Comparison of the High-Temperature Oxidation Behavior of Subsolvus and Supersolvus Treated Advanced Powder Metallurgy Disk Alloys
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Overview of the PM-HIP work performed on stainless steel 316H as part of the microreactor program. High temperature mechanical testing was performed, with concerns identified with the creep-fatigue performance. Variations in feedstock and processing parameters did not conclusively identify the primary factor in the reduced creep-fatigue performance.
Advanced manufacturing routes such as electron beam welding and powder metallurgy with hot isostatic pressing are increasingly used across energy and aerospace industries, where the reliable prediction of weld behavior and heat affected zone (HAZ) evolution is critical. This study examines how fabrication routes and post-weld heat treatments influence phase distribution, crystallite size, microstrain, and dislocation density in nuclear reactor pressure vessel steels using synchrotron X-ray diffraction (SXRD). Retained austenite occurs only in samples that did not undergo austenitization, whereas an austenitizing heat treatment fully eliminates retained austenite and produces a more uniform microstructure across the weldment in terms of phase fraction, dislocation density, and microstrain. The Rosenthal solution underestimates the HAZ width for powder metallurgy samples. A newly proposed modified Rosenthal solution, reducing density by accounting for porosity, matches the SXRD-measured HAZ width with a 0.65% error. Structure–property correlations reveal that dislocation density correlates strongly with nanohardness in homogenous microstructures, while in heterogenous weldments nanohardness is further influenced by the presence of dissimilar phase boundaries. These findings provide new insight into the thermal and microstructural response of powder metallurgy fabricated steels and offer a framework for optimizing welding procedures and heat treatments in advanced manufacturing applications.
The physical metallurgy of near-solidus integranular cracking in Inconel 718 welds was investigated. The data, although inconclusive, suggest at least two mechanisms which might explain intergranular cracking (microfissuring) in the heat-affected zone of several high temperature alloys. One theory is based on the separation of intergranular liquid while the other involves mechanical failure of solid ligaments surrounded by intergranular liquid. Both mechanisms concentrate strain in the grain boundaries resulting in low strain (1%) intergranular brittleness. The mechanisms reported might also pertain to the physical metallurgy of casting, powder metallurgy sintering and hot isostatic pressing.
The advantages of rapid solidification processing over ingot metallurgy processing in the development of 2XXX aluminum alloy compositions were evaluated using a similarly processed ingot metallurgy (IM) control alloy. The powder metallurgy (PM) alloy extrusions showed a reduced age-hardening response in comparison with similar IM compositions, with higher tensile properties for naturally aged extrusions but lower properties for artificially aged ones. However, the tensile properties of naturally and artificially aged PM alloy extrusions based on a version of IM 2034 alloy, but containing 0.6 weight percent zirconium, were comparable to those of the IM control extrusions and had significantly superior combinations of strength and toughness. The tensile properties of this PM alloy showed even greater advantage in 6.4-mm (0.25-in.) and 1.8-mm (0.070-in.) plate and sheet, the yield strength being about 68 MPa (10 ksi) greater than reported values for the IM 2034 alloy sheet. An artificially aged PM alloy based on 2219 alloy also showed a strength and strength-toughness combination comparable to those of the PM Al-Cu-Mg-Zr alloy, substantially outperforming the IM 2219 alloy. These results show that rapid solidification offers the flexibility needed to modify conventional IM compositions to produce new alloy compositions with superior mechanical properties.
The copper-8 atomic percent chromium-4 atomic percent niobium (CuCrNb) alloy was developed by Glenn Research Center (formally Lewis Research Center) as an improved alloy for combustion chamber liners. In comparison to NARloy-Z, the baseline (as in Space Shuttle Main Engine) alloy for such liners, CuCrNb demonstrates mechanical and thermophysical properties equivalent to NARloy-Z, but at temperatures 100 C to 150 C (180 F to 270 F) higher. Anticipated materials related benefits include decreasing the thrust cell liner weight 5% to 20%, increasing the service life at least two fold over current combustion chamber design, and increasing the safety margins available to designers. By adding an oxidation and thermal barrier coating to the liner, the combustion chamber can operate at even higher temperatures. For all these benefits, however, this alloy cannot be formed using conventional casting and forging methods because of the levels of chromium and niobium, which exceed their solubility limit in copper. Until recently, the only forming process that maintains the required microstructure of CrNb intermetallics is powder metallurgy formation of a billet from powder stock, followed by extrusion. This severely limits its usefulness in structural applications, particularly the complex shapes required for combustion chamber liners. Vacuum plasma spray (VPS) has been demonstrated as a method to form structural articles including small combustion chambers from the CuCrNb alloy. In addition, an oxidation and thermal barrier layer can be formed integrally on the hot wall of the liner that improve performance and extend service life. This paper discusses the metallurgy and thermomechanical properties of VPS formed CuCrNb versus the baseline powder metallurgy process, and the manufacturing of small combustion chamber liners at Marshall Space Flight Center using the VPS process. The benefits to advanced propulsion initiatives of using VPS to fabricate combustion chamber liners while maintaining the superior CuCrNb properties are also presented.
High hardness, high carbide powder metallurgy tools steels such as M62 enable the operation of ball bearings at extremely high load and stress levels. Operation under such conditions increases the potential for rolling contact fatigue failure attributed to ceramic particle inclusions. To address this challenge, industry has sought steel made from ever increasing levels of cleanliness but the results have been uneven owing to the random nature of the occurrence of material flaws. One common approach is to rely upon careful ingot inspections prior to bearing manufacture. By selecting the cleanest portion of an ingot, it is expected that bearings relatively free from material flaws will result. This approach is not always successful because detrimental flaws that exist deep within an ingot can pass inspection undetected potentially causing subsequent failure. Recent efforts to commercialize an intermetallic material, 60NiTi, for rolling element bearings demonstrates a pathway to produce bearing steel that is free from unwanted ceramic particle inclusions. In this paper, the process used to make bearing grade ceramic-free NiTi alloys is described and applied to steelmaking. At its core, the NiTi process differs from steel making in one key aspect. NiTi alloys are made from elementally pure starting materials that are melted, blended and processed in equipment absolutely free from exposure to oxygen and ceramics ensuring a ceramic particle-free product. In contrast, the predominant method to make bearing steel is to employ a successive series of purification steps to reduce contamination levels below required thresholds. This paper describes the processes developed and applied to high carbide tool steel, M62. The resulting material and microstructures are evaluated and compared to M62 prepared by conventional powder metallurgy techniques. It is hoped that the application of materials manufacturing techniques used for fracture sensitive ceramics and intermetallic materials like NiTi can provide a pathway to Ultra-Clean, Ceramic-Inclusion free steels for rolling element bearings and other failure critical applications.
Iron-chromium-aluminum (FeCrAl) alloys are potential accident tolerant fuel (ATF) cladding candidates for light-water reactors but are difficult to fabricate as thin-walled tubes via conventional cast-and-wrought routes. Powder metallurgy (PM) offers a manufacturing alternative with improved compositional control, but its transient accident performance has not been directly benchmarked against wrought variants. This study evaluates the burst behavior of commercially developed PM-processed FeCrAl alloys, PM-C26M (Fe-12Cr-6Al-2Mo) and the high precipitate density FA-SMT (Fe-22Cr-5Al-3Mo), under simulated light-water reactor accident transient conditions. Burst testing was conducted using the Severe Accident Test Station with heating rates of 5 °C/s and 50 °C/s and internal pressures ranging from 25 MPa to 100 MPa. PM-C26M reproduced wrought C26M burst behavior within 7–37 °C across the stress range, indicating that PM processing does not compromise transient strength. FA-SMT exhibited markedly higher burst temperatures and reduced heating-rate sensitivity, consistent with its engineered precipitate strengthening. FA-SMT rupture exhibited axial "unzipping" rather than the lateral tearing characteristic of PM- and wrought C26M. Post-test EBSD and fractography indicate that this behavior is strongly correlated with strain-gated intergranular void nucleation associated with the dense precipitate architecture of FA-SMT, a response absent in the comparatively clean PM-C26M matrix and consistent with rupture morphologies reported for oxide-dispersion strengthened (ODS) FeCrAl of similar base-matrix chemistry to PM-C26M. These findings highlight the potential of powder metallurgy as a viable fabrication route for ATF claddings from an accident performance standpoint.
The development of effective neutron shielding materials is of paramount importance for the progression of fusion technologies with the aim of producing clean and sustainable energy for future generations. This study demonstrates the successful fabrication of a promising candidate material for shielding applications, hafnium hydride, through the powder metallurgy process. Powder metallurgy fabrication resulted in the production of 91% dense, crack-free, ε-phase HfH 2 pellets with a hydrogen-to-metal ratio of 1.89 to 2.00. Resonant ultrasound spectroscopy (RUS) was used to measure a Young’s modulus of 34.52 ± 2.70 GPa and a shear modulus of 12.25 ± 0.18 GPa. Nanoindentation techniques have been used to establish a hardness value of 4.45 ± 1.63 GPa, and a Young’s modulus of 47.8 ± 6.4 GPa was determined using Poison’s ratio from RUS. Hydrogen release was measured using thermogravimetric analysis and appeared to occur in three different regimes as the sample transitioned through the ε- and δ-phases. Heat capacity matched literature data up to 600 K, after which a rapid increase was observed due to phase transformations occurring with hydrogen loss.
This study presents an advancement in high-temperature Raman spectroscopy, specifically for analyzing molten materials. It introduces an approach by integrating a fiber-optic Raman probe with a copper block protection system designed to endure extreme thermal conditions. The copper block features an open port designed to accommodate an external telescope with a 3 cm focal length, enabling Raman spectra collection in challenging high-temperature environments. A built-in gas channel ensures a continuous flow of argon gas to prevent flux intrusion. The robust copper block acts as a reliable shield, safeguarding the fiber-optic Raman probe within molten materials. This enhancement maintains the probe's integrity and significantly improves its resilience, making it ideal for rigorous investigations of molten substances. This advancement is particularly relevant in metallurgy, where flux materials impact production quality and efficiency. The ability to acquire Raman signals under elevated thermal conditions offers opportunities for studying molecular dynamics, compositional changes, and chemical interactions within molten substances. This introduced direct immersion probing technique has implications, benefiting both scientific and industrial fields. It holds promise for advancing research and exploration in various contexts, from fundamental scientific inquiries to practical applications in metallurgical processes, where flux materials are critical for optimizing production quality and efficiency. Furthermore, this approach enhances the capabilities of high-temperature Raman spectroscopy, making it a valuable tool for investigating molten materials and their properties in diverse settings.
An evaluation of the cyclic behavior of three aircraft engine turbine disk materials was conducted to compare their relative crack initiation and crack propagation resistance. The disk alloys investigated were Inconel 718, hot isostatically pressed and forged powder metallurgy Rene '95, and as-hot-isostatically pressed Rene '95. The objective was to compare the hot isostatically pressed powder metallurgy alloy forms with conventionally processed superalloys as represented by Inconel 718. Cyclic behavior was evaluated at 650 C both under continuously cycling and a fifteen minute tensile hold time cycle to simulate engine conditions. Analysis of the test data were made to evaluate the strain range partitioning and energy exhaustion concepts for predicting hold time effects on low cycle fatigue.
A study was undertaken in order to adapt IIB-11 (an experimental wrought superalloy with high temperature strength) to manufacture via powder metallurgy techniques, and to improve its microstructural stability. Three compositional modifications were produced and evaluated. Among the conclusions reached it was found that: (1) IIB-11 having a low C and low Hf alloy content is suitable for advanced temperature turbine disks, and is applicable to fabrication by powder metallurgy techniques, (2) IIB-11, when compared to modifications with higher C and/or higher Hf, is somewhat weaker in tension at intermediate temperatures but superior in tensile ductility, rupture strength and ductility, and stability during long-time heating, (3) increases in the cross-rolling temperature increase the grain size of alloys after solution treatment, and (4) both the lower C modifications develop larger grain sizes than the higher C modification.
Developments of particulate metallurgy of alloyed materials where the final products is a fully dense body are discussed. Particulates are defined as powders, flakes, foils, silvers, ribbons and strip. Because rapid solidification is an important factor in particulate metallurgy, all of the particulates must have at least one dimension which is very fine, sometimes as fine as 10 to 50 microns, but move typically up to several hundred microns, provided that the dimension permits a minimum solidification rate of at least 100 K/s.
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.
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.
Literature survey was conducted to determine the effects of different microstructural features and different load histories on fatigue crack initiation and propagation of aluminum alloys. Comparison of microstructure and monotonic and cyclic properties between powder metallurgy (P/M) and ingot metallurgy (I/M) alloys is presented. The two alloys that are representative of each process on which the comparison is focused are X7091 and 7050. Included is a detailed description of the microstructure produced through the P/M and I/M proesses. The effect of each pertinent microstructural feature on monotonic and cyclic properties, such as yield strength, toughness, crack initiation and propagation is discussed. Also discussed are the proposed mechanisms for crack initiation and propagation, as well as the effects of aggressive environments on these cyclic properties. The effects of variable amplitude loadin on fatigue crack propagation and the various models proposed to predict load interaction effects are discussed.