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At least 397 records · Page 22

Solid Phase Gradient Alloying Method via ShAPE

Alloying has been used to confer desirable properties to various metallic systems since the bronze age. For example, Ni, Mn, and Cr are alloyed into an Fe matrix to make steel, which has improved strength and corrosion resistance (as displayed in Fig. 1). In addition to the type of alloying elements, the amount of alloying elements added into a matrix is also very critical for a material’s mechanical property, physical property, machinability, and cost. Conventionally, new alloys are discovered by combining alloy precursors and elemental constituents into a mixture and melting them together. The solidified product or ingot represents a usually non-homogeneous combination of the chemistry with a microstructure dictated by the physics of solidification. It is time and energy intensive to optimize the alloying amounts via the casting process and hence, economically not conducive to rapid alloy discovery. In addition, the cast microstructure seen in the as-cast ingot is often not the ideal, nor even desired structure for optimized performance. Cast materials often need further processing such as homogenization, annealing, and deformation work put in through rolling, forging, extruding, etc. to have favorable microstructures and properties. A faster method to discover new alloy combinations and evaluate them in their worked or processed form is needed. Recently, Laser Engineered Net Shaping was applied to fabricate gradient compositional material for alloy designing. However, the mechanical properties of this gradient alloy were poor due to the existence of impurities, oxidation and cracks that are inherent in the melt-solidification process. Because of these limitations, we propose to use a solid-phase process (ShAPE) to create bulk materials (extrudates) that vary in composition from one end of the extruded solid to the other. Various manufacturing methods for alloy design including conventional casting method, laser based combinatorial method and current solid phase gradient alloying method are displayed and compared in Fig. 2. ShAPE machine and a schematic of ShAPE process are displayed in Fig. 3. Starting material is processed by a rotating and plunging die to form an extrudate. We are proposing through this methodology to invent a new, bulk-scale combinatorial technique. With this novel technique, alloying element can be dissolved into the matrix with a continued gradient without bulk melting. Formation of inter-metallics and defects originating from melt processing can be avoided. In addition, the ShAPE process creates the mixed alloy chemistry, and meanwhile subjects the material to severe plastic strain, which induces the favorable “worked” microstructure. Products from the ShAPE process can be tested in hardness directly providing a path to rapid evaluation of mechanical properties. The ability to create graded structures using friction stir processing (FSP) has been demonstrated, however using the ShAPE process we believe will lead to much faster and higher fidelity results. When combined with high throughput screening methods of physical, mechanical and microstructural property characterization, efficiency and accuracy of alloy design can be significantly improved.

36 MATERIALS SCIENCE↗

Approximate formula for recalescence in binary eutectic alloys

Supercooling of a liquid prior to the nucleation of a solid and the subsequent rapid growth are necessary conditions for producing novel microstructures including metastable phases which are not formed by conventional solidification processes. Since containerless techniques, such as levitation and free fall of a sample, are capable of achieving a significant supercooling level of liquids, they are under consideration as possible techniques for material processing on earth and in space.

ALLOY STRUCTURE FORMATION↗

Bright and durable field-emission source derived from frozen refractory-metal Taylor cones

A novel method for creating conical field-emission structures possessing unusual and desirable physical characteristics is described. This process is accomplished by solidification of electrostatically formed high-temperature Taylor cones created on the ends of laser melted refractory-metal wires. Extremely rapid freezing ensures that the resultant solid structures preserve the shape and surface smoothness of the flawless liquid Taylor-cones to a very high degree. The method also enables in situ and rapid restoration of the frozen cones to their initial pristine state after undergoing physical degradation during use. This permits maximum current to be delivered without excessive concern for any associated reduction in field-emitter lifetime resulting from operation near or even above the damage threshold. In addition to the production of field emitters using polycrystalline wires as a substrate, the feasibility of producing monocrystalline frozen Taylor-cones having reproducible crystal orientation by growth on single-crystal wires was demonstrated. Finally, the development of the basic field-emission technology, progress to incorporate it into a pulsed electron gun employing laser-assisted field emission for ultrafast experiments, and some additional advances and opportunities are discussed.

36 MATERIALS SCIENCE↗

Facilities and experiment results of the NASA sounding rocket program

The NASA rocket program on reduced gravity materials experiments is reported, including experimental results obtained from the single-stage Black Brant VC sounding rockets first flight and the developed equipment. The first flight was made on 11 December 1975, and nine different experiments were done in the five min of weightlessness. All systems operated satisfactorily and each experiment generated interesting results and recorded phenomena that have been reported. Each of the experiments will be flown again in modified form to obtain additional data or check unexpected results on the multiple rocket launches planned each year. General-purpose apparatus and facilities are being developed and built to allow repeated experimentation of various materials by different investigators. For example, multiple-cavity furnaces with rapid heat-up and cool-down possibilities, providing isothermal and gradient thermal profiles, will accommodate a wide variety of solidification experiments. Special hardware satisfying specific individual requirements is also being developed.

Snyder, R. S.↗

Research on metal solidification in zero-g state

The containerless solidification of several pure metals and metallic alloys was studied in a low gravity environment. The tests were performed in the MSFC 4.2 s drop tower using a rapid wire melting apparatus designed and built for this purpose. Pure iron and nickel, and alloys of iron-nickel, iron-carbon, nickel-aluminum and tungsten-rhenium were all melted and solidified at a gravity level of approximately 100.000/-4 g. Interpretation of the results has led to an appreciation of the factors controlling the successful execution of this drop test experiment and to a delineation of the limits of applicability of the apparatus. Preliminary metallurgical evaluations are presented of the overall shapes, lattice parameters, surface microstructure,, cross-sectional microstructures, solidification and transformation sequences, evaporative segregation, and localized solute redistribution observed in the low-gravity specimens. The effects of low gravity on metallic solidification are discussed with particular emphasis on observations of spontaneous undercooling and evaporative segregation in uncontained melts.

Papazian, J. M.↗

Effect of Marangoni Convection Generated by Voids on Segregation During Low-G and 1-G Solidification

Solidification experiments, especially microgravity solidification experiments are often hampered by the evolution of unwanted voids or bubbles in the melt. Although these voids and/or bubbles are highly undesirable, there are currently no effective means of preventing their formation or eliminating their adverse effects, particularly, during low-g experiments. Marangoni Convection caused by these voids can drastically change the transport processes in the melt and, therefore, introduce enormous difficulties in interpreting the results of the space investigations. Recent microgravity experiments by Matthiesen, Andrews, and Fripp are all good examples of how the presence of voids and bubbles affect the outcome of costly space experiments and significantly increase the level of difficulty in interpreting their results. In this work we examine mixing caused by Marangoni convection generated by voids and bubbles in the melt during both 1-g and low-g solidification experiments. The objective of the research is to perform a detailed and comprehensive combined numerical-experimental study of Marangoni convection caused by voids during the solidification process and to show how it can affect segregation and growth conditions by modifying the flow, temperature, and species concentration fields in the melt. While Marangoni convection generated by bubbles and voids in the melt can lead to rapid mixing that would negate the benefits of microgravity processing, it could be exploited in some terrestrial processing to ensure effective communication between a melt/solid interface and a gas phase stoichiometry control zone. Thus we hope that this study will not only aid us in interpreting the results of microgravity solidification experiments hampered by voids and bubbles but to guide us in devising possible means of minimizing the adverse effects of Marangoni convection in future space experiments or of exploiting its beneficial mixing features in ground-based solidification.

Kassemi, M.↗

Low shear process for producing polymer composite fibers

A method for producing a polymer composite fiber comprised of a polymer matrix with filaments incorporated therein whose lengthwise dimensions are substantially oriented with the axial dimension of the composite fiber, the method comprising subjecting a melt comprised of a polymer matrix and filaments to an extrusion process in which the melt is extruded into a fibrous form in the absence of screw extruders and in the substantial absence of shear forces that result in breakage of the filaments, followed by cooling and solidification of the extruded melt to provide the polymer composite fiber. Integration of these polymer composite fibers with additive manufacturing technologies, particularly rapid prototyping methods, such as FFF and 3D printing, are also described. The resulting polymer composite fibers and articles made thereof are also described.

36 MATERIALS SCIENCE↗

Effect of Microstructural Bands on the Localized Corrosion of Laser Surface-melted 316L Stainless Steel

The localized corrosion of laser surface melted (LSM) 316L stainless steel is investigated by a combination of potentiodynamic anodic polarization in 0.1M HCl and microscopic investigation of the initiation and propagation of localized corrosion. The pitting potential of LSM 316L is significantly lower than the pitting potential of wrought 316L. The LSM microstructure is highly banded as a consequence of the high laser power density and high linear energy density. The bands are composed of zones of changing modes of solidification, cycling between very narrow regions of primary austenite solidification and very wide regions of primary ferrite solidification. Pits initiate in the outer edge of each band where the mode of solidification is primary austenite plane front solidification and primary austenite cellular solidification. The primary austenite regions have low chromium concentration (and possibly low molybdenum concentration), which explains their susceptibility to pitting corrosion. The ferrite is enriched in chromium, which explains the absence of pitting in the primary ferrite regions. The presence of the low chromium regions of primary austenite solidification explains the lower pitting resistance of LSM 316L relative to wrought 316L. The influence of banding on localized corrosion is applicable to other rapidly solidified processes such as additive manufacturing.

36 MATERIALS SCIENCE↗

Modeling supercritical CO 2 flow and mineralization in reactive host rocks with PFLOTRAN v7.0

Understanding the flow and reactivity of CO 2 injected into geological reservoirs is important for many subsurface applications including secure geologic carbon storage (GCS), critical mineral extraction, enhanced geothermal systems (EGS), and enhanced oil recovery (EOR). Traditionally, subsurface CO 2 injection for GCS applications has focused on geologic formations with favorable subsurface configurations for CO 2 migration and trapping through non-reactive mechanisms such as structural, solubility, and petrophysical trapping. Recently, CO 2 -reactive rocks such as mafic and ultramafic basalts have been investigated for their potential to react with injected CO 2 in situ to simultaneously dissolve host rock minerals and mineralize CO 2 as carbonates. Engineering rapid CO 2 mineralization in the subsurface is attractive because of the increased density of stored CO 2 , the additional safety factors associated with solidification, and the potential to extract valuable critical minerals. Here we present recent developments in the parallel flow and reactive transport simulator PFLOTRAN to model coupled CO 2 -brine flow and reactive transport for a wide range of injection and production applications involving reactive CO 2 -brine systems. These developments are based on the well established and trusted CO 2 flow capabilities in the STOMP-CO 2 simulator. New capabilities added to PFLOTRAN include new CO 2 -brine equations of state with optional thermal coupling, several new constitutive relationships like capillary pressure smoothing and scanning path hysteresis, a fully implicit well model, and native linkage with PFLOTRAN's well-established reactive transport libraries. A series of benchmarks between PFLOTRAN and STOMP-CO 2 verify the newly developed CO 2 -brine flow capabilities. Demonstrations of coupled CO 2 -brine flow modeling and reactive transport show how CO 2 mineralization can be engineered in reactive host rocks. Finally, an example use case involving copper leaching by CO 2 and critical mineral extraction is presented to showcase the strengths of this new implementation. Several limitations still remain, including limited availability of field data to parameterize models. Future work should constrain the evolution of mineral surface area during mineralization and the temperature and/or pH dependence of geochemical reactions for specific systems of interest.

Critical Minerals↗

Study on solidification of immisible alloys (M-10)

Alloying of immiscible alloys under microgravity is of interest in metallurgical processes. Several experiments investigating the alloying of immiscible alloys, such as Al-In, Al-Bi, Zn-Bi, and Zn-Pb, were done in space. Homogeneous distribution of small L2 particles in the matrix, such as an emulsion structure, was expected in the space-solidifed alloys. However, the alloys demonstrated an extremely segregated structure. To date insufficient information was obtained to explain these unexpected results. Our experiment was proposed to clarify the solidification manner of immiscible alloys and to obtain fundamental information concerning structural control of the alloys. In space, density differences between the two liquids separated in immiscible regions can be neglected, so that no sedimentation of L(sub 2) phase will take place. When the growth of the alloys is interrupted and this status is frozen by an adequate rapid cooling procedure, it will provide much information concerning decomposing homogeneous liquid and the interaction between the monotectic growth front morphology and the distribution of L(sub 2) phase. It is anticipated that the results will be useful for elucidating the monotectic solidification manner and it will be instructive to explain the segregated structures obtained in the past space experiments.

Kamio, Akihiko↗

The convective liquidus in a solidifying magma chamber - A fluid dynamic investigation

An experimental study of the solidification of a layer of paraffin cooled from above is reported. When the fluid is superheated, convection sets in at the beginning of cooling but rapidly decreases in intensity. Once the layer has lost its superheat, convection ceases and further cooling is by conduction. The interior temperature then remains constant until encountered by the upper crust. The convective liquidus is defined as the temperature threshold below which convection is very weak or nonexistent. In natural basaltic systems the convective liquidus, although strictly unknown, may be very close to the true liquidus. Rapid convection may therefore not be a dominant process during the crystallization of many magmna chambers; instead, convection is part of an overall intimate balance between phase equilibria, crystal growth, and heat transfer.

Brandeis, Genevieve↗

Additively-manufactured Al-0.3Zr-0.2Ce-0.2Cu alloy with high creep resistance and electrical conductivity

Here, a new, solute-lean Al-0.3Zr-0.2Ce-0.2Cu (wt.%) alloy is developed for additive manufacturing that overcomes the classical tradeoff between conductivity and creep resistance. The rapid-cooling-enabled supersaturation of Zr, and its uniform distribution in α-Al matrix, along with formation of submicron (Ce,Cu)-rich intermetallic particles on solidification lead to unusually high creep resistance at 200 °C. Near-zero secondary creep rates are achieved up to the alloy yield stress (YS) of 65 MPa at 200 °C in as-fabricated state. The Zr-solute-induced dislocation-climb suppression mechanism underlying this improvement also restricts dynamic recovery above YS, as noted from appreciable primary creep and its transitioning to near-zero secondary creep rates. A combination of relatively coarse, epitaxially-grown α-Al grains, low Zr concentration in α-Al, and the impurity-scavenging effect of Ce to purify α-Al matrix produces high electrical conductivity of ∼48 %IACS. Aging precipitation of L1 2 -Al 3 Zr nanoprecipitates doubles the YS (to ∼150 MPa) at room temperature and increases alloy conductivity to ∼58 %IACS, but loss of solid-solution Zr out of α-Al matrix leads to activation of dislocation climb, degrading the creep properties as compared to the supersaturated Al-Zr solid solution in the as-fabricated state. Compared to L1 2 -Al 3 Zr nanoprecipitates, submicron (Ce,Cu)-rich particles formed on solidification are more effective at impeding dislocation climb, producing a threshold stress for dislocation creep of ∼ 50 MPa at 200 °C. The new alloy design concepts, especially solute-induced dislocation-climb suppression for creep resistance, explored here may pave way for the design of new metallic alloys for thermal/electrical conductors and other high-temperature applications.

Additive Manufacturing↗

Accretion timescale and impact history of Mars deduced from the isotopic systematics of martian meteorites

High precision Sm-Nd isotopic analyses have been completed on a suite of 11 martian basaltic meteorites in order to better constrain the age of silicate differentiation on Mars associated with the formation of their mantle sources. Our data is used to evaluate the merits and disadvantages of various mathematical approaches that have been employed in previous work on this topic. Ages determined from the Sm-Nd isotopic systematics of individual samples are strongly dependent on the assumed Nd isotopic composition of the bulk planet. This assumption is problematic given differences observed between the Nd isotopic composition of Earth and chondritic meteorites and the fact that these materials are both commonly used to represent bulk planetary Nd isotopic compositions. Ages determined from the slope of Sm-146-Nd-142 whole rock isochrons are not dependent on the assumed Nd-142/Nd-144 ratio of the planet, but require the sample suite to be derived from complementary, contemporaneously-formed reservoirs. In this work, we present a mathematical expression that defines the age of formation of the source regions of such a suite of samples that is based solely on the slope of a Nd-143-Nd-142 whole rock isochron and is also independent of any a priori assumptions regarding the bulk isotopic composition of the planet. This expression is also applicable to mineral isochrons and has been used to successfully calculate Nd-143-Nd-142 model crystallization ages of early refractory solids as well as lunar samples. This permits ages to be obtained using only Nd isotopic measurements without the need for Sm-147/Nd-144 isotope dilution determinations. When used in conjunction with high-precision Nd isotopic measurements completed on martian meteorites this expression yields an age of formation of the martian basaltic meteorite source regions of 4504 +/- 6 Ma. Because the Sm-Nd model ages for the formation of martian source regions are commonly interpreted to record the age at which large scale mantle reservoirs formed during planetary differentiation associated with magma ocean solidification, the age determined here implies that magma ocean solidification occurred several tens of millions of years after the beginning of the Solar System. Recent thermal models, however, suggest that Mars-sized bodies cool rapidly in less than similar to 5 Ma after accretion ceases, even in the presence of a thick atmosphere. In assuming these models are correct, an extended period of accretion is necessary to provide a mechanism to keep portions of the martian mantle partially molten until 4504 Ma. Late accretional heating of Mars could either be associated with protracted accretion occurring at a quasi-steady state or alternatively be associated with a late giant impact. If this scenario is correct, then accretion of Mars-sized bodies takes up to 60 Ma and is likely to be contemporaneous with the core formation and possibly the onset of silicate differentiation. This further challenges the concept that isotopic equilibrium is attained during primordial evolution of planets, and may help to account for geochemical evidence implying addition of material into planetary interiors after core formation was completed.

58 GEOSCIENCES↗

Compression Freezing Kinetics of Water to Ice VII

Time-resolved x-ray diffraction (XRD) of compressed liquid water shows transformation to ice VII in 6 nsec, revealing crystallization rather than amorphous solidification during compression freezing. Application of classical nucleation theory indicates heterogeneous nucleation and one-dimensional (e.g., needlelike) growth. In conclusion, these first XRD data demonstrate rapid growth kinetics of ice VII with implications for fundamental physics of diffusion-mediated crystallization and thermodynamic modeling of collision or impact events on ice-rich planetary bodies.

36 MATERIALS SCIENCE↗

Use of a CO2 laser to prepare chondrule-like spherules from supercooled molten oxide and silicate droplets.

Chondrule-like spherules were formed from individual freely falling subcooled droplets of alumina, enstatite, forsterite, enstatite-albite and forsterite-albite mixtures that had been melted with a focused continuous CO2 laser beam. Their textures (rimmed, excentro-radial, barred, glassy) are strikingly similar to those of many meteoritic chondrules. It is suggested that the phenomena associated with rapid crystallization from the supercooled melt are responsible for the various textures observed in the artificial spherules as well as in similar meteoritic chondrules. It is suggested that the textures observed would also result from rapid crystallization of relatively slowly cooling molten droplets that may have been produced in larger scale events, including condensation from a nebula of solar composition and solidification in an ambient medium of high temperature.

Nelson, L. S.↗

Kinetics of the Formation of a Disordered Crystal Structure during High-Speed Solidification

A phase–field description is given for the kinetic transition in the structure of a binary ordering crystal growing from a supercooled liquid. The results are interpreted on the basis of the solution of the phasefield dynamics equation and the relaxation equation for the long-range order parameter at the diffuse crystal–liquid interface and in the bulk of the crystal. The critical temperatures for the variation of the growth rate and the long-range order parameter of a growing A{sub 50}B{sub 50} crystal are determined. A qualitative difference and analogies are found between the processes of nonequilibrium impurity trapping and the formation of a disordered structure of rapidly growing crystals. The results of the study are analyzed in comparison with the results of the theory of kinetic phase transitions [A.A. Chernov, Sov. Phys. JETP 26, 1182 (1967)] and the experimental data on the high-speed solidification of congruently melting samples [H. Hartmann et al., Europhys. Lett. 87, 40007 (2009)].

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Improved the microstructures and properties of M3:2 high-speed steel by spray forming and niobium alloying

The microstructures and properties of spray formed (SF) high-speed steels (HSSs) with or without niobium (Nb) addition were studied. Particular emphasis was placed on the effect of Nb on the solidification microstructures, decomposition of M{sub 2}C carbides, thermal stability and mechanical properties. The results show that spray forming can refine the cell size of eutectic carbides due to the rapid cooling effect during atomization. With Nb addition, further refinement of the eutectic carbides and primary austenite grains are obtained. Moreover, the Nb addition can accelerate the decomposition of M{sub 2}C carbides and increase the thermal stability of high-speed steel, and also can improve the hardness and bending strength with slightly decrease the impact toughness. The high-speed steel made by spray forming and Nb alloying can give a better tool performance compared with powder metallurgy M3:2 and commercial AISI M2 high-speed steels. - Highlights: • Spray forming can effectively refine the microstructure of M3:2 steel. • Niobium accelerates the decomposition of M{sub 2}C carbides. • Niobium increases the hardness and bending strength of spray formed M3:2 steel. • Spray-formed niobium-containing M3:2 steel has the best tool performance.

36 MATERIALS SCIENCE↗

Microstructure evolution and mechanical characterization of Nd:YAG laser beam welded titanium tubes

Highlights: • Joining of thin titanium tubes using laser beam welding. • Fusion zone exhibited coarse granular like grains with serrated and irregular boundaries. • Large spherical and irregular shape pores were observed at lower welding speeds. • Misorientation angle distribution indicated substructure boundaries along with single β grain formation from double α grains. • Fusion zone strengthened by substructure boundaries, solid solution strengthening and dislocation density. - Abstract: Grade 2 titanium tubes of outer diameter 60 mm and wall thickness 3.9 mm were effectively joined by Nd:YAG laser. The welding speed was varied in five levels (2.50, 2.75, 3.00, 3.25 and 3.50 m/min). The microstructure evolution was studied using optical microscopy and advanced characterization techniques. The bead geometry changed from parallel shape to wedge shape with increased welding speed due to changes in surface tension. The macrographs showed three zones namely fusion zone, heat affected zone (HAZ) and base metal. Coarse granular structure with irregular and serrated contours was observed in the fusion zone. Acicular α grains were observed at the extreme outer edge of the fusion zone due to rapid cooling. Spherical and irregular shaped pores were observed near the centerline of the fusion zone at lower welding speeds due to large amount of entrapped gases and downward sweeping solidification front. The grain size decreased with increased welding speed due to higher cooling rate. The misorientation angle distribution map showed three distinct regions. The increase in welding speed caused an increase in low angle boundaries and a reduction in very high angle boundaries. High density of dislocations was observed in the fusion zone due to thermal stresses caused by solidification. The microhardness of the fusion zone was recorded to be higher than base metal due to substructure boundaries, solute elements and dislocations. The increase in welding speed shifted the fracture location from fusion zone to base metal and fracture mode from brittle to ductile.

36 MATERIALS SCIENCE↗