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Massey, Caleb

Publications and source records attributed to Massey, Caleb.

50 records · Page 3

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗

In situ synchrotron tensile investigations on ultrasonic additive manufactured (UAM) zirconium

The microstructure evolution during room temperature uniaxial tensile straining of ultrasonic additive manufactured (UAM) zirconium was evaluated using the Advanced Photon Source (APS) facility. Miniature dog-bone tensile specimens of two orientations were cut from a UAM-fabricated zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stages of plastic deformation, which become candidate necking positions and eventually lead to failure. Additionally, fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvements of the UAM zirconium fabrication process.

36 MATERIALS SCIENCE↗

Effect of heavy ion irradiation dose rate and temperature on α' precipitation in high purity Fe-18%Cr alloy

Cr-rich alpha prime precipitates (CrRP) induce hardening and embrittlement of FeCr alloys, but the kinetics of CrRP formation due to particle irradiation are not well understood. In this study, Fe18wt.%Cr alloy in solid solution state and pre-aged to produce relatively coarse CrRP was irradiated with 8 MeV Fe ions. The irradiation conditions involved two midrange doses of 0.37 and 3.7 displacements per atom (dpa), a wide range of dose rates (10 -5 –10 -3 dpa/s) and temperatures (300–450 °C). The distributions of CrRP after irradiation were studied with atom probe tomography (APT). The critical irradiation conditions to suppress CrRP formation were identified as 300 °C and 10-3 dpa/s; CrRP formation occurred readily at lower dose rates or higher temperatures. From 0.37 to 3.7 dpa, CrRP were observed to slightly grow at 350 °C and strongly coarsen at 450 °C. Specimens with pre-existing CrRP evolved into a similar precipitate distribution as detected after ion irradiation on solution annealed specimens at 300–350 °C to 0.37 dpa, indicating that the precipitate microstructure approaches a quasi-equilibrium for doses <1 dpa. Limited shrinking of pre-existing CrRP was observed after irradiation at 450 °C to 0.37 dpa, indicating a higher recovery rate at this temperature. Additionally, the evolution of CrRP is quantitatively explained by employing corrections to the historic Nelson-Hudson-Mazey precipitate stability model, and a radiation modified precipitation mechanism is proposed to account for the competition between radiation enhanced diffusion and ballistic dissolution which results in the modifications on both size and solute concentration of CrRP.

36 MATERIALS SCIENCE↗

Investigation of deformation mechanisms in an advanced FeCrAl alloy using in-situ SEM-EBSD testing

The deformation mechanisms associated with uniaxial tensile testing are observed by conducting tensile experiments of an FeCrAl alloy using scanning electron microscopy (SEM) coupled with electron backscattered diffraction (EBSD). Prior to the deformation, investigated alloy was consisting grain and precipitate size of ~63.0 μm and ~6.7 μm, respectively. The recorded SEM micrographs and EBSD data at increasing levels of strains revealed the complex phenomena of slip bands’ formation in the presence of surface grain morphology evolution and their (001), (110) and (111) crystallographic planes distortions. The grains with orientation (110)||tensile direction (TD) shows higher shape change; however, (001)||TD and (111)||TD oriented grains show higher lattice gradient formation. Extracted information from the EBSD indicates that the crystallographic rotations drive towards specific, fiber-like texture in relation to the loading direction. Postmortem analysis of the recorded microstructure during the tensile deformation explains the phenomena of crack formation in the hard-intermetallic particles before the ultimate tensile strength (UTS). However, after the UTS, pores were identified in the neck that resulted from extensive plastic deformation. In-depth analysis was carried out to identify the cause of cracks and pores formation phenomena during the tensile test.

36 MATERIALS SCIENCE↗

An Atom Probe Tomography Study of the Through Wall Attenuation Effect on Cu-rich Precipitate Formation in a Reactor Pressure Vessel Steel

In this study, high-Cu weld material harvested from an ex service reactor pressure vessel (RPV) steel from Unit 1 of the decommissioned Zion Nuclear Generating Station has been characterized using atom probe tomography. Samples taken from 4 different positions through the thicknesses of the pressure vessel wall from the water-side to the air-side were characterized, along with an unirradiated baseline material. In the baseline material, no precipitates were found and the Cu was observed to be fully in solid solution; however, scanning transmission electron microscopy combined with energy dispersive spectroscopy (STEM-EDS) revealed the presence of ϵ -Cu that form during processing of the material and results in the concomitant decrease of matrix Cu. Following irradiation, a high number density of nano-scale Cu-rich precipitates (CRPs) were observed, uniformly distributed throughout the matrix. The Cu content within the CRPs was found to be ~30-35 at.% regardless of location in the wall. No statistically significant variation in the compositions, mean radius, number density, or volume fraction as a function of location within the wall was observed. The measured matrix Cu level excluding CRPs contribution was found to be ~90 appm higher than the solubility limit suggesting that further nucleation and growth of the CRPs under continued operations would have occurred. These results clearly demonstrate that the neutron energy attenuation has no significant effect on the precipitation kinetics of CRPs regardless of location in the wall in high-Cu RPV steels under irradiation.

36 MATERIALS SCIENCE↗

Microchemical evolution of irradiated additive-manufactured HT9

The microstructural responses under 5 MeV Fe2 + single-ion-beam irradiation of three conditions of additive-manufactured (AM) HT9 steel using a powder-based directed energy deposition (DED) technique with and without postbuild heat treatments were investigated. Besides the observed dislocation loop formation and the absence of cavities at the irradiation condition of 50 dpa at 460 °C, Ni/Si/Mn-rich precipitates are found to form in all three conditions of AM-HT9, whereas Cu-rich clusters that arise from Cu uptake from the DED process are only observed in the heat-treated conditions, and not in the as-built (ASB) condition. Coprecipitation of the Cu- and Ni/Si/Mn-rich clusters occur near defect sinks such as line dislocations and grain boundaries in the heat-treated AM-HT9. The variation in microchemical evolution can be directly linked to the starting sink strength of the three AM-HT9 conditions, and the ASB condition with higher sink strength suppressed the responses observed in the postbuild heat-treated specimens.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ultrasonic additive manufacturing of zirconium: Pilot results

Ultrasonic additive manufacturing (UAM) was successfully applied to the Zirconium material system to create a three-dimensional component prototype. The UAM process resulted in grain size refinement and significant localized deformation. Electron backscatter diffraction analysis revealed activated slip systems only applicable at high deformation temperatures, while texture analysis showed a decrease in measurable texture of the UAM build in comparison to the initial Zr-foil. Average tensile strengths in the X (sonotrode travel), Y (vibration), and Z (build) directions averaged 435 MPa, 458 MPa, and 359 MPa, respectively, demonstrating the viability of UAM for Zr-based materials. Furthermore, the delamination of some Z specimens along foil boundaries during loading suggests an interplay between interfacial Ti impurities introduced during welding and the spatial dependence of weld quality for this material system.

36 MATERIALS SCIENCE↗

In Situ Synchrotron Tensile Investigations on Ultrasonic Additive Manufactured (UAM) Zirconium

The microstructure evolution of ultrasonic additive manufactured (UAM) zirconium under room temperature uniaxial tensile straining is reported. Miniature dog-bone tensile specimens of two orientations were cut from a UAM zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning at the Advanced Photon Source (APS) at Argonne National Laboratory was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stage of plastic deformation, which become candidate necking positions and eventually lead to failure. Fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvement of the UAM zirconium process.

36 MATERIALS SCIENCE↗

Extensive nanoprecipitate morphology transformation in a nanostructured ferritic alloy due to extreme thermomechanical processing

Nano-oxide precipitates in a modern nanostructured ferritic alloy were investigated after extreme thermomechanical processing into a thin-walled tube geometry. It was found that the morphology of the precipitates changed from spherical to rod-shaped, with some increasing to aspect ratios of up to 9, despite the precipitate volume fraction (0.3%) and number density (> 10 23 m -3 ) of precipitates remaining unchanged. High-resolution electron microscopy showed that the precipitates likely remained coherent with the Fe-matrix, while atom probe tomography confirmed that the precipitate compositions remained unaffected by the transformation. The morphological change was attributed to the shearable nature of the (Y,Ti,O)-rich precipitates, indicating they should be considered as “soft” obstacles to dislocation motion. The elongation was most pronounced in larger (>5 nm) precipitates, which may be caused by preferential dissolution of the smallest (1–3 nm) precipitates followed by the competition between re-precipitation and solute diffusion to larger precipitates during recovery heat treatments.

36 MATERIALS SCIENCE↗

The effect of Zr on precipitation in oxide dispersion strengthened FeCrAl alloys

Oxide dispersion strengthened (ODS) FeCrAl alloys are promising candidate materials for advanced nuclear reactor applications requiring high-temperature strength, corrosion resistance, and irradiation tolerance. As these alloys have increased in compositional complexity through attempts to use highly reactive elements such as Zr to refine particle sizes and optimize nanoprecipitate dispersion characteristics, much debate has ensued as to the effects of these alloying element additions on alloy properties. In an attempt to reconcile differences in nanoprecipitate distributions reported in the literature over the past decade, a detailed investigation of a recently developed ODS FeCrAl alloy with nominal composition Fe–10Cr-6.1Al-0.3Zr+0.3Y 2 O 3 is presented here using a combination of atom probe tomography (APT), scanning/transmission electron microscopy (S/TEM), and computational thermodynamics modeling. It is illustrated that based on the amount of Zr available in the lattice, Zr competes with Al and Cr to form carbides and nitrides as opposed to oxygen-rich precipitates. This alloy system has a high number density (>10 23 m -3 ) of ~2–4 nm diameter (Y,Al,O)-rich nanoprecipitates, but it is shown that due to the compositional spread and unknown partitioning of Al between the matrix and precipitates, significant challenges still exist for quantifying the exact compositions of these precipitates using APT. However, the noted compositional spread is supported by identified complex oxides yttrium aluminum monoclinic (YAM) and yttrium aluminum garnet (YAG) using S/TEM. As a result of these findings, researchers developing ODS FeCrAl with reactive element additions must pay careful attention to C and N impurities when optimizing reactive element additions.

electron microscopy↗