Deformation processed Al/Ca nano-filamentary composite conductors for HVDC applications
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Engineering topics
Publications and source records attributed to Anderson, Iver.
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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 and 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.
The charge for each gas atomization experiment was provided by Alcoa and consisted of cast blocks cut into 1 inch by 1 inch square rods of the chosen aluminum alloys. The atmosphere in the melting chamber and connected atomization system was evacuated with a mechanical pump prior to backfilling with ultrahigh purity (UHP grade) Ar. The melt was contained in a bottom tapped alumina crucible with an alumina stopper rod to seal the exit while heating to a pouring temperature of 1000 – 1400°C. When the desired superheat was reached, the stopper rod was lifted and melt flowed through pour tube and was atomized with Ar from a 45-22-052-409 gas atomization nozzle (or atomization die), having a jet apex angle of 45 degrees with 22 cylindrical gas jets (each with diameter of 1.32 mm or 0.052 inches) arrayed around the axis of a 10.4 mm central bore. The Ar atomization gas supply regulator pressure was set to produce nozzle manifold pressures for the series of runs at pressures of 250-650 psi. Secondary gas halos of Ar+O 2 and He also were added to the interior of the spray chamber at various downstream locations for additional cooling of the atomized droplets, surface passivation, and to prevent coalescence of the resulting powder.
Light, strong materials with high conductivity are desired for many applications such as power transmission conductors, fly-by-wire systems, and downhole power feeds. However, it is difficult to obtain both high strength and high conductivity simultaneously in a material. In this study, an Al/Ca (20 vol%) nanofilamentary metal-metal composite was produced by powder metallurgy and severe plastic deformation. Fine Ca metal powders (~200 µm) were produced by centrifugal atomization, mixed with pure Al powder, and deformed by warm extrusion, swaging, and wire drawing to a true strain of 12.9. The Ca powder particles became fine Ca nanofilaments that reinforce the composite substantially by interface strengthening. The conductivity of the composite is slightly lower than the rule-of-mixtures prediction due to minor quantities of impurity inclusions. As a result, the elevated temperature performance of this composite was also evaluated by differential scanning calorimetry and resistivity measurements.
A method and apparatus for generating transpiration cooling using an oxidized porous HTA layer metallurgically bonded to a substrate having micro-channel architectures. The method and apparatus generates a porous HTA layer by spreading generally spherical HTA powder particles on a substrate, partially sintering under O.sub.2 vacuum until the porous HTA layer exhibits a porosity between 20% and 50% and a neck size ratio between 0.1 and 0.5, followed by a controlled oxidation generating an oxidation layer of alumina, chromia, or silica at a thickness of about 20 to about 500 nm. In particular embodiments, the oxidized porous HTA layer and the substrate comprise Ni as a majority element. In other embodiments, the oxidized porous HTA layer and the substrate further comprise Al, and in additional embodiments, the oxidized porous HTA layer and the substrate comprise .gamma.-Ni+.gamma.'-Ni.sub.3Al.
Fabrication methods are being developed and tested for producing fuel clad tubing of the advanced ODS 14YWT and FCRD-NFA1 ferritic alloys. Three fabrication methods were based on plastically deforming a machined thick-wall tube sample of the ODS alloys by pilgering, hydrostatic extrusion or drawing to decrease the outer diameter and wall thickness and increase the length of the final tube. The fourth fabrication method consisted of the additive manufacturing approach involving solid-state spray deposition (SSSD) of ball milled and annealed powder of 14YWT for producing thin-wall tubes. Of the four fabrication methods, two methods were successful at producing tubing for further characterization: production of tubing by high-velocity oxy-fuel spray forming and production of tubing using high-temperature hydrostatic extrusion. The characterization described shows through neutron diffraction the texture produced during extrusion while maintaining the beneficial oxide dispersion. In this research, the parameters for innovative thermal spray deposition and hot extrusion processing methods have been developed to produce the final nanostructured ferritic alloy (NFA) tubes having approximately 0.5 mm wall thickness. Effect of different processing routes on texture and grain boundary characteristics has been investigated. It was found that hydrostatic extrusion results in combination of plane strain and shear deformations which generate rolling textures of α- and γ-fibers on {001}<110> and {111}<110> together with a shear texture of ζ-fiber on {011}<211> and {011}<011>. On the other hand, multi-step plane strain deformation in cross directions leads to a strong rolling textures of θ- and ε-fiber on {001}<110> together with weak γ-fiber on {111}<112>. Even though the amount of the equivalent strain is similar, shear deformation leads to much lower texture indexes compared to the plane strain deformations. Moreover, while 50% of hot rolling brings about a large number of high-angle grain boundaries (HAB), 44% of shear deformation results in large amount of low-angle boundaries (LAB) showing the incomplete recrystallization.
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Iver Anderson and his team invented lead-free solder.
Recently, a novel Al/Ca composite was produced by severe plastic deformation of Al powders and Ca granules for possible use as a high-voltage power transmission conductor. Since the strength of such composites is inversely proportional to the Ca filament size, fine Ca powders (less than ~250 μm) are needed to achieve the desired high strength for the powder metallurgy production of an Al-matrix composite reinforced by nano-scale Ca filaments. However, fine Ca powders are not commercially available. Therefore, we have developed a method to produce fine Ca powders via centrifugal atomization to supply Ca powder for prototype development of Al/Ca composite conductor. A secondary goal of the project was to demonstrate that Ca powder can be safely prepared, stored, and handled and could potentially be scaled for commercial production. Our results showed that centrifugal atomization can yield as much as 83 vol. % Ca powder particles smaller than 250 μm. The mean particle size sometimes matches, sometimes deviates substantially from the predictions of the Champagne & Anger equation likely due to unexpected secondary atomization. The particle size distribution is typical for a ligament-disintegration atomization mode. Scanning electron micrographs showed that the morphology of these Ca powders varied with powder size. Spark testing and auto-ignition tests indicated that the atomized powders were difficult to ignite, providing confidence that this material can be handled safely in air.
The charge components for each gas atomization experiment (GA-1-230, GA-1-232, and GA-1-238) was provided by Aegis and consisted of elemental materials, while MPC provided the master alloy arc melted button castings that were added to yield a charge composition of (Co35Fe65)88Zr7B4Cu. The atmosphere in the melting chamber and connected atomization system was evacuated with a mechanical pump prior to backfilling with ultrahigh purity (UHP grade) Ar. The melt was contained in a bottom tapped zirconia crucible with an alumina stopper rod to seal the exit while heating to a pouring temperature of 1550 – 1575oC. When the desired superheat was reached, the stopper rod was lifted and melt flowed through a yttria stabilized zirconia (YSZ) pour tube with a 3.2 mm orifice and was atomized with Ar from a 45-22-052-409 gas atomization nozzle (or atomization die), having a jet apex angle of 45 degrees with 22 cylindrical gas jets (each with diameter of 1.32 mm or 0.052 inches) arrayed around the axis of a 10.4 mm central bore. The Ar atomization gas supply regulator pressure was set to produce nozzle manifold pressures for the series of runs at a pressure of 450 psi. Secondary gas halos of Ar and He also were added to the interior of the spray chamber at various downstream locations for additional cooling of the atomized droplets and to prevent coalescence of the resulting powder. Powder size analysis and size classification were performed with a full set of ASTM sieves, starting with the 106 µm screen and proceeding down through the 20 µm screen. A Microtrac particle size analyzer was used to verify the size classification results of the particulate resulting from the runs. The resulting powder size distribution results are provided with this report labeled with their respective run numbers (GA-1-230, GA-1-232, and GA-1-238). It should be noted that the size distribution results of the first atomization run were quite acceptable and the same parameters were used for the second and third runs to test the reproducibility for technology transfer purposes.
Liquid-phase diffusion bonding (LPDB) is being studied as the primary phenomena occurring in the development of a high temperature lead-free composite solder paste composed of gas-atomized Cu-10Ni, wt.% (Cu-11Ni, at.%) powder blended with Sn-0.7Cu-0.05Ni-0.01Ge (Sn-1.3Cu-0.1Ni-0.02Ge, at.%) Nihon-Superior SN100C solder powder. Powder compacts were used as a model system. LPDB promotes enhanced interdiffusion of the low-melting alloy matrix with the solid Cu-10Ni reinforcement powder above the matrix liquidus temperature. The initial study involved the effective intermetallic compound (IMC) compositions and microstructures that occur at varying reflow temperatures and times between 250-300°C and 30-60s, respectively. Certain reflow temperatures encourage adequate interdiffusion to form a continuous highly-conductive network throughout the composite solder joints. The diffusion of nickel, in particular, has a disperse pattern that foreshadows the possibility of a highly-conductive low-melting solder that can be successfully utilized at high temperatures.
Deformation processed metal–metal (matrix–reinforcement) composites (DMMCs) are high-strength, high-conductivity in situ composites produced by severe plastic deformation. The electrical resistivity of DMMCs is rarely investigated mechanistically and tends to be slightly higher than the rule-of-mixtures prediction. In this paper, we analyze several possible physical mechanisms (i.e. phonons, interfaces, mutual solution, grain boundaries, dislocations) responsible for the electrical resistivity of DMMC systems and how these mechanisms could be affected by processing conditions (i.e. temperature, deformation processing). As an innovation, we identified and assembled the major scattering mechanisms for specific DMMC systems and modeled their electrical resistivity in combination. From this analysis, it appears that filament coarsening rather than dislocation annihilation is primarily responsible for the resistivity drop observed in these materials after annealing and that grain boundary scattering contributes to the resistivity at least at the same magnitude as does interface scattering.
A novel gas atomization reaction synthesis (GARS) method was developed in this project to enable production (at our partner’s facility) a precursor Ni-Cr-Y-Ti powder with a surface oxide and an internal rare earth (RE) containing intermetallic compound (IMC) phase. Consolidation and heat-treatment experiments were performed at Ames Lab to promote the exchange of oxygen from the surface oxide to the RE intermetallic to form nano-metric oxide dispersoids. Alloy selection was aided by an internal oxidation and serial grinding experiments at Ames Lab and found that Hf-containing alloys may form more stable dispersoids than Ti-containing alloy, i.e., the Hf-containing system exhibited five different oxide phases and two different intermetallics compared to the two oxide phases and one intermetallic in the Ti-containing alloys. Since the simpler Ti-containing system was less complex to characterize, and make observations on the effects of processing parameters, the Ti-containing system was selected by Ames Lab for experimental atomization trials at our partner. An internal oxidation model was developed at Ames Lab and used to predict the heat treatment times necessary for dispersoid formation as a function of powder size and temperature. A new high-pressure gas atomization (HPGA) nozzle was developed at Ames Lab with the aim of promoting fine powder production at scales similar to that of the high gas-flow and melt-flow of industrial atomizers. The atomization nozzle was characterized using schlieren imaging and aspiration pressure testing at Ames Lab to determine the optimum melt delivery tip geometry and atomization pressure to promote enhanced secondary atomization mechanisms. Six atomization trials were performed at our partner to investigate the effects of: gas atomization pressure and reactive gas concentration on the particle size distribution (PSD) and the oxygen content of the resulting powder. Also, the effect on the rapidly solidified microstructure (as a function of powder size) was investigated at Ames Lab as a function of reactive gas composition and bulk alloy composition. The results indicated that the pulsatile gas atomization mechanism and a significantly enhanced yield of fine powders reported in the literature for this type of process were not observed. Also it was determined that reactive gas may marginally improve the fine powder yield but further experiments are required. The oxygen content in the gas also did not have any detrimental effect on the microstructure (i.e. did not significantly reduce undercooling). On the contrary, the oxygen addition to the atomization gas may have mitigated some potent catalytic nucleation sites, but not enough to significantly alter the microstructure vs. particle size relationship. Overall the downstream injection of oxygen was not found to significantly affect either the particle size distribution or undercooling (as inferred from microstructure and XRD observations) but injection further upstream, including in the gas atomization nozzle, remains to be investigated in later work.
Deformation processed metal–metal composites (DMMCs) are high-strength, high-electrical conductivity composites developed by severe plastic deformation of two ductile metal phases. The extraordinarily high strength of DMMCs is underestimated using the rule of mixture (or volumetric weighted average) of conventionally work-hardened metals. A dislocation-density-based, strain–gradient–plasticity model is proposed to relate the strain-gradient effect with the geometrically necessary dislocations emanating from the interface to better predict the strength of DMMCs. The model prediction was compared with our experimental findings of Cu–Nb, Cu–Ta, and Al–Ti DMMC systems to verify the applicability of the new model. The results show that this model predicts the strength of DMMCs better than the rule-of-mixture model. The strain-gradient effect, responsible for the exceptionally high strength of heavily cold worked DMMCs, is dominant at large deformation strain since its characteristic microstructure length is comparable with the intrinsic material length.
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The microstructure-strength relationship in a deformation processed Al-Ca composite
With the advent of high-flux density permanent magnets based on rare earth elements such as neodymium (Nd) in the 1980s, permanent magnet-based electric machines had a clear performance and cost advantage over induction machines when weight and size were factors such as in hybrid electric vehicles and wind turbines. However, the advantages of the permanent magnet-based electric machines may be overshadowed by supply constraints and high prices of their key constituents, rare earth elements, which have seen nearly a 10-fold increase in price in the last 5 years and the imposition of export limits by the major producing country, China, since 2010. We outline the challenges, prospects, and pitfalls for several potential alloys that could replace Nd-based permanent magnets with more abundant and less strategically important elements.
Of Pb-free solder choices, an array of solder alloys based on the Sn-Ag-Cu (SAC) ternary eutectic (T eut = 217°C) composition have emerged with potential for broad use, including ball grid array (BGA) joints that cool slowly. This work investigated minor substitutional additions of Al (<0.25 wt.%) to Sn-3.5Ag-0.95Cu (SAC3595) solders to promote more consistent solder joint microstructures and to avoid deleterious product phases, e.g., Ag3Sn “blades,” for BGA cooling rates, since such Al additions to SAC had already demonstrated excellent thermal aging stability. Consistent with past work, blade formation was suppressed for increased Al content (>0.05Al), but the suppression effect faded for >0.20Al. Undercooling suppression did not correlate specifically with blade suppression since it became significant at 0.10Al and increased continuously with greater Al to 0.25Al. Surprisingly, an intermediate range of Al content (0.10 wt.% to 0.20 wt.% Al) promoted formation of significant populations of 2-μm to 5-μm faceted Cu-Al particles, identified as Cu33Al17, that clustered at the top of the solder joint matrix and exhibited extraordinary hardness. Clustering of Cu33Al17 was attributed to its buoyancy, from a lower density than Sn liquid, and its early position in the nucleation sequence within the solder matrix, permitting unrestricted migration to the top interface. Joint microstructures and implications for the full nucleation sequence for these SAC + Al solder joints are discussed, along with possible benefits from the clustered particles for improved thermal cycling resistance.