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At least 1,351 records · Page 75

Helium-implantation-induced lattice strains and defects in tungsten probed by X-ray micro-diffraction

Tungsten is the main candidate material for plasma-facing armour components in future fusion reactors. Bombardment with energetic fusion neutrons causes collision cascade damage and defect formation. Interaction of defects with helium, produced by transmutation and injected from the plasma, modifies defect retention and behaviour. Here we investigate the residual lattice strains caused by different doses of helium-ion-implantation into tungsten and tungsten-rhenium alloys. Energy and depth-resolved synchrotron X-ray micro-diffraction uniquely permits the measurement of lattice strain with sub-micron 3D spatial resolution and ~10 -4 strain sensitivity. Increase of helium dose from 300 appm to 3000 appm increases volumetric strain by only ~2.4 times, indicating that defect retention per injected helium is ~3 times higher at low helium doses. This suggests defect retention is not a simple function of implanted helium dose, but strongly depends on material composition and presence of impurities. Conversely, analysis of W-1 wt% Re alloy samples and of different crystal orientations shows that both the presence of rhenium, and crystal orientation, have a comparatively small effect on defect retention. These insights are key for the design of armour components in future reactors where it will be essential to account for irradiation-induced dimensional change when predicting component lifetime and performance.

36 MATERIALS SCIENCE↗

Structural and optical effects induced by gamma irradiation on NdPO{sub 4}: X-ray diffraction, spectroscopic and luminescence study

Highlights: • Inorganic NdPO{sub 4} crystal was grown first time using potassium polyphosphate (K{sub 6}P{sub 4}O{sub 13}) flux. • NdPO{sub 4} crystal is insoluble in water, non-hygroscopic and high radiation resistance favoring for actinides host. • Actinide immobilization can be made at 1273 K. • High yield of 1061 nm photon emission. - Abstract: Rare earth orthophosphate (NdPO{sub 4}) monazite single crystals were grown using high temperature flux growth method employing K{sub 6}P{sub 4}O{sub 13} (K{sub 6}) as molten solvent. Their structural parameters were studied using single crystal X-ray diffraction (XRD) method. The grown crystals were examined by SEM and EDX techniques for their homogeniousity and inclusion in the crystals. The influence of gamma irradiation in structural and optical absorption properties were studied by the powder XRD, FTIR and reflectance spectroscopy. The effect of gamma irradiation on luminescence properties was recorded. No significant structural change is observed up to 150 kGy gamma dose. The gamma ray induced charge trap in the crystal was saturated to 40 kGy dose. The luminescence intensity decreases with an increase in the irradiation. The emission of luminescence intensity stabilizes above 40 kGy gamma dose.

36 MATERIALS SCIENCE↗

In situ neutron diffraction analyses of temperature and stresses during friction stir processing of Mg-3Al-1Zn magnesium alloy

In this paper, the evolution of temperature and thermal stresses were examined during friction stir processing of a magnesium alloy using in situ neutron diffraction. Measured total lattice strains were de-convoluted into the thermal and stress components. Finally, it shows the maximum temperature of 464 °C and compressive stress distributions up to -52 MPa underneath the tool via the thermo-mechanical deformation in terms of the Zener-Hollomon parameter of 4.51 × 10 10 s -1 .

36 MATERIALS SCIENCE↗

Residual stress distribution in an additively manufactured complex structure by neutron diffraction measurement

Residual stress in an aerodynamically shaped Ni-based superalloy airfoil fabricated by laser powder bed fusion was measured by neutron diffraction. The experiment was conducted by considering the complex shape, implementing computer aided experiment planning, and automatic alignment at each rapid measurement. The 3-dimensional (3D) residual stress distribution in the airfoil is presented in this work, which lacks symmetry due to the complex geometry of the airfoil. In conclusion, the results provide theoretical thermal processing models a complete residual stress dataset of simulation validation on 3D shape complex structure.

Residual stress↗

Probing lead acetate in solution using X-ray diffraction

Here, for the purpose of water purification involving toxic metal sensing and removal, high energy X-ray diffraction experiments have been performed on lead acetate Pb(Ac) 2 solutions, liquid and amorphous glutathione disulfide (GSSG), and their mixtures. The data have been interpreted using Empirical Potential Structure Refinement and pair distribution function analysis. At the highest concentration of 1 M Pb(Ac) 2 in water, the lead molecules are found to cluster and the second shell in the water structure becomes slightly more ordered as the water molecules become compressed. Liquid and amorphous GSSG are found to hydrogen bond primarily via OH-O interactions, while NH-O bonds are much more distorted. Aqueous solutions of Pb(Ac) 2 + GSSG show the closest Pb-O (carboxyl) and Pb-N (amine) bonds both at a distance of 2.5 ± 0.1 Å at a concentration of 1 M Pb(Ac) 2 in water. At 0.75 M Pb(Ac) 2 in water, strong Pb-S bonds are found at a distance of 2.8 ± 0.1 Å. The implications for lead removal using capacitive deionization are discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In-situ TOF neutron diffraction studies of cyclic softening in superelasticity of a NiFeGaCo shape memory alloy

Real-time in-situ neutron diffraction was conducted during uniaxial cycling compression of a Ni 49.3 Fe 18 Ga 27 Co 5.7 shape memory alloy to explore the mechanism on its superelasticity at room temperature, which was manifested by the almost recoverable large strains and the apparent cyclic softening. Based on the Rietveld refinements, the real-time evolution of volume fraction of martensite was in-situ monitored, indicating the incremental amount of residual martensite with increasing load cycles. Real-time changes in intensities and lattice strains of { hkl } reflections for individual phase were obtained through fitting individual peaks, which reveal the quantitative information on phase transformation kinetics as a function of grain orientation and stress/strain partitioning. Moreover, a large compressive residual stress was evidenced in the parent phase, which should be balanced by the residual martensite after the second unloading cycle. As a result, the large compressive residual stress found in the parent austenite phase may account for the cyclic effect on critical stress required for triggering the martensitic transformation in the subsequent loading.

36 MATERIALS SCIENCE↗

Study on the residual stress relaxation in girth-welded steel pipes under bending load using diffraction methods

This research is dedicated to the experimental investigation of the residual stress relaxation in girth-welded pipes due to quasi-static bending loads. Ferritic-pearlitic steel pipes are welded with two passes, resulting in a characteristic residual stress state with high tensile residual stresses at the weld root. Also, four-point bending is applied to generate axial load stress causing changes in the residual stress state. These are determined both on the outer and inner surfaces of the pipes, as well as in the pipe wall, using X-ray and neutron diffraction. Focusing on the effect of tensile load stress, it is revealed that not only the tensile residual stresses are reduced due to exceeding the yield stress, but also the compressive residual stresses for equilibrium reasons. Furthermore, residual stress relaxation occurs both parallel and perpendicular to the applied load stress.

36 MATERIALS SCIENCE↗

In situ neutron diffraction in quantifying deformation behaviors of nano-sized carbide strengthened UFG ferritic steel

Here, the microstructures and mechanical properties of a low-alloy medium-carbon steel with a duplex microstructure composed of nanoscale spheroidized carbides in ultrafine-grained (UFG) ferritic steel are examined. The average grain size of the studied steel is ~ 430 nm, and these grains coexist with numerous carbides. Neutron diffraction reveals that the intensity of (011) and (022) peaks for the UFG sample is significantly enhanced, suggesting that the (011)//RD texture is a result of the warm rolling process. The lattice parameter of UFG steel is smaller than that of a martensitic steel (M steel) counterpart, indicating a lower carbon concentration in the lattice. The estimated dislocation densities for M steel and UFG steel are 2.59 × 10 14 cm –2 and 1.76 × 10 12 cm –2 , respectively. The UFG steel reveals a nearly isotropic lattice strain response under initial tension from 0 to 450 MPa, where the lattice strains of the (110), (002), and (112) planes are identical. The increase of lattice strain of the (110) plane becomes smaller than that of the (002) and (112) planes as the stress exceeds 450 MPa, suggesting that the nanosized carbides contribute to the hardening ability by promoting the accumulation of geometrically necessary dislocations around the particles, and the (110) lattice becomes harder compared to the other two planes.

36 MATERIALS SCIENCE↗

In situ high-energy X-ray diffraction investigation of the micromechanical behavior of Fe-0.1C-10Mn-0/2Al steel at room and elevated temperatures

The micromechanical behavior of medium-Mn transformation-induced-plasticity (TRIP) steels with nominal chemical compositions of Fe-0.1C-10Mn (mass%) (0Al steel) and Fe-0.1C-10Mn-2Al (mass%) (2Al steel) fabricated by intercritical annealing 600 degrees C for 1 h and 650 degrees C for 1 h, respectively, was investigated using in situ high-energy X-ray diffraction (HE-XRD) with uniaxial tensile tests at 25 degrees C and 100 degrees C. We found that Liiders band propagation promoted lower volume fraction of austenite transformation to martensite in 0Al steel than 2Al steel at 25 degrees C while higher volume fraction of austenite transformation to martensite in 0Al steel than 2Al steel at 100 degrees C. Portevin-Le Chatelier (PLC) band propagation promoted higher volume fraction of austenite transformation to martensite in 0Al steel than 2Al steel during deformation at 25 degrees C and 100 degrees C. Moreover, the addition of Al obviously suppresses the formation of intermediate epsilon martensite during tensile deformation, thus the zigzag change in lattice strain of austenite was completely depressed in 2Al steel. Due to the controlled stability of metastable austenite, the 2Al steel demonstrated the best combination of ultimate tensile strength and total elongation at 25 degrees C.

36 MATERIALS SCIENCE↗

A brittle fracture mechanism in thermally aged duplex stainless steels revealed by in situ high-energy X-ray diffraction

A direct relationship between the microstructural evolution and macroscopic fracture behaviors of a thermally aged (at 475 °C for 400 h) duplex stainless steel (DSS) has been established with experimental results from atom probe tomography (APT), nanoindentation and in situ synchrotron-based high-energy X-ray diffraction (HE-XRD). Furthermore, the APT experiments demonstrate that ferrite in DSS spinodally decomposes into Cr-enriched and Cr-depleted domains during thermal aging, which leads to a severe hardening effect in ferrite. The lattice strain development during deformation acquired with the in situ HE-XRD measurements confirms the cleavage fracture of α{110} and α{200} ferrite grains aligned perpendicular to loading direction. The thermally aged DSS can be readily fractured by connecting the cleavage cracks in ferrite. Conclusively, the spinodal-decomposition-induced hardening in ferrite and the premature failure of ferrite control the final brittle fracture in the aged DSS.

36 MATERIALS SCIENCE↗

In situ investigation of the deformation behaviors of Fe 20 Co 30 Cr 25 Ni 25 and Fe 20 Co 30 Cr 30 Ni 20 high entropy alloys by high-energy X-ray diffraction

In situ synchrotron-based high-energy X-ray diffraction (HE-XRD) technique was employed to investigate the mechanical behaviors and microstructural evolution of face-centered cubic (FCC) Fe 20 Co 30 Cr 25 Ni 25 and Fe 20 Co 30 Cr 30 Ni 20 high entropy alloys (HEAs) during tensile deformation. Fe 20 Co 30 Cr 30 Ni 20 HEA has a good combination of strength (ultimate tensile strength of 864 ± 35 MPa) and ductility (elongation of 0.627 ± 0.021). The HE-XRD investigation reveals that Fe 20 Co 30 Cr 30 Ni 20 HEA has the transformation-induced plasticity (TRIP) effect, which starts at a critical stress of ~555 MPa. Furthermore, transmission electron microscopy confirmed this deformation-induced new phase is hexagonal-close-packed structured ε-martensite, which follows an orientation relationship of {111} γ //(0001) ε , and (110) γ //[11 2 ¯ 0] ε with the FCC γ matrix. The observation of deformation twins in the deformed samples of the two studied HEAs proves that twinning-induced plasticity (TWIP) effect occurs in both HEAs. The combination of TRIP and TWIP effects lead to the high strength, large ductility and improved strain hardening behavior of Fe 20 Co 30 Cr 30 Ni 20 HEA.

36 MATERIALS SCIENCE↗

In-situ neutron diffraction investigation of two-stage martensitic transformation in a 13%Mn steel with serrated deformation

Two stage austenite →ε-martensite →α-martensite phase transformation, phase-specific lattice strain evolution and load sharing during tensile deformation of a 13%Mn hot-rolled austenitic steel are revealed by in-situ neutron diffraction. In conclusion, direct evidence is provided that serrated deformation behavior is attributed to discontinuous martensitic transformation.

Austenitic steel↗

The formation and evolution of Ni 2 Cr precipitates in Ni–Cr model alloys as a function of stoichiometry characterized by synchrotron x-ray diffraction

Ni-based alloys containing significant amounts of Cr, may precipitate new phases during long-term service at elevated temperatures. In Ni–Cr model alloys, the formation of Ni 2 Cr has been found to impact the material properties, including the strength and ductility after isothermal aging below the critical temperature of 590°C. In this work, we quantify the formation and evolution of long-range ordering in four Ni–Cr binary model alloys (Ni/Cr = 1.8, 2.0, 2.2, 2.4) after isothermal aging up to 10,000h at temperatures between 373 and 475°C. The alloys were characterized by hardness testing and synchrotron-based x-ray diffraction to quantify the impact of Ni 2 Cr phase fraction and precipitate size on mechanical properties. After 500h of isothermal aging, the formation of Ni 2 Cr was detected in all four alloys at 475°C. In the stochiometric alloy samples (Ni/Cr = 2.0), the formation of Ni 2 Cr was found after 500 and 3000h aging at 418 and 373°C, respectively. We found that the matrix lattice contraction and Ni 2 Cr phase fraction both saturate after early aging times. This is in stark contrast to the hardness and Ni 2 Cr precipitate size that both continue to increase with increasing aging time. Our results highlight that changes in hardness correlate linearly with Ni 2 Cr precipitate size rather than phase fraction. This important structure-property relationship can potentially help define Ni–Cr-based component lifetimes directly through an understanding of how Ni 2 Cr formation impacts strength and ductility. Here, we find that a precipitation hardening model for critical resolved shear stress with weakly coupled dislocations shows good agreement with the material property changes quantified from experimental measurements.

36 MATERIALS SCIENCE↗

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↗

Understanding the asymmetric orientations and stress states in polycrystalline NiTi SMA by in-situ synchrotron-based high-energy X-ray diffraction

The stress-induced martensite transformations (SIMTs) dramatically affect the recoverable strain and mechanical response of polycrystalline NiTi. An in-depth understanding of the propagation manner and orientation preference of SIMTs is therefore crucial. Here, in this work, we present a unique asymmetric anisotropy of SIMTs and lattice strains induced by Lüders-type deformation in polycrystalline NiTi, achieved through a combination of in-situ synchrotron X-ray diffraction and uniaxial tensile loading and unloading experiments. Our experimental findings reveal that in polycrystalline NiTi under uniaxial deformation, the asymmetry of SIMTs is attributed to the inhomogeneous strain field caused by the Lüders-type mechanism. The asymmetrical SIMT starts with the forward Lüder band and disappears along with the backward Lüder band. The austenite with the favored orientation of $\langle$110$\rangle$ A //loading direction (LD) transformed and recovered back at a higher rate compared to other orientations during both loading and unloading.

36 MATERIALS SCIENCE↗

High temperature neutron diffraction investigation of U 3 Si 2

The U-Si system is actively undergoing studies due to its promise as a component of an accident tolerant nuclear fuel. In this work, the crystal structure of the U 3 Si 2 compound in the U-Si system was investigated as a function of temperature from room temperature to 1298 K for a sample of approximately 42.02 at.% Si composition and 1373 K for a sample with approximately 42.10 at.% Si using high temperature time-of-flight neutron diffraction on the High-Pressure Preferred Orientation (HIPPO) diffractometer at Los Alamos Neutron Science Center (LANSCE). The simultaneous Rietveld refinement of five histograms from the five HIPPO detector backs (40°, 60°, 90°, 120°, and 145°) provided datasets for the lattice parameters, anisotropic atomic displacement parameters, and atomic positions as a function of temperature. To explore the possibility of a homogeneity range, two sample compositions were analyzed, a 40.02 at.% Si (near stoichiometric) and a potentially hyperstoichiometric (40.10 at.% Si) sample. While minor differences in the anisotropic atomic displacement parameters between the two samples were observed, over the entire investigated temperature range no additional phases were found indicative of a single phase sample and the ability of the U 3 Si 2 compound to accommodate nonstoichiometry, suggesting that the U 3 Si 2 compound is not a line compound confirming previous determinations. However, the differences observed in the average coefficient of linear thermal expansion identified between the two compositions warrant future investigation.

36 MATERIALS SCIENCE↗

Understanding the interaction of extension twinning and basal-plate precipitates in Mg-9Al using precession electron diffraction

Precession electron diffraction is used to characterize the interaction between ${10\bar{1}2}$ tensile twins and basal plate-like precipitates in a post-deformed, precipitate-dispersed Mg-9Al micropillar. We observed a heterogeneous distribution of precipitates in the micropillar sample, which enabled the study of the different stages involved in twin precipitate interactions. We show that twin nucleation was promoted, taking place on the surface, as well as from the interior of the micropillar. Twin tip propagation and twin growth were hindered by the precipitates. Twin tips either were arrested by precipitates and new twins formed on the other side of the precipitate, or continued to grow around the precipitate without the re-nucleation events. During twin thickening, the precipitates did not significantly alter the shear-dominant twin boundary migration mechanism, as evidenced by the relatively flat twin boundaries around the partially embedded precipitates. However, the twin boundary migration was retarded by the precipitates, especially in regions confined by closely-spaced precipitates.

36 MATERIALS SCIENCE↗

Detector requirements and simulation results for the EIC exclusive, diffractive and tagging physics program using the ECCE detector concept

This article presents a collection of simulation studies using the ECCE detector concept in the context of the EIC’s exclusive, diffractive, and tagging physics program, which aims to further explore the rich quark–gluon structure of nucleons and nuclei. To successfully execute the program, ECCE proposed to utilize the detector system close to the beamline to ensure exclusivity and tag ion beam/fragments for a particular reaction of interest. Preliminary studies confirm the proposed technology and design satisfy the requirements. Further, the projected physics impact results are based on the projected detector performance from the simulation at 10 or 100 fb -1 of integrated luminosity. Additionally, insights related to a potential second EIC detector are documented, which could serve as a guidepost for future development.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗