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A method of forming a nanocomposite thermoelectric material having microstructural stability at temperatures greater than 1000 C. The method includes creating nanocrystalline powder by cryomilling. The method is particularly useful in forming SiGe alloy powder.
This work quantifies the plastic deformation in terms of dislocation density for a series of cold sprayed Al-Cu coatings with copper contents from 2 mass% to 5 mass%. The success of the deposition and consolidation of the feedstock powders during the cold spray process rely on the occurrence of significant plastic deformation. Inert gas atomized Al-Cu alloy powders were sprayed onto substrates made of an Al-Cu-Mg-Mn alloy (AA2024) to produce dense coatings using a low pressure cold spray system with helium as the carrier gas. X-ray diffraction patterns were obtained from the Al-Cu feedstock powder material and the cold sprayed coatings using a monochromatic X-ray source, and the dislocation density was determined via an X-ray whole profile analysis. Increasing the Cu alloy content (from 2 mass% to 5 mass%) systematically increased the dislocation density in the Al-Cu coatings from (4.3 ± 0.5) × 10 14 m -2 to (7.5 ± 0.8) × 10 14 m -2 . The dislocation densities in the feedstock powders ranging from (0.4 ± 0.1) × 10 14 m -2 to (1.8 ± 0.2) × 10 14 m -2 were all lower than the dislocation densities in the corresponding coatings. The increasing deformation level in the Al-Cu coatings with Cu additions were confirmed by the classic and modified Williamson-Hall analyses of X-ray diffraction data, and peak breadth measurements from neutron diffraction data. Finally, a high density of dislocations was also observed in these coatings via electron backscatter diffraction and transmission electron microscopy.
Arc heating process for preparation of dispersion strengthened nickel base alloy powder
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.
Nanotechnology based thermoelectric materials are considered attractive for developing highly efficient thermoelectric devices. Nano-structured thermoelectric materials are predicted to offer higher ZT over bulk materials by reducing thermal conductivity and increasing electrical conductivity. Consolidation of nano-structured powders into dense materials without losing nanostructure is essential towards practical device development. Using the gas atomization process, amorphous nano-structured powders were produced. Shockwave consolidation is accomplished by surrounding the nanopowder-containing tube with explosives and then detonating. The resulting shock wave causes rapid fusing of the powders without the melt and subsequent grain growth. We have been successful in generating consolidated nano-structured bismuth telluride alloy powders by using the shockwave technique. Using these consolidated materials, several types of thermoelectric power generating devices have been developed. Shockwave consolidation is anticipated to generate large quantities of nanostructred materials expeditiously and cost effectively. In this paper, the technique of shockwave consolidation will be presented followed by Seebeck Coefficient and thermal conductivity measurements of consolidated materials. Preliminary results indicate a substantial increase in electrical conductivity due to shockwave consolidation technique.
New alloys and materials are potentially possible through additive manufacturing’s unique thermal history. Current literature explores the fabrication of eutectic and solid solution strengthened alloys through in-situ alloying, to take advantage of AM’s unique thermal history. The resulting lessons learned by in-situ alloying currently available materials will likely lead to the development of novel materials solely possible through in-situ alloying. This work will expand the application of in-situ alloying via additive manufacturing to NASA’s GRCop-42 (Cu-4at% Cr-2at% Nb), a high temperature copper alloy which has shown success in additively manufactured combustion chambers from pre-alloyed powders. GRCop-42 is unique to literature because a reaction to form the Cr2Nb dispersoids is required during the in-situ alloying. Both reaction completion rate and how input energy from the AM process influences the reaction progress will be evaluated. Ultimately, expansion of in-situ alloying capabilities provides further insight to develop novel materials using AM.
Precipitation-strengthened, nickel-based superalloys are widely used in the aerospace and energy industries due to their excellent environmental resistance and outstanding mechanical properties under extreme conditions. Powder-bed additive manufacturing (AM) technologies offer the potential to revolutionize the processing of superalloy turbine components by eliminating the need for extensive inventory or expensive legacy tooling. Like selective laser melting (SLM), electron beam melting (EBM) constructs three-dimensional dense components layer-by-layer by melting and solidification of atomized, pre-alloyed powder feedstock within 50-200 micron layers. While SLM has been more widely used for AM of nickel alloys like 718, EBM offers several distinct advantages, such as less retained residual stress, lower risk of contamination, and faster build rates with multiple-electron-beam configurations. These advantages are particularly attractive for turbine disks, for which excessive residual stress and contamination can shorten disk life during high-temperature operation. In this presentation, we will discuss the feasibility of fabricating disk superalloy components using EBM AM. Originally developed using powder metallurgy forging processing, disk superalloys contain a higher refractory content and precipitate volume fraction than alloy 718, thus making them more prone to thermal cracking during AM. This and other challenges to produce homogeneous builds with desired properties will be presented. In particular, the quality of lab-scale samples fabricated via a design of experiments, in which the beam current, build temperature, and beam velocity were varied, will be summarized. The relationship between processing parameters, microstructure, grain orientation, and mechanical response will be discussed.
Four ODS FeCrAl alloys with base alloy composition Fe-16Cr-4Al-2Mo-0.2Y (wt.%) were mechanically alloyed with minor additions of CeO 2 and Y 2 O 3 additions and were successfully extruded into rectangular-shaped bars. Two oxide compositions were explored, which were designated NC with oxide addition of 0.5CeO 2 plus 0.2Yin solution of the base alloy powder and PC with additions of 0.5CeO 2 and 0.7Y 2 O 3 to elevate the O level. The microstructure of both alloys revealed by SEM and EBSD to consist of very small grains with sizes of ~450-520 nm and weak texture components. Sub-size tensile specimens fabricated from both alloys were tensile tested from room temperature to 800ºC. The results for both alloys from room temperature to 400ºC showed very high strengths, but low ductilities, especially uniform strain. From 500ºC to 800ºC, the strengths decreased rapidly, and the ductilities increased significantly. The reason for the rapid decreases in tensile strengths above 500ºC for both alloys is not clear, but will require advanced characterization techniques including atom probe tomography, to determine the size and number density of the nano-size oxide particles, and TEM/EFTEM, for investigating the dispersion of nano-size oxide particles on grain boundaries to assess the Zener grain boundary pinning effect, which will hinder grain coarsening at high temperatures that may enhance the Hall Petch strengthening mechanism.
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.
In collaboration with other laboratories, Idaho National Laboratory has investigated additively manufactured alloys for applications in advanced nuclear reactors. The primary focus has been on nickel alloys, as well as “other” alloys, which are alloys not considered steel nor nickel-based alloys, manufactured by laser powder bed fusion. Suitability of investigated alloys were considered against a matrix of properties of interest, developed jointly with the collaborating laboratories. For the nickel alloys, Alloys 282 and 625 are considered promising due to their properties, existing data, and availability of commercial powder feedstock. Haynes 244 is also of interest for its molten salt corrosion resistance, however there is no current feedstock supply chain, and no experience with this alloy as an additively manufactured material. Iron-chrome-aluminum alloys, titanium alloys, zirconium alloys, ceramics, and ceramic inclusions were all considered within the other alloys category. The results and discussions within this report will be compiled with the investigations from the other collaborating laboratories and compiled into a final report later this year (2023).
The ferrite memory arrays are made from pre-formed metal conductors for the ferrite arrays. The conductors are made by forming a thin sheet of a metallizing paste of metal alloy powder, drying the paste layer, bisque firing the dried sheet at a first temperature, and then punching the conductors from the fired sheet. During the bisque firing, the conductor sheet shrinks to 58 percent of its pre-fired volume and the alloy particles sinter together. The conductors are embedded in ferrite sheet material and finally fired at a second higher temperature during which firing the conductors shrink approximately the same degree as the ferrite material.
This research aims to explore an accelerated development path for oxide dispersion-strengthened (ODS) alloys by integrating additive manufacturing (AM) technologies with recent advances in ODS materials and traditional manufacturing methods. Novel AM and post-build processing routes have been developed for ODS austenitic alloys, specifically Fe-Cr-Ni alloys like 316L and 316H. Electron microscopy and mechanical characterizations were conducted to evaluate the effects of process variables on microstructure and properties, aiming for an economically feasible route property optimization. Traditionally, ODS alloy production involves multi-day high-energy mechanical milling of alloy powder with yttria (Y 2 O 3 ) followed by powder consolidation via extrusion or other methods and additional thermomechanical processing (TMP) for property control. Here, to address these challenges associated with this complex and costly approach, we propose exploring alternative, cost-effective processing routes focusing on AM and traditional TMP methods. The new ODS alloy processing routes have achieved up to a 400% increase in yield strength and a 60% increase in ultimate tensile strength compared to wrought stainless steels while still maintaining significant ductility and fracture toughness. This paper details the novel and economical AM-based processing routes for ODS austenitic alloys, combined with post-build TMPs, and discusses the mechanical and microstructural characteristics of the developed materials.
This work package within the Advanced Materials and Manufacturing Technologies (AMMT) program focused on the mechanical and microstructural characterization of oxide dispersion strengthened (ODS) stainless steels produced using advanced manufacturing techniques. The research aimed to identify an accelerated development path for ODS alloys by integrating additive manufacturing (AM) technologies with recent advancements in ODS materials and traditional manufacturing methods. For FY 24, the research specifically targeted exploring an accelerated development path for ODS alloys by combining AM technologies with these advancements. Novel AM and post-build processing routes were developed for ODS austenitic alloys, including Fe-Cr-Ni alloys such as 316L and 316H. Electron microscopy and mechanical characterizations were conducted to evaluate the impact of process variables on microstructure and properties, with the goal of optimizing these properties economically. Traditionally, producing ODS alloys involves multi-day, high-energy mechanical milling of alloy powder with yttria powder, followed by milled-powder consolidation through extrusion or other methods, and additional thermomechanical processing (TMP) for property control. To overcome the challenges associated with this complex and costly approach, we propose exploring alternative, cost-effective processing routes that emphasize AM and traditional TMP methods. The new processing routes for ODS alloys have achieved significantly higher strengths—several times greater than those of wrought stainless steels—while maintaining substantial ductility and fracture toughness. This report outlines the novel and economical AM-based processing routes for ODS austenitic alloys, combined with post-build TMPs, and discusses the mechanical and microstructural characteristics of the developed materials.
The present investigation examines the effects of manufacturing process on the total axial strain controlled low cycle fatigue behavior of polycrystalline NiAl at 1000 K, a temperature above the monotonic Brittle-to-Ductile Transition Temperature (BDTT). The nickel aluminide samples were produced by three different processing routes: hot isostatic pressing of pre- alloyed powders, extrusion of prealloyed powders, and extrusion of vacuum induction melted ingots. The LCF behavior of the cast plus extruded material was also determined at room temperature (below the BD77) for comparison to the high temperature data. The cyclic stress response, cyclic stress-strain behavior, and strain-life relationships were influenced by the alloy preparation technique and the testing temperature. Detailed characterization of the LCF tested samples was conducted by optical and electron microscopy to determine the variations in fracture and deformation modes and to determine any microstructural changes that occurred during LCF testing. The dependence of LCF properties on processing route was rationalized on the basis of starting microstructure, brittle-to-ductile transition temperature, deformation induced changes in the basic microstructure, deformation substructure, and synergistic interaction between the damage modes.
A thermogravimetry system designed to study the reduction of oxides in metal and alloy powders to be used in dispersion strengthened materials is described. The apparatus was devised for use at high temperatures with controlled atmospheres. Experimental weight change and moisture evolution results for the thermal decomposition of calcium oxalate monohydrate in dry helium, and experimental weight change results for the reduction of nickel oxide in dry hydrogen and hydrogen containing 15,000 PPM water vapor are presented. The system is currently being successfully applied to the evaluation of the reduction characteristics and the removal of impurities from metals and alloys to be used for dispersion strengthening.
A thermogravimetry system, designed to study the reduction of oxides in metal and alloy powders to be used in dispersion strengthened materials, is described. The apparatus was devised for use at high temperatures with controlled atmospheres. Experimental weight change and moisture evolution results for the thermal decomposition of calcium oxalate monohydrate in dry helium, and experimental weight change results for the reduction of nickel oxide in dry hydrogen and hydrogen containing 15,000 p.p.m. water vapor are presented. The system is currently being successfully applied to the evaluation of the reduction characteristics and the removal of impurities from metals and alloys to be used for dispersion strengthening.
Metal additive manufacturing (AM) processes are being used to enable economical manufacturing of legacy alloys as well as advancing new alloys. Laser powder bed fusion (L-PBF) is a metal AM process that has high maturity and being used to produce a variety of parts for space applications including complex propulsion components. The National Aeronautics and Space Administration (NASA) has identified the need to develop and advance new materials in unique space applications such as high-pressure hydrogen environments. NASA HR-1 is a high strength Fe-Ni based superalloy designed to resist high pressure hydrogen environment embrittlement (HEE), oxidation, and corrosion that has been successfully adapted to laser powder directed energy deposition (LP-DED). Insights gained from the NASA HR-1 development for LP-DED have guided the development process for L-PBF. However, adapting NASA HR-1 to L-PBF posed new challenges due to the distinct differences between the additive manufacturing processes. During parameter development, sensitivities were observed in post-processing that necessitated additional optimization of heat treatments. Additionally, the variations in thickness and how it influenced the microstructural response during heat treatment was characterized. Understanding these sensitivities is important to qualification of the material in a L-PBF machine. This ensures that the microstructures and properties of the material maintain consistency in production. This presentation will cover parameter development along with post-processing challenges and solutions will be discussed in addition to key material properties as it pertains to application performance and qualification per NASA-STD-6030. Improvements made by developing a derivative alloy, NASA HR-2, will be highlighted through preliminary small scale parameter development, material characterization, and initial property testing.
sCO2 turbomachinery that operates above 650°C requires the use of γ' strengthened Ni-based superalloys, leading to high cost and barrier of market adoption. Near-net-shape (NNS) HIP manufacturing with 282® alloy powder is being developed for sCO2 turbine components, with a significant estimated cost reduction. Tensile, creep, low cycle fatigue properties of argon gas atomized and plasma atomized powders were evaluated and compared to sand cast HAYNES® 282®. While tensile strength and fatigue life outperformed sand cast material, a 10~25% debit in the creep stress capability was observed due to the fine grain size and presence of prior particle boundaries (PPBs). Finite element model calibrated by powder rheological properties accurately predicted the nonuniform shrinkage during HIP, providing HIP tooling design to achieve the target dimension. A 20 lbs. turbine nozzle ring was successfully demonstrated within 0.01 inch dimensional tolerance at the vanes. A 1700lbs. turbine casing with complex internal struts and manifolds was also demonstrated being close to the target dimension.