficient to produce Y-Ti-O NFs in the size range below 3 nm. TEM showed that the low O resulted in fewer and larger oxide phases that are more highly enriched in Y, resulting in low Vicker's hardness values 250 kg/mm^2 compared to 443 kg/mm^2 in an alloy consolidated from the preliminary powders with higher O content. In order to overcome the problem of O deficiency, FeO additions during 40 h attritor milling were made to increase the O content to a nominal value of 0.135%. The annealed powder and corresponding 1150°C HIP and 850°C extrusion consolidated alloy showed a very uniform distribution of fine scale NFs. The HIP consolidated alloy had promising high temperature creep strength, but low toughness and a high ductile to brittle transition temperature (DBTT). An extruded and cross-rolled alloy processed at 850ºC, however, exhibited a lower DBTT. Also investigated were the effects of Ti and Y content on the NFs in alloys produced from conventionally milled powders that varied Y2O3 from 0.2 to 0.5 wt.% while maintaining Ti/Y atom ratios of 1.6, 2.4, and 3.1. SANS showed the volume fraction and number density of the NFs increases with Y and to a lesser extent Ti. Notably, the NF size and composition are relatively independent of the alloy Y and Ti content, except at the lowest Y2O3 concentration of 0.2 wt.%. An APT characterization of MA957 joined by friction stir welding (FSW) showed that this solid sate joining procedure had only a modest effect on the NF number density (N) and average diameter () compared to an as extruded sample. FSW appears to rearrange the NFs, which become highly aligned with sub-boundary and dislocation structures to an extent that are not observed in the as extruded case. The aligned NF structures are less apparent, but seem to persist after post weld annealing at 1150ºC for 3 h following which reduces N, consistent with a significant reduction in hardness. Lastly, several NFA materials, including MA957 and various 14YWT alloys, have been included in irradiation experiments performed at the Advanced Test Reactor, the JOYO sodium cooled fast reactor, the High Flux Isotope Reactor, and the SINQ spallation neut« less

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.

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.

Biaxially textured articles formed by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.

2001-01-01

A biaxially textured alloy article comprises Ni powder and at least one powder selected from the group consisting of Cr, W, V, Mo, Cu, Al, Ce, YSZ, Y, Rare Earths, (RE), MgO, CeO.sub.2, and Y.sub.2 O.sub.3 ; compacted and heat treated, then rapidly recrystallized to produce a biaxial texture on the article. In some embodiments the alloy article further comprises electromagnetic or electro-optical devices and possesses superconducting properties.

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

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

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

2016-03-30

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

Method for refining contaminated iridium

DOEpatents

Heshmatpour, B.; Heestand, R.L.

1982-08-31

Contaminated iridium is refined by alloying it with an alloying agent selected from the group consisting of manganese and an alloy of manganese and copper, and then dissolving the alloying agent from the formed alloy to provide a purified iridium powder.

Effects of Bi Addition on the Microstructure and Mechanical Properties of Nanocrystalline Ag Coatings.

PubMed

Wang, Yuxin; Cheng, Guang; Tay, See Leng; Guo, Yunxia; Sun, Xin; Gao, Wei

2017-08-10

In this study we investigated the effects of Bi addition on the microstructure and mechanical properties of an electrodeposited nanocrystalline Ag coating. Microstructural features were investigated with transmission electron microscopy (TEM). The results indicate that the addition of Bi introduced nanometer-scale Ag-Bi solid solution particles and more internal defects to the initial Ag microstructures. The anisotropic elastic-plastic properties of the Ag nanocrystalline coating with and without Bi addition were examined with nanoindentation experiments in conjunction with the recently-developed inverse method. The results indicate that the as-deposited nanocrystalline Ag coating contained high mechanical anisotropy. With the addition of 1 atomic percent (at%) Bi, the anisotropy within Ag-Bi coating was very small, and yield strength of the nanocrystalline Ag-Bi alloy in both longitudinal and transverse directions were improved by over 100% compared to that of Ag. On the other hand, the strain-hardening exponent of Ag-Bi was reduced to 0.055 from the original 0.16 of the Ag coating. Furthermore, the addition of Bi only slightly increased the electrical resistivity of the Ag-Bi coating in comparison to Ag. Results of our study indicate that Bi addition is a promising method for improving the mechanical and physical performances of Ag coating for electrical contacts.

Defect structure in electrodeposited nanocrystalline Ni layers with different Mo concentrations

NASA Astrophysics Data System (ADS)

Kapoor, Garima; Péter, László; Fekete, Éva; Gubicza, Jenő

2018-05-01

The effect of molybdenum (Mo) alloying on the lattice defect structure in electrodeposited nanocrystalline nickel (Ni) films was studied. The electrodeposited layers were prepared on copper substrate at room temperature, with a constant current density and pH value. The chemical composition of these layers was determined by EDS. In addition, X-ray diffraction line profile analysis was carried out to study the microstructural parameters such as the crystallite size, the dislocation density and the stacking fault probability. It was found that the higher Mo content yielded more than one order of magnitude larger dislocation density while the crystallite size was only slightly smaller. In addition, the twin boundary formation activity during deposition increased with increasing Mo concentration. The results obtained on electrodeposited layers were compared with previous research carried out on bulk nanocrystalline Ni-Mo materials with similar compositions but processed by severe plastic deformation.

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

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

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

Microstructure study of direct laser fabricated Ti alloys using powder and wire

NASA Astrophysics Data System (ADS)

Wang, Fude; Mei, J.; Wu, Xinhua

2006-11-01

A compositionally graded material has been fabricated using direct laser fabrication (DFL). Two types of feedstock were fed simultaneously into the laser focal point, a burn resistant (BurTi) alloy Ti-25V-15Cr-2Al-0.2C powder and a Ti-6Al-4V wire. The local composition of the alloy was changed by altering the ratio of powder to wire by varying the feed rate of the powder whilst maintaining a fixed feed rate of wire-feed. For the range of compositions between about 20% and 100% BurTi only the beta phase was observed and the composition and lattice parameter varied monotonically. The grain size was found to be much finer in these functionally graded samples than in laser fabricated Ti64. Some samples were made using the wire-feed alone, where it was found that the microstructure is different from that found when using powder feed alone. The results are discussed in terms of the power requirements for laser fabrication of powder and wire samples.

Lattice dynamics and thermoelectric properties of nanocrystalline silicon-germanium alloys: Lattice dynamics and thermoelectric properties of nc Si-Ge alloys

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

Claudio, Tania; Stein, Niklas; Petermann, Nils

2015-10-26

The lattice dynamics and thermoelectric properties of sintered phosphorus-doped nanostructured silicon–germanium alloys obtained by gas-phase synthesis were studied. Measurements of the density of phonon states by inelastic neutron scattering were combined with measurements of the elastic constants and the low-temperature heat capacity. A strong influence of nanostructuring and alloying on the lattice dynamics was observed. The thermoelectric transport properties of samples with different doping as well as samples sintered at different temperature were characterized between room temperature and 1000°C. A peak figure of merit zT=0.88 at 900°C is observed and is comparatively insensitive to the aforementioned parameter variations.

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

PubMed

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

2017-04-06

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

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

PubMed Central

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

2017-01-01

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

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.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Fe-Cr-Mo based ODS alloys via spark plasma sintering: A combinational characterization study by TEM and APT

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

Y. Q. Wu; K. N. Allahar; J. Burns

2013-08-01

Nanoscale oxides play an important role in oxide dispersion strengthened (ODS) alloys for improved high temperature creep resistance and enhanced radiation damage tolerance. In this study, transmission electron microscopy (TEM) and atom probe tomography (APT) were combined to investigate two novel Fe-16Cr-3Mo (wt.%) based ODS alloys. Spark plasma sintering (SPS) was used to consolidate the ODS alloys from powders that were milled with 0.5 wt.% Y2O3 powder only or with Y2O3 powder and 1 wt.% Ti. TEM characterization revealed that both alloys have a bimodal structure of nanometer-size (~ 100 – 500 nm) and micron-size grains with nanostructured oxide precipitatesmore » formed along and close to grain boundaries with diameters ranging from five to tens of nanometers. APT provides further quantitative analyses of the oxide precipitates, and also reveals Mo segregation at grain boundaries next to oxide precipitates. The alloys with and without Ti are compared based on their microstructures.« less

The influence of laser alloying on the structure and mechanical properties of AlMg5Si2Mn surface layers

NASA Astrophysics Data System (ADS)

Pakieła, W.; Tański, T.; Brytan, Z.; Labisz, K.

2016-04-01

The goal of this paper was focused on investigation of microstructure and properties of surface layer produced during laser surface treatment of aluminium alloy by high-power fibre laser. The performed laser treatment involves remelting and feeding of Inconel 625 powder into the aluminium surface. As a base metal was used aluminium alloy AlMg5Si2Mn. The Inconel powder was injected into the melt pool and delivered by a vacuum feeder at a constant rate of 4.5 g/min. The size of Inconel alloying powder was in the range 60-130 µm. In order to remelt the aluminium alloy surface, the fibre laser of 3 kW laser beam power has been used. The linear laser scan rate of the beam was set 0.5 m/min. Based on performed investigations, it was possible to obtain the layer consisting of heat-affected zone, transition zone and remelted zone, without cracks and defects having much higher hardness value compared to the non-alloyed material.

Expected values and variances of Bragg peak intensities measured in a nanocrystalline powder diffraction experiment

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

Öztürk, Hande; Noyan, I. Cevdet

A rigorous study of sampling and intensity statistics applicable for a powder diffraction experiment as a function of crystallite size is presented. Our analysis yields approximate equations for the expected value, variance and standard deviations for both the number of diffracting grains and the corresponding diffracted intensity for a given Bragg peak. The classical formalism published in 1948 by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] appears as a special case, limited to large crystallite sizes, here. It is observed that both the Lorentz probability expression and the statistics equations used in the classical formalism are inapplicable for nanocrystallinemore » powder samples.« less

Expected values and variances of Bragg peak intensities measured in a nanocrystalline powder diffraction experiment

DOE PAGES

Öztürk, Hande; Noyan, I. Cevdet

2017-08-24

A rigorous study of sampling and intensity statistics applicable for a powder diffraction experiment as a function of crystallite size is presented. Our analysis yields approximate equations for the expected value, variance and standard deviations for both the number of diffracting grains and the corresponding diffracted intensity for a given Bragg peak. The classical formalism published in 1948 by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] appears as a special case, limited to large crystallite sizes, here. It is observed that both the Lorentz probability expression and the statistics equations used in the classical formalism are inapplicable for nanocrystallinemore » powder samples.« less

Mechanochemical processing for metals and metal alloys

DOEpatents

Froes, Francis H.; Eranezhuth, Baburaj G.; Prisbrey, Keith

2001-01-01

A set of processes for preparing metal powders, including metal alloy powders, by ambient temperature reduction of a reducible metal compound by a reactive metal or metal hydride through mechanochemical processing. The reduction process includes milling reactants to induce and complete the reduction reaction. The preferred reducing agents include magnesium and calcium hydride powders. A process of pre-milling magnesium as a reducing agent to increase the activity of the magnesium has been established as one part of the invention.

Influence of Hydrogen on Atomized Titanium Powders Sintering

NASA Astrophysics Data System (ADS)

Senkevich, K. S.

2018-07-01

The aim of this work is to study the effect of hydrogen reversible alloying (thermohydrogen processing, THP) on low-temperature sintering of atomized titanium powders. It is stated that alloying with 0.2 to 0.8 wt pct of hydrogen beneficially affects titanium powders sintering. The effect is caused by phase transformations occurring upon hydrogen saturation of powders and dehydrogenation, which substantially intensifies sintering at temperatures from 800 °C to 900 °C. The role of certain THP stages (sintering in hydrogenated state and upon dehydrogenation) on formation of sintered contacts in porous materials is shown.

Influence of Hydrogen on Atomized Titanium Powders Sintering

NASA Astrophysics Data System (ADS)

Senkevich, K. S.

2018-05-01

The aim of this work is to study the effect of hydrogen reversible alloying (thermohydrogen processing, THP) on low-temperature sintering of atomized titanium powders. It is stated that alloying with 0.2 to 0.8 wt pct of hydrogen beneficially affects titanium powders sintering. The effect is caused by phase transformations occurring upon hydrogen saturation of powders and dehydrogenation, which substantially intensifies sintering at temperatures from 800 °C to 900 °C. The role of certain THP stages (sintering in hydrogenated state and upon dehydrogenation) on formation of sintered contacts in porous materials is shown.

Influence of small particles inclusion on selective laser melting of Ti-6Al-4V powder

NASA Astrophysics Data System (ADS)

Gong, Haijun; Dilip, J. J. S.; Yang, Li; Teng, Chong; Stucker, Brent

2017-12-01

The particle size distribution and powder morphology of metallic powders have an important effect on powder bed fusion based additive manufacturing processes, such as selective laser melting (SLM). The process development and parameter optimization require a fundamental understanding of the influence of powder on SLM. This study introduces a pre-alloyed titanium alloy Ti-6Al-4V powder, which has a certain amount of small particles, for SLM. The influence of small particle inclusion is investigated through microscopy of surface topography, elemental and microstructural analysis, and mechanical testing, compared to the Ti-6Al-4V powder provided by SLM machine vendor. It is found that the small particles inclusion in Ti-6Al-4V powder has a noticeable effect on extra laser energy absorption, which may develop imperfections and deteriorate the SLM fatigue performance.

Thixoforming of Stellite Powder Compacts

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

Hogg, S. C.; Atkinson, H. V.; Kapranos, P.

2007-04-07

Thixoforming involves processing metallic alloys in the semi-solid state. The process requires the microstructure to be spheroidal when part-solid and part-liquid i.e. to consist of solid spheroids surrounded by liquid. The aim of this work was to investigate whether powder compacts can be used as feedstock for thixoforming and whether the consolidating pressure in the thixoformer can be used to remove porosity from the compact. The powder compacts were made from stellite 6 and stellite 21 alloys, cobalt-based alloys widely used for e.g. manufacturing prostheses. Isothermal heat treatments of small samples in the consolidated state showed the optimum thixoforming temperaturemore » to be in the range 1340 deg. C-1350 deg. C for both materials. The alloys were thixoformed into graphite dies and flowed easily to fill the die. Porosity in the thixoformed components was lower than in the starting material. Hardness values at various positions along the radius of the thixoformed demonstrator component were above the specification for both alloys.« less

Self-passivating bulk tungsten-based alloys manufactured by powder metallurgy

NASA Astrophysics Data System (ADS)

López-Ruiz, P.; Ordás, N.; Lindig, S.; Koch, F.; Iturriza, I.; García-Rosales, C.

2011-12-01

Self-passivating tungsten-based alloys are expected to provide a major safety advantage compared to pure tungsten, which is at present the main candidate material for the first wall armour of future fusion reactors. WC10Si10 alloys were manufactured by mechanical alloying (MA) in a Planetary mill and subsequent hot isostatic pressing (HIP), achieving densities above 95%. Different MA conditions were studied. After MA under optimized conditions, a core with heterogeneous microstructure was found in larger powder particles, resulting in the presence of some large W grains after HIP. Nevertheless, the obtained microstructure is significantly refined compared to previous work. First MA trials were also performed on the Si-free system WCr12Ti2.5. In this case a very homogeneous structure inside the powder particles was obtained, and a majority ternary metastable bcc phase was found, indicating that almost complete alloying occurred. Therefore, a very fine and homogeneous microstructure can be expected after HIP in future work.

Development of a Power Metallurgy Superalloy for Use at 1800-2000 F (980-1090 C)

NASA Technical Reports Server (NTRS)

Kortovich, C. S.

1973-01-01

A program was conducted to develop a powder metallurgy nickel-base superalloy for 1800-2000 F (980-1090 C) temperature applications. The feasibility of a unique concept for alloying carbon into a superalloy powder matrix and achieving both grain growth and a discrete particle grain boundary carbide precipitation was demonstrated. The process consisted of blending metastable carbides with a carbon free base alloy and consolidating this blend by hot extrusion. This was followed by heat treatment to grow a desired ASTM No. 2-3 grain size and to solution the metastable carbides to allow precipitation of discrete particle grain boundary carbides during subsequent aging heat treatments. The best alloy developed during this program was hydrogen-atomized, thermal-mechanically processed, modified MAR-M246 base alloy plus VC (0.28 w/o C). Although below those for cast MAR-M246, the mechanical properties exhibited by this alloy represent the best combination offered by conventional powder metallurgy processing to date.

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.

Grain Nucleation and Growth in Deformed NiTi Shape Memory Alloys: An In Situ TEM Study

NASA Astrophysics Data System (ADS)

Burow, J.; Frenzel, J.; Somsen, C.; Prokofiev, E.; Valiev, R.; Eggeler, G.

2017-12-01

The present study investigates the evolution of nanocrystalline (NC) and ultrafine-grained (UFG) microstructures in plastically deformed NiTi. Two deformed NiTi alloys were subjected to in situ annealing in a transmission electron microscope (TEM) at 400 and 550 °C: an amorphous material state produced by high-pressure torsion (HPT) and a mostly martensitic partly amorphous alloy produced by wire drawing. In situ annealing experiments were performed to characterize the microstructural evolution from the initial nonequilibrium states toward energetically more favorable microstructures. In general, the formation and evolution of nanocrystalline microstructures are governed by the nucleation of new grains and their subsequent growth. Austenite nuclei which form in HPT and wire-drawn microstructures have sizes close to 10 nm. Grain coarsening occurs in a sporadic, nonuniform manner and depends on the physical and chemical features of the local environment. The mobility of grain boundaries in NiTi is governed by the local interaction of each grain with its microstructural environment. Nanograin growth in thin TEM foils seems to follow similar kinetic laws to those in bulk microstructures. The present study demonstrates the strength of in situ TEM analysis and also highlights aspects which need to be considered when interpreting the results.

Magnetic softening and nanocrystallization in amorphous Co-rich alloys

NASA Astrophysics Data System (ADS)

Buttino, G.; Cecchetti, A.; Poppi, M.

1997-02-01

In this work we have analyzed the changes of the magnetic properties in the Co-based Metglas 2714A (made by Allied Chem. Corp., USA) caused by isothermal heat treatments in the range of temperature from room temperature to conventional crystallization temperature Tcr = 550°C. The nominal composition of the amorphous alloy is Co 66Fe 4Ni 1B 14Si 15. The analysis is made on toroidal samples prepared by winding lengths of amorphous ribbon of about 20 cm. The magnetic properties undergo variations depending on the treatment temperature, except for the saturation magnetization which remains unchanged. For heat treatments of about half an hour around 500°C, superior soft magnetic properties are obtained. Particularly, the initial permeability reaches values up to ten times the value of permeability in the as-received sample. Analysis by the transmission electron microscopy of the sample annealed around 500°C reveals the formation of a nanocrystalline phase, with average grain size of 2 nm, embedded in a residual amorphous matrix. The occurrence of permeability increases in concomitance with the formation of the nanocrystalline phase is ascribed to a drastic reduction in the local magnetocrystalline anisotropy randomly averaged out by the exchange interactions, similar to the case of the annealed Fe-based alloys containing Cu.

Free Form Low Cost Fabrication Using Titanium

DTIC Science & Technology

2007-06-29

Compaction Metals) "* CP Ti (International Titanium Powders, LLC) "* Gas Atomized Ti-6AI- 4V (Carpenter Powder Products, Bridgeville, PA) "* Gas Atomized CP...analytical data for the titanium alloys represented in this report Alloy Al C Fe H Mo N2 02 al V TI CP-Ti Grade II 0.1 0.3 0.015 0.03 025 Balance TI-6AI- 4V ...Ti-6A1- 4V is titanium alloyed with 6% Aluminum and 4% Vanadium. This alloy has a melting point range of 1604-1660’C, which is not suitable for

Powder-Metallurgy Process And Product

NASA Technical Reports Server (NTRS)

Paris, Henry G.

1988-01-01

Rapid-solidification processing yields alloys with improved properties. Study undertaken to extend favorable property combinations of I/M 2XXX alloys through recently developed technique of rapid-solidification processing using powder metallurgy(P/M). Rapid-solidification processing involves impingement of molten metal stream onto rapidly-spinning chill block or through gas medium using gas atomization technique.

Retraction Note to: Ultra-High Strength and Ductile Lamellar-Structured Powder Metallurgy Binary Ti-Ta Alloys

NASA Astrophysics Data System (ADS)

Liu, Yong; Xu, Shenghang; Wang, Xin; Li, Kaiyang; Liu, Bin; Wu, Hong; Tang, Huiping

2018-05-01

The editors and authors have retracted the article, "Ultra-High Strength and Ductile Lamellar-Structured Powder Metallurgy Binary Ti-Ta Alloys" by Yong Liu, Shenghang Xu, Xin Wang, Kaiyang Li, Bin Liu, Hong Wu, and Huiping Tang (https://doi.org/10.1007/s11837-015-1801-1).

Specific Adaptation of Gas Atomization Processing for Al-Based Alloy Powder for Additive Manufacturing

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

Anderson, Iver; Siemon, John

The initial three atomization attempts resulted in “freeze-outs” within the pour tubes in the pilot-scale system and yielded no powder. Re-evaluation of the alloy liquidus temperatures and melting characteristics, in collaboration with Alcoa, showed further superheat to be necessary to allow the liquid metal to flow through the pour tube to the atomization nozzle. A subsequent smaller run on the experimental atomization system verified these parameters and was successful, as were all successive runs on the larger pilot scale system. One alloy composition froze-out part way through the atomization on both pilot scale runs. SEM images showed needle formation andmore » phase segregations within the microstructure. Analysis of the pour tube freeze-out microstructures showed that large needles formed within the pour tube during the atomization experiment, which eventually blocked the melt stream. Alcoa verified the needle formation in this alloy using theoretical modeling of phase solidification. Sufficient powder of this composition was still generated to allow powder characterization and additive manufacturing trials at Alcoa.« less

Synthesizing Aluminum alloys by double mechanical alloying

NASA Astrophysics Data System (ADS)

Froyen, L.; Delaey, L.; Niu, X. P.; Le Brun, P.; Peytour, C.

1995-03-01

A new synthesis technique, namely double mechanical alloying (dMA), has been developed to fabricate aluminum alloys containing the finely distributed intermetallic compounds and inert dispersoids Al4C3 and Al2O3 The technique consists mainly of three steps: a primary milling stage of elemental powders (MAI) followed by a heat treatment to promote the formation of intermetallic phases, a secondary milling stage (MA2) to refine the microstructure, and consolidation of the produced powders. The results of mechanical and tribological properties of the resulting materials indicate that the dMA is a promising technique for the fabrication of aluminum alloys for applications requiring wear resistance and high-temperature performance.

Applications of high-temperature powder metal aluminum alloys to small gas turbines

NASA Technical Reports Server (NTRS)

Millan, P. P., Jr.

1982-01-01

A program aimed at the development of advanced powder-metallurgy (PM) aluminum alloys for high-temperature applications up to 650 F using the concepts of rapid solidification and mechanical alloying is discussed. In particular, application of rapidly solidified PM aluminum alloys to centrifugal compressor impellers, currently used in auxiliary power units for both military and commercial aircraft and potentially for advanced automotive gas turbine engines, is examined. It is shown that substitution of high-temperature aluminum for titanium alloy impellers operating in the 360-650 F range provides significant savings in material and machining costs and results in reduced component weight, and consequently, reduced rotating group inertia requirements.

Solidification of nanosuspensions for the production of solid oral dosage forms and inhalable dry powders.

PubMed

Malamatari, Maria; Somavarapu, Satyanarayana; Taylor, Kevin M G; Buckton, Graham

2016-01-01

Nanosuspensions combine the advantages of nanotherapeutics (e.g. increased dissolution rate and saturation solubility) with ease of commercialisation. Transformation of nanosuspensions to solid oral and inhalable dosage forms minimises the physical instability associated with their liquid state, enhances patient compliance and enables targeted oral and pulmonary drug delivery. This review outlines solidification methods for nanosuspensions. It includes spray and freeze drying as the most widely used techniques. Fluidised-bed coating, granulation and pelletisation are also discussed as they yield nanocrystalline formulations with more straightforward downstream processing to tablets or capsules. Spray-freeze drying, aerosol flow reactor and printing of nanosuspensions are also presented as promising alternative solidification techniques. Results regarding the solid state, in vitro dissolution and/or aerosolisation efficiency of the nanocrystalline formulations are given and combined with available in vivo data. Focus is placed on the redispersibility of the solid nanocrystalline formulations, which is a prerequisite for their clinical application. A few solidified nanocrystalline products are already on the market and many more are in development. Oral and inhalable nanoparticle formulations are expected to have great potential especially in the areas of personalised medicine and delivery of high drug doses (e.g. antibiotics) to the lungs, respectively.

Mechanical Properties of β-Ti-35Nb-2.5Sn Alloy Synthesized by Mechanical Alloying and Pulsed Current Activated Sintering

NASA Astrophysics Data System (ADS)

Omran, Abdel-Nasser; Woo, Kee-Do; Lee, Hyun Bom

2012-12-01

A developed Ti-35 pct Nb-2.5 pct Sn (wt pct) alloy was synthesized by mechanical alloying using high-energy ball-milled powders, and the powder consolidation was done by pulsed current activated sintering (PCAS). The starting powder materials were mixed for 24 hours and then milled by high-energy ball milling (HEBM) for 1, 4, and 12 hours. The bulk solid samples were fabricated by PCAS at 1073 K to 1373 K (800 °C to 1100 °C) for a short time, followed by rapid cooling to 773 K (500 °C). The relative density of the sintered samples was about 93 pct. The Ti was completely transformed from α to β-Ti phase after milling for 12 hours in powder state, and the specimen sintered at 1546 K (1273 °C) was almost transformed to β-Ti phase. The homogeneity of the sintered specimen increased with increasing milling time and sintering temperature, as did its hardness, reaching 400 HV after 12 hours of milling. The Young's modulus was almost constant for all sintered Ti-35 pct Nb-2.5 pct Sn specimens at different milling times. The Young's modulus was low (63.55 to 65.3 GPa) compared to that of the standard alloy of Ti-6Al-4V (100 GPa). The wear resistance of the sintered specimen increased with increasing milling time. The 12-hour milled powder exhibited the best wear resistance.

Photoluminescent spectroscopy measurements in nanocrystalline praseodymium doped zirconia powders

NASA Astrophysics Data System (ADS)

Ramos-Brito, F.; Murrieta S, H.; Hernández A, J.; Camarillo, E.; García-Hipólito, M.; Martínez-Martínez, R.; Álvarez-Fragoso, O.; Falcony, C.

2006-05-01

Praseodymium doped zirconia powder (ZrO2: (0.53 at%) Pr3+) was prepared by a co-precipitation technique and annealed in air at a temperature Ta = 950 °C. The x-ray diffraction pattern shows a nanocrystalline structure composed of 29.6% monoclinic and 70.4% cubic-tetragonal phases. Medium infrared and Raman analysis confirms the monoclinic/cubic-tetragonal crystalline structure and proves the absence of praseodymium aggregates in the material. Photoluminescent spectroscopy over excitations of 457.9 and 514.9 nm (at 20 K), shows two emission spectra composed of many narrow peaks in the visible-near infrared region (VIS-NIR) of the electromagnetic spectrum, associated with 4f inter-level electronic transitions in praseodymium ions incorporated in the zirconia. Excitation and emission spectra show the different mechanisms of the direct and non-direct excitation of the dopant ion (Pr3+), and the preferential relaxation of the material by charge transfer from the host (zirconia) to the 4f5d band and the 4f inter-level of the dopant ion (Pr3+). No evidence of energy transfer from the host to the dopant was observed.

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

NASA Technical Reports Server (NTRS)

Glasgow, T. K.

1975-01-01

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

The luminescence properties of nanocrystalline phosphors Mg2SiO4:Eu3+

NASA Astrophysics Data System (ADS)

Kolomytsev, A. Y.; Mamonova, D. V.; Manshina, A. A.; Kolesnikov, I. E.

2017-11-01

Nanocrystalline Eu3+-doped Mg2SiO4 powders were prepared with combined Pechini-solid phase synthesis. The structural properties were investigated with XRD, SEM and Raman spectroscopy. XRD pattern indicated that Mg2SiO4:Eu3+ were obtained with formation of other phase: MgO. Raman spectrum revealed good homogeneity and crystallinity of synthesized nanopowders. The luminescence properties were studied with measurement of excitation and emission spectra and decay curves. The effect of Eu3+ concentration on 5D0 level lifetime was studied. Most probably, the observed shortening of 5D0 level lifetime with Eu3+ concentration is caused by increase of nonradiative process probability.

Surface treatment process of Al-Mg alloy powder by BTSPS

NASA Astrophysics Data System (ADS)

Zhao, Ran; Gao, Xinbao; Lu, Yanling; Du, Fengzhen; Zhang, Li; Liu, Dazhi; Chen, Xuefang

2018-04-01

The surface of Al-Mg alloy powder was treated by BTSPS(bis(triethoxysilylpropyl)tetrasulfide) in order to avoid easy oxidation in air. The pH value, reaction temperature, reaction time, and reaction concentration were used as test conditions. The results show that the BTSPS can form a protected film on the surface of Al-Mg alloy powder. Select the best test solution by orthogonal test. The study found that the reaction time and reaction temperature have the biggest influence on the two indexes of the orthogonal test (melting enthalpy of heat and enthalpy of oxidation). The optimal conditions were as follows: pH value is 8, reaction concentration is 2%, reaction temperature is 25 °C, reaction time is 2 h. The oxidation weight gain of the alloy reached 74.45% and the decomposition temperature of silane film is 181.8 °C.

Forming a single layer of a composite powder based on the Ti-Nb system via selective laser melting (SLM)

NASA Astrophysics Data System (ADS)

Saprykin, A. A.; Sharkeev, Yu P.; Ibragimov, E. A.; Babakova, E. V.; Dudikhin, D. V.

2016-07-01

Alloys based on the titanium-niobium system are widely used in implant production. It is conditional, first of all, on the low modulus of elasticity and bio-inert properties of an alloy. These alloys are especially important for tooth replacement and orthopedic surgery. At present alloys based on the titanium-niobium system are produced mainly using conventional metallurgical methods. The further subtractive manufacturing an end product results in a lot of wastes, increasing, therefore, its cost. The alternative of these processes is additive manufacturing. Selective laser melting is a technology, which makes it possible to synthesize products of metal powders and their blends. The point of this technology is laser melting a layer of a powdered material; then a sintered layer is coated with the next layer of powder etc. Complex products and working prototypes are made on the base of this technology. The authors of this paper address to the issue of applying selective laser melting in order to synthesize a binary alloy of a composite powder based on the titanium-niobium system. A set of 10x10 mm samples is made in various process conditions. The samples are made by an experimental selective laser synthesis machine «VARISKAF-100MB». The machine provides adjustment of the following process variables: laser emission power, scanning rate and pitch, temperature of powder pre-heating, thickness of the layer to be sprinkled, and diameter of laser spot focusing. All samples are made in the preliminary vacuumized shielding atmosphere of argon. The porosity and thickness of the sintered layer related to the laser emission power are shown at various scanning rates. It is revealed that scanning rate and laser emission power are adjustable process variables, having the greatest effect on forming the sintered layer.

Evaluation of the radiopacity of calcium silicate cements containing different radiopacifiers.

PubMed

Camilleri, J; Gandolfi, M G

2010-01-01

To identify the suitable ratio of alternative radiopacifiers to impart the necessary radiopacity to calcium silicate cements (CSC) and assess the purity of the radiopacifying agents. Alternative radiopacifying materials for incorporation into CSC included barium sulphate, titanium oxide, zinc oxide, gold powder and silver/tin alloy. The chemical composition of the alternative radipacifying materials and bismuth oxide, which is used in mineral trioxide aggregate (MTA), was determined using energy dispersive X-ray analysis. In addition, using an aluminium step-wedge and densitometer, the radiopacity of each material was evaluated as recommended by international standards. The optical density was compared with the relevant thickness of aluminium (Al). A commercial MTA and CSC were used as controls. Statistical analysis comparing the radiodensity of the different cements to MTA was performed using anova with P = 0.05 and post hoc Tukey test. All percentage replacements of bismuth oxide, gold and silver-tin alloy powder, and the 25% and 30% replacements with barium sulphate and zinc oxide had radiopacities greater than 3 mm thickness of aluminium (Al) recommended by ISO 6876 (2002). The 25% replacement of cement with gold powder and 20% replacement of cement with silver/tin alloy powder exhibited radiopacity values of 8.04 mm Al and 7.52 mm Al, respectively, similar to MTA (P > 0.05). The cement replaced with 20% bismuth oxide showed a radiopacity of 6.83 mm Al, lower than MTA (P = 0.003). Silver/tin alloy and gold powder imparted the necessary radiopacity to a calcium silicate-based cement. Barium sulphate was also a suitable radiopacifier together with a lower concentration of silver/tin alloy and gold powder that achieved the radiodensity recommended by ISO 6876. Further research is required to investigate the broader properties of the calcium silicate-based cement with the different radiopacifiers.

Formation and magnetic properties of the L10 phase in bulk, powder and hot compacted Mn-Ga alloys

NASA Astrophysics Data System (ADS)

Mix, T.; Müller, K.-H.; Schultz, L.; Woodcock, T. G.

2015-10-01

The formation and stability of the L10 phase in Mn-Ga binary alloys with compositions in the range 50-75 at% Mn (in steps of 5 at%) has been studied. Of these, single-phase L10 structure was successfully produced in the 55, 60 and 65 at% Mn alloys by annealing the high temperature phases, which had been retained to room temperature following arc melting. Further annealing and thermal analysis were used to determine the phase transformation temperatures in the alloys and the results were used to guide further processing. The saturation magnetisation, Ms, and the anisotropy field, Ha, were determined in applied fields up to 14 T. For Mn55Ga45, μ0Ms=0.807 T and μ0Ha=4.4 T were observed. Mechanically milled Mn55Ga45 powder had coercivity of μ0Hc=0.393 T, which was a twentyfold increase compared to the bulk material but the magnetisation was reduced (cf. powder: μ0M5 T=0.576 T, bulk: μ0M5 T=0.780 T). Annealing the powder at 400 °C led to recovery of the magnetisation but reduced the coercivity, which was still 10 times as high as the bulk value. A degree of texture of 0.45 was achieved by magnetic alignment of the powder particles, leading to a remanence of 0.526 T. Furthermore, isotropic hot compacts of powders were produced with packing density from 83% to 99%, in which the improved coercivity of the powders was partially retained.

Relationship of Powder Feedstock Variability to Microstructure and Defects in Selective Laser Melted Alloy 718

NASA Technical Reports Server (NTRS)

Smith, T. M.; Kloesel, M. F.; Sudbrack, C. K.

2017-01-01

Powder-bed additive manufacturing processes use fine powders to build parts layer by layer. For selective laser melted (SLM) Alloy 718, the powders that are available off-the-shelf are in the 10-45 or 15-45 micron size range. A comprehensive investigation of sixteen powders from these typical ranges and two off-nominal-sized powders is underway to gain insight into the impact of feedstock on processing, durability and performance of 718 SLM space-flight hardware. This talk emphasizes an aspect of this work: the impact of powder variability on the microstructure and defects observed in the as-fabricated and full heated material, where lab-scale components were built using vendor recommended parameters. These typical powders exhibit variation in composition, percentage of fines, roughness, morphology and particle size distribution. How these differences relate to the melt-pool size, porosity, grain structure, precipitate distributions, and inclusion content will be presented and discussed in context of build quality and powder acceptance.

Effects of N precursor on the agglomeration and visible light photocatalytic activity of N-doped TiO2 nanocrystalline powder.

PubMed

Hu, Yulong; Liu, Hongfang; Rao, Qiuhua; Kong, Xiaodong; Sun, Wei; Guo, Xingpeng

2011-04-01

N-doped TiO2 nanocrystalline powders were prepared by the sol-gel method using various N precursors, including triethylamine, hydrazine hydrate, ethylenediamine, ammonium hydroxide, and urea. The samples were characterized by X-ray diffraction, N2 adsorption isotherms, transmission electron microscopy, ultraviolet-visible diffuse reflectance spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The photocatalytic activities of as-prepared samples under irradiation of visible light (lambda > 405 nm) were evaluated by photodecomposition of methyl orange. The alkalinity of N precursor was found to play a key role in the gel process. The N precursor with moderate alkalinity causes TiO2 nanoparticles to be sol-transformed into a loosely agglomerated gel. This transformation facilitates the preparation of an N-doped TiO2 powder with small nanocrystal size, large specific surface area, and high N doping level and results in high visible light photocatalytic activity. The N in TiO2 with N is binding energy at 399-400 eV may be assigned to the N-H species located in interstitial sites of TiO2 lattice which is the active N species responsible for the visible light photocatalytic activity. The N species of N 1s peak at 402 and 405 eV are ineffective to the visible light photocatalytic activity and may inhibit the photocatalytic activity. Moreover, a TiO2 nanoparticle powder with large specific area can be achieved by using urea as a template and then by using ammonium hydroxide to transform the sol into gel.

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

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

PubMed

Prakash, B Shri; Varma, K B R

2008-11-01

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

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.

Physics of the multi-functionality of lanthanum ferrite ceramics

NASA Astrophysics Data System (ADS)

Bhargav, K. K.; Ram, S.; Majumder, S. B.

2014-05-01

In the present work, we have illustrated the physics of the multifunctional characteristics of nano-crystalline LaFeO3 powder prepared using auto-combustion synthesis. The synthesized powders were phase pure and crystallized into centro-symmetric Pnma space group. The temperature dependence of dielectric constant of pure LaFeO3 exhibits dielectric maxima similar to that observed in ferroelectric ceramics with non-centrosymmetric point group. The dielectric relaxation of LaFeO3 correlates well with small polaron conduction. The occurrence of polarization hysteresis in LaFeO3 (with centro-symmetric Pnma space group) is thought to be spin current induced type. The canting of the Fe3+ spins induce weak ferromagnetism in nano-crystalline LaFeO3. Room temperature saturation magnetization of pure LaFeO3 is reported to be 3.0 emu/g. Due to the presence of both ferromagnetic as well as polarization ordering, LaFeO3 behaves like a single phase multiferroic ceramics. The magneto-electric coupling in this system has been demonstrated through the magneto-dielectric measurements which yield about 0.8% dielectric tuning (at 10 kHz) with the application of 2 T magnetic field. As a typical application of the synthesized nano-crystalline LaFeO3 powder, we have studied its butane sensing characteristics. The efficient butane sensing characteristics have been correlated to their catalytic activity towards oxidation of butane. Through X-ray photoelectron spectroscopy analyses, we detect the surface adsorbed oxygen species on LaFeO3 surface. Surface adsorbed oxygen species play major role in their low temperature butane sensing. Finally, we have hypothesized that the desorbed H2O and O2 (originate from surface adsorbed hydroxyl and oxygen) initiate the catalytic oxidative dehydrogenation of n-butane resulting in weakening of the electrostatics of the gas molecules.

High Pressure X-Ray Diffraction Studies of Nanocrystalline Materials

NASA Technical Reports Server (NTRS)

Palosz, B.; Stel'makh, S.; Grzanka, E.; Gierlotka, S.; Palosz, W.

2004-01-01

Experimental evidence obtained for a variety of nanocrystalline materials suggest that the crystallographic structure of a very small size particle deviates from that in the bulk crystals. In this paper we show the effect of the surface of nanocrystals on their structure by the analysis of generation and distribution of macro- and micro-strains at high pressures and their dependence on the grain size in nanocrystalline powders of Sic. We studied the structure of Sic nanocrystals by in-situ high-pressure powder diffraction technique using synchrotron and neutron sources and hydrostatic or isostatic pressure conditions. The diffraction measurements were done in HASYLAB at DESY using a Diamond Anvil Cell (DAC) in the energy dispersive geometry in the diffraction vector range up to 3.5 - 4/A and under pressures up to 50 GPa at room temperature. In-situ high pressure neutron diffraction measurements were done at LANSCE in Los Alamos National Laboratory using the HIPD and HIPPO diffractometers with the Paris-Edinburgh and TAP-98 cells, respectively, in the diffraction vector range up to 26 Examination of the response of the material to external stresses requires nonstandard methodology of the materials characterization and description. Although every diffraction pattern contains a complete information on macro- and micro-strains, a high pressure experiment can reveal only those factors which contribute to the characteristic diffraction patterns of the crystalline phases present in the sample. The elastic properties of powders with the grain size from several nm to micrometers were examined using three methodologies: (l), the analysis of positions and widths of individual Bragg reflections (used for calculating macro- and micro-strains generated during densification) [I], (2). the analysis of the dependence of the experimental apparent lattice parameter, alp, on the diffraction vector Q [2], and (3), the atomic Pair Distribution Function (PDF) technique [3]. The results of our studies show, that Sic nanocrystals have the features of two phases, each with its distinct elastic properties. and under pressures up to 8 GPa.

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

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

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

Powder metallurgy approaches to high temperature components for gas turbine engines

NASA Technical Reports Server (NTRS)

Probst, H. B.

1974-01-01

Research is reported for the tensile strength, ductility, and heat performance characterisitics of powder metallurgy (p/m) superalloys. Oxide dispersion strengthened alloys were also evaluated for their strength during thermal processing. The mechanical attributes evident in both p/m supperalloys and dispersion strengthened alloys are discussed in terms of research into their possible combination.

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.

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.

Alternating current transport and dielectric relaxation of nanocrystalline graphene oxide

NASA Astrophysics Data System (ADS)

Zedan, I. T.; El-Menyawy, E. M.

2018-07-01

Graphene oxide (GO) has been synthesized from natural graphite using modified Hummer's method and is subjected to sonication for 1 h. X-ray diffraction (XRD) showed that the prepared GO has nanocrystalline structure with particle size of about 5 nm and high-resolution transmission electron microscope showed that it had a layered structure. The nanocrystalline GO powder was pressed as a disk and the alternating current (AC) electrical conductivity, σAC, and dielectric properties have been investigated in the frequency range 50Hz-5 MHz and temperature range 298-523K using parallel plate spectroscopic technique. Analysis of σ AC as a function of frequency shows that the relation follows Jonscher's universal law with frequency exponent decreases with increasing temperature in which the correlated barrier hopping model is applicable to describe the behavior. The dielectric constant and dielectric loss are studied as functions of frequency and temperature. The dielectric modulus formalism is used for describing the relaxation process in which the relaxation time and its activation energy were evaluated.

Anisotropic nanocrystalline MnBi with high coercivity at high temperature

NASA Astrophysics Data System (ADS)

Yang, J. B.; Yang, Y. B.; Chen, X. G.; Ma, X. B.; Han, J. Z.; Yang, Y. C.; Guo, S.; Yan, A. R.; Huang, Q. Z.; Wu, M. M.; Chen, D. F.

2011-08-01

Magnetic hard nanocrystalline MnBi has been prepared by melt spinning and subsequent low temperature annealing. A coercivity of 2.5 T can be achieved at 540 K for MnBi with an average grain size of about 20-30 nm. The coercivity iHc, mainly controlled by the coherent magnetization rotation, shows a strong dependence on the time of grinding and exhibits a positive temperature coefficient from 100 up to 540 K. The unique temperature dependent behavior of the coercivity (magnetocrystalline anisotropy) has a relationship with the variations in the crystal lattice ratio of c/a with temperatures. In addition, discontinuity can not be found in the lattice parameters of a, c, and c/a ratio at the magnetostructural transition temperature. The nanocrystalline MnBi powder fixed in an epoxy resin and under an applied magnetic field of 24 kOe shows a maximum energy product of 7.1 MGOe at room temperature and shows anisotropic characteristics with high Mr/Ms ratio up to 560 K.

Multiscale understanding of tricalcium silicate hydration reactions.

PubMed

Cuesta, Ana; Zea-Garcia, Jesus D; Londono-Zuluaga, Diana; De la Torre, Angeles G; Santacruz, Isabel; Vallcorba, Oriol; Dapiaggi, Monica; Sanfélix, Susana G; Aranda, Miguel A G

2018-06-04

Tricalcium silicate, the main constituent of Portland cement, hydrates to produce crystalline calcium hydroxide and calcium-silicate-hydrates (C-S-H) nanocrystalline gel. This hydration reaction is poorly understood at the nanoscale. The understanding of atomic arrangement in nanocrystalline phases is intrinsically complicated and this challenge is exacerbated by the presence of additional crystalline phase(s). Here, we use calorimetry and synchrotron X-ray powder diffraction to quantitatively follow tricalcium silicate hydration process: i) its dissolution, ii) portlandite crystallization and iii) C-S-H gel precipitation. Chiefly, synchrotron pair distribution function (PDF) allows to identify a defective clinotobermorite, Ca 11 Si 9 O 28 (OH) 2 . 8.5H 2 O, as the nanocrystalline component of C-S-H. Furthermore, PDF analysis also indicates that C-S-H gel contains monolayer calcium hydroxide which is stretched as recently predicted by first principles calculations. These outcomes, plus additional laboratory characterization, yielded a multiscale picture for C-S-H nanocomposite gel which explains the observed densities and Ca/Si atomic ratios at the nano- and meso- scales.

Characterization of Localized Filament Corrosion Products at the Anodic Head on a Model Mg-Zn-Zr Alloy Surface

DOE PAGES

Rossouw, David; Fu, Dong; Leonard, Donovan N.; ...

2017-02-15

In this study, localized filament corrosion products at the anodic head on a model Mg-1%Zn-0.4%Zr alloy surface were characterized by electron microscopy techniques of site-specific lamella prepared by focused ion beam milling. It is revealed that the anodic head propagates underneath a largely intact thin and dense MgO surface film and comprises dense aggregates of nano-crystalline MgO within a nano-porous Mg(OH) 2 network. In conclusion, the findings contribute new supportive direct imaging insight into the source of the enhanced H 2 evolution that accompanies anodic dissolution of Mg and its alloys.

Lattice dynamics and thermoelectric properties of nanocrystalline silicon-germanium alloys

DOE PAGES

Claudio, Tania; Stein, Niklas; Peterman, Nils; ...

2015-10-26

The lattice dynamics and thermoelectric properties of sintered phosphorus-doped nanostructured silicon- germanium alloys obtained by gas-phase synthesis were studied. Measurements of the density of phonon states by inelastic neutron scattering were combined with measurements of the elastic constants and the low- temperature heat capacity. A strong influence of nanostructuring and alloying on the lattice dynamics was observed. The thermoelectric transport properties of samples with different doping as well as samples sintered at different temperature were characterized between room temperature and 1000C. A peak figure of merit zT = 0:88 at 900C is observed and comparatively insensitive to the aforementioned param-more » eter variations.« less

Characterization of Localized Filament Corrosion Products at the Anodic Head on a Model Mg-Zn-Zr Alloy Surface

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

Rossouw, David; Fu, Dong; Leonard, Donovan N.

In this study, localized filament corrosion products at the anodic head on a model Mg-1%Zn-0.4%Zr alloy surface were characterized by electron microscopy techniques of site-specific lamella prepared by focused ion beam milling. It is revealed that the anodic head propagates underneath a largely intact thin and dense MgO surface film and comprises dense aggregates of nano-crystalline MgO within a nano-porous Mg(OH) 2 network. In conclusion, the findings contribute new supportive direct imaging insight into the source of the enhanced H 2 evolution that accompanies anodic dissolution of Mg and its alloys.

The thermal stability of the nanograin structure in a weak solute segregation system.

PubMed

Tang, Fawei; Song, Xiaoyan; Wang, Haibin; Liu, Xuemei; Nie, Zuoren

2017-02-08

A hybrid model that combines first principles calculations and thermodynamic evaluation was developed to describe the thermal stability of a nanocrystalline solid solution with weak segregation. The dependence of the solute segregation behavior on the electronic structure, solute concentration, grain size and temperature was demonstrated, using the nanocrystalline Cu-Zn system as an example. The modeling results show that the segregation energy changes with the solute concentration in a form of nonmonotonic function. The change in the total Gibbs free energy indicates that at a constant solute concentration and a given temperature, a nanocrystalline structure can remain stable when the initial grain size is controlled in a critical range. In experiments, dense nanocrystalline Cu-Zn alloy bulk was prepared, and a series of annealing experiments were performed to examine the thermal stability of the nanograins. The experimental measurements confirmed the model predictions that with a certain solute concentration, a state of steady nanograin growth can be achieved at high temperatures when the initial grain size is controlled in a critical range. The present work proposes that in weak solute segregation systems, the nanograin structure can be kept thermally stable by adjusting the solute concentration and initial grain size.

Examining the influence of grain size on radiation tolerance in the nanocrystalline regime

DOE PAGES

Barr, Christopher M.; Li, Nan; Boyce, Brad L.; ...

2018-05-01

Here, nanocrystalline materials have been proposed as superior radiation tolerant materials in comparison to coarse grain counterparts. However, there is still a limited understanding whether a particular nanocrystalline grain size is required to obtain significant improvements in key deleterious effects resulting from energetic irradiation. This work employs the use of in-situ heavy ion irradiation transmission electron microscopy experiments coupled with quantitative defect characterization and precession electron diffraction to explore the sensitivity of defect size and density within the nanocrystalline regime in platinum. Under the explored experimental conditions, no significant change in either the defect size or density between grain sizesmore » of 20 and 100 nm was observed. Furthermore, the in-situ transmission electron microscopy irradiations illustrate stable sessile defect clusters of 1–3 nm adjacent to most grain boundaries, which are traditionally treated as strong defect sinks. The stability of these sessile defects observed in-situ in small, 20–40 nm, grains is the proposed primary mechanism for a lack of defect density trends. Lastly, this scaling breakdown in radiation improvement with decreasing grain size has practical importance on nanoscale grain boundary engineering approaches for proposed radiation tolerant alloys.« less

Examining the influence of grain size on radiation tolerance in the nanocrystalline regime

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

Barr, Christopher M.; Li, Nan; Boyce, Brad L.

Here, nanocrystalline materials have been proposed as superior radiation tolerant materials in comparison to coarse grain counterparts. However, there is still a limited understanding whether a particular nanocrystalline grain size is required to obtain significant improvements in key deleterious effects resulting from energetic irradiation. This work employs the use of in-situ heavy ion irradiation transmission electron microscopy experiments coupled with quantitative defect characterization and precession electron diffraction to explore the sensitivity of defect size and density within the nanocrystalline regime in platinum. Under the explored experimental conditions, no significant change in either the defect size or density between grain sizesmore » of 20 and 100 nm was observed. Furthermore, the in-situ transmission electron microscopy irradiations illustrate stable sessile defect clusters of 1–3 nm adjacent to most grain boundaries, which are traditionally treated as strong defect sinks. The stability of these sessile defects observed in-situ in small, 20–40 nm, grains is the proposed primary mechanism for a lack of defect density trends. Lastly, this scaling breakdown in radiation improvement with decreasing grain size has practical importance on nanoscale grain boundary engineering approaches for proposed radiation tolerant alloys.« less

Physical and Mechanical Properties of W-Ni-Fe-Co Metal Foam Modified by Titanium Tungsten Carbide Alloying

NASA Astrophysics Data System (ADS)

Ishchenko, A. N.; Tabachenko, A. N.; Afanas'eva, S. A.; Belov, N. N.; Biryukov, Yu. A.; Burkin, V. V.; D'yachkovskii, A. S.; Rogaev, K. S.; Skosyrskii, A. B.; Yugov, N. T.

2018-02-01

The paper studies physical and mechanical properties of tungsten-nickel-iron-cobalt metal foam alloyed with titanium tungsten carbide. Test specimens are obtained by the liquid phase sintering of powder materials, including those containing tungsten nanopowders. High porosity metal foams are prepared through varying the porosity of powder specimens and the content of filling material. The penetration capability of cylinder projectiles made of new alloys is explored in this paper. It is shown that their penetration depth exceeds that of the prototype with relevant weight and size, made of tungsten-nickel-iron alloy, other factors being equal.

Transmission electron microscopy characterization of microstructural features of Al-Li-Cu alloys

NASA Technical Reports Server (NTRS)

Avalos-Borja, M.; Pizzo, P. P.; Larson, L. A.

1983-01-01

A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitation events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significant alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

Transmission electron microscopy characterization of microstructural features in aluminum-lithium-copper alloys

NASA Technical Reports Server (NTRS)

Avalos-Borja, M.; Larson, L. A.; Pizzo, P. P.

1984-01-01

A transmission electron microscopy (TEM) examination of aluminum-lithium-copper alloys was conducted. The principal purpose is to characterize the nature, size, and distribution of stringer particles which result from the powder metallurgy (P/M) processing of these alloys. Microstructural features associated with the stringer particles are reported that help explain the stress corrosion susceptibility of the powder metallurgy-processed Al-Li-Cu alloys. In addition, matrix precipitaton events are documented for a variety of heat treatments and process variations. Hot rolling is observed to significantly alter the nature of matrix precipitation, and the observations are correlated with concomitant mechanical property variations.

Effects of Bi Addition on the Microstructure and Mechanical Properties of Nanocrystalline Ag Coatings

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

Wang, Yuxin; Cheng, Guang; Tay, See Leng

Here in this study we investigated the effects of Bi addition on the microstructure and mechanical properties of an electrodeposited nanocrystalline Ag coating. Microstructural features were investigated with transmission electron microscopy (TEM). The results indicate that the addition of Bi introduced nanometer-scale Ag-Bi solid solution particles and more internal defects to the initial Ag microstructures. The anisotropic elastic-plastic properties of the Ag nanocrystalline coating with and without Bi addition were examined with nanoindentation experiments in conjunction with the recently-developed inverse method. The results indicate that the as-deposited nanocrystalline Ag coating contained high mechanical anisotropy. With the addition of 1 atomicmore » percent (at%) Bi, the anisotropy within Ag-Bi coating was very small, and yield strength of the nanocrystalline Ag-Bi alloy in both longitudinal and transverse directions were improved by over 100% compared to that of Ag. On the other hand, the strain-hardening exponent of Ag-Bi was reduced to 0.055 from the original 0.16 of the Ag coating. Furthermore, the addition of Bi only slightly increased the electrical resistivity of the Ag-Bi coating in comparison to Ag. Lastly, results of our study indicate that Bi addition is a promising method for improving the mechanical and physical performances of Ag coating for electrical contacts.« less

Effects of Bi Addition on the Microstructure and Mechanical Properties of Nanocrystalline Ag Coatings

DOE PAGES

Wang, Yuxin; Cheng, Guang; Tay, See Leng; ...

2017-08-10

Here in this study we investigated the effects of Bi addition on the microstructure and mechanical properties of an electrodeposited nanocrystalline Ag coating. Microstructural features were investigated with transmission electron microscopy (TEM). The results indicate that the addition of Bi introduced nanometer-scale Ag-Bi solid solution particles and more internal defects to the initial Ag microstructures. The anisotropic elastic-plastic properties of the Ag nanocrystalline coating with and without Bi addition were examined with nanoindentation experiments in conjunction with the recently-developed inverse method. The results indicate that the as-deposited nanocrystalline Ag coating contained high mechanical anisotropy. With the addition of 1 atomicmore » percent (at%) Bi, the anisotropy within Ag-Bi coating was very small, and yield strength of the nanocrystalline Ag-Bi alloy in both longitudinal and transverse directions were improved by over 100% compared to that of Ag. On the other hand, the strain-hardening exponent of Ag-Bi was reduced to 0.055 from the original 0.16 of the Ag coating. Furthermore, the addition of Bi only slightly increased the electrical resistivity of the Ag-Bi coating in comparison to Ag. Lastly, results of our study indicate that Bi addition is a promising method for improving the mechanical and physical performances of Ag coating for electrical contacts.« less

High-strength, creep-resistant molybdenum alloy and process for producing the same

DOEpatents

Bianco, R.; Buckman, R.W. Jr.; Geller, C.B.

1999-02-09

A wet-doping process for producing an oxide-dispersion strengthened (ODS), creep-resistant molybdenum alloy is disclosed. The alloy is made by adding nitrate or acetate salts of lanthanum, cerium, thorium, or yttrium to molybdenum oxide to produce a slurry, heating the slurry in a hydrogen atmosphere to produce a powder, mixing and cold isostatically pressing the powder, sintering in a hydrogen atmosphere, and thermomechanically processing (swaging, extruding, cold drawing) the product. The ODS molybdenum alloy produced by the process contains 2--4% by volume (ca. 1--4% by weight) of an oxide of lanthanum, cerium, thorium, or yttrium. The alloy has high strength and improved creep-resistance at temperatures greater than 0.55T{sub m} of molybdenum. 10 figs.

High-strength, creep-resistant molybdenum alloy and process for producing the same

DOEpatents

Bianco, Robert; Buckman, Jr., R. William; Geller, Clint B.

1999-01-01

A wet-doping process for producing an oxide-dispersion strengthened (ODS), creep-resistant molybdenum alloy is disclosed. The alloy is made by adding nitrate or acetate salts of lanthanum, cerium, thorium, or yttrium to molybdenum oxide to produce a slurry, heating the slurry in a hydrogen atmosphere to produce a powder, mixing and cold isostatically pressing the powder, sintering in a hydrogen atmosphere, and thermomechanically processing (swaging, extruding, cold drawing) the product. The ODS molybdenum alloy produced by the process contains 2-4% by volume (.about.1-4% by weight) of an oxide of lanthanum, cerium, thorium, or yttrium. The alloy has high strength and improved creep-resistance at temperatures greater than 0.55T.sub.m of molybdenum.

Comparison of different pressing techniques for the preparation of n-type silicon-germanium thermoelectric alloys

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

Harringa, J.L.; Cook, B.A.

1996-06-01

Improvements to state-of-the-art Si{sub 80}Ge{sub 20} thermoelectric alloys have been observed in laboratory-scale samples by the powder metallurgy techniques of mechanical alloying and hot pressing. Incorporating these improvements in large scale compacts for the production of thermoelectric generator elements is the next step in achieving higher efficiency RTGs. This paper discusses consolidation of large quantities of mechanically alloyed powders into production size compacts. Differences in thermoelectric properties are noted between the compacts prepared by the standard technique of hot uniaxial pressing and hot isostatic pressing. Most significant is the difference in carrier concentration between the alloys prepared by the twomore » consolidation techniques.« less

Thermogravimetric feasibility study of argon purification using powders of titanium alloys with molybdenum and vanadium

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

Eremeev, A.P.; Veselovskii, P.F.

1987-10-20

The high adsorption and chemical activity of titanium alloy powders (TiMo > TiV) having specific size and chemical compositions, and the nature of the surface and its specific energy characteristics permit one to use them effectively for the purification of argon and other inert gases from impurities such as water vapor, carbon dioxide gas, oxygen, and nitrogen. In agreement with the developed activity series the irreversible adsorption of impurities (1 vol. %) by the indicated powders can be controlled using powders or filters pressed from these powders by heating to temperatures of 500-700/sup 0/. The thickness of the filters canmore » be established on the basis of the rate constants of the chemical reactions of the impurities with the TiMo and TiV powders obtained in this study.« less

Development and characterization of Powder Metallurgy (PM) 2XXX series Al alloy products and Metal Matrix Composite (MMC) 2XXX Al/SiC materials for high temperature aircraft structural applications

NASA Technical Reports Server (NTRS)

Chellman, D. J.; Gurganus, T. B.; Walker, J. A.

1992-01-01

The results of a series of material studies performed by the Lockheed Aeronautical Systems Company over the time period from 1980 to 1991 are discussed. The technical objective of these evaluations was to develop and characterize advanced aluminum alloy materials with temperature capabilities extending to 350 F. An overview is given of the first five alloy development efforts under this contract. Prior work conducted during the first five modifications of the alloy development program are listed. Recent developments based on the addition of high Zr levels to an optimum Al-Cu-Mg alloy composition by powder metallurgy processing are discussed. Both reinforced and SiC or B4C ceramic reinforced alloys were explored to achieve specific target goals for high temperature aluminum alloy applications.

Properties and rapid low-temperature consolidation of nanocrystalline Fe-ZrO2 composite by pulsed current activated sintering

NASA Astrophysics Data System (ADS)

Kang, Hyun-Su; Ko, In-Yong; Yoon, Jin-Kook; Doh, Jung-Mann; Hong, Kyung-Tae; Shon, In-Jin

2011-02-01

Nanopowders of Fe and ZrO2 were synthesized from Fe2O3 and Zr by high-energy ball milling. The powder sizes of Fe and ZrO2 were 70 nm and 12 nm, respectively. Highly dense nanostructured 4/3Fe-ZrO2 composite was consolidated by a pulsed current activated sintering method within 1 minute from the mechanically synthesized powders (Fe-ZrO2) and horizontal milled Fe2O3+Zr powders under the 1 GPa pressure. The grain sizes of Fe and ZrO2 in the composite were calculated. The average hardness and fracture toughness values of nanostuctured 4/3Fe-ZrO2 composite were investigated.

Phase composition and microstructure of WC-Co alloys obtained by selective laser melting

NASA Astrophysics Data System (ADS)

Khmyrov, Roman S.; Shevchukov, Alexandr P.; Gusarov, Andrey V.; Tarasova, Tatyana V.

2018-03-01

Phase composition and microstructure of initial WC, BK8 (powder alloy 92 wt.% WC-8 wt.% Co), Co powders, ball-milled powders with four different compositions (1) 25 wt.% WC-75 wt.% Co, (2) 30 wt.% BK8-70 wt.% Co, (3) 50 wt.% WC-50 wt.% Co, (4) 94 wt.% WC-6 wt.% Co, and bulk alloys obtained by selective laser melting (SLM) from as-milled powders in as-melted state and after heat treatment were investigated by scanning electron microscopy and X-ray diffraction analysis. Initial and ball-milled powders consist of WC, hexagonal α-Co and face-centered cubic β-Co. The SLM leads to the formation of major new phases W3Co3C, W4Co2C and face-centered cubic β-Co-based solid solution. During the heat treatment, there occurs partial decomposition of the face-centered cubic β-Co-based solid solution with the formation of W2C and hexagonal α-Co solid solution. The microstructure of obtained bulk samples, in general, corresponds to the observed phase composition.

Synthesis of Nano-Polycrystalline Synroc-B Powders as a High Level Radioactive Wastes Ceramic Forms by a Solution Combustion Synthesis.

PubMed

Han, Young-Min; Lee, Sang-Jin; Kim, Yeon-Ku; Jung, Choong-Hwan

2016-02-01

Synroc (Synthetic Rock) consists of four main titanate phases: peroveskite (CaTiO3), zirconolite (CaZrTi2O7), hollandite (BaAl2Ti6O16) and rutile (TiO2). Nano-polycrystalline synroc powders were made by a synthesis combustion process. The combustion process, an externally initiated reaction is self-sustained owing to the exothermic reaction. A significant volume of gas is evolved during the combustion reaction and leads to loosely agglomerated powders. This exothermic reaction provides necessary heat to further carry the reaction in forward direction to produce nanocrystalline powders as the final product. Glycine is used as a fuel, being oxidized by nitrate ions. It is inexpensive, has high energy efficiency, fast heating rates, short reaction times and high compositional homogeneity. In this study, combustion synthesis of nano-sized synroc-B powder is introduced. The fabrication of synroc-B powder result of observation XRD were prepared for polycrystalline (perovskite, zirconolite, hollandite, rutile) structures. The characterization of the synthesized powders is conducted by using XRD, SEM/EDS and TEM.

Microscale mechanical characterization of materials for extreme environments

NASA Astrophysics Data System (ADS)

Ozerinc, Sezer

Nanocrystalline metals are promising materials for applications that require outstanding strength and stability in extreme environments. Further improvements in the desirable mechanical properties of these materials require a better understanding of the relationship between their microstructure and grain boundary deformation behavior. Previous molecular dynamics simulations suggested that solute additions to grain boundaries can enhance the strength of nanocrystalline metals, but there has been a lack of experimental studies investigating this prediction. This dissertation presents mechanical and microstructural characterization of nanocrystalline Cu alloys and demonstrate that addition of Nb solutes to grain boundaries greatly enhances the strength of Cu. The measured hardness of Cu90Nb10 alloy is 5.6 GPa which is more than double the hardness of nanocrystalline pure Cu. Microstructural characterization through transmission electron microscopy and energy-dispersive X-ray spectroscopy on these alloys indicates a strong correlation between the grain boundary composition and the hardness. Variation of measured hardness with measured grain boundary composition is in very good agreement with previous molecular dynamics simulation predictions. The results of this work provide experimental evidence that grain boundary doping enhances the strength of nanocrystalline Cu far beyond that predicted by classical Hall-Petch strengthening and decreasing grain boundary energy through solute additions is the key to reaching theoretical strength in nanocrystalline metals. Irradiation induced creep is a deformation mechanism that takes place under combined stress and particle bombardment. Effective characterization of this phenomenon on nanostructured materials is crucial for the assessment of their potential use in next generation nuclear power plants. Direct measurements of irradiation induced creep under MeV-heavy ion bombardment have not been feasible until recently due to the requirements of micron-sized specimens, muN-level force sensitivity, and nm-level displacement sensitivity. A recently developed mechanical characterization technique, micropillar compression, has enabled the testing of miniaturized specimens; however, there has been no demonstration of the application of this technique to irradiation induced creep measurements. This dissertation presents the development of an in situ measurement apparatus for compression testing of micron-sized cylindrical specimens under MeV-heavy ion bombardment. The apparatus has a force resolution of 1 muN and a displacement resolution of 1 nm. The apparatus measured irradiation induced creep in four different amorphous materials and the findings clarified the significance of different creep mechanisms in these materials. In amorphous metals and amorphous Si, the measured irradiation induced fluidity is ≈ 3 dpa-1GPa-1 (dpa: displacements per atom). The measured fluidity is in excellent agreement with previous molecular dynamics simulation predictions, providing experimental evidence for point defect mediated plastic flow under ion bombardment. For amorphous SiO2, stress relaxation through thermal spikes further contribute to the creep response, resulting in higher fluidities up to ≈ 83 dpa-1GPa -1. Finally, this dissertation presents the further development of the creep testing apparatus for high temperature measurements. The apparatus demonstrated good thermal and mechanical stability and measured irradiation induced creep of nanocrystalline Cu at 200°C. Resulting irradiation induced fluidity is ≈ 10% of the fluidity of the amorphous metals, in agreement with previous measurements on free-standing films. Understanding the creep behavior of nanostructured metals under heavy ion bombardment at elevated temperatures is important for identifying the governing creep mechanisms in these materials. The developed apparatus provides a new and effective method of accelerated mechanical characterization of such promising materials for their potential use in future nuclear applications.

Effects of surface crystallization and oxidation in nanocrystalline FeNbCuSiB(P) ribbons

NASA Astrophysics Data System (ADS)

Butvinová, B.; Butvin, P.; Brzózka, K.; Kuzminski, M.; Maťko, I.; Švec, P., Sr.; Chromčíková, M.

2017-02-01

Si-poor Fe74Nb3Cu1Si8B14-xPx, (x=0, 3) nanocrystalline ribbon-form alloys often form surfaces, which exert in-plane force on underlying ribbon interior when nanocrystallized in even modest presence of oxygen. Mostly unwanted hard-ribbon-axis magnetic anisotropy is standard result. Essential sources of the surface-caused stress have been sought and influence of P instead of B substitution on this effect was studied too. Preferred surface crystallization (PSC) was found to be the major reason. However P substitution suppresses PSC and promotes Fe-oxide formation, which eases the stress, softens the surfaces and provides different annealing evolution of surface properties.

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.

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.

Development of casting investment preventing blackening of noble metal alloys part 1. Application of developed investment for Ag-Pd-Cu-Au alloy.

PubMed

Kakuta, Kiyoshi; Nakai, Akira; Goto, Shin-ichi; Wakamatsu, Yasushi; Yara, Atushi; Miyagawa, Yukio; Ogura, Hideo

2003-03-01

The objective of this study is to develop a casting investment that prevents the blackening of the cast surface of noble metal alloys. The experimental investments were prepared using a gypsum-bonded investment in which the metallic powders such as boron (B), silicon (Si), aluminum (Al) and titanium (Ti) were added as oxidizing agents. An Ag-Pd-Cu-Au alloy was cast into the mold made of the prepared investment. The effect of the addition of each metal powder was evaluated from the color difference between the as-cast surface and the polished surface of the cast specimen. The color of the as-cast surface approached that of the polished surface with increasing B and Al content. A lower mean value in the color difference was obtained at 0.25-1.00 mass% B content. B and Al are useful as an additive in a gypsum-bonded investment to prevent the blackening of an Ag-Pd-Cu-Au alloy. The effects of Si and Ti powder addition could not be found.

Grain Growth in Nanocrystalline Mg-Al Thin Films

NASA Astrophysics Data System (ADS)

Kruska, Karen; Rohatgi, Aashish; Vemuri, Rama S.; Kovarik, Libor; Moser, Trevor H.; Evans, James E.; Browning, Nigel D.

2017-12-01

An improved understanding of grain growth kinetics in nanocrystalline materials, and in metals and alloys in general, is of continuing interest to the scientific community. In this study, Mg-Al thin films containing 10 wt pct Al and with 14.5 nm average grain size were produced by magnetron sputtering and subjected to heat treatments. The grain growth evolution in the early stages of heat treatment at 423 K, 473 K, and 573 K (150 °C, 200 °C, and 300 °C) was observed with transmission electron microscopy and analyzed based upon the classical equation developed by Burke and Turnbull. The grain growth exponent was found to be 7 ± 2 and the activation energy for grain growth was 31.1 ± 13.4 kJ/mol, the latter being significantly lower than in bulk Mg-Al alloys. The observed grain growth kinetics are explained by the Al supersaturation in the matrix and the pinning effects of the rapidly forming beta precipitates and possibly shallow grain boundary grooves. The low activation energy is attributed to the rapid surface diffusion which is dominant in thin film systems.

Nanocrystalline diamond protects Zr cladding surface against oxygen and hydrogen uptake: Nuclear fuel durability enhancement.

PubMed

Škarohlíd, Jan; Ashcheulov, Petr; Škoda, Radek; Taylor, Andrew; Čtvrtlík, Radim; Tomáštík, Jan; Fendrych, František; Kopeček, Jaromír; Cháb, Vladimír; Cichoň, Stanislav; Sajdl, Petr; Macák, Jan; Xu, Peng; Partezana, Jonna M; Lorinčík, Jan; Prehradná, Jana; Steinbrück, Martin; Kratochvílová, Irena

2017-07-25

In this work, we demonstrate and describe an effective method of protecting zirconium fuel cladding against oxygen and hydrogen uptake at both accident and working temperatures in water-cooled nuclear reactor environments. Zr alloy samples were coated with nanocrystalline diamond (NCD) layers of different thicknesses, grown in a microwave plasma chemical vapor deposition apparatus. In addition to showing that such an NCD layer prevents the Zr alloy from directly interacting with water, we show that carbon released from the NCD film enters the underlying Zr material and changes its properties, such that uptake of oxygen and hydrogen is significantly decreased. After 100-170 days of exposure to hot water at 360 °C, the oxidation of the NCD-coated Zr plates was typically decreased by 40%. Protective NCD layers may prolong the lifetime of nuclear cladding and consequently enhance nuclear fuel burnup. NCD may also serve as a passive element for nuclear safety. NCD-coated ZIRLO claddings have been selected as a candidate for Accident Tolerant Fuel in commercially operated reactors in 2020.

Surface nanocrystalline and hardening effects of Ti-Al-V alloy by electropulsing ultrasonic shock

NASA Astrophysics Data System (ADS)

Ye, Xiaoxin

2015-04-01

The effect of electropulsing ultrasonic shock (EUS) on the surface hardening and microstructure of Ti6Al4V alloy was studied. It was found that electropulsing improved the microhardness dramatically both in the influential depth and maximum value, compared with the only ultrasonic-shocked sample. It's indicated that refined surface layer with nanocrystalline and improved microhardness were obtained on account of surface severe plastic deformation, dynamic recrystallization (DRX) and phase change, which was implemented at relative low temperature and high strain rate/capacity due to the coupling of the thermal and athermal effects of EUS. It's different from conventional experiments and theory. It's discussed that the positive contributions of EPT in the thermodynamics and kinetics of microstructure and properties change were attributed to the reduction of nucleation energy barrier and acceleration of atomic diffusion. Therefore, it's supposed that EUS is an energy-saving and high-efficiency method of surface treatment technique with the help of high-energy electropulses, which is promising in cost reduction of the surface engineering and energy management.

[Influence of different sol-gel system on the luminescence of nanocrystalline ZnO powder].

PubMed

Guo, Shu-xia; Zhang, Xing-tang; Zhang, Zhong-suo; Zhao, Hui-ling; Li, Yun-cai; Huang, Ya-bin; Du, Zu-liang

2005-08-01

ZnO nanopowders were prepared by the sol-gel techniques with two kinds of solvent. Microstructure of powder samples was examined by XRD and TEM. The results indicate that the two ZnO samples have the same crystal and energy band structure. Their photoluminescence (PL) spectra in ultraviolet region are analogous, but their photoluminescence (PL) spectra in visible region are different. The reason is that the two kinds of solvent with different polarity result in the difference in configuration and distribution of the sample surface states in the two systems.

Structural transformations, strengthening, and wear resistance of titanium nickelide upon abrasive and adhesive wear

NASA Astrophysics Data System (ADS)

Korshunov, L. G.; Pushin, V. G.; Chernenko, N. L.; Makarov, V. V.

2010-07-01

Wear resistance and structural transformations upon abrasive and adhesive wear of titanium nickelide Ti49.4Ni50.6 in microcrystalline (MC) and submicrocrystalline (SMC) states have been investigated. It has been shown that the abrasive wear resistance of this alloy exceeds that of the steel 12Kh18N9 by a factor of about 2, that of the steel 110G13 (Hadfield steel), by a factor of 1.3, and is close to that of the steel 95Kh18. Upon adhesive wear in a testing-temperature range from -50 to +300°C, the Ti49.4Ni50.6 alloy, as compared to the steel 12Kh18N9, is characterized by the wear rate that is tens of times smaller and by a reduced (1.5-2.0 times) friction coefficient. The enhanced wear resistance of the Ti49.4Ni50.6 alloy is due to the development of intense strain hardening in it and to a high fracture toughness, which is a consequence of effective relaxation of high contact stresses arising in the surface layer of the alloy. The SMC state produced in the alloy with the help of equal-channel angular pressing (ECAP) has no effect on the abrasive wear resistance of the alloy. The favorable effect of ECAP on the wear resistance of the Ti49.4Ni50.6 alloy takes place under conditions of its adhesive wear at temperatures from -25 to +70°C. The electron-microscopic investigation showed that under conditions of wear at negative and room temperatures in the surface layer (1-5 μm thick) of titanium nickelide there arises a mixed structure consisting of an amorphous phase and nanocrystals of supposedly austenite and martensite. Upon friction at 200-300°C, a nanocrystalline structure of the B2 phase arises near the alloy surface, which, as is the case with the amorphous-nanocrystalline structure, is characterized by significant effective strength and wear resistance.

Development of a Tabletop Model for the Generation of Amorphous/ Microcrystalline Metal Powders

DTIC Science & Technology

1980-04-30

Voltage Characteristics for Wetting (si) and Non-wetting (AZ 4.5% Cu ) EHD Spray 2-57 28 Schematic of the Process of Electrohydrodynamic Droplet...Microscope Image of a Deposit , Fine Powders and "Matrix" Film of Fe-Ni-B-P Metallic Glass Alloy Produced by the EHD Technique 3-9 45 Selected Area...Transmission Electron Microscope Image of a Deposit , Fine Powders and "Matrix" Film of Fe-Ni-B-P Metallic Glass Alloy Produced by the EHD Technique 3-11 xi

Method for forming biaxially textured articles by powder metallurgy

DOEpatents

Goyal, Amit; Williams, Robert K.; Kroeger, Donald M.

2002-01-01

A method of preparing a biaxially textured alloy article comprises the steps of preparing a mixture comprising Ni powder and at least one powder selected from the group consisting of Cr, W, V, Mo, Cu, Al, Ce, YSZ, Y, Rare Earths, (RE), MgO, CeO.sub.2, and Y.sub.2 O.sub.3 ; compacting the mixture, followed by heat treating and rapidly recrystallizing to produce a biaxial texture on the article. In some embodiments the alloy article further comprises electromagnetic or electro-optical devices and possesses superconducting properties.

Discussion on the application of high additional value of high purity and high quality direct reduced iron

NASA Astrophysics Data System (ADS)

Yue, Chongfeng; Bai, Lu; Hong, Yicheng; Xu, Lijun

2018-03-01

The high purity and high quality direct reduced iron(DRI) products which were produced by high grade and high quality iron powder, with a high grade and low impurity characteristics. This article introduced the application of high purity and high quality DRI in the fields of amorphous base material, atomized iron powder, powder superalloy, high purity and ultra-low carbon special metallurgy products, precision casting, super alloy and various iron-based alloys. It provides a reference for the high added value utilization of DRI.

FABRICATION OF URANIUM-ALUMINUM ALLOYS

DOEpatents

Saller, H.A.

1959-12-15

A process is presented for producing a workable article of a uranium- aluminum alloy in which the uranium content is between 14 and 70% by weight; aluminum powder and powdered UAl/sub 2/, UAl/sub 3/, UAl/sub 5/, or UBe/sub 9/ are mixed, and the mixture is compressed into the shape desired and sintered at between 450 and 600 deg C.

Line profile analysis of ODS steels Fe20Cr5AlTiY milled powders at different Y2O3 concentrations

NASA Astrophysics Data System (ADS)

Afandi, A.; Nisa, R.; Thosin, K. A. Z.

2017-04-01

Mechanical properties of material are largely dictated by constituent microstructure parameters such as dislocation density, lattice microstrain, crystallite size and its distribution. To develop ultra-fine grain alloys such as Oxide Dispersion Strengthened (ODS) alloys, mechanical alloying is crucial step to introduce crystal defects, and refining the crystallite size. In this research the ODS sample powders were mechanically alloyed with different Y2O3 concentration respectively of 0.5, 1, 3, and 5 wt%. MA process was conducted with High Energy Milling (HEM) with the ball to powder ratio of 15:1. The vial and the ball were made of alumina, and the milling condition is set 200 r.p.m constant. The ODS powders were investigated by X-Ray Diffractions (XRD), Bragg-Brentano setup of SmartLab Rigaku with 40 KV, and 30 mA, step size using 0.02°, with scanning speed of 4°min-1. Line Profile Analysis (LPA) of classical Williamson-Hall was carried out, with the aim to investigate the different crystallite size, and microstrain due to the selection of the full wide at half maximum (FWHM) and integral breadth.

Hot Corrosion Behavior of Bare, Cr3C2-(NiCr) and Cr3C2-(NiCr) + 0.2wt.%Zr Coated SuperNi 718 at 900 °C

NASA Astrophysics Data System (ADS)

Mudgal, Deepa; Singh, Surendra; Prakash, Satya

2015-01-01

Corrosion in incinerators, power plants, and chemical industries are frequently encountered due to the presence of salts containing sodium, sulphur, and chlorine. To obviate this problem, bare and coated alloys were tested under environments simulating the conditions present inside incinerators and power plants. 0.2 wt.% zirconium powder was incorporated in the Cr3C2-(NiCr) coating powder. The original powder and Zr containing powder was sprayed on Superni 718 alloy by D-gun technique. The bare and coated alloys were tested under Na2SO4 + K2SO4 + NaCl + KCl and Na2SO4 + NaCl environment. The corrosion rate of specimens was monitored using weight change measurements. Characterization of the corrosion products has been done using FE-SEM/EDS and XRD techniques. Bare and coated alloys showed very good corrosion resistance under given molten salt environments. Addition of 0.2wt.%Zr in Cr3C2-25%(NiCr) coating further greatly reduced the oxidation rate as well as improved the adherence of oxide scale to the coating surface during the time of corrosion.

Process for alloying uranium and niobium

DOEpatents

Holcombe, Cressie E.; Northcutt, Jr., Walter G.; Masters, David R.; Chapman, Lloyd R.

1991-01-01

Alloys such as U-6Nb are prepared by forming a stacked sandwich array of uraniun sheets and niobium powder disposed in layers between the sheets, heating the array in a vacuum induction melting furnace to a temperature such as to melt the uranium, holding the resulting mixture at a temperature above the melting point of uranium until the niobium dissolves in the uranium, and casting the uranium-niobium solution. Compositional uniformity in the alloy product is enabled by use of the sandwich structure of uranium sheets and niobium powder.

Bioaccessibility of micron-sized powder particles of molybdenum metal, iron metal, molybdenum oxides and ferromolybdenum--Importance of surface oxides.

PubMed

Mörsdorf, Alexander; Odnevall Wallinder, Inger; Hedberg, Yolanda

2015-08-01

The European chemical framework REACH requires that hazards and risks posed by chemicals, including alloys and metals, that are manufactured, imported or used in different products (substances or articles) are identified and proven safe for humans and the environment. Metals and alloys need hence to be investigated on their extent of released metals (bioaccessibility) in biologically relevant environments. Read-across from available studies may be used for similar materials. This study investigates the release of molybdenum and iron from powder particles of molybdenum metal (Mo), a ferromolybdenum alloy (FeMo), an iron metal powder (Fe), MoO2, and MoO3 in different synthetic body fluids of pH ranging from 1.5 to 7.4 and of different composition. Spectroscopic tools and cyclic voltammetry have been employed to characterize surface oxides, microscopy, light scattering and nitrogen absorption for particle characterization, and atomic absorption spectroscopy to quantify released amounts of metals. The release of molybdenum from the Mo powder generally increased with pH and was influenced by the fluid composition. The mixed iron and molybdenum surface oxide of the FeMo powder acted as a barrier both at acidic and weakly alkaline conditions. These findings underline the importance of the surface oxide characteristics for the bioaccessibility of metal alloys. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

Benefits of rapid solidification processing of modified LaNi{sub 5} alloys by high pressure gas atomization for battery applications

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

Anderson, I.E.; Pecharsky, V.K.; Ting, J.

1997-12-31

A high pressure gas atomization approach to rapid solidification has been employed to investigate simplified processing of Sn modified LaNi{sub 5} powders that can be used for advanced Ni/metal hydride (Ni/MH) batteries. The current industrial practice involves casting large ingots followed by annealing and grinding and utilizes a complex and costly alloy design. This investigation is an attempt to produce powders for battery cathode fabrication that can be used in an as-atomized condition without annealing or grinding. Both Ar and He atomization gas were tried to investigate rapid solidification effects. Sn alloy additions were tested to promote subambient pressure absorption/desorptionmore » of hydrogen at ambient temperature. The resulting fine, spherical powders were subject to microstructural analysis, hydrogen gas cycling, and annealing experiments to evaluate suitability for Ni/MH battery applications. The results demonstrate that a brief anneal is required to homogenize the as-solidified microstructure of both Ar and He atomized powders and to achieve a suitable hydrogen absorption behavior. The Sn addition also appears to suppress cracking during hydrogen gas phase cycling in particles smaller than about 25 {micro}m. These results suggest that direct powder processing of a LaNi{sub 5{minus}x}Sn{sub x} alloy has potential application in rechargeable Ni/MH batteries.« less

Benefits of rapid solidification processing of modified LaNi{sub 5} alloys by high pressure gas atomization for battery applications

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

Anderson, I.E.; Pecharsky, V.K.; Ting, J.

1998-07-01

A high pressure gas atomization approach to rapid solidification has been employed to investigate simplified processing of Sn modified LaNi{sub 5} powders that can be used for advanced Ni/metal hydride (Ni/MH) batteries. The current industrial practice involves casting large ingots followed by annealing and grinding and utilizes a complex and costly alloy design. This investigation is an attempt to produce powders for battery cathode fabrication that can be used in an as-atomized condition without annealing or grinding. Both Ar and He atomization gas were tried to investigate rapid solidification effects. Sn alloy additions were tested to promote subambient pressure absorption/desorptionmore » of hydrogen at ambient temperature. The resulting fine, spherical powders were subject to microstructural analysis, hydrogen gas cycling, and annealing experiments to evaluate suitability for Ni/MH battery applications. The results demonstrate that a brief anneal is required to homogenize the as-solidified microstructure of both Ar and He atomized powders and to achieve a suitable hydrogen absorption behavior. The Sn addition also appears to suppress cracking during hydrogen gas phase cycling in particles smaller than about 25{micro}m. These results suggest that direct powder processing of a LaNi{sub 5{minus}x}Sn{sub x} alloy has potential application in rechargeable Ni/MH batteries.« less

Apparatus for making environmentally stable reactive alloy powders

DOEpatents

Anderson, I.E.; Lograsso, B.K.; Terpstra, R.L.

1996-12-31

Apparatus and method are disclosed for making powder from a metallic melt by atomizing the melt to form droplets and reacting the droplets downstream of the atomizing location with a reactive gas. The droplets are reacted with the gas at a temperature where a solidified exterior surface is formed thereon and where a protective refractory barrier layer (reaction layer) is formed whose penetration into the droplets is limited by the presence of the solidified surface so as to avoid selective reduction of key reactive alloyants needed to achieve desired powder end use properties. The barrier layer protects the reactive powder particles from environmental constituents such as air and water in the liquid or vapor form during subsequent fabrication of the powder to end-use shapes and during use in the intended service environment. 7 figs.

Stress-corrosion behavior of aluminum-lithium alloys in aqueous salt environments

NASA Technical Reports Server (NTRS)

Pizzo, P. P.; Galvin, R. P.; Nelson, H. G.

1984-01-01

The stress corrosion susceptibility of two powder metallurgy (P/M) alloys, Al-Li-Cu and Al-Li-Cu-Mg; two mechanically attrited (M/A) alloys, Al-Li-Cu and Al-Li-Mg; and two wrought, ingot alloys, X-2020 and AA7475, are compared. Time-dependent fracture in an aqueous sodium chloride environment under alternate immersion condition was found to vary significantly between alloys. The stress corrosion behavior of the two powder metallurgy processed alloys was studied in detail under conditions of crack initiation, static crack growth, and fatigue crack growth. A variety of stress corrosion tests were performed including smooth surface, time-to-failure tests; potentiostatic tests on smooth surfaces exposed to constant applied strain rates; and fracture mechanics-type tests under static and cyclic loads. Both alloys show surface pitting and subsequent intergranular corrosion. Pitting is more severe in the magnesium-bearing alloy and is associated with stringer particles strung along the extrusion direction as a result of P/M processing.

Stress-corrosion behavior of aluminum-lithium alloys in aqueous environments

NASA Technical Reports Server (NTRS)

Pizzo, P. P.; Galvin, R. P.; Nelson, H. G.

1983-01-01

The stress corrosion susceptibility of two powder metallurgy (P/M) alloys, Al-Li-Cu and Al-Li-Cu-Mg two mechanically attrited (M/A) alloys, Al-Li-Cu and Al-Li-Mg; and two wrought, ingot alloys, X-2020 and AA7475, are compared. Time-dependent fracture in an aqueous sodium chloride environment under alternate immersion condition was found to vary significantly between alloys. The stress corrosion behavior of the two powder metallurgy processed alloys was studied in detail under conditions of crack initiation, static crack growth, and fatigue crack growth. A variety of stress corrosion tests were performed including smooth surface, time-to-failure tests; potentiostatic tests on smooth surfaces exposed to constant applied strain rates; and fracture mechanics-type tests under static and cyclic loads. Both alloys show surface pitting and subsequent intergranular corrosion. Pitting is more severe in the magnesium-bearing alloy and is associated with stringer particles strung along the extrusion direction as a result of P/M processing.

Grain boundary phase transformations in PtAu and relevance to thermal stabilization of bulk nanocrystalline metals

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

O’Brien, C. J.; Barr, C. M.; Price, P. M.

There has recently been a great deal of interest in employing immiscible solutes to stabilize nanocrystalline microstructures. Existing modeling efforts largely rely on mesoscale Monte Carlo approaches that employ a simplified model of the microstructure and result in highly homogeneous segregation to grain boundaries. However, there is ample evidence from experimental and modeling studies that demonstrates segregation to grain boundaries is highly non-uniform and sensitive to boundary character. This work employs a realistic nanocrystalline microstructure with experimentally relevant global solute concentrations to illustrate inhomogeneous boundary segregation. Furthermore, experiments quantifying segregation in thin films are reported that corroborate the prediction thatmore » grain boundary segregation is highly inhomogeneous. In addition to grain boundary structure modifying the degree of segregation, the existence of a phase transformation between low and high solute content grain boundaries is predicted. In order to conduct this study, new embedded atom method interatomic potentials are developed for Pt, Au, and the PtAu binary alloy.« less

Grain boundary phase transformations in PtAu and relevance to thermal stabilization of bulk nanocrystalline metals

DOE PAGES

O’Brien, C. J.; Barr, C. M.; Price, P. M.; ...

2017-10-31

There has recently been a great deal of interest in employing immiscible solutes to stabilize nanocrystalline microstructures. Existing modeling efforts largely rely on mesoscale Monte Carlo approaches that employ a simplified model of the microstructure and result in highly homogeneous segregation to grain boundaries. However, there is ample evidence from experimental and modeling studies that demonstrates segregation to grain boundaries is highly non-uniform and sensitive to boundary character. This work employs a realistic nanocrystalline microstructure with experimentally relevant global solute concentrations to illustrate inhomogeneous boundary segregation. Furthermore, experiments quantifying segregation in thin films are reported that corroborate the prediction thatmore » grain boundary segregation is highly inhomogeneous. In addition to grain boundary structure modifying the degree of segregation, the existence of a phase transformation between low and high solute content grain boundaries is predicted. In order to conduct this study, new embedded atom method interatomic potentials are developed for Pt, Au, and the PtAu binary alloy.« less

Beating Homogeneous Nucleation and Tuning Atomic Ordering in Glass-Forming Metals by Nanocalorimetry.

PubMed

Zhao, Bingge; Yang, Bin; Abyzov, Alexander S; Schmelzer, Jürn W P; Rodríguez-Viejo, Javier; Zhai, Qijie; Schick, Christoph; Gao, Yulai

2017-12-13

In this paper, the amorphous Ce 68 Al 10 Cu 20 Co 2 (atom %) alloy was in situ prepared by nanocalorimetry. The high cooling and heating rates accessible with this technique facilitate the suppression of crystallization on cooling and the identification of homogeneous nucleation. Different from the generally accepted notion that metallic glasses form just by avoiding crystallization, the role of nucleation and growth in the crystallization behavior of amorphous alloys is specified, allowing an access to the ideal metallic glass free of nuclei. Local atomic configurations are fundamentally significant to unravel the glass forming ability (GFA) and phase transitions in metallic glasses. For this reason, isothermal annealing near T g from 0.001 s to 25,000 s following quenching becomes the strategy to tune local atomic configurations and facilitate an amorphous alloy, a mixed glassy-nanocrystalline state, and a crystalline sample successively. On the basis of the evolution of crystallization enthalpy and overall latent heat on reheating, we quantify the underlying mechanism for the isothermal nucleation and crystallization of amorphous alloys. With Johnson-Mehl-Avrami method, it is demonstrated that the coexistence of homogeneous and heterogeneous nucleation contributes to the isothermal crystallization of glass. Heterogeneous rather than homogeneous nucleation dominates the isothermal crystallization of the undercooled liquid. For the mixed glassy-nanocrystalline structure, an extraordinary kinetic stability of the residual glass is validated, which is ascribed to the denser packed interface between amorphous phase and ordered nanocrystals. Tailoring the amorphous structure by nanocalorimetry permits new insights into unraveling GFA and the mechanism that correlates local atomic configurations and phase transitions in metallic glasses.

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

Mukhametkaliyev, T., E-mail: mtm91@mail.ru; Surmeneva, M., E-mail: feja-mari@yandex.ru; Surmenev, R., E-mail: rsurmenev@gmail.com

A thin film of hydroxyapatite (HA) was deposited on AZ31 and Mg-Ca alloys by using radio frequency (RF) magnetron sputtering. The thickness of the HA coating was determined to be 750 nm. The phase composition, microstructure, and surface morphology of the HA coatings were investigated using X-ray diffraction and scanning electron microscopy. In vitro degradation behaviour of the HA coated alloys was evaluated in simulated body fluid (SBF) and 3.5wt.% NaCl solution using electrochemical method. The coatings homogeneously covered the entire surface of the substrates. The coating structure corresponded to a nanostructured HA. The ultrathin coating significantly improved the degradationmore » resistance of the alloy. Nanocrystalline HA coating significantly improved the corrosion resistance of the Mg-Ca and AZ31 magnesium alloys. The polarization resistance (Rp) of the coated Mg-Ca alloy was more than two-order of magnitude higher and the corrosion current density I{sub corr} reduced by ∼ 98% as compared to the base alloy.« less

Structure and Mechanical and Corrosion Properties of a Magnesium Mg-Y-Nd-Zr Alloy after High Pressure Torsion

NASA Astrophysics Data System (ADS)

Lukyanova, E. A.; Martynenko, N. S.; Serebryany, V. N.; Belyakov, A. N.; Rokhlin, L. L.; Dobatkin, S. V.; Estrin, Yu. Z.

2017-11-01

The structure and the properties of an Mg-Y-Nd-Zr alloy (WE43) are studied after high pressure torsion (HPT) in the temperature range 20-300°C. Structure refinement proceeds mainly by deformation twinning with the formation of a partial nanocrystalline structure with a grain size of 30-100 nm inside deformation twins. The WE43 alloy is shown to be aged during heating after HPT due to the decomposition of a magnesium solid solution. HPT at room temperature and subsequent aging causes maximum hardening. It is shown that HPT significantly accelerates the decomposition of a magnesium solid solution. HPT at all temperatures considerably increases the tensile strength and the yield strength upon tensile tests and significantly decreases plasticity. Subsequent aging additionally hardens the WE43 alloy. A potentiodynamic study shows that the corrosion resistance of this alloy after HPT increases. However, subsequent aging degrades the corrosion properties of the alloy.

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.

Mechanical process for enhancing metal hydride for the anode of a Ni-MH secondary battery

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

Ikeya, T.; Kumai, K.; Iwahori, T.

1993-11-01

This study attempted to find a simpler method for modifying hydrogen storage alloys that are used as anodes in Ni-MH batteries to prolong their cycle life. The alloy was modified by mechanical grinding with cobalt metal powder. A short grinding time yielded samples with a higher discharge capacity and longer cycle life than those of the alloy which was mixed with the cobalt powder without the mechanical treatment. However, prolonged grinding caused a decrease in the discharge capacity because of amorphization of the alloy by mechanical stress. The authors believed the formation of a cobalt compound on the alloy surfacemore » plus closer contact between particle enhanced the cyclic durability and discharge capacity of metal hydride anodes.« less

Gas response properties of citrate gel synthesized nanocrystalline MgFe{sub 2}O{sub 4}: Effect of sintering temperature

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

Patil, J.Y.; Mulla, I.S.; Suryavanshi, S.S., E-mail: sssuryavanshi@rediffmail.com

2013-02-15

Graphical abstract: Display Omitted Highlights: ► Synthesis of nanocrystalline MgFe{sub 2}O{sub 4} by economical citrate gel combustion method. ► Structural, morphological, and gas response properties of MgFe{sub 2}O{sub 4}. ► Enhancement in selectivity of MgFe{sub 2}O{sub 4} towards LPG with sintering temperature. ► Use of MgFe{sub 2}O{sub 4} to detect different gases at different operating temperatures. -- Abstract: Spinel type MgFe{sub 2}O{sub 4} material was synthesized by citrate gel combustion method. The effect of sintering temperature on structural, morphological, and gas response properties was studied. The powder X-ray diffraction pattern and transmission electron microscope study confirms nanocrystalline spinel structure ofmore » the synthesized powder. The material was tested for response properties to various reducing gases like liquid petroleum gas (LPG), acetone, ethanol, and ammonia. The results demonstrated n-type semiconducting behavior of MgFe{sub 2}O{sub 4} material. It was revealed that MgFe{sub 2}O{sub 4} sintered at 973 K was most sensitive to LPG at 648 K and to acetone at 498 K. However MgFe{sub 2}O{sub 4} sintered at 1173 K exhibited higher response and selectivity to LPG with marginal increase in the operating temperature. Furthermore, the sensor exhibited a fast response and a good recovery. It was observed that the particles size, porosity, and surface activity of the sensor material is affected by the sintering temperature.« less

Mechanochemical stabilization and sintering of nanocrystalline the (ZrO2)0.97 (Y2O3)0.03 solid solution from pure oxides

NASA Astrophysics Data System (ADS)

Rendtorff, N. M.; Suárez, G.; Sakka, Y.; Aglietti, E. F.

2011-10-01

The mechanochemical activation processing has proved to be an effective technique to enhance a solid-state reaction at relatively low temperatures. In such a process, the mechanical effects of milling, such as reduction of particle size and mixture homogenization, are accompanied by chemical effects, such as partial decomposition of salts or hydroxides resulting in very active reactants. The objective of the present work is to obtain (ZrO2)0.97(Y2O3)0.03 nanocrystalline tetragonal solid solution powders directly using a high energy milling on a mixture of the pure oxides. A second objective is to evaluate the efficiency of the processing proposed and to characterize both textural and structural evolution of the mixtures during the milling processes and throughout posterior low temperature treatments. The Textural and structural evolution were studied by XRD analysis, specific area measurements (BET) and SEM. Firstly a decrease of the crystallinity of the reactants was observed, followed by the disappearance of Y2O3 diffraction peaks and the partial appearance of the tetragonal phase at room temperature. The solid solution proportion was increased with the high energy milling time, obtaining complete stabilization of the tetragonal solid solution with long milling treatments (60 min).The obtained powders were uniaxially pressed and sintered at different temperatures (600-1400°C) the influence of the milling time was correlated with the sinterization degree and final crystalline composition of the materials. Finally, fully stabilized nanocrystalline zirconia materials were obtained satisfactorily by the proposed method.

Structural characterization, electrical conductivity and open circuit voltage studies of the nanocrystalline La10Si6O27 electrolyte material for SOFCs

NASA Astrophysics Data System (ADS)

Jena, Paramananda; Jayasubramaniyan, S.; Patro, P. K.; Lenka, R. K.; Sinha, Amit; Muralidharan, P.; Srinadhu, E. S.; Satyanarayana, N.

2018-02-01

Nanocrystalline La10Si6O27 apatite-type sample was synthesized by the co-precipitation method. Thermal behavior, phase, structure, morphology and elemental composition of La, O and Si of the synthesized La10Si6O27 sample were investigated through TG/DTA, XRD, FTIR, Raman spectroscopy and SEM-EDX measurements respectively. Formation of phase purity of the nanocrystalline La10Si6O27 sample was confirmed by analysing the measured X-ray powder diffraction (XRD) pattern using Rietveld refinement and the calculated average crystallite size of the La10Si6O27 sample was found to be 33 nm. The electrical conductivity of the sintered La10Si6O27 pellet was investigated as a function of temperature ranging from 200 to 800 °C under air and it was found to be 1.92 × 10-3 S cm-1 at 800 °C. The chemical stability of La10Si6O27 powder under oxidizing and reducing atmospheres was confirmed from the analysis of the measured XRD pattern and Raman spectral results. Open circuit potential of a button cell, made up of the La10Si6O27 sample, was tested up to 800 °C with both oxygen and hydrogen at opposite sides of the cell and was found to 1 V. Hence, the results demonstrate that La10Si6O27 could be a promising solid electrolyte material for the solid oxide fuel cell (SOFC) applications.

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.

Process for manufacturing a lithium alloy electrochemical cell

DOEpatents

Bennett, William R.

1992-10-13

A process for manufacturing a lithium alloy, metal sulfide cell tape casts slurried alloy powders in an organic solvent containing a dissolved thermoplastic organic binder onto casting surfaces. The organic solvent is then evaporated to produce a flexible tape removable adhering to the casting surface. The tape is densified to increase its green strength and then peeled from the casting surface. The tape is laminated with a separator containing a lithium salt electrolyte and a metal sulfide electrode to form a green cell. The binder is evaporated from the green cell at a temperature lower than the melting temperature of the lithium salt electrolyte. Lithium alloy, metal sulfide and separator powders may be tape cast.

Microstructures and properties of rapidly solidified alloys

NASA Technical Reports Server (NTRS)

Shechtman, D.; Horowitz, E.

1984-01-01

The microstructure and properties of rapidly solidified aluminum alloys were researched. The effects of powder and flake chemistry and morphology and alternative consolidation processing parameters are being conducted. Samples of the powders being utilized were obtained for comprehensive metallurgical characterization. Seven aluminum alloys in the form of thin foils were studied by a variety of techniques including optical metallography, scanning electron microscope, and transmission electron microscope. Details of the microstructural characteristics are presented along with a discussion of the solidification process. A better understanding of the microstructure of the rapidly solidified aluminum alloys prepared by a variety of techniques such as roller quenching, the vacuum atomized procedure, ultrasonically atomized in inert atmospheres, and atomized in flue gas was provided.