Yaqiao Wu

A lanthana-containing nanostructured ferritic steel (NFS) was processed via mechanical alloying (MA) of Fe-14Cr-1Ti-0.3Mo-0.5La2O3 (wt.%) and consolidated via spark plasma sintering (SPS). In order to study the consolidation behavior via SPS, sintering temperature and dwell time were correlated with microstructure, density, microhardness and shear yield strength of the sintered specimens. A bimodal grain size distribution including both micron-sized and nano-sized grains was observed in the microstructure of specimens sintered at 850, 950 and 1050 oC for 45 min. Significant densification occurred at temperatures greater than 950 oC with a relative density higher than 98%. A variety of nanoparticles, some enriched in Fe and Cr oxides and copious nanoparticles smaller than 10 nm with faceted morphology and enriched in La and Ti oxides were observed. After SPS at 950 oC, the number density of Cr-Ti-La-O enriched nanoclusters with an average radius of 1.5 nm was estimated to be 1.2 ×10^24 m^-3 . The La + Ti : O ratio was close to 1 after SPS at 950 and 1050 C; however, the number density of nanoclusters decreased at 1050 C. With SPS above 950 C, the density improved but the microhardness and shear yield strength decreased due to partial coarsening of the grains and nanoparticles.

Atom probe tomography (APT) was performed to study the effects of Cr concentrations, irradiation doses and irradiation temperatures on α′ phase formation in Fe–Cr model alloys (10–16 at.%) irradiated at 300 and 450 °C to 0.01, 0.1 and 1 dpa. For 1 dpa specimens, α′ precipitates with an average radius of 1.0–1.3 nm were observed. The precipitate density varied significantly from 1.1 × 1023 to 2.7 × 1024 1/m3, depending on Cr concentrations and irradiation temperatures. The volume fraction of α′ phase in 1 dpa specimens qualitatively agreed with the phase diagram prediction. For 0.01 dpa and 0.1 dpa, frequency distribution analysis detected slight Cr segregation in high-Cr specimens, but not in Fe–10Cr specimens. Proximity histogram analysis showed that the radial Cr concentration was highest at the center of α′ precipitates. For most precipitates, the Cr contents were significantly lower than that predicted by the phase diagram. The Cr concentration at precipitate center increased with increasing precipitate size.

Ni-based weld alloys 52, 52M and 152 are extensively used in repair and mitigation of primary water stress corrosion cracking (SCC) in nuclear power plants. In the present study, a series of microstructure and microchemistry at the SCC tips of these alloys were examined with scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), scanning transmission electron microscopy (STEM) and energy filtered transmission electron microscopy (EFTEM). The specimens have similar chemical compositions and testing conditions. Intergranular (IG) and transgranular (TG) SCC was observed in all of them. The cracks were filled with nickel-oxides and partial precipitations of chrome carbides (CrCs), niobium carbides (NbCs), titanium nitrides (TiNs) and silicon carbides (SiCs), while iron (Fe) was largely dissolved into the solution. However, the crack densities, lengths and distributions were different for all three specimens.

Microstructural changes resulted from neutron irradiation and post-irradiation annealing in a high-temperature ultra-fine precipitate strengthened (HT-UPS) stainless steel were characterized using transmission electron microscopy (TEM) and atom probe tomography (APT). Three HT-UPS samples were neutron-irradiated to 3 dpa at 500?°C, and after irradiation, two of them were annealed for 1?h?at 600?°C and 700?°C, respectively. Frank dislocation loops were the dominant defect structure in both the as-irradiated and 600?°C post-irradiation-annealed (PIAed) samples, and the loop sizes and densities were similar in these two samples. Unfaulted dislocation loops were observed in the 700?°C PIAed sample, and the loop density was greatly reduced in comparison with that in the as-irradiated sample. Nano-sized MX precipitates were observed under TEM in the 700?°C PIAed sample, but not in the 600?°C PIAed or the as-irradiated samples. The titanium-rich clusters were identified in all three samples using APT. The post-irradiation annealing (PIA) caused the growth of the Ti-rich clusters with a stronger effect at 700?°C than at 600?°C. The irradiation caused elemental segregations at the grain boundary and the grain interior, and the grain boundary segregation behavior is consistent with observations in other irradiated austenitic steels. APT results showed that PIA reduced the magnitude of irradiation induced segregations.

Irradiation induced phase transformation of γ-austenite to α-ferrite has been observed in austenitic steels for the past several decades. This transformation can be detrimental to structural materials in a nuclear reactor environment as the increased fraction of the ferritic phase can increase corrosion and embrittlement and lead to stress corrosion cracking. This transformation is caused by both strain induced martensite transformation as well as radiation induced segregation and precipitation. In this study, two radiation tolerant nanostructured 304L austenitic steels (one ultrafine grained and one nanocrystalline) were manufactured using severe plastic deformation. These nanostructured 304L steels were compared to conventional coarse-grained 304L, after self-ion irradiation at 500°C up to a peak damage of 50 displacements per atom. Phase fraction after irradiation was analyzed using grazing incidence x-ray diffraction, precession electron diffraction, and electron backscatter diffraction. Nanostructured 304L steels showed significant resistance to irradiation induced austenite to ferrite transformation. This resistance was shown to be due to a decrease in defect formation, as well as a reduction in radiation induced segregation and precipitation.

This study explored solid-state additive friction stir deposition (AFSD) as a modular manufacturing technology, with the aim of enabling a more rapid and streamlined on-site fabrication process for large meter-scale nuclear structural components with fully dense parts. Austenitic 316 stainless steel (SS) is an excellent candidate to demonstrate AFSD, as it is a commonly-used structural material for nuclear applications. The microstructural evolution and concomitant changes in mechanical properties after 5 MeV Fe++ ion irradiation were studied comprehensively via transmission electron microscopy and nanoindentation. AFSD-processed 316 SS led to a fine-grained and ultrafine-grained microstructure that resulted in a simultaneous increase in strength, ductility, toughness, irradiation resistance, and corrosion resistance. The AFSD samples did not exhibit voids even at 100 dpa dose at 600 °C. The enhanced radiation tolerance as compared to conventional SS was reasoned to be due to the high density of grain boundaries that act as irradiation-induced defect sinks.

To enable the life extension of Light Water Reactors (LWRs) beyond 60 years, it is critical to gain adequate knowledge for making conclusive predictions to assure the integrity of duplex stainless steel reactor components, e.g. primary pressure boundary and reactor vessel internal. Microstructural changes in the ferrite of thermally aged, neutron irradiated only, and neutron irradiated after being thermally aged cast austenitic stainless steels (CASS) were investigated using atom probe tomography. The thermal aging was performed at 400 °C for 10,000 h and the irradiation was conducted in the Halden reactor at ~315 °C to 0.08 dpa (5.6 × 1019 n/cm2, E > 1 MeV). Low dose neutron irradiation at a dose rate of 5 × 10-9 dpa/s was found to induce spinodal decomposition in the ferrite of as-cast microstructure, and further to enhance the spinodal decomposition in the thermally aged cast alloys. Regarding the G-phase precipitates, the neutron irradiation dramatically increases the precipitate size, and alters the composition of the precipitates with increased, Mn, Ni, Si and Mo and reduced Fe and Cr contents. The results have shown that low dose neutron irradiation can further accelerate the degradation of ferrite in a duplex stainless steel at the LWR relevant condition.

A lanthana-containing nanostructured ferritic steel (NFS) was processed via mechanical alloying (MA) of Fe-14Cr-1Ti-0.3Mo-0.5La2O3 (wt.%) and consolidated via spark plasma sintering (SPS). In order to study the consolidation behavior via SPS, sintering temperature and dwell time were correlated with microstructure, density, microhardness and shear yield strength of the sintered specimens. A bimodal grain size distribution including both micron-sized and nano-sized grains was observed in the microstructure of specimens sintered at 850, 950 and1050 °C for 45 min. Significant densification occurred at temperatures greater than 950 °C with a relative density higher than 98%. A variety of nanoparticles, some enriched in Fe and Cr oxides and copious nanoparticles smaller than 10 nm with faceted morphology and enriched in La and Ti oxides were observed. After SPS at 950 °C, the number density of Cr–Ti–La–O-enriched nanoclusters with an average radius of 1.5 nm was estimated to be 1.2 × 1024 m−3. The La + Ti:O ratio was close to 1 after SPS at 950 and 1050 °C; however, the number density of nanoclusters decreased at 1050 °C. With SPS above 950 °C, the density improved but the microhardness and shear yield strength decreased due to partial coarsening of the grains and nanoparticles.

A novel nanostructured ferritic steel powder with the nominal composition Fe–14Cr–1Ti–0.3Mo–0.5La2O3 (wt.%) was developed via high energy ball milling. La2O3 was added to this alloy instead of the traditionally used Y2O3. The effects of varying the ball milling parameters, such as milling time, steel ball size and ball to powder ratio, on the mechanical properties and microstructural characteristics of the as-milled powder were investigated. Nanocrystallites of a body-centered cubic ferritic solid solution matrix with a mean size of approximately 20 nm were observed by transmission electron microscopy. Nanoscale characterization of the as-milled powder by local electrode atom probe tomography revealed the formation of Cr–Ti–La–O-enriched nanoclusters during mechanical alloying. The Cr:Ti:La:O ratio is considered “non-stoichiometric”. The average size (radius) of the nanoclusters was about 1 nm, with number density of 3.7x10^24 m^-3. The mechanism for formation of nanoclusters in the as-milled powder is discussed. La2O3 appears to be a promising alternative rare earth oxide for future nanostructured ferritic steels.

This article presents the comprehensive mechanical testing data archive from a neutron irradiation campaign of nuclear structural alloys fabricated by powder metallurgy with hot isostatic pressing (PM-HIP). The irradiation campaign was designed to facilitate a direct comparison of PM-HIP to conventional casting or forging. Five common nuclear structural alloys were included in the campaign: 316L stainless steel, SA508 pressure vessel steel, Grade 91 ferritic steel, and Ni-base alloys 625 and 690. Irradiations were carried out in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) to target doses of 1 and 3 displacements per atom (dpa) at target temperatures of 300 and 400 °C. This article contains the data collected from post-irradiation uniaxial tensile tests following ASTM E8 specifications, fractography of these tensile bars, and nanoindentation. By making this systematic and valuable neutron irradiated mechanical behavior dataset openly available to the nuclear materials research community, researchers may now use this data to populate material performance databases, validate material performance and hardening models, design follow-on experiments, and enable future nuclear code-qualification of PM-HIP techniques.

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. This work reports the effect of transmission electron microscope (TEM) lamella thickness on the quality of data and establishes a baseline comparison to SiC grain boundary characteristics, in an unirradiated TRISO particle, determined previously using a conventional electron backscatter diffraction (EBSD) scanning electron microscope (SEM)-based technique. In general, it was determined that the lamella thickness produced using the standard focused ion beam (FIB) fabrication process (∼80 nm), is sufficient to provide reliable PED measurements, although thicker lamellae (∼120 nm) were found to produce higher quality orientation data. Also, analysis of SiC grain boundary character from the TEM-based PED data showed a much lower fraction of low-angle grain boundaries compared to SEM-based EBSD data from the SiC layer of a TRISO-coated particle made using the same fabrication parameters and a SiC layer deposited at a slightly lower temperature from a surrogate TRISO particle. However, the fractions of high-angle and coincident site lattice (CSL)-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm (Kirchhofer et al., 2013), depending on the fabrication parameters, and since grain boundary fission product precipitates in irradiated TRISO fuel can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low-angle, high-angle, and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed needs to be significantly greater than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas would be required than those used in this study.

Nano-structured ferritic steels (NFSs) with 12-14 wt% Cr have attracted widespread interest for potential high temperature structural and fuel cladding applications in advanced nuclear reactors. They have excellent high temperature mechanical properties and high resistance to radiation-induced damage. The properties of the NFSs depend on the composition that mainly consists of Cr, Ti, W or Mo, and Y2O3 as alloying constituents. In this study, a novel nano-structured ferritic steel (Fe-14Cr-1Ti-0.3Mo-0.5La2O3, wt%) termed as 14LMT was developed via high energy ball milling and spark plasma sintering. Vickers microhardness values were measured. Microstructural studies of the developed NFSs were performed by EBSD and TEM, which revealed a bimodal grain size distribution. A significant number density of nano-precipitates was observed in the microstructure. The diameter of the precipitates varied between 2-70 nm and the morphology from the spherical to faceted shape. The Cr-La-Ti-O-enriched nano-clusters were identified by APT studies.

Elemental powder mixture of Fe–14Cr–1Ti–0.3Mo–0.5La2O3(wt%) composition is mechanicallyalloyed for different milling durations (5, 10 and 20 h) and subsequently consolidated via spark plasmasintering under vacuum at 950?C for 7 min. The effects of milling time on the densi?cation behaviorand density/microhardness are studied. The sintering activation energy is found to be close to that ofgrain boundary diffusion. The bimodal grain structure created in the milled and sintered material isfound to be a result of milling and not of sintering alone. The oxide particle diameter varies between2 and 70 nm. Faceted precipitates smaller than 10 nm in diameter are found to be mostly La–Ti–Cr-enriched complex oxides that restrict further recrystallization and related phenomena

Here, we report atom probe tomography results of the nanoclusters in a neutron-irradiated oxide dispersion strengthened alloy. Following irradiation to 5 dpa at target temperatures of 300 °C and 450 °C, fewer large nanoclusters were found and the residual nanoclusters tend to reach an equilibrium Guinier radius of 1.8 nm. With increasing dose, evident decrease in peak oxygen and titanium (but not yttrium) concentrations in the nanoclusters was observed, which was explained by atomic weight, solubility, diffusivity, and chemical bonding arguments. The chemical modifications indicate the equilibrium size is indeed a balance of two competing processes: radiation enhanced diffusion and collisional dissolution.

Historic and recent post-irradiation-examination from the German AVR and Advanced Gas Reactor Fuel Development and Qualification Project have shown that 110 m Ag is released from intact tristructural isotropic (TRISO) fuel. Although TRISO fuel particle research has been performed over the last few decades, little is known about how metallic fission products are transported through the SiC layer, and it was not until March 2013 that Ag was first identified in the SiC layer of a neutron-irradiated TRISO fuel particle. The existence of Pd- and Ag-rich grain boundary precipitates, triple junction precipitates, and Pd nano-sized intragranular precipitates in neutron-irradiated TRISO particle coatings was investigated using Scanning Transmission Electron Microscopy and Energy Dispersive Spectroscopy analysis to obtain more information on the chemical composition of the fission product precipitates. A U-rich fission product honeycomb shape precipitate network was found near a micron-sized precipitate in a SiC grain about ∼5 μm from the SiC-inner pyrolytic carbon interlayer, indicating a possible intragranular transport path for uranium. A single Ag-Pd nano-sized precipitate was found inside a SiC grain, and this is the first research showing such finding in irradiated SiC. This finding may possibly suggest a possible Pd-assisted intragranular transport mechanism for Ag and may be related to void or dislocation networks inside SiC grains. Preliminary semi-quantitative analysis indicated the micron-sized precipitates to be Pd2Si2U with carbon existing inside these precipitates. However, the results of such analysis for nano-sized precipitates may be influenced by the SiC matrix. The results reported in this paper confirm the co-existence of Cd with Ag in triple points reported previously.

The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe2+ ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension =100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

thermal neutron absorber material composed of Al3Hf particles in an aluminum matrix is under development for the Advanced Test Reactor. This metal matrix composite was fabricated via hot pressing of high-purity aluminum and micrometer-size Al3Hf powders at volume fractions of 20.0, 28.4, and 36.5%. Room temperature tensile and hardness testing of unirradiated specimens revealed a linear relationship between volume fraction and strength, while the tensile data showed a strong decrease in elongation between the 20 and 36.5% volume fraction materials. Tensile tests conducted at 200 °C on unirradiated material revealed similar trends. Evaluations were then conducted on specimens irradiated at 66 to 75 °C to four dose levels ranging from approximately 1 to 4 dpa. Tensile properties exhibited the typical increase in strength and decrease in ductility with dose that are common for metallic materials irradiated at ≤0.4Tm. Hardness also increased with neutron dose. The difference in strength between the three different volume fraction materials was roughly constant as the dose increased. Nanoindentation measurements of Al3Hf particles in the 28.4 vol% material showed the expected trend of increased hardness with irradiation dose. Transmission electron microscopy revealed oxygen at the interface between the Al3Hf particles and aluminum matrix in the irradiated material. Scanning electron microscopy of the exterior surface of tensile tested specimens revealed that deformation of the material occurs via plastic deformation of the Al matrix, cracking of the Al3Hf particles, and to a lesser extent, tearing of the matrix away from the particles. The fracture surface of an irradiated 28.4 vol% specimen showed failure by brittle fracture in the particles and ductile tearing of the aluminum matrix with no loss of cohesion between the particles and matrix. The coefficient of thermal expansion decreased upon irradiation, with a maximum change of −6.3% for the annealed irradiated 36.5 vol% specimen.