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At least 163 records · Page 9

Stress effects on flow and transport in three-dimensional fracture networks

We investigate the effects of various external stress regimes on fracture apertures, fluid flow, and solute transport in three-dimensional fracture networks. We use well-established geomechanics equations coupled with discrete fracture network modeling to characterize changes in primary flow paths within a complex network as a function of stress magnitude and orientation. These changes manifest in the alterations of the fluid flow field and are measured in terms of Eulerian and Lagrangian flow observables including solute transport, which is a key problem in many hydrologic applications. Changes in primary flow paths affect the solute transport in the network by promoting anomalously early arrival or long tailing behavior. However, early time arrival is not ubiquitous in anisotropically stressed networks and in most cases there is a delayed arrival of solute, which is attributed to (i) the presence of low-velocity zones normal to the flow direction, (ii) the angle between flow direction and major compressive principal stress directions, and (iii) changes in the primary flow paths (i.e., increases in tortuosity and active network structure). Overall, flows become more channelized in anisotropically stressed fracture networks than in unstressed and isotropically stressed networks.

58 GEOSCIENCES↗

Correlation between microstructure and residual stress formation in friction stir welded armor steels characterized by neutron diffraction

Friction stir welding (FSW) is a solid-state joining process that minimizes the heat-affected zone (HAZ) compared with fusion-based arc welding, making it well suited for joining martensitic armor steels where hardness and ballistic resistance are critical. This study investigates residual stress formation in three defect-free FSW butt-joint configurations relevant to armored-vehicle fabrication: similar rolled homogeneous armor (RHA–RHA, Case 1), similar high-hardness armor (HHA–HHA, Case 2), and dissimilar HHA–RHA (Case 3) joints produced under temperature-controlled conditions (770 °C). Neutron diffraction was employed to quantify the magnitude and spatial distribution of residual stresses in the longitudinal, transverse, and normal directions and to correlate them with weld microstructure and hardness. Tensile residual stresses were concentrated in the softened HAZ, reaching approximately 300 MPa for Case 2 and 400 MPa for Case 1 (≈50–70 % of the base-metal yield strength; ∼581 MPa for RHA and ∼566 MPa for HHA), while compressive residual stresses dominated the stir zone. The spatial extent of tensile stresses scaled with the width of the softened HAZ, which was largest in the dissimilar HHA–RHA joint and smallest in the HHA–HHA joint. Full-width-at-half-maximum (FWHM) analysis revealed low microstrain in overtempered HAZ regions and high microstrain in the stir zone associated with severe plastic deformation and fresh martensite formation. This work demonstrates that residual stress evolution in FSW of martensitic armor steels is governed not primarily by peak temperature or thermal contraction, as inferred from fusion-welding analogies, but by the competition between transformation-induced volumetric expansion and tempering-induced stress relaxation. The relative dominance of these mechanisms is shown to depend on alloy hardenability and local thermal history, leading to more extensive HAZ softening and broader tensile stress regions in the lower-hardenability RHA steel. These findings establish a transferable mechanistic framework for optimizing solid-state joining strategies in high-strength steels and other transformation-hardening alloys beyond armor applications.

Friction stir welding↗

Thermodynamic and electrical transport properties of UTe 2 under uniaxial stress

Despite intense experimental efforts, the nature of the unconventional superconducting order parameter of UTe 2 remains elusive. This puzzle stems from reports of either a single or a double superconducting transition at ambient pressure as well as a complex pressure-temperature phase diagram. To address this issue, we measured the heat capacity and electrical resistivity of UTe 2 under compressive uniaxial stress σ applied along different crystallographic directions. We find that the critical temperature T c of the single observed bulk superconducting transition decreases with σ along [100] and [110] but increases with σ along [001]. Aside from its effect on T c , c-axis stress leads to a significant piezoresistivity. Importantly, an in-plane shear stress σ xy does not induce any observable splitting of the superconducting transition over a stress range of σ xy ≈ 0.17GPa. Furthermore, this result suggests that the superconducting order parameter of UTe 2 may be single component at ambient pressure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of rice husk ash-derived activator on the structural build-up of alkali activated materials

Highlights: • Filtered and unfiltered sodium silicate solutions were synthesised from RHA. • The dissolution efficiency of RHA in NaOH solution was 76.3%. • RHA-derived activator showed a structural build-up comparable to the commercial activator in AAM pastes. • The undissolved residues in the unfiltered RHA-derived activator increased the yield stress. • Comparable compressive strength and early age gel formation were observed from both commercial and RHA-derived solutions. Waste-derived sodium silicates (SSs) were synthesised from rice husk ash (RHA) to produce alkali activated materials (AAMs) using fly ash and slag as precursors. The effects of these SSs on the structural build-up were investigated by monitoring the evolution of the viscoelasticity, ultrasonic pulse waves, setting time, and infrared spectra. Two types of RHA derived SSs (filtered SS and unfiltered SS) were prepared to investigate the effect of the undissolved residue on the hardening process. The derived SS contained a large portion of monomer silicate species. The results showed that the structural build-up mechanism was comparable between the AAMs activated by the filtered SS and a commercial SS. The unfiltered SS increased the yield stress of the paste by up to 10 times. However, the residues in the unfiltered SS had insignificant impacts on the gel formation and compressive strength when using identical SiO{sub 2}/Na{sub 2}O and Na{sub 2}O/binder ratios in the mix design.

36 MATERIALS SCIENCE↗

Effects of rhodium doping on dislocation nucleation in a [001] SrNi 2 P 2 single crystal under spherical nanoindentation

Nanoindentation was performed on SrNi 2 P 2 single crystals and their dilute solid solutions, Sr(Ni 1–x Rh x ) 2 P 2 (x = 0 ~ 0.055), under [001] loading to investigate the effects of elemental doping on Young’s modulus and dislocation nucleation stress. The results show that Young’s modulus and the dislocation nucleation stress decrease as the Rh content increases, and their Rh content dependence also varies with the Rh content. Electron diffraction analysis and the anisotropic lattice distortion calculations revealed that a local structural transition from the orthorhombic superstructure to the tetragonal structure and local compressive residual stresses could be the main reasons for the decrease in Young’s modulus and dislocation nucleation stress, respectively. The overlap of stress–strain fields between Rh atoms and the associated local structural transition contribute to their Rh content dependence. Here, the results also indicate that elemental doping does not necessarily strengthen materials if the incipient plasticity is controlled by dislocation nucleation, unlike conventional solid solution strengthening.

36 MATERIALS SCIENCE↗

Smart material based multilayered microbeam structures for spatial self-deployment and reconfiguration: A residual stress approach

Alleviation of the potentially damaging effects induced by residual stresses was comprehensively investigated in previous research. Here, this paper, however, presents a spatially self-deployable and reconfigurable multilayered microbeam which takes advantage of residual stresses and shape memory effects. Reconfigurable mechanism of a typical four-layered microbeam composed of Pt\Ni 50 Ti 50 \Ni 50 Ti 50 \Pt is introduced, followed by analytical modeling of the maximum distance of the self-deployed gap as functions of variable structural and material parameters, including compressive residual stress in Pt layers and tensile residual stress in Ni 50 Ti 50 layers. Analytical solutions given by the static model agree well with the results obtained via finite element models (FEMs). Fabrication, characterization, and in-situ experiments were carried out to validate the feasibility of deployment of the as-released four-layered microbeam. The maximum distance of the gap was measured to be 41.39 μm at 20 °C, which could be increased to 51.73 μm thanks to controllable reconfiguration driven by shape memory effects. Theoretical analysis of such self-deployment and reconfiguration suggested a tensile residual stress increase by 52 MPa in Ni 50 Ti 50 layers. The multilayered microbeam structure with capabilities of self-deployment and reconfiguration offers great potential for various emerging applications, such as micro robotics, medical drug delivery devices, and intelligent chip scale spacecraft.

36 MATERIALS SCIENCE↗

Modeling Sequences of Earthquakes and Aseismic Slip (SEAS) in Elasto-Plastic Fault Zones With a Hybrid Finite Element Spectral Boundary Integral Scheme

We present a coupled finite element spectral boundary integral framework for modeling sequences of earthquakes and aseismic slip on a 2-D planar rate-and-state fault with off-fault visco-plastic response in the plane strain approximation. The model resolves both slow aseismic deformation and inertia effects during rapid slip. As an application, we perform two sets of simulations with different choices of cohesion to explore the co-evolution of fault slip, bulk plasticity and local stress fields. The first set implements a relatively large value of the cohesion parameter, which results in limiting inelastic strain accumulation to dynamic rupture phases. The second set implements a smaller cohesion, allowing for plastic strain to accumulate in both seismic and aseismic phases. For the first model, our results indicate that the extent and distribution of plastic strain depend on the angle of maximum compressive principal stress. At larger angles, inelastic strain accumulates on the extensional side of a dynamically propagating rupture. At smaller angles, the extent of plasticity is limited to the compressional side of the domain. At smaller cohesion values, off-fault plasticity may occur during aseismic slip, which alters the nucleation characteristics and earthquake sequence pattern. Furthermore, our results at lower cohesion values indicate that plastic strain accumulation may occur in both the extensional and compressional sides of the off-fault bulk even at higher angles of maximum compression. In conclusion, this produces damage patterns that deviate from the traditional off-fault fan-like distribution observed in dynamic rupture simulations and emphasizes the significance of long-term deformation in interpreting observations.

58 GEOSCIENCES↗

Designing the stripe-ordered cuprate phase diagram through uniaxial-stress

The ability to efficiently control charge and spin in the cuprate high-temperature superconductors is crucial for fundamental research and underpins technological development. Here, we explore the tunability of magnetism, superconductivity and crystal structure in the stripe phase of the cuprate La 2-x Ba x CuO 4 , with x = 0.115 and 0.135, by employing temperature-dependent (down to 400 mK) muon-spin rotation and AC susceptibility, as well as X-ray scattering experiments under compressive uniaxial stress in the CuO 2 plane. A sixfold increase of the 3-dimensional (3D) superconducting critical temperature T c and a full recovery of the 3D phase coherence is observed in both samples with the application of extremely low uniaxial stress of 0.1 GPa. This finding demonstrates the removal of the well-known 1/8-anomaly of cuprates by uniaxial stress. On the other hand, the spin-stripe order temperature as well as the magnetic fraction at 400 mK show only a modest decrease under stress. Moreover, the onset temperatures of 3D superconductivity and spin-stripe order are very similar in the large stress regime. However, a substantial decrease of the magnetic volume fraction and a full suppression of the low-temperature tetragonal structure is found at elevated temperatures, which is a necessary condition for the development of the 3D superconducting phase with optimal T c . Our results evidence a remarkable cooperation between the long-range static spin-stripe order and the underlying crystalline order with the three-dimensional fully coherent superconductivity. Overall, these results suggest that the stripe- and the SC order may have a common physical mechanism.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effects of elevated temperature exposure on the residual stress state and microstructure of PVD Cr coatings on SiC investigated via in situ X-ray diffraction and transmission electron microscopy

Pure Cr coatings are being considered as corrosion-resistant layers for SiC-SiC f composite fuel cladding in light water reactors. The residual stress state and interdiffusion behavior of Cr coatings deposited on SiC substrates using bipolar high-power impulse magnetron sputtering (B-HiPIMS) and direct current impulse magnetron sputtering (DCMS) were studied using in situ X-ray diffraction experiments at 300 °C, 700 °C, and 1200 °C. After elevated temperature exposure, evolution of the coating microstructure and coating/substrate interdiffusion was characterized by transmission electron microscopy. The compressive residual stress of the dense B-HiPIMS coating at room temperature was gradually relieved at 300 °C, while the stress transitioned to a tensile state at 700 °C. Grain growth of the Cr coating and a Cr–SiC interdiffusion layer consisting of newly formed Cr–C and Cr–Si phases were observed in the B-HiPIMS coating after exposure at 700 °C. The phases in the interdiffusion layer were identified to be Cr 7 C 3 , Cr 3 Si, and Cr 5 Si 3 C x experimentally and by thermodynamic predictions. For the DCMS coating, however, changes in residual stress and microstructure at the elevated temperatures were limited by the inherent porosity and inhomogeneous structure of the as-deposited coating. At 1200 °C, both coating types interacted rapidly with the underlying SiC substrate in the early stages of the experiment. The results from this study suggest that the characteristics of the Cr coatings do not significantly change at the reactor operating temperature of 300 °C, while changes in microstructure and stress state are expected in off-normal conditions of 700 °C and 1200 °C. Finally the results from this study suggest the B-HiPIMS coating is best-suited as a protective coating for SiC fuel cladding.

36 MATERIALS SCIENCE↗

FY2025 Status Report: Model 9975 O Ring Fixture Long-Term Leak Performance

Leak testing experiments to monitor the aging performance of Viton® GLT and GLT-S O-rings used in the model 9975 shipping package have been ongoing since 2004 at Savannah River National Laboratory. Seventy tests using mock-up 9975 primary containment vessels (PCVs) with GLT O-rings were assembled and heated to temperatures ranging from 200 to 450 °F. Due to material substitution, fourteen tests with GLT-S O-rings were initiated in 2008 and heated to temperatures ranging from 200 to 400 °F. The conditioning temperatures are elevated compared to the calculated maximum O-ring temperature in a 9975 package in storage, 158 °F, to accelerate aging and enable observations of O-ring failures in a reasonable time frame. The mock-up PCV fixtures are leak tested periodically, and all GLT O-ring fixtures aged at 350 °F or above have failed to maintain a leak-tight seal. Eight GLT O-ring fixtures aged at 300 °F have failed after 2.8 to 5.7 years at temperature while the remaining fixtures at 300 °F were retired from testing following more than five years of aging without failure. Two of these retired fixtures were returned to testing and heated to 350 °F to evaluate the impact of additional heating at higher temperature for aged O-rings. Fixture #20 failed after 3 months while fixture #18 failed after 9 months at 350 °F. These O-rings demonstrated that aged and in-service O-rings can continue to be used, even at higher temperatures, after being in storage, and their leak performance are consistent with other samples at 350 °F. There has been one GLT O-ring fixture which failed after 13.4 years of aging at 200 °F. However, 20 other GLT O-rings aging at 200 °F have remained leak-tight for over 16.9 years and remain in test. There are two GLT O-ring fixtures at 270 °F; one fixture has failed after 12.9 years while the other fixture remains in test after 12.5 years. All GLT-S O-ring fixtures aged at 300 °F or above have failed their leak test. No failures have yet been observed in GLT-S O-ring fixtures aging at 250 °F for 14.9 years, while one GLT-S O-ring fixture failed after 12.4 years at 200 °F. The leak testing data to date suggest the GLT and GLT-S O-rings aging in the K-Area Complex (KAC) storage at temperatures of 158 °F might maintain a leak-tight seal for up to 59 years. Data from the O-ring fixtures are generally consistent with results from compression stress-relaxation testing and provide confidence in the predictive models based on those results. However, uncertainty exists in extrapolating these elevated temperature results to the lower temperatures of interest for normal storage in KAC. The collective data from these test efforts suggest the minimum O-ring service life at KAC normal storage conditions should be at least 34 years for GLT and GLT-S O-rings. Measurement of compression set in O-rings removed from failed fixtures, compared to that from KAC surveillance O-rings, indicate significant margin remains for O-rings still in service in 9975 packages in KAC. Aging and periodic leak testing will continue for the remaining 24 mock-up PCV fixtures.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Evolution of Microstructure, Residual Stress, and Tensile Properties of Additively Manufactured Stainless Steel Under Heat Treatments

This study investigated the microstructure, residual stress and tensile properties of the directed energy deposited stainless steel 316L (SS316L) under thermal annealing. Microstructure characterization shows the as-printed sample has laser-generated patterns where dendritic structure is observed at the edge of the patterns and cellular structure dominates the interior region. Here, the thermal annealing at 983 and 1093°C effectively removes the dendritic/cellular structures. Synchrotron X-ray diffraction reveals that the as-fabricated SS316L exhibits compressive residual stress of -197.4 MPa. The stress is greatly relieved to -53.8 MPa after annealing at 1093°C. The room temperature tensile testing indicates that the yield strength and ultimate tensile strength drop from 378 and 502 MPa in the as-printed sample to 258 and 446 MPa in the annealed samples (1093°C), respectively. Our study provides insights into the relationship between microstructure, residual stress, and tensile properties of laser additive manufactured SS316L.

36 MATERIALS SCIENCE↗

Correlating energy density induced residual stress, porosity, and mechanical property variations in directed energy deposition using neutron diffraction and imaging techniques

In a directed energy deposition (DED) process, the energy density deposited into the materials drives the structure and properties. The energy density is influenced by several printing parameters, such as laser power, hatch spacing, scanning speed, etc. In this study, 316L stainless steels samples were fabricated with varying hatch spacing aiming to induce variations in sample microstructure and properties. A combination of techniques including engineering neutron diffraction, neutron computed tomography, and tensile testing, were employed to correlate the structure and macroscopic properties. Porosity was predominantly observed at the bottom of the deposited materials and was effectively reduced by decreased hatch spacing. Correlatively, compressive residual stress was observed at the bottom of the specimens, while internal stress is largely determined by the hatch spacing. The residual stress in general decreases as the hatch spacing decreases. The maximum ultimate tensile strength (UTS) was found to increase from 517.4 to 528.6 MPa with a strain increased from 0.847 to 0.897 as the hatch spacing decreased from 0.45 to 0.42 mm. However, further increase in energy density by reducing the hatch spacing resulted in a significant decrease in UTS (as low as 452 MPa). This work provides new insights from bulk non-destructive techniques into correlating energy density induced residual stress, porosity, and mechanical property variations in directed energy deposition.

316L stainless steel↗

Pervasive symmetry-lowering nanoscale structural fluctuations in the cuprate La 2−𝑥 ⁢Sr 𝑥 ⁢Cu⁢O 4

The cuprate superconductors are among the most widely studied quantum materials, yet there remain fundamental open questions regarding their electronic properties and the role of structural degrees of freedom. Recent neutron and x-ray scattering measurements uncovered exponential scaling with temperature of the strength of orthorhombic fluctuations in the tetragonal phase of La 2−𝑥⁢ Sr 𝑥 ⁢Cu⁢O 4 and Tl 2 ⁢Ba 2 ⁢Cu⁢O 6+𝛿 , unusual behavior that closely resembles prior results for the emergence of superconducting fluctuations, and that points to a common origin rooted in inherent correlated structural inhomogeneity. Here, in this study, we use neutron and x-ray diffuse scattering to provide further insight into structural fluctuations in La 2−𝑥 ⁢Sr 𝑥 ⁢Cu⁢O 4 . We perform measurements up to temperatures that approach the melting point of the undoped parent compound, and we investigate the effects of in situ in-plane uniaxial elastic stress and plastic deformation. Our neutron scattering results for the parent compound La 2 ⁢Cu⁢O 4 reveal that short-range orthorhombic fluctuations persist to the maximum experimental temperature of nearly 1000 K, i.e., to a significant fraction of the crystallization temperature. At this temperature, the spatial characteristic length extracted from the momentum-space data is still about three lattice constants. The neutron scattering experiment enables quasistatic discrimination and reveals that the response is increasingly dynamic at higher temperatures. We also find that neither compressive elastic stress along the tetragonal [110] direction nor irreversible plastic deformation activating the ⟨100⟩⁢[001] slip system significantly alter the robust orthorhombic fluctuations. Overall, these results support the notion that these fluctuations couple to subtle, underlying inhomogeneity that underpins the cuprate phase diagram. Finally, in La 1.8⁢ Sr 0.2⁢ Cu⁢O 4 , we uncover low-energy structural fluctuations at a nominally forbidden reflection that are distinct from the orthorhombic distortions. While the origin of these fluctuations is not clear, they might be related to the presence of extended defects such as dislocations or stacking faults.

Spieker, R. J. [Univ. of Minnesota, Minneapolis, M↗

Model 9975 O-Ring Fixture Long-Term Leak Performance (FY2020 Status Report)

Leak testing experiments to monitor the aging performance of Viton GLT and GLT-S O-rings used in the model 9975 shipping package has been ongoing since 2004 at Savannah River National Laboratory. Seventy tests using mock-up 9975 primary containment vessels (PCVs) with GLT O-rings were assembled and heated to temperatures ranging from 200 to 450 °F. In addition, fourteen tests with GLT-S O-rings were initiated in 2008 and heated to temperatures ranging from 200 to 400 °F. The conditioning temperatures are elevated compared to the calculated maximum O-ring temperature in a 9975 package in storage, 158 °F, to accelerate aging and enable observations of O-ring failures in a reasonable time frame. The fixtures are leak tested periodically and all GLT O-ring fixtures aging at 350 °F or above have failed to maintain a leak-tight seal. Eight GLT O-ring fixtures aging at 300 °F have failed after 2.8 to 5.7 years at temperature while the remaining fixtures at 300 °F were retired from testing following more than five years without failure. No failures have yet been observed in GLT O-ring fixtures aging at 200 °F for 12 to 14 years or aging at 270 °F for 8.5 years. All GLT-S O-ring fixtures aging at 300 °F or above have failed their leak test. No failures have yet been observed in GLT-S O-ring fixtures aging at 200 and 250 °F for 10 to 10.5 years. Data from the O-ring fixtures are generally consistent with results from compression stress-relaxation testing, and provide confidence in the predictive models based on those results. However, uncertainty exists in extrapolating these elevated temperature results to the lower temperatures of interest for normal storage in K-Area Complex (KAC). Oxygen consumption testing, which includes results from temperatures near KAC normal storage temperatures, is ongoing to provide further confidence and corroborate these extrapolations. The collective data from these test efforts suggest the minimum O-ring service life at KAC normal storage conditions should be at least 34 years for GLT and GLT-S O-rings. Measurement of compression set in O-rings removed from failed fixtures, compared to that from KAC surveillance O-rings, indicates margin remains for O-rings still in service. Aging and periodic leak testing will continue for the remaining PCV fixtures.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Model 9975 O Ring Fixture LongTerm Leak Performance (FY2021 Status Report)

Leak testing experiments to monitor the aging performance of Viton® GLT and GLT-S O-rings used in the model 9975 shipping package has been ongoing since 2004 at Savannah River National Laboratory. Seventy tests using mock-up 9975 primary containment vessels (PCVs) with GLT O-rings were assembled and heated to temperatures ranging from 200 to 450 °F. Due to material substitution, fourteen tests with GLT-S O-rings were initiated in 2008 and heated to temperatures ranging from 200 to 400 °F. The conditioning temperatures are elevated compared to the calculated maximum O-ring temperature in a 9975 package in storage, 158 °F, to accelerate aging and enable observations of O-ring failures in a reasonable time frame. The fixtures are leak tested periodically and all GLT O-ring fixtures aging at 350 °F or above have failed to maintain a leak-tight seal. Eight GLT O-ring fixtures aging at 300 °F have failed after 2.8 to 5.7 years at temperature while the remaining fixtures at 300 °F were retired from testing following more than five years without failure. There has been one GLT O-ring fixture which failed after 13.4 years aging at 200 °F. However, 19 other GLT O-rings aging at 200 °F have remained leak-tight for over 14 years and remain in test. No failures have yet been observed in GLT O-ring fixtures aging at 270 °F for 9.5 years. All GLT-S O-ring fixtures aging at 300 °F or above have failed their leak test. No failures have yet been observed in GLT-S O-ring fixtures aging at 200 and 250 °F for 11.5 years. Data from the O-ring fixtures are generally consistent with results from compression stress-relaxation testing, and provide confidence in the predictive models based on those results. However, uncertainty exists in extrapolating these elevated temperature results to the lower temperatures of interest for normal storage in K-Area Complex (KAC). Oxygen consumption testing, which includes results from temperatures near KAC normal storage temperatures, is ongoing to provide further confidence and corroborate these extrapolations. The collective data from these test efforts suggest the minimum O-ring service life at KAC normal storage conditions should be at least 34 years for GLT and GLT-S O-rings. Measurement of compression set in O-rings removed from failed fixtures, compared to that from KAC surveillance O-rings, indicate significant margin remains for O-rings still in service in 9975 packages in KAC. Aging and periodic leak testing will continue for the remaining 26 mock-up PCV fixtures.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Model 9975 O-Ring Fixture Long-Term Leak Performance (FY2022 Status Report)

Leak testing experiments to monitor the aging performance of Viton® GLT and GLT-S O-rings used in the model 9975 shipping package has been ongoing since 2004 at Savannah River National Laboratory. Seventy tests using mock-up 9975 primary containment vessels (PCVs) with GLT O-rings were assembled and heated to temperatures ranging from 200 to 450 °F. Due to material substitution, fourteen tests with GLT-S O-rings were initiated in 2008 and heated to temperatures ranging from 200 to 400 °F. The conditioning temperatures are elevated compared to the calculated maximum O-ring temperature in a 9975 package in storage, 158 °F, to accelerate aging and enable observations of O-ring failures in a reasonable time frame. The fixtures are leak tested periodically and all GLT O-ring fixtures aging at 350 °F or above have failed to maintain a leak-tight seal. Eight GLT O-ring fixtures aging at 300 °F have failed after 2.8 to 5.7 years at temperature while the remaining fixtures at 300 °F were retired from testing following more than five years without failure. There has been one GLT O-ring fixture which failed after 13.4 years aging at 200 °F. However, 20 other GLT O-rings aging at 200 °F have remained leak-tight for over 14 years and remain in test. No failures have yet been observed in GLT O-ring fixtures aging at 270 °F for 10.4 years. All GLT-S O-ring fixtures aging at 300 °F or above have failed their leak test. No failures have yet been observed in GLT-S O-ring fixtures aging at 250 °F for 12.5 years. This year, one GLT-S O-ring fixture failed after 12.4 years aging at 200 °F. Data from the O-ring fixtures are generally consistent with results from compression stress-relaxation testing, and provide confidence in the predictive models based on those results. However, uncertainty exists in extrapolating these elevated temperature results to the lower temperatures of interest for normal storage in K-Area Complex (KAC). Oxygen consumption testing, which includes results from temperatures near KAC normal storage temperatures, is ongoing to provide further confidence and corroborate these extrapolations. The collective data from these test efforts suggest the minimum O-ring service life at KAC normal storage conditions should be at least 34 years for GLT and GLT-S O-rings. Measurement of compression set in O-rings removed from failed fixtures, compared to that from KAC surveillance O-rings, indicate significant margin remains for O-rings still in service in 9975 packages in KAC. Aging and periodic leak testing will continue for the remaining 25 mock-up PCV fixtures.

36 MATERIALS SCIENCE↗

Modeling Validation of Mechanical and Thermal Borehole Breakouts From Polyaxial Laboratory Tests to Determine Maximum Horizontal in Situ Stress

To accurately assess rock behavior in the deep subsurface, it is necessary to measure the in situ stress directions and magnitudes. The current methods for measuring the in situ stress state in the deep subsurface primarily include hydraulic fracturing tests (i.e., the minimum horizontal stress) or occasionally observing existing compressive borehole breakouts (i.e., the maximum horizontal stress) that have occurred naturally from drilling. If there are no existing compressive breakouts in a borehole, the maximum horizontal in situ stress cannot be estimated with much confidence. In response to this data gap, a new thermal breakout technology is being developed that will provide a method for thermally inducing borehole breakouts and obtaining consistent measurements of the maximum horizontal stress magnitude. This thermal breakout technology involves heating the borehole and increasing the thermoelastic compressive stress in the rock until a breakout develops, which is directly correlated to the maximum horizontal stress magnitude. In support of developing the thermal breakout technology, polyaxial laboratory tests have been performed on small-scale boreholes within rock blocks where mechanically- and thermally-induced borehole breakouts have been created. Numerical models along with the principal of superposition were created and used to analyze the polyaxial laboratory tests to predict the maximum horizontal stress, given the same data that would be obtained in an actual subsurface borehole thermal breakout test. Multiple failure criteria were used to evaluate the best prediction of the breakout onset and maximum horizontal stress. The maximum horizontal stress predictions were compared to the actual maximum horizontal stress applied at breakout using acoustic events recorded from emission sensors in the polyaxial tests. The results showed consistent results that could be used to refine the modeling approach and failure criterion that are used to make the maximum horizontal stress predictions. This study provided insight and validation for the thermal breakout stress measurement concept.

Jones, Matt↗

Dynamic response of 17-4 stainless steel as a function of manufacturing method and heat treatment

We present a series of plate-impact experiments on 17-4 stainless steel to study the effect of manufacturing method and heat treatment on the Hugoniot elastic limit (HEL), Hugoniot, phase transformation stress, and spallation strength. Two traditional manufacturing methods were considered, wrought processing and casting, as well as two additive manufacturing methods, laser powder-bed fusion (LPBF) and wire-fed electron beam (EBAM). For both LPBF and EBAM 17-4 stainless steel variants, two billets were printed, enabling the application of two unique heat treatments. The HEL stress depended heavily on the thermal history, with the HEL increasing after the formation of Cu-rich precipitates via heat treatment. The Hugoniot response both below and above the phase transition was unaffected by the manufacturing method or heat treatment. The phase transition stress depended heavily on the thermal history, with its variation being attributed to the presence of various microstructural features. This is supported by a marked increase in the phase transition stress after precipitation hardening. These results suggest that the notion of the phase transition stress being dictated by bulk composition is an oversimplification and the stress fields generated by the meso-scale structure are a dominant force. The spallation strength was lower in the cast material compared to all other 17-4 stainless steel variants due to the presence of brittle δ-ferrite inclusions. Additionally, a drop in the tensile strain-rate was observed in the spallation response above the phase transition stress, which was hypothesized to stem from the kinetics of the reversion to the low-pressure phase during spall.

Compressive stress↗