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At least 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Microstructural evolution of a uranium-10 wt.% molybdenum alloy for nuclear reactor fuels

Low-enriched uranium-10 wt.% molybdenum (LEU-10wt.%Mo) is of interest for the fabrication of monolithic fuels to replace highly-enriched uranium (HEU) dispersion fuels in high performance research and test reactors around the world. In this work, depleted uranium-10wt.%Mo (DU- 10wt.%Mo) is used to simulate the solidification and microstructural evolution of LEU- 10wt.%Mo. Electron backscatter diffraction (EBSD) and complementary electron probe microanalysis (EPMA) reveal significant microsegregation present in the metastable γ-phase after solidification. Homogenization is performed at 800 and 1000 °C for times ranging from 1 to 32 h to explore the time-temperature combinations that will reduce the extent of microsegregation, as regions of higher and lower Mo content may influence local mechanical properties and provide preferred regions for γ-phase decomposition. We show for the first time that EBSD can be used to qualitatively assess microstructural evolution in DU-10wt.%Mo after homogenization treatments. Complementary EPMA is used to quantitatively confirm this finding. Homogenization at 1000 °C for 2 to 4 h reduces the regions that contain 8 wt.% Mo or lower, whereas homogenization at 1000 °C for longer than 8 h effectively saturates Mo chemical homogeneity, but results in substantial grain growth. The appropriate homogenization time will depend upon additional microstructural considerations, such as grain growth and intended subsequent processing. Higher carbon LEU-10wt.%Mo generally contains more inclusions within the grains and at grain boundaries after solidification. The effect of these inclusions on microstructural evolution (e.g. grain growth) during homogenization and as potential γ-phase decomposition nucleation sites is unclear, but likely requires additional study.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Post-irradiation characterization of a high burnup mixed oxide fuel rod with minor actinides

The Advanced Fuels Campaign performed a series of irradiation tests of minor actinide-bearing mixed oxide fuel (MA-MOX), the so-called AFC-2C&D experiments, to investigate the transmutation of long-lived transuranic actinide isotopes contained in spent nuclear fuel via fast reactor technology at burnups exceeding 10 % fission of initial metallic atoms. This manuscript reports the test results derived from one of the five MA-MOX rodlets taken to higher burnup in the AFC-2D irradiation. This includes both non-destructive investigations, such as gamma and neutron spectrometry, and destructive investigations, such as fission gas release, ceramography, and chemical burnup analysis. In addition, the microstructure of the fuel was investigated using advanced electron microscopy techniques including electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Here, it was observed with EBSD that the pellet had subdivision of the grains and the TEM observed migration of cladding material into the 5 metal precipitates in the fuel which could have been from the higher than desired oxygen/metal ratio. The TEM also showed an enrichment of Cr in fuel clad chemical interaction (FCCI) layer.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

A study on texture stability and the biaxial creep behavior of as-hydrided CWSR Zircaloy-4 cladding at the effective stresses from 55 MPa to 65 MPa and temperatures from 300°C to 400°C

The creep rupture of high burnup used nuclear fuel (> 45 GWD/MTU) cladding is regarded as one of the failure mechanisms during long-term dry storage. A high amount of zirconium hydride in the cladding matrix would degrade the mechanical properties of the cladding especially leading to delayed hydride cracking. To better understand the influence of zirconium hydride on the biaxial thermal creep performance and the crystalline texture stability of Zircaloy-4 cladding, the pressurized tube technique is applied to test the durability of the as-hydrided material. Tests were performed on as-received Zircaloy-4 tubular specimens as well as-hydrided ones with targeted 300 wt parts per million (wppm) or 750 wppm hydrogen. The biaxial creep experiments were conducted at temperatures from 300 degrees C to 400 degrees C and at equivalent stresses at mid-wall from 55 MPa to 65 MPa. The hydridation process prior to creep tests induces the formation of FCC delta-hydride platelets along the circumferential direction of the tube. This alignment and phase structure of hydride show no significant change after biaxial creep tests. The creep strain-rate negatively depends on the hydrogen content. The synchrotron wide-angle X-ray diffraction (WAXD) technique and electron backscatter diffraction (EBSD) analysis were applied for the study of the crystallographic orientation relationship. zirconium-to-hydride grain orientation follows Shoji-Nishiyama crystallographic relationship. This relationship is stable before and after creep deformation. These results of creep performance and texture stability of Zircaloy-4 claddings can help support the design basis of interim and long-term dry storage facilities.

creep↗
DOE OSTI2023

Investigating microstructural evolution in SolidStir™ extruded oxide dispersion strengthened 14YWT alloy fuel cladding tube

Structural components for extreme environments require advanced materials and manufacturing processes. One such advanced material is oxide dispersion strengthened (ODS) Fe–14 wt.%Cr–3W–0.4Ti–0.3Y 2 O 3 (14YWT), which is developed for components to be used in Gen IV and fusion nuclear reactors. However, the conventional manufacturing processes to produce components, such as fuel cladding tubes, either do not retain the desired microstructural attributes or are costly and less efficient. As a result, a more attractive option is a novel manufacturing process developed on the principle of friction stir welding or processing (FSW/P) and commercially referred to as SolidStir™ Extrusion (SSE). Here this study used the SSE technique to study the manufacturing and microstructural evolution of a fuel cladding tube made of ODS 14YWT alloy. The cladding extrusion by the SSE technique involved the use of ball-milled 14YWT powders with Y, Ti, and O in the solid solution and the use of a specially designed W-25Re-Hf tool for consolidation and extrusion of the powders. A scanning electron microscope (SEM), electron backscattered diffraction (EBSD), and transmission electron microscope (TEM) were utilized for microstructural characterization. A Keyence microscope captured macrostructural photographs of the extruded tube. EBSD examination of the extruded tube on both transverse and longitudinal cross-sections showed the presence of dynamically recrystallized grains and revealed that the average grain size of the transverse cross-section was smaller than that of the longitudinal cross-section. The texture was weak and consisted of some amount of shear texture. The presence of nano-oxide clusters or precipitates of Y, Ti, and O (pyrochlores) in the extruded tube was determined by TEM. Aging heat treatment caused the average precipitate size to decrease and the density to increase compared to the as-processed condition. The results indicated that SSE is a viable tool for manufacturing fuel cladding tubes with the desired microstructural attributes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Gas tungsten arc welding and friction stir welding of ultrafine grained AISI 304L stainless steel: Microstructural and mechanical behavior characterization

In the present study, an ultrafine grained (UFG) AISI 304L stainless steel with the average grain size of 650 nm was successfully welded by both gas tungsten arc welding (GTAW) and friction stir welding (FSW). GTAW was applied without any filler metal. FSW was also performed at a constant rotational speed of 630 rpm and different welding speeds from 20 to 80 mm/min. Microstructural characterization was carried out by High Resolution Scanning Electron Microscopy (HRSEM) with Electron Backscattered Diffraction (EBSD) and Transmission Electron Microscopy (TEM). Nanoindentation, microhardness measurements and tensile tests were also performed to study the mechanical properties of the base metal and weldments. The results showed that the solidification mode in the GTAW welded sample is FA (ferrite–austenite) type with the microstructure consisting of an austenite matrix embedded with lath type and skeletal type ferrite. The nugget zone microstructure in the FSW welded samples consisted of equiaxed dynamically recrystallized austenite grains with some amount of elongated delta ferrite. Sigma phase precipitates were formed in the region ahead the rotating tool during the heating cycle of FSW, which were finally fragmented into nanometric particles and distributed in the weld nugget. Also there is a high possibility that the existing delta ferrite in the microstructure rapidly transforms into sigma phase particles during the short thermal cycle of FSW. These suggest that high strain and deformation during FSW can promote sigma phase formation. The final austenite grain size in the nugget zone was found to decrease with increasing Zener–Hollomon parameter, which was obtained quantitatively by measuring the peak temperature, calculating the strain rate during FSW and exact examination of hot deformation activation energy by considering the actual grain size before the occurrence of dynamic recrystallization. Mechanical properties observations showed that the welding efficiency of the FSW welded sample is around 70%, which is more than 20% higher than the GTAW welded sample. - Highlights: • Microstructure and mechanical properties of UFG 304L stainless steel were studied during GTAW and FSW. • Sigma phase formation mechanism was studied during FSW of 304L stainless steel. • THERMOCALC analysis was performed to obtain possible formation temperatures for sigma phase. • Nano-mechanical twins were found in the TMAZ region.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterization of the effects of different tempers and aging temperatures on the precipitation behavior of Al-Mg (5.25at.%)-Mn alloys

We investigated the effects of different tempers (H131 and H116) and different aging temperatures (50 and 70 °C) on the precipitation behavior of Al-Mg (5.25 at.%)-Mn (Al 5083) alloys aged for a long time (41 and 30 months) using electron backscatter diffraction(EBSD), scanning transmission electron microscopy(STEM), energy-dispersive X-ray spectroscopy(EDS), atom probe tomography (APT), and small angle neutron scattering (SANS). Results for the GP zones and β'' phases were found in Al 5083 H116 aged at 50 °C for 24 months using APT. EDS and SANS revealed that a phase transformation process from GP zones to β'/β phases occurred for precipitates formed in both Al 5083 H131 and H116 aged at 70 °C. The effective diffusion coefficient of Mg in Al 5083 H131 is 1.8 times of that in Al 5083 H116 aged at 70 °C. The precipitation process in Al 5083 H116 aged at 50 °C is much slower than that in the sample aged at 70 °C. Finally, we identified the coarsening process in Al 5083 H131 and H116 aged at 70 °C for > 9 months.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Heterogeneous microstructural evolution during hydrodynamic penetration of a high-velocity copper microparticle impacting copper

Microparticle hydrodynamic penetration (HDP) may be associated with the erosion regime in cold spray processing and other high-velocity impact events. Here, in an experimental approach where we can individually launch particles and study the impact sites, we explore copper microparticles impacted on copper substrates at velocities above 900 m/s where HDP begins. We lift cross-sectional lamellae from the impact sites with a focused-ion beam for further microstructural characterization using electron backscatter diffraction and scanning transmission electron microscopy. Due to the gradients of strain, strain rate, and temperature associated with HDP, heterogeneous microstructures result. The structural evolution processes observed include deformation twinning and multiple dislocation-mediated grain recrystallization mechanisms—geometric dynamic recrystallization (gDRX), discontinuous DRX (dDRX), and meta DRX (mDRX). The higher strains at the interface lead to the most significant structural changes and complex mechanisms. In contrast, there is a gradient to more conventional dislocation plasticity away from the interface (on either the particle or substrate side). Here, these microstructural observations are consistent with the deformation map for copper and extend the observations of impact-induced recrystallization across new regimes of behavior.

Cold spray process↗
DOE OSTI2012

Twinning and martensite in a 304 austenitic stainless steel

The microstructure characteristics and deformation behavior of 304L stainless steel during tensile deformation at two different strain rates have been investigated by means of interrupted tensile tests, electron-backscatter-diffraction (EBSD) and transmission electron microscopy (TEM) techniques. The volume fractions of transformed martensite and deformation twins at different stages of the deformation process were measured using X-ray diffraction method and TEM observations. It is found that the volume fraction of martensite monotonically increases with increasing strain but decreases with increasing strain rate. On the other hand, the volume fraction of twins increases with increasing strain for strain level less than 57%. Beyond that, the volume fraction of twins decreases with increasing strain. Careful TEM observations show that stacking faults (SFs) and twins preferentially occur before the nucleation of martensite. Meanwhile, both {var_epsilon}-martensite and {alpha}{prime}-martensite are observed in the deformation microstructures, indicating the co-existence of stress induced- transformation and strain-induced-transformation. We also discussed the effects of twinning and martensite transformation on work-hardening as well as the relationship between stacking faults, twinning and martensite transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Study of growth twins produced through heat treatment of fine-grained magnesium

This study investigated the microstructural features of magnesium after the fine-grained magnesium sample was heat treated at 400 °C for 2 h. Both fine-grained and heat-treated magnesium samples were observed using the electron backscatter diffraction technique in scanning electron microscopy. The results show that the grains were substantially coarsened, the local strain and the local misorientation was significantly reduced, and a large number of twins were observed in the heat-treated magnesium sample. The misorientation angle analysis determined that the twins were oriented about 86.3° away from the orientation of their corresponding matrices, and the twins were the variants of $\{1 0 \bar{1} 2\}$ tensile twins. The relative orientation analysis also identified that the fast growth directions of the twins were closely along the $<2 \bar{1} \bar{1} 0>$ or $<1 0 \bar{1} 0>$ directions in the basal plane. The twins can merge or impinge onto each other. Most boundaries between the twins have the misorientation angle of about 7.4°.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of annealing treatment on the dry sliding wear behavior of copper

We report the effect of annealing on the wear behavior of commercial grade pure copper (Cu) was evaluated by performing unlubricated pin-on-disc wear tests of as-received and annealed samples under 0.1-10 kgf normal load. It was found that annealing at 800 °C for 24 h led to an increase of grain size of Cu from ~ 6.7 to ~ 15.3 μm and a decrease in hardness. Wear rates of both samples increased while the friction coefficients decreased with increasing normal load. Subsurface microstructure evolution and wear debris were characterized by high resolution electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) after wear tests. Dynamic recrystallization and abnormal subsurface grain growth were observed in both samples under high load. Finally, the effect of annealing on the microstructure evolution and wear resistance of Cu were discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Understanding Phase and Interfacial Effects of Spall Fracture in Additively Manufactured Ti-5Al-5V-5Mo-3Cr

Additive manufactured Ti-5Al-5V-5Mo-3Cr (Ti-5553) is being considered as an AM repair material for engineering applications because of its superior strength properties compared to other titanium alloys. Here, we describe the failure mechanisms observed through computed tomography, electron backscatter diffraction (EBSD), and scanning electron microscopy (SEM) of spall damage as a result of tensile failure in as-built and annealed Ti-5553. We also investigate the phase stability in native powder, as-built and annealed Ti-5553 through diamond anvil cell (DAC) and ramp compression experiments. We then explore the effect of tensile loading on a sample containing an interface between a Ti-6Al-V4 (Ti-64) baseplate and additively manufactured Ti-5553 layer. Post-mortem materials characterization showed spallation occurred in regions of initial porosity and the interface provides a nucleation site for spall damage below the spall strength of Ti-5553. Preliminary peridynamics modeling of the dynamic experiments is described. Finally, we discuss further development of Stochastic Parallel PARticle Kinteic Simulator (SPPARKS) Monte Carlo (MC) capabilities to include the integration of alpha (α)-phase and microstructural simulations for this multiphase titanium alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Application of Nano-Indentation Test in Estimating Constituent Phase Properties for Microstructure-Based Modeling of Multiphase Steels

For multiphase advanced high strength steels (AHSS), the constituent phase properties play a crucial role in determining the overall mechanical behaviors. Therefore, it is important to accurately measure/estimate the constituent phase properties in the research of AHSS. In this study, a new nanoindentation-based inverse method that we developed was adopted in estimating the phase properties of a low alloy Quenching and Partitioning (Q&P) steel. A microstructure-based Finite Element (FE) model was also generated based on the Electron BackScatter Diffraction (EBSD) and Scanning Electron Microscopy (SEM) images of the Q&P steel. The phase properties estimated from nanoindentation were first compared with those estimated from in-situ High Energy X-Ray Diffraction (HEXRD) test and, then, employed in the generated FE model to examine whether they can be appropriately used as the input properties for the model. The results show that the estimated phase properties from the inverse method are similar to those from HEXRD, and that the Ultimate Tensile Strength (UTS) and Uniform Elongation (UE) predicted from the FE model based on the estimated phase properties are also similar to those of tensile experiment of the Q&P steel. Based on the results in this study, the nanoindentation-based inverse method appears to be a viable way in determining the phase properties of complex multiphase steels with submicrometer grain sizes.

Cheng, Guang↗
NASA NTRS2008

Andreyivanovite: A Second New Phosphide from the Kaidun Meteorite

Andreyivanovite (ideally FeCrP) is another new phosphide species from the Kaidun meteorite, which fell in South Yemen in 1980. Kaidun is a unique breccia containing an unprecedented variety of fragments of different chondritic as well as achondritic lithologies. Andreyivanovite was found as individual grains and linear arrays of grains with a maximum dimension of 8 m within two masses of Fe-rich serpentine. In one sample it is associated with Fe-Ni-Cr sulfides and florenskyite (FeTiP). Andreyivanovite is creamy white in reflected light, and its luster is metallic. The average of nine electron microprobe analyses yielded the formula Fe(Cr0.587 Fe0.150 V0.109 Ti0.081 Ni0.060 Co0.002)P. Examination of single grains of andreyivanovite using Laue patterns collected by in-situ synchrotron X-ray diffraction (XRD), and by electron backscattered diffraction revealed that it is isostructural with florenskyite; we were unable to find single crystals of sufficient quality to perform a complete structure analysis. Andreyivanovite crystallizes in the space group Pnma, and has the anti-PbCl2 structure. Previously-determined cell constants of synthetic material [a = 5.833(1), b = 3.569(1), c = 6.658(1) A] were consistent with our XRD work. We used the XPOW program to calculate a powder XRD pattern; the 5 most intense reflections are d = 2.247 (I = 100), 2.074 (81), 2.258 (46), 1.785 (43), and 1.885 A (34). Andreyivanovite is the second new phosphide to be described from the Kaidun meteorite. Andreyivanovite could have formed as a result of cooling and crystallization of a melted precursor consisting mainly of Fe-Ni metal enriched in P, Ti, and Cr. Serpentine associated with andreyivanovite would then have formed during aqueous alteration on the parent asteroid. It is also possible that the andreyivanovite could have formed during aqueous alteration, however, artificial FeTiP has been synthesized only during melting experiments, at low oxygen fugacity, and there is no evidence that a hydrothermal genesis is reasonable.

Zolensky, Michael↗
NASA NTRS2018

Lath Structured Monazite from Haughton Dome, Canada Reveals Shock-Induced Tetragonal High Pressure Polymorph of REEPO4

Shock deformed monazite, mono-clinic rare earth element (REE) phosphate, from the Haughton Dome impact structure, Nunavut, Canada, contain lath-structured lamellae. Microstructural phase heritage indicate the former presence of a previously unreported, shock-produced, tetragonal-structured, high pressure polymorph of REEPO4. This study presents an electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) study of shock deformed monazite from the historic sample DIG-9, a shock stage III, biotite sillimanite gneiss sample from near the central uplift of the Haughton Dome (75°22'20"N, 89°40'50"W), in which shock features in monazite were first described.

Erickson, T. M.↗
NASA NTRSDate not supplied

TPSAS-NF1676L-31770-DND

HREBSD (high resolution electron backscatter diffraction) is a scanning electron microscope based diffraction technique that measures stress, elastic strain and dislocation density in crystalline materials with a spatial resolution on the order of tens of nanometers. This information represents a glut of quantitative data that may be directly incorporated in microscale crystal plasticity models. However, concerns over the accuracy of HREBSD make integration of microscopy data with material models problematic. This presentation addresses a number of issue concerning the accuracy of HREBSD, including pattern center error, cross-correlation error and random noise. Additionally, a computational framework is presented that allows for rapid, non-deterministic calibration of material models. Finally, several tests cases are presented where HREBSD is cross-validated with other diffraction techniques: X-ray diffraction, electron channeling contrast imaging and transmission electron microscopy. The accuracy of HREBSD, when incorporating these new techniques, is sufficient to measure local stress to below 10 MPa and to detect individual dislocations.

Timothy J Ruggles↗
DOE OSTI2026

Impact of Molten Gallium on the Microstructure and Corrosion Behavior of Aluminum and Uranium-Aluminum Alloys for Used Nuclear Fuel Reprocessing

Test reactors around the world utilize highly enriched uranium fuel to achieve high neutron fluxes for materials testing. Once spent, the remaining uranium is a valuable resource for subsequent fuel fabrication. However, some of these test reactor cores consist of curved plate-type fuel elements, fabricated using aluminum alloy 6061 (AA6061) cladding to encapsulate a uranium-aluminum alloy (UAlx) fuel matrix. These assemblies require non-standard reprocessing approaches for uranium recovery, as aluminum dissolves readily in acidic solutions, generating large volumes of waste and complicating downstream chemical separations. In this work, we investigate a novel chemical decladding strategy based on the interaction between AA6061/UAlx and molten gallium (Ga). Ga is known to induce severe degradation of aluminum metal through liquid metal embrittlement (LME), even at relatively low Ga concentrations. By penetrating the aluminum crystal lattice, Ga disrupts grain cohesion and facilitates fracture or dissolution of the aluminum matrix. Thermodynamic analysis of the Al–Ga binary phase diagram suggests that Ga may offer a viable pathway to selectively weaken or dissolve the AA6061 cladding, and potentially the aluminum component of the UAlx fuel matrix within. To this end, parametric experiments were performed at 50 °C and 100 °C across a range of Al–Ga atomic fractions. At lower Al fractions, the AA6061 was completely molten after 2 hours of exposure to the Ga metal. In contrast, samples with higher Al fractions (0.9 Al, 0.1 Ga) contained residual solids after 2 hours, which were characterized by microstructural examination using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). These Al-Ga compositions were also evaluated using FactSage thermodynamic modeling to further elucidate the relationship between phase diagram behavior and LME.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Mitigation of tin whisker growth by inserting Ni nanocones

Highlights: • Tin whisker growth is mitigated effectively by inserting Ni nanocones. • Ni nanocones impede Sn dynamic recrystallization by blocking dislocation motions. • The inhibition method and mechanism are important to the study of tin whisker. - Abstract: An innovative controllable way has been proposed to mitigate tin whisker growth by inserting Ni nanocones prepared by electrodeposition. The results reveal that, after inserting Ni nanocones, tin whisker formation is mitigated effectively for 1.6 μm Sn coating but there is no inhibition effect for 4.5 μm Sn coating. The coatings are characterized by X-ray diffraction, scanning electron microscopy, energy dispersive spectrometer and electron backscatter diffraction (EBSD). The EBSD results show that Sn grain size without Ni nanocones increases significantly after indentation test compared with Sn grains with Ni nanocones. The inhibition effect of Ni nanocones on whisker growth can be ascribed to its specific structure which prevents dynamic recrystallization and produces horizontal grain boundaries of Sn grains. The structural inhibition method and mechanism proposed are of great importance to the research of tin whisker.

77 NANOSCIENCE AND NANOTECHNOLOGY↗