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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 1,243 records · Page 69
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Three-Dimensional Model of Holographic Formation of Inhomogeneous PPLC Diffraction Structures

A three-dimensional theoretical model of holographic formation of inhomogeneous diffraction structures in composite photopolymer - liquid crystal materials is presented considering both the nonlinearity of recording and the amplitude-phase inhomogeneity of the recording light field. Based on the results of numerical simulation, the kinematics of formations of such structures and their spatial profile are investigated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Measuring grain boundary character distributions in Ni-base alloy 725 using high-energy diffraction microscopy

We use high-energy X-ray diffraction microscopy (HEDM) to characterize the microstructure of Ni-base alloy 725. HEDM is a non-destructive technique capable of providing three-dimensional reconstructions of grain shapes and orientations in polycrystals. The present analysis yields the grain size distribution in alloy 725 as well as the grain boundary character distribution (GBCD) as a function of lattice misorientation and boundary plane normal orientation. We find that the GBCD of Ni-base alloy 725 is similar to that previously determined in pure Ni and other fcc-base metals. We find an elevated density of Σ9 and Σ3 grain boundaries. We also observe a preponderance of grain boundaries along low-index planes, with those along (1 1 1) planes being the most common, even after Σ3 twins have been excluded from the analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2017

In Situ Neutron Diffraction Study of the Influence of Microstructure on the Mechanical Response of Additively Manufactured 304L Stainless Steel

In situ neutron diffraction measurements were completed for this study during tensile and compressive deformation of stainless steel 304L additively manufactured (AM) using a high power directed energy deposition process. Traditionally produced wrought 304L material was also studied for comparison. The AM material exhibited roughly 200 MPa higher flow stress relative to the wrought material. Crystallite size, crystallographic texture, dislocation density, and lattice strains were all characterized to understand the differences in the macroscopic mechanical behavior. The AM material’s initial dislocation density was about 10 times that of the wrought material, and the flow strength of both materials obeyed the Taylor equation, indicating that the AM material’s increased yield strength was primarily due to greater dislocation density. Finally, a ~50 MPa flow strength tension/compression asymmetry was observed in the AM material, and several potential causes were examined.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Determination of γ/γ' Lattice Misfit in Ni-Based Single-Crystal Superalloys at High Temperatures by Neutron Diffraction

Constrained γ/γ' lattice misfit as a function of temperature (room temperature, 871 °C, 982 °C, 1093 °C, and 1204 °C) is measured by neutron diffraction on the first-generation Ni-based single-crystal superalloy René N4 and second-generation superalloys René N5, CMSX4, and PWA1484. All the alloys studied show negative misfit at temperatures above 871 °C. For René N4, René N5, and PWA1484, the misfit becomes less negative at temperatures above 1093 °C, possibly due to either the chemistry effect or internal stress relaxation. The magnitude of the misfit shows a qualitative agreement with Caron’s misfit model based on Vegard’s coefficients. The Re-free alloy René N4 was found to have a larger γ lattice parameter and γ/γ' misfit due to higher fractions of Cr, Ti, and Mo. After 100 hours of annealing at high temperatures, René N5 shows a more negative misfit than the misfit after the standard heat treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Neutron Diffraction and Neutron Radiography Investigation into Powder Sintering of Ti/Al and TiH{sub 2}/Al Compacts

Sintering behaviors of two types of powder compact, i.e., Ti/Al and TiH{sub 2}/Al, under vacuum were studied using in situ neutron diffraction, in situ thermal dilatometric measurement, and ex situ neutron radiography. Their densification, microstructure, hydrogen concentration, and phase transformation features were compared. The results indicate that the predominant phase identified in the samples sintered from both compacts is γ-TiAl phase with minor Ti{sub 3}Al phase. Dehydrogenation of TiH{sub 2} plays a decisive role in the sintering behavior and the resultant microstructure. In comparison with the Ti/Al compact, dehydrogenation occurring in the TiH{sub 2}/Al compact leads to a higher level of densification and faster sintering kinetics.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Electron Backscattered Diffraction Study of Microstructural Evolution During Isothermal Deformation of High-N Mn18Cr18 Alloy

In order to understand the dynamic recrystallization (DRX) mechanism of Mn18Cr18N austenitic stainless steel during hot deformation, the investigation of microstructure evolution is significant. Isothermal compression tests were conducted on a Gleeble-3500 thermomechanical simulator in the temperature range of 950 °C to 1150 °C and strain rate range between 0.001 and 1 s{sup −1}. Optical microscopy (OM) and electron backscattered diffraction (EBSD) were employed to study the resultant microstructures. More grain boundary information of hot-deformed specimens was provided by EBSD. It was found that the fraction of low-angle grain boundaries (LAGBs) increases with the decrease of deformation temperature or the increase of strain rate and can be expressed as a function of the Zener–Hollomon parameter. DRX easily occurs at the high deformation temperature and low strain rate. From the flow stress curves, the occurrence of single peak behavior and multiple transient steady-state (MTSS) behavior illustrated the existence of different DRX mechanisms. The EBSD analysis indicated that both continuous dynamic recrystallization (CDRX) and discontinuous dynamic recrystallization (DDRX) existed during hot deformation. For the low fraction of 10 to 15 deg misorientation, CDRX is the minor DRX mechanism while DDRX is the major DRX mechanism for the studied steel.

36 MATERIALS SCIENCE↗
DOE OSTI2018

X-ray Diffraction Investigation of Annealing Behavior of Peened Surface Deformation Layer on Precipitation Hardening Stainless Steel

In order to investigate the recrystallization behavior of peened surface deformation layer of precipitation hardening stainless steel, a classic x-ray diffraction line profile analysis, Voigt method, was carried out on peened 17-4PH with different isothermal annealing temperatures. The activation energy of domain boundary migration (Q{sub a}) and the activation energy of microstrain relaxation (Q{sub b}) were calculated by regression analysis in different annealing temperature conditions. The results show that the value of Q{sub a} decreases with annealing temperature increasing, which is due to the influence of precipitation (ε-Cu) size on the movements of grain and subgrain boundaries. The maximum growth rate of ε-Cu particles occurs during 400 to 500 °C interval. Compared with growth behavior of domain size, microstrain relaxation behavior is less sensitive to precipitation particle size. The effects of annealing temperature and time on dislocation density are both significant when annealing temperature is lower than 500 °C. However, the effect of annealing temperature on dislocation density becomes insignificant when annealing temperature is higher than 500 °C. 300 °C annealing temperature only leads to the microstrain relaxation but nearly cannot lead to the domain size growth even if prolonging annealing time. Microstructure enhancement effect still exists in plastic deformation layer when 300 °C annealing temperature lasts for 60 min but nearly disappears when 600 °C annealing temperature lasts for 20 min.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Electron Backscattered Diffraction Study of Pulse Electrodeposited Cu-Y{sub 2}O{sub 3} Composite Coating

The current investigation is an effort of correlating the grain growth, crystallographic orientation and second-phase Y{sub 2}O{sub 3} particles to the mechanical properties of the electrodeposited pure copper (Cu) and Cu-Y{sub 2}O{sub 3} coatings. Energy-dispersive spectrum and elemental mapping confirm the codeposition of Y{sub 2}O{sub 3} in the composite coating matrix, which indeed justifies the composite (Cu-Y{sub 2}O{sub 3}) coating. Both pure Cu and Cu-Y{sub 2}O{sub 3} coatings have (101) preferred orientation; however, the volume fraction is found comparatively lower in composite coating. Both microstructural and textural characterization through electron backscattered diffraction technique show significant grain refinement in case of Cu-Y{sub 2}O{sub 3} composite coating compared to pure Cu coating, and prominent 〈011〉 fiber texture is observed in case of pure Cu coating compared to composite coating. By the addition of second-phase Y{sub 2}O{sub 3} in the matrix, the 〈011〉 fiber texture is disintegrated and concentrated at ϕ{sub 1} = 37°, ϕ = 45°, ϕ{sub 2} = 0°. Despite lower volume fraction of 〈011〉 fiber texture, better mechanical properties (hardness and wear resistance) of the composite coating compared to pure Cu coating can be attributed to finer grain size, higher misorientation angle and incorporation of second-phase Y{sub 2}O{sub 3} particles.

36 MATERIALS SCIENCE↗
DOE OSTI2018

The Determination of Residual Stress in Quenched and Cold-Compressed 7050 Aluminum Alloy T-Section Forgings by the Contour Method and Neutron Diffraction

Residual stresses were determined through the thickness of quenched and quenched followed by cold compression 7050 aluminum alloy T-section forgings using the contour method and neutron diffraction. 7050 T-section forgings are used for the manufacture of the connecting joints of wing and fuselage. Inevitably high residual stresses are introduced during the quenching process of 7050 T-section forgings, which could be reduced by cold compression to overcome the effect of residual stress on machining deformation. The longitudinal residual stresses obtained by the two techniques achieved good agreement in both trend and magnitude in both the quenched and quenched followed by cold compression 7050 T-section forgings. The stress-free lattice spacing of Al(311), the Bragg reflection used for the neutron measurements, was obtained from a 5-mm slice using the plane-stress condition, and its variation through the thickness is insignificant in both the quenched specimen and quenched followed by cold compression specimen. A comparison of the residual stresses in the quenched specimen and quenched followed by cold compression specimen showed significant changes in range of residual stresses from (− 304, 262 MPa) induced by quenching process to (− 125, 142 MPa) due to 3% cold compression. The percentage reduction in residual stress in the quenched specimen due to 3% cold compression was (46, 59%).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Ambient and High-Temperature Bulk Characterization of Additively Manufactured Ti-6Al-4V Using Neutron Diffraction

Characterization of the bulk microstructure using neutron diffraction has been applied to investigate the phase fractions and textures of α- and β-phases in Ti-6Al-4V fabricated by additive manufacturing. The microstructure of a specimen cut from a fan structure, built by either electron beam melting (EBM) or selective laser melting, indicated that predominantly the build direction and not the fan angle determines the microstructure. In situ heating experiments of specimens from a rod built using EBM provided insight into the lattice strain, phase fraction, and texture evolution, providing a rich picture of the microstructure changes during heat treatment of additively manufactured Ti-6Al-4V. Finally, a remarkably low weight fraction of β-phase at lower temperatures, deviations from thermal expansion behavior attributed to vanadium repartitioning, as well as texture strengthening were observed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Cryogenic Stress-Driven Grain Growth Observed via Microcompression with in situ Electron Backscatter Diffraction

The deformation of materials at cryogenic temperature is of interest for space, arctic, and fundamental science applications. In this work, a custom-built cooling system attached to a commercial picoindenter was used for in situ cryogenic microcompression testing of equal-channel angular-pressed copper with real-time electron backscatter diffraction. Stress-driven grain growth at cryogenic temperatures was observed during a series of elastic and plastic deformations. Finally, these results provide direct evidence for the previously predicted phenomenon, whereas previous ex situ examinations demonstrated coarsening after cryogenic loading when samples were not maintained at cryogenic temperatures between deformation and characterization.

36 MATERIALS SCIENCE↗
DOE OSTI2021

AFRL Additive Manufacturing Modeling Series: Challenge 1, Characterization of Residual Strain Distribution in Additively-Manufactured Metal Parts Using Energy-Dispersive Diffraction

A machine component fabricated by additive manufacturing (AM) of metal powders often possesses steep residual stress gradients with significant magnitudes due to large temperature gradients that transpire within a localized area during fabrication. These processing-induced residual stresses can cause distortion of the part, and if they are of significant magnitude, they could induce cracking of the component, degrade printability, and/or diminish subsequent mechanical performance. The ability to predict these residual stresses imparted by AM is an important step in permeating AM technology for advanced manufacturing. Calibration and validation of AM process models used for prediction are, therefore, a critical step in understanding the origin and mitigating the challenges associated with residual stresses inherent to the AM process. In the present work, the residual strain distributions in components with simple geometries fabricated by a laser powder bed fusion (LBPF) process were characterized non-destructively using energy-dispersive X-ray diffraction in support of the US Air Force Research Laboratory Additive Manufacturing Modeling Challenge Series Groeber et al. (JOM 70:441-448, 2018). The measurement setup and approach are described in detail so that the data can be used as a benchmark to calibrate and validate models for the prediction of macro-scale residual stresses due to the LPBF process.

36 MATERIALS SCIENCE↗
DOE OSTI2024

High-Throughput Microstructural Characterization and Process Correlation Using Automated Electron Backscatter Diffraction

The need to optimize the processing conditions of additively manufactured (AM) metals and alloys has driven advances in throughput capabilities for material property measurements such as tensile strength or hardness. High-throughput (HT) characterization of AM metal microstructure has fallen significantly behind the pace of property measurements due to intrinsic bottlenecks associated with the artisan and labor-intensive preparation methods required to produce highly polished surfaces. This inequality in data throughput has led to a reliance on heuristics to connect process to structure or structure to properties for AM structural materials. In this study, we show a transformative approach to achieve laser powder bed fusion (LPBF) printing, HT preparation using dry electropolishing and HT electron backscatter diffraction (EBSD). This approach was used to construct a library of > 600 experimental EBSD sample sets spanning a diverse range of LPBF process conditions for AM Kovar. This vast library is far more expansive in parameter space than most state-of-the-art studies, yet it required only approximately 10 labor hours to acquire. Build geometries, surface preparation methods, and microscopy details, as well as the entire library of >600 EBSD data sets over the two sample design versions, have been shared with intent for the materials community to leverage the data and further advance the approach. Using this library, we investigated process–structure relationships and uncovered an unexpected, strong dependence of microstructure on location within the build, when varied, using otherwise identical laser parameters.

Characterization and Analytical Technique↗
DOE OSTI2016

Synchrotron X-ray microbeam diffraction measurements of full elastic long range internal strain and stress tensors in commercial-purity aluminum processed by multiple passes of equal-channel angular pressing

Synchrotron X-ray microbeam diffraction was used to measure the full elastic long range internal strain and stress tensors of low dislocation density regions within the submicrometer grain/subgrain structure of equal-channel angular pressed (ECAP) aluminum alloy AA1050 after 1, 2, and 8 passes using route B C . This is the first time that full tensors were measured in plastically deformed metals at this length scale. The maximum (most tensile or least compressive) principal elastic strain directions for the unloaded 1 pass sample for the grain/subgrain interiors align well with the pressing direction, and are more random for the 2 and 8 pass samples. The measurements reported here indicate that the local stresses and strains become increasingly isotropic (homogenized) with increasing ECAP passes using route BC. The average maximum (in magnitude) LRISs are -0.43 σ a for 1 pass, -0.44 σ a for 2 pass, and 0.14 σ a for the 8 pass sample. Furthermore, these LRISs are larger than those reported previously because those earlier measurements were unable to measure the full stress tensor. Significantly, the measured stresses are inconsistent with the two-component composite model.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Direct measurement of critical resolved shear stress of prismatic and basal slip in polycrystalline Ti using high energy X-ray diffraction microscopy

Knowledge of the critical resolved shear stress (CRSS) values of different slip modes is important for accurately modeling plastic deformation of hexagonal materials. Here, we demonstrate that CRSS can be directly measured with an in-situ high energy X-ray diffraction microscopy (HEDM) experiment. A commercially pure Ti tensile specimen was deformed up to 2.6% strain. In-situ far-field HEDM experiments were carried out to track the evolution of crystallographic orientations, centers of masses, and stress states of 1153 grains in a material volume of 1.1mm×1mm×1mm. Predominant prismatic slip was identified in 18 grains, where the orientation change occurred primarily by rotation around the c-axis during specimen deformation. By analyzing the resolved shear stress on individual slip systems, the estimated CRSS for prismatic slip is 96±18 MPa. Predominant basal slip was identified in 22 other grains, where the 2 orientation change occurred primarily by tilting the c-axis about an axis in the basal plane. The estimated CRSS for basal slip is 127±33 MPa. The ratio of CRSS basal /CRSS prismatic is in the range of 1.7-2.1. From indirect assessment, the CRSS for pyramidal < c+a > slip is likely greater than 240MPa. Lastly, grain size and free surface effects on the CRSS value in different grains are also examined.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2017

Investigation of fatigue crack initiation from a non-metallic inclusion via high energy x-ray diffraction microscopy

Crack initiation at inclusions is a dominant, unavoidable and life-limiting failure mechanism of important structural materials. Fatigue progresses in a complex manner to find the ‘weakest link’ in the microstructure, leading to crack nucleation. In this study, fully 3-D characterization methods using high-energy synchrotron x-rays are combined with in-situ mechanical testing to study the crack initiation mechanism in a Ni-based superalloy specimen. The specimen was produced via powder metallurgy and seeded with a non-metallic inclusion. Two x-ray techniques were employed: absorption contrast computed micro-tomography (μ-CT) to determine the morphology of the inclusion and its location in the gauge section of the specimen; and far-field high-energy diffraction microscopy (FF-HEDM) to resolve the centroids, average orientations, and lattice strains of the individual grains comprising the microstructure surrounding the inclusion. Sequential μ-CT and FF-HEDM scans were carried out at both peak and zero applied stress following schedules of cyclic deformation. The µ-CT data showed the onset and location of crack initiation, and the FF-HEDM data provided temporal and spatial evolution of the intergranular strains. Strain partitioning and the associated stress heterogeneities that develop are shown to stabilize within a few loading cycles. Elasto-viscoplastic fast Fourier transform simulations were utilized to supplement interpretation of the experimental stress distributions and compared with the experimental stress distributions. In conclusion, appropriate conditions for crack nucleation in the form of stress gradients were demonstrated and created by virtue of the inclusion, specifically the residual stress state and local bonding state at the inclusion-matrix interface.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Temperature-dependent micromechanical behavior of medium-Mn transformation-induced-plasticity steel studied by in situ synchrotron X-ray diffraction

The temperature-dependent micromechanical behavior of medium-Mn transformation-induced-plasticity (TRIP) steel with a nominal chemical composition of Fe-0.1C-10Mn-2Al (mass%) fabricated by intercritical annealing 650 ºC for 1 h after cold-rolling, was investigated using in situ high-energy X-ray diffraction (HE-XRD) with uniaxial tensile tests at temperatures of 100, 25 and -50 ºC. We find that as the deformation temperature decreases, the Luders strain decreases and more austenite transforms to martensite during Luders band propagation. The Luders bands are associated with sudden changes of lattice strain in austenite. At 100 ºC, austenite is too stable to transform to martensite, resulting in limited work-hardening capability and a relatively low strain to failure. At 25 ºC, the austenite is found to transform in bursts during applied loading. These transformations correlate with stepwise peak broadening in the austenite phase and are attributed to Portevin-Le Chatelier (PLC) band propagation. At -50 ºC, we then observe a more intense TRIP effect which suppresses PLC band formation and leads to a high ultimate tensile strength. In addition to the TRIP effect, we find that work hardening in the deformation-induced martensite phase plays an important role in the plastic stability at low temperature, by accommodating stress compatibility between grains and phases. Our studies provide the first direct experimental evidence for the existence of large stress concentrations in the austenite phase near the Luders band propagation front. These observations help to deepen understanding of the complex temperature-dependent micromechanical behaviors of advanced medium-Mn TRIP steels.

36 MATERIALS SCIENCE↗