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At least 181 records · Page 10

Hardening mechanisms in a dynamic strain aging alloy, Hastelloy X, during isothermal and thermomechanical cyclic deformation

The relative contributions of the hardening mechanisms in Hastelloy X during cyclic deformation were investigated by conducting isothermal cyclic deformation tests within a total strain range of +/-0.3 pct and at several temperatures and strain rates, and thermomechanical tests within several different temperature limits. The results of the TEM examinations and special constant structure tests showed that the precipitation on dislocations of Cr23C6 contributed to hardening, but only after sufficient time above 500 C. Solute drag alone produced very considerable cyclic hardening. Heat dislocation densities, peaking around 10 exp 11 per sq cm, were found to develop at temperatures producing the greatest cyclic hardening.

Miner, R. V.↗

On the use of charged particles to characterize precipitation in irradiated reactor pressure vessel steels with a wide range of compositions

Nuclear reactor lifetimes may be limited by nano-scale Cu-Mn-Ni-Si precipitates (CRPs and MNSPs) that form under neutron irradiation (NI) of pressure vessel (RPV) steels, resulting in hardening and ductile to brittle transition temperature increases (embrittlement). Physical models of embrittlement must be based on characterization of precipitation as a function of the combination of metallurgical and irradiation variables. Here we focus on rapid and convenient charged particle irradiations (CPI) to both: a) compare to precipitates formed in NI; and, b) use CPI to efficiently explore precipitation in steels with a very wide range of compositions. Atom probe tomography (APT) comparisons show NI and CPI for similar bulk steel solute contents yield nearly the same precipitate compositions, albeit with some differences in their number density, size and volume fraction (f) dose (dpa) dependence. Yet, the overall precipitate evolutions are very similar. Advanced high Ni (>3 wt%) RPV steels, with superior unirradiated properties, were also investigated at high CPI dpa. For typical Mn contents, MNSPs have Ni 16 Mn 6 Si 7 or Ni 3 Mn 2 Si phase type compositions, with f values that are close to the equilibrium phase separated values. In contrast, in steels with very low Mn and high Ni, Ni 2-3 Si silicide phase type precipitate compositions are observed; and when Ni is low, the precipitate compositions are close to the MnSi phase field. Low Mn significantly reduces, but does not eliminate, precipitation in high Ni steels. A comparison of dispersed barrier model predictions with measured hardening data suggests that the Ni-Si dominated precipitates are weaker dislocation obstacles than the G phase type MNSPs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Study of X-ray diffraction on aging alloys with different degrees of volume discrepancy between the precipitation phase and the matrix

Study of the diffraction patterns of X rays diffracted by dispersion-hardened alloys with various degrees of difference between the specific atomic volumes of their precipitation phases and matrices. Experiments were performed on aging alloys KhN77TIuR (nimonic) and KhN67VMTIuO, which have the same types of gamma solid solutions and precipitating gamma prime phases, but differ considerably with respect to the volume factor. It is found that in the decay of supersaturated solid solutions for which the difference between the specific atomic volumes of the precipitation phase and the matrix is small (alloy KhN67VMTIuO) the nature of the intensity distribution of the diffraction lines remains practically unchanged regardless of the aging, while in cases where the volume discrepancy is large (alloy KhN77TIuR) significant changes in the appearance of the diffraction lines are recorded.-

Gitgarts, M. I.↗

Correlating microstructure and mechanical properties of harvested high dose Zorita light water reactor internals

Here, in this study, microstructural studies and micro-mechanical testing of an ex-plant material harvested from the decommissioned pressurized water reactor (PWR) is carried out. Irradiated 304 stainless steel (SS) components were harvested by the Electric Power Research Institute, U.S. Nuclear Regulatory Commission, and members of the José Cabrera Nuclear Power Station (Zorita) in Spain. The bi-crystalline micro-tensile specimens, atom probe tomography (APT) tips, and transmission electron microscopy (TEM) lamellae were fabricated from the baffle plate materials irradiated to 0.05, 15 and 50 dpa to elucidate microstructural, microchemical, and local mechanical properties changes as a function of dose. TEM and APT studies reveal radiation induced Ni, Cr, and Si rich precipitates in the 15 dpa sample that become smaller and partially redissolve into the matrix of the 50 dpa sample (decreasing size and number density). Dislocation loop and cavity number density and size were quantified as a function of dose as well as swelling. Intergranular Ni and Si enrichments with concomitant Fe and Cr depletion were observed in the 15 dpa sample and were more pronounced in the 50 dpa sample. Micro-tensile testing performed in the scanning electron microscope (SEM) at room temperature and 300 °C shows that the material's local yield strength and ultimate tensile strength decreases with increased dose and elevated test temperature and provides further insights via localized strain mapping. Current and previous mechanical data was compared with calculated values using the dispersed barrier hardening model with inputs of dislocation loops, precipitates, and cavities from microstructural characterization.

36 MATERIALS SCIENCE↗

Post-irradiation examination of commercial tantalum alloys following neutron irradiation

Post irradiation examination of two commercial tantalum alloys (based on Ta-8 %W) revealed significant irradiation hardening following neutron irradiation in the High Flux Isotope Reactor at Oak Ridge National Laboratory. Tensile samples of commercial Ta alloys T-111 and ASTAR-811C were irradiated to a total neutron fluence (E > 0.1 MeV) in the range (2–4)x10 21 n/cm 2 (0.39–0.75 dpa) at an irradiation temperature near 900 °C. Tensile testing conducted at room temperature and at 800 °C revealed significant irradiation hardening under all test conditions. Samples that were tensile tested at room temperature exhibited brittle failure, whereas ductility was maintained for elevated temperature testing. The irradiation hardening and embrittlement noted for both alloys was attributed to irradiation-induced dislocation loop formation as confirmed through scanning transmission electron microscopy analysis. Corresponding energy dispersive x-ray spectroscopy revealed radiation-induced segregation of Hf in these loop populations. This Hf enrichment is shown to result in eventual co-precipitation of elongated (Hf,O)-rich precipitates along the dislocation loops. Further, these results show that irradiation hardening is enhanced via irradiation-enhanced precipitation at elevated irradiation temperatures. Consequently, the minimum recommended operating temperature window for Ta alloys should be increased to account for observed hardening/embrittlement at irradiation temperatures as high as 900 °C (1,173 K).

36 MATERIALS SCIENCE↗

Defect formation and transmutation behaviors in irradiated tungsten under thermal-neutron shielded and mixed spectrum conditions

Here, this study investigates the microstructural evolution of pure tungsten irradiated under thermal-neutron shielded and mixed spectrum conditions in the High Flux Isotope Reactor (HFIR). Four samples were irradiated at temperatures from 570 °C to 1130 °C up to 0.73 dpa. Neutron spectrum significantly influenced the accumulation of transmutation products, with Re+Os content estimated at ∼0.3–0.6% under thermal-neutron shielded conditions and ∼5.2% under the mixed spectrum condition. Irradiation temperature strongly influences tungsten’s microstructure, with dislocation loops and fine voids forming at lower temperatures and only larger voids and Re/Os segregation observed at higher temperature. Under thermal-neutron shielded conditions, dislocation loops and voids were observed at 570 °C and 790 °C. At the highest irradiation temperature (1130 °C), dislocation loops were no longer observed, while larger but less dense voids remained. Re and Os segregation to void surfaces was evident at 790 °C and 1130 °C, though no precipitation was observed. In contrast, under the mixed-spectrum condition, both spherical and needle-like Re/Os-rich precipitates were observed, frequently accompanied by large voids. Dislocation loops were not observed, but loop-like contrast within the precipitates suggests they may have nucleated on pre-existing loops. Irradiation-induced hardening was assessed for the shielded samples at 570 °C and 790 °C. Dispersed barrier hardening (DBH) analysis, based on TEM-resolved defects, revealed that voids were the dominant contributors to hardening, consistent with literature results. A schematic model is proposed to describe defect and precipitate evolution in tungsten under fusion-relevant transmutation-to-dpa conditions.

Dislocation loops↗

The effect of Ti content on age hardening and mechanical properties of uranium-titanium alloys

Here, the effect of Ti content on age hardening and the resulting mechanical properties are described for -quenched U-Ti alloys containing 0.3 wt.% to 2.0 wt.%Ti. Age hardening occurs between ~250°C and ~450°C. Overaging occurs at higher temperatures by cellular decomposition. Age hardening kinetics suggest that different mechanisms occur depending on Ti content and initial microstructure. Strengthening in 'a acicular martensites begins by the formation of Ti clusters which evolve into thin U 2 Ti disc shaped precipitates and later mature into continuous U 2 Ti rods beginning at peak hardness. The mechanism of hardening in 'b banded martensite is more elusive, as significant hardening occurs where atomic mobility is lower than that required for precipitate formation, similar to that reported for age hardening in ''b banded martensite in U-6%Nb. The activation energy for aging varies with Ti content and microstructure. In fully martensitic alloys containing 0.75% to 2.0%Ti it is in the vicinity of ~44 kcal/mole (184 kJ/mole). But it is lower in alloys containing less than 0.6%Ti where quenched microstructures are less than fully martensitic. Tensile ductility is high prior to aging, decreases with age hardening, is effectively zero at peak hardness, and remains low in overaged conditions. Attractive combinations of strength and ductility are best obtained in alloys containing 0.6% to 1.0%Ti which have been partially aged to fractional hardening levels no greater than ~0.6. This corresponds to the very early stages of aging, associated with clustering and the earliest stages of U 2 Ti disc formation. Alloys containing 0.45%Ti or less are not as responsive to age hardening. Alloys containing 1.5% and 2.0%Ti can be aged to higher strengths, but extreme quench rate sensitivity prevents them from being effectively heat treated in realistic section thicknesses.

36 MATERIALS SCIENCE↗

A novel microstructural approach for TRIP/TWIP β-Ti alloys using intermetallic precipitation

Interest in metastable β-Ti has grown, due to the exceptional work hardening caused by TRansformation and TWinning Induced Plasticity (TRIP/TWIP). A current challenge is increasing the yield strength, while maintaining the benefits of TRIP/TWIP. This study presents the first report of TRIP/TWIP in a metastable β-Ti alloy containing intermetallic compounds, specifically Ti silicide precipitates. Silicon (Si) additions enable the formation of silicide particles, which can be precipitated, dissolved, and controlled through tailored heat treatments. In-situ synchrotron x-ray diffraction during tensile testing reveals primary {332}<113> twinning activates first, followed by TRIP, leading to extensive work hardening and uniform elongation in the solutionized state. In conclusion, these findings open a novel microstructural approach to the design of multiphase TRIP/TWIP titanium alloys, relying on intermetallic precipitation rather than allotropes such as α or ω phase, and lay the groundwork for future studies on intermetallic precipitation strengthening.

Materials science↗

NiAl alloys for structural uses

Alloys based on the intermetallic compound NiAl are of technological interest as high temperature structural alloys. These alloys possess a relatively low density, high melting temperature, good thermal conductivity, and (usually) good oxidation resistance. However, NiAl and NiAl-base alloys suffer from poor fracture resistance at low temperatures as well as inadequate creep strength at elevated temperatures. This research program explored macroalloying additions to NiAl-base alloys in order to identify possible alloying and processing routes which promote both low temperature fracture toughness and high temperature strength. Initial results from the study examined the additions of Fe, Co, and Hf on the microstructure, deformation, and fracture resistance of NiAl-based alloys. Of significance were the observations that the presence of the gamma-prime phase, based on Ni3Al, could enhance the fracture resistance if the gamma-prime were present as a continuous grain boundary film or 'necklace'; and the Ni-35Al-20Fe alloy was ductile in ribbon form despite a microstructure consisting solely of the B2 beta phase based on NiAl. The ductility inherent in the Ni-35Al-20Fe alloy was explored further in subsequent studies. Those results confirm the presence of ductility in the Ni-35Al-20Fe alloy after rapid cooling from 750 - 1000 C. However exposure at 550 C caused embrittlement; this was associated with an age-hardening reaction caused by the formation of Fe-rich precipitates. In contrast, to the Ni-35Al-20Fe alloy, exploratory research indicated that compositions in the range of Ni-35Al-12Fe retain the ordered B2 structure of NiAl, are ductile, and do not age-harden or embrittle after thermal exposure. Thus, our recent efforts have focused on the behavior of the Ni-35Al-12Fe alloy. A second parallel effort initiated in this program was to use an alternate processing technique, mechanical alloying, to improve the properties of NiAl-alloys. Mechanical alloying in the conventional sense requires ductile powder particles which, through a cold welding and fracture process, can be dispersion strengthened by submicron-sized oxide particles. Using both the Ni-35Al-Fe alloys to contain approx. 1 v/o Y2O3. Preliminary results indicate that mechanically alloyed and extruded NiAl-Fe + Y2O3 alloys when heat treated to a grain-coarsened condition, exhibit improved creep resistance at 1000 C when compared to NiAl; oxidation resistance comparable to NiAl; and fracture toughness values a factor of three better than NiAl. As a result of the research initiated on this NASA program, a subsequent project with support from Inco Alloys International is underway.

Koss, D. A.↗

Hierarchical microstructures and deformation behavior of laser direct-metal-deposited Cu–Fe alloys

Cu25Fe75 and Cu50Fe50 (nominal composition, at. %) alloys were fabricated using laser direct metal deposition (DMD) based additive manufacturing technique. These alloys exhibit hierarchical microstructures with bi-phasic Cu and Fe dendrites that contain nanoscale precipitates of varying sizes and structures. In the Cu25Fe75 alloy, Fe dendrites contained nanoscale, coherent, metastable BCC Cu and semi-coherent FCC Cu precipitates while the Cu matrix had nanoscale, coherent, metastable FCC Fe precipitates. In the Cu50Fe50 alloy, Fe dendrites only contained nanoscale semi-coherent FCC Cu precipitates while the Cu matrix had nanoscale coherent metastable FCC Fe precipitates. Both alloys exhibited enhanced flow strengths in the range of 750 – 980 MPa and significant plasticity, in compression. Here, the Cu25Fe75 alloy had lower yield strength than Cu50Fe50 alloy but higher maximum compressive strength due to higher strain hardening resulting from slightly coarser dendrites with hierarchy of nanoscale precipitation.

36 MATERIALS SCIENCE↗

Effect of Sn microalloying on the nucleation of L1 2 Al 3 Zr precipitates in a dilute aluminum-zirconium alloy

While L1 2 -Al 3 Zr nanoprecipitates provide a balance between strengthening and good electrical conductivity, the precipitation of L1 2 -Al 3 Zr in aluminum requires aggressive heat treatments. An improved age-hardening response was observed during isochronal aging of an Al-0.24Zr (wt%) alloy when microalloyed with Sn. A new mechanism termed Low melting point Element-Assisted Nucleation (LEAN) is proposed to explain the lower temperature nucleation of L1 2 -Al 3 Zr precipitates observed in this alloy based on the addition of a low melting point element, such as Sn. Characterization verified the first-principles density functional theory prediction that Zr and Sn atoms cluster during homogenization owing to the favorable binding energy of Zr-Sn-vacancy triplets. Direct microstructural observations revealed these clusters form Sn nanoprecipitates that assist the nucleation of L1 2 -Al 3 Zr at 200°C, where L1 2 -Al 3 Zr precipitation is not expected due to the low diffusivity of Zr atoms in Al. At higher temperatures (≳350°C), the acceleration of L1 2 -Al 3 Zr precipitation is driven by faster Zr diffusion in Al with Sn microalloying and the nuclei formed via the LEAN mechanism. In conclusion, this combination of mechanisms explains the improvement in age hardening through L1 2 -Al 3 Zr precipitation with Sn microalloying.

36 MATERIALS SCIENCE↗

Multiscale hierarchical and heterogeneous mechanical response of additively manufactured novel Al alloy investigated by high-resolution nanoindentation mapping

Smart alloying and microstructural engineering mitigate challenges associated with laser-powder bed fusion additive manufacturing (L-PBFAM). A novel Al–Ni–Ti–Zr alloy utilized grain refinement by heterogeneous nucleation and eutectic solidification to achieve superior performance-printability synergy. Conventional mechanical testing cannot delineate complex micromechanics of such alloys. This study combined multiscale nanomechanical and microstructural mapping to illustrate mechanical signatures associated with hierarchical heat distribution and rapid solidification of L-PBFAM. The disproportionate hardening effect imparted by Al 3 (Ti,Zr) precipitates in the pool boundaries and the semi-solid zone was successfully demonstrated. Nanomechanical response associated with heterogeneity in particle volume fraction and coherency across melt pool was interpreted from nanoindentation force–displacement curves. The hardness map effectively delineated the weakest and strongest sections in the pool with microscopic accuracy. The presented approach serves as a high throughput methodology to establish the chemistry-processing-microstructure-properties correlation of newly designed alloys for L-PBFAM.

36 MATERIALS SCIENCE↗

The low cycle fatigue deformation response of a single-crystal superalloy at 650 C

The cyclic stress-strain response and the associated deformation structure of the single crystal nickel-base superalloy PWA 1480 were investigated. Specimens of various crystallographic orientations were tested in low-cycle fatigue (LCF) at 650 C, resulting in a significant tension-compression anisotropy in initial yield strength associated with the shearing of gamma-prime precipitates by dislocation pairs, and a LCF cyclic hardening of the crystals associated with dislocation interactions occurring in the gamma phase. In specimens deforming by slip on a single slip system, dislocations of the primary slip system accumulated in the gamma matrix and formed seesile entanglements. In specimens deforming by slip on several slip systems, the dislocations of the different operative slip systems intersected in the gamma matrix and formed sessile arrangements.

Gabb, T. P.↗

Design of a V–Ti–Ni alloy with superelastic nano-precipitates

Stress-induced martensitic transformations enable metastable alloys to exhibit enhanced strain hardening capacity, leading to improved formability and toughness. As is well-known from transformation-induced plasticity (TRIP) steels, however, the resulting martensite can limit ductility and fatigue life due to its intrinsic brittleness. In this work, we explore an alloy design strategy that utilizes stress-induced martensitic transformations but does not retain the martensite phase. This strategy is based on the introduction of superelastic nano-precipitates, which exhibit reverse transformation after initial stress-induced forward transformation. To this end, utilizing ab-initio simulations and thermodynamic calculations we designed and produced a V 45 Ti 30 Ni 25 (at%) alloy. In this alloy, TiNi is present as nano-precipitates uniformly distributed within a ductile V-rich base-centered cubic (bcc) β matrix, as well as being present as a larger matrix phase. We characterized the microstructure of the produced alloy using various scanning electron microscopy (SEM) and transmission electron microscopy (TEM) methods. Furthermore, the bulk mechanical properties of the alloy are demonstrated through tensile tests, and the reversible transformation in each of the TiNi morphologies were confirmed by in-situ TEM micro-pillar compression experiments, in-situ high-energy diffraction synchrotron cyclic tensile tests, indentation experiments, and differential scanning calorimetry experiments. The observed transformation pathways and variables impacting phase stability are critically discussed.

59 BASIC BIOLOGICAL SCIENCES↗

Dislocation-θ' (Al2Cu) interactions during creep deformation of an Al-Cu alloy

While precipitate-dislocation interactions are well-understood for Al-Cu alloys in tension, creep behavior has seen far less study. New, thermally-stabilized Al-Cu alloys have θ' (Al 2 Cu) as strengthening precipitates that remain stable up to 300 °C (~60% of the melting temperature) and higher, where creep becomes essential to the mechanical behavior. This investigation identifies the precipitate-dislocation interactions in such an Al-Cu alloy using in-situ neutron diffraction and scanning transmission electron microscopy. Significant load transfer to the θ' precipitates occurs, which can be attributed to dislocation loops on the interfaces of θ' and the Al matrix. Thus, Orowan looping is identified to be the primary activity for precipitate-dislocation interactions. As Orowan looping and load transfer are associated with significant strain hardening, these results explain the excellent creep resistance seen in this alloy, and provide insights into the design of precipitation strengthened alloys with superior creep performance.

36 MATERIALS SCIENCE↗

Using post-processing heat treatments to elucidate precipitate strengthening of additively manufactured superalloy 718

The poor machinability and extensive work hardening of Ni-based superalloys makes additive manufacturing an attractive option for producing geometrically complex components with distinct microstructures. Although previous studies show recovery of high strength at room temperature, very few studies demonstrate successful properties at elevated temperatures required for industrial applications. Here, the objectives of this study are to present a post-build heat treatment for high strength across a wide temperature range, determine the strength contribution of nanoscale precipitating phases to the overall mechanical properties of superalloy 718, and from these, provide a comprehensive microstructure-property relationship for wrought and AM 718 to guide efforts to simulate the properties of AM components. Laser powder bed fusion–produced superalloy 718 was characterized at multiple length scales using scanning electron microscopy and transmission electron microscopy in the as-built condition and with multiple heat treatments designed to form combinations of γ', γ", and δ precipitates. Uniaxial tensile tests performed from room temperature to 600 °C on subsize specimens determined the yield strength, elastic modulus, ultimate tensile strength, fracture stress, and uniform elongation. Precipitates in this work proved to be weak barriers to dislocation motion through a dispersed barrier model, but they provided strength to the alloy through their consistent high density. The relative contribution to the yield strength from γ" remained consistent between 48% and 57% of the total strength up to 600 °C, the primary influence on the high temperature strength of superalloy 718. The strength factors for γ" and δ precipitates were found to trend inversely with tensile test temperature and may be attributable to the differences in precipitate coherency. A post-build heat treatment is recommended to maintain high strength at elevated temperatures. A quantitative microstructure-property relationship, dependent on precipitate size, density, and morphology, was derived and can estimate the yield strength across a wide temperature range applicable to the operational regimes for superalloy 718.

36 MATERIALS SCIENCE↗

Atomic faulting drives exceptional toughness in low thermal expansion chromium alloys

Endowing functional properties with mechanical responses in traditional metals has been a frontier topic, akin to transforming base metal into gold. Chromium and its alloys, with their functional deficiencies and limited ductility, serve as typical examples. Herein, we report a Cr96Fe4Ge1.3B1 alloy that unifies low thermal expansion (LTE, αl = 1.79 × 10-6 K-1, 200 − 315 K) with exceptional toughness (240.2 J·cm-3). The enhancement in mechanical responses is primarily attributed to layered Cr2B intermetallic precipitates, which ameliorate interfacial cohesion and simultaneously refine the grain structure. The weakened interlayer interactions within the Cr-B layers facilitate the nucleation and movement of numerous tiny stacking faults in precipitates, efficiently alleviating strain energy and resulting in marked work-hardening ability. Additionally, antiferromagnetic fluctuations in the BCC matrix contribute to the unique LTE behavior. This paves the way for the design of high-performance alloys featuring layered-symmetry precipitates.

Yu, Chengyi [University of Science and Technology ↗

Defect-specific strength factors and superposition model for predicting strengthening of ion irradiated Fe18Cr alloy

Here, a high-purity binary alloy Fe18Cr was subjected to heavy-ion irradiation in order to provide improved understanding of the irradiation effect on radiation hardening associated with dislocation loop and network formation, α’ precipitation. The specimens were irradiated with 8 MeV Fe ions (~2 μm ion range) to midrange doses of 0.37 and 3.7 dpa at 300, 350 and 450 °C using dose rates of ~10 –5 –10 –3 dpa/s. Nanoindentation testing was performed to extract the bulk equivalent hardness at low depth from these ion irradiated specimens. High-quality transmission electron microscopy (TEM) images were acquired by utilizing a flash electropolishing method on the Focused Ion Beam (FIB) prepared liftouts. An accurate calculation of the strength factor was provided based on detailed TEM characterization of the irradiated microstructures. A newly refined hardening superposition method was applied to combine the strengthening components from each microstructure. The good agreement between microstructure predicted strength and measured strength further demonstrated the fidelity to use hardening model to quantify the mechanical properties of ion irradiated materials.

36 MATERIALS SCIENCE↗