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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 1,657 records · Page 92
All sourcesNASA NTRSDOE OSTI
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↗
DOE OSTI2018

Glancing-incidence focussed ion beam milling: A coherent X-ray diffraction study of 3D nano-scale lattice strains and crystal defects

Here, this study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defects than normal incidence milling at the same energy. However the resulting residual lattice strains have similar magnitude and extend up to ~50 nm into the sample. At the edges of the milled surface, where the ion-beam tails impact the sample at near-normal incidence, large dislocation loops with a range of Burgers vectors are formed. Further glancing incidence FIB polishing with 5 keV ion energy removes these dislocation loops and reduces the lattice strains caused by higher energy FIB milling. However, even at the lower ion energy, damage-induced lattice strains are present within a ~20 nm thick surface layer. These results highlight the need for careful consideration and management of FIB damage. They also show that low-energy FIB-milling is an effective tool for removing FIB-milling induced lattice strains. This is important for the preparation of micro-mechanical test specimens and strain microscopy samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

In situ synchrotron X-ray diffraction investigations of the physical mechanism of ultra-low strain hardening in Ti-30Zr-10Nb alloy

A warm-rolled, metastable beta-type Ti-30Zr-10Nb alloy exhibited a peculiar two-stage yielding behavior under uniaxial tensile loading, showing a first plastic stage with obvious strain hardening at 0.4%-10.4% strain and a second plastic stage with ultra-low strain hardening at 10.4%-23.5% strain. In situ high-energy X-ray diffraction (HE-XRD) was used to reveal the stress-induced martensitic transformation scenarios and physical mechanism of the different strain hardening rates. It was found that the deformation-induced phase transformation dominated the onset of the first plastic stage corresponding to the selection of favorable martensitic variants, and their elastic interaction contributed to the obvious strain hardening. HE-XRD experiments further verified that the ultra-low strain hardening rate in the second plastic stage was related to an interesting superelasticity of the martensite, which was characterized by the reversible, stress-induced reorientation of the martensite variants. This reorientation of the martensite variants was primarily due to the rigid lattice rotation of similar to 23 degrees about the [110](α '') axis toward the tensile direction. Here, our investigations provide in-depth understanding of the mechanism of the excellent plasticity with ultra-low strain hardening in beta-type titanium alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Electric-field-induced structure and domain texture evolution in PbZrO 3 -based antiferroelectric by in-situ high-energy synchrotron X-ray diffraction

Antiferroelectrics (AFEs) have a great potential for modern electronic devices by virtue of the large strain during the antiferroelectric-to-ferroelectric (AFE-FE) phase transition under external electric fields. Although the fascinating macroscopic properties of AFE materials have been extensively studied, it is still unclear how the underlying structure evolution engenders their defining properties. Here we employ an electric biasing in-situ high-energy synchrotron X-ray diffraction technique to reveal the phase, domain texture, and lattice evolution in a high performance PbZrO 3 -based AFE material. During the reversible AFE-FE transition triggered by electric fields, the evolution of the superstructure for AFE pseudo-tetragonal and FE rhombohedral phase is found to display strong dependence on the angle with respect to the field direction. In contrast to previous prediction, it is found that there is no obvious domain reorientation in the AFE phase, when the system is far away from the AFE-FE transitions. The electric-field-induced FE rhombohedral phase exhibits an unusual microscopic behavior, distinguished from the normal one, presenting small changes in domain texture and lattice strain with electric field, and leading to a small piezoelectric response. The longitudinal, transverse, and volume strains estimated from the XRD peak profiles are well consistent with the macroscopic strain measurements. It is demonstrated that the large strain arises from the structural change associated with anisotropic lattice strain and highly preferential domain reorientation during the AFE-FE transitions. Finally, the AFE-FE switching sequence is constructed based on the present study, which provides a further understating of AFE materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Elucidating the temperature dependence of TRIP in Q&P steels using synchrotron X-Ray diffraction, constituent phase properties, and strain-based kinetics models

Understanding the deformation-induced martensitic transformation (DIMT) is critical for interpreting the structure-property relationships that govern the performance of transformation-induced plasticity (TRIP) assisted steels. However, modern TRIP-assisted steels often exhibit DIMT kinetics that are not easily captured by existing empirical models based on bulk tensile strain. We address this challenge by combined bulk uniaxial tensile tests and in-situ high energy synchrotron X-ray diffraction, which resolved the phase volume fractions, stress-strain response, and microstructure evolution of each constituent phase. A modification of the Olson-Cohen model is implemented, which describes the martensitic transformation kinetics as a function of the estimated partitioned strain in austenite, rather than the bulk tensile strain. This DIMT kinetic model is used as a framework to clarify the root cause of an insufficiently understood toughness trough reported for TRIP-assisted steels during deformation at elevated temperatures. Here, the importance of the temperature-dependent toughness is discussed, based on the opportunity to modify deformation processes to tailor the DIMT kinetics and mechanical properties during forming and in service.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Solidification modes during additive manufacturing of steel revealed by high-speed X-ray diffraction

Solidification during fusion-based additive manufacturing (AM) is characterized by high solidification velocities and large thermal gradients, two factors that control the solidification mode of metals and alloys. Using two synchrotron-based, in situ setups, we perform high-speed X-ray diffraction measurements to investigate the impact of the solidification velocities and thermal gradients on the solidification mode of a hot-work tool steel over a wide range of thermal conditions of relevance to AM of metals. The solidification mode of primary δ-ferrite is observed at a cooling rate of 2.12x10 4 K/s, and at a higher cooling rate of 1.5x10 6 K/s, δ-ferrite is sup-pressed, and primary austenite is observed. The experimental thermal conditions are evaluated and linked to a Kurz-Giovanola-Trivedi (KGT) based solidification model. The modelling results show that the predictions from the multicomponent KGT model agree with the experimental observations. This work highlights the role of in situ XRD measurements for a fundamental understanding of the microstructure evolution during AM and for vali-dation of computational thermodynamics and kinetics models, facilitating parameter and alloy development for AM processes.

36 MATERIALS SCIENCE↗
DOE OSTI2023

A spall and diffraction study of nanosecond pressure release across the iron ε-α phase boundary

The extreme response of polycrystalline iron at high pressures and high strain rates is revealed by means of high-power laser pulses. The compression portion of the pulse coupled with x-ray diffraction identifies the expected body-centered cubic (α) to hexagonal close packed (ε) displacive transformation. Upon release, observation shows that the complete reverse transformation takes approximately 8 ns and that the structure returns to its initial microstructural configuration, in a reversible transformation path. This is in good agreement with molecular dynamics (MD) simulations which predict an inverse dependence between transformation time and strain rate. The grain size is reduced from μm to nm range during compression and begins increasing back to the original grain size on decompression. The kinetics of the transition is dictated by heterogenous nucleation as it follows the Johnson-Mehl-Avrami-Kolmogorov equation with the appropriate time exponent of ~1. This is confirmed by MD simulations which also identify profuse twinning and dislocation generation. Here, the tensile pulse generated upon reflection at the free surface is captured by time-resolved free surface velocity measurements from which a peak tensile stress of 7 GPa is obtained, in stark contrast with its quasi-static value of ~200 MPa. At these strain rates, the strength of grain interiors, which is determined by twinning and slip exceeds the strength of the boundaries, and failure initiates preferentially in the latter.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Thermostructural evolution of boron carbide characterized using in-situ x-ray diffraction

Boron carbide, with a nominal stoichiometry of B 4 C, is a highly desired ceramic candidate for armor applications due to its high hardness derived from the complex crystal structure. However, stress-induced local amorphization can lead to failure and is a known challenge for this material which must be addressed for applications in ballistic environments. Understanding boron carbide's atomic structural behavior and bonding environment is critical in determining effective strategies to mitigate these issues. Here, in this work, the thermo-structural behavior of B 4 C has been studied in detail using a conical nozzle levitator system coupled with in-situ synchrotron X-ray diffraction. Lattice expansion and the resulting thermal expansion coefficients (CTEs) were determined from 25-2100 °C. Rietveld refinements showed anisotropic atomic displacement for each of the 4 unique sites as a function of temperature. An exceptionally large z-axis displacement for the boron chain center is linked to bond weakness and may be linked to faster expansion of the α 33 relative to α 11 CTEs. Thermally induced lattice changes can inform the use of boron carbide at elevated temperatures as well as help develop strategies for mitigating structural failure for armor applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Real-time evolution of texture and temperature during friction stir processing of a magnesium alloy: An operando neutron diffraction study

The real-time development of texture and the evolution of temperature during friction stir processing (FSP) of a Mg alloy were investigated using an operando neutron diffraction measurement. A novel approach was applied in this study where the real-time, quasi-steady state measurements performed as a function of position during FSP are converted to a Lagrangian dataset that reveals the transient behavior as a function of time. The in-situ FSP was carried out under two different thermo-mechanical processing conditions represented by the Zener-Hollomon parameter, Z. Further, the results show that: (i) a shear texture develops from the initial strong basal texture with the peak temperature reaching about 774 K during a low-Z processing and (ii) a strong off-normal texture develops with a peak temperature of 616 K during a high-Z processing. Moreover, time-temperature-texture diagrams were established to reveal the real-time development of the texture during the processing for both the low Z and high Z processing conditions. The changes in texture will be discussed in terms of plastic deformation mechanisms active during various stages of the FSP under the two different processing conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Multi-stage load partitioning in additively manufactured Al6061+TiC nanocomposite characterized by in-situ neutron diffraction

Metal matrix composites (MMCs), combining metal matrix and ceramic particles, exhibit high mechanical strength and stiffness compared to conventional metallic materials. During fusion-based additive manufacturing (AM), MMCs undergo a rapid heating and cooling thermal history, which affects the interfacial bonding, thermal misfit stress and mechanical load transfer behavior between the metal matrix and particles, thus impacting the bulk mechanical performance. Here, we investigate the deformation dynamics and phase-specific load transfer in fusion-based AMed Al6061 +TiC MMCs through in-situ neutron diffraction. By calculating the phase-specific lattice strains, a multi-stage load transfer and deformation behavior during uniaxial compression is revealed: (1) elastic deformation in Stage I for both phases; (2) sudden stress rebalance between two phases in Stage II, evidenced by a sudden decrease in Al lattice strain and increase in TiC; (3) active load carrying by both phases in Stage III, with both phases experiencing an increase in lattice strains. Further, the deformation mechanism of each stage is deducted by correlating the evolutions of the interphase stresses and peaks’ broadening and intensity of the Al matrix. The local plastic deformation of the Al matrix near the phase interface is triggered and leads to stress rebalancing in Stage II. The global plastic deformation subsequently propagates throughout the Al matrix in Stage III, and the composite is further hardened through both dislocation multiplication and load transfer. The findings offer valuable insights into deformation and load-sharing behavior in AMed MMCs.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Assessment of Barium Sulphate Formation and Inhibition at Surfaces with Synchrotron X-ray Diffraction (SXRD)

The precipitation of barium sulphate from aqueous supersaturated solutions is a well-known problem in the oil industry often referred to as 'scaling'. The formation and growth of barite on surfaces during the oil extraction process can result in malfunctions within the oil facilities and serious damage to the equipment. The formation of barium sulphate at surfaces remains an important topic of research with the focus being on understanding the mechanisms of formation and means of control. In situ synchrotron X-ray diffraction (SXRD) was used to investigate the formation of barium sulphate on a stainless steel surface. The effect of Poly-phosphinocarboxylic acid (PPCA) and Diethylenetriamine-penta-methylenephosphonic acid (DETPMP) which are two commercial inhibitors for barium sulphate was examined. The in situ SXRD measurements allowed the identification of the crystal faces of the deposited barite in the absence and presence of the two inhibitors. The preferential effect of the inhibitors on some crystal planes is reported and the practical significance discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Analysis of the turbostratic structures in PAN-based carbon fibers with wide-angle x-ray diffraction

Carbon fiber (CF) is a versatile material renowned for its excellent mechanical, thermal, and electrical properties. Polyacrylonitrile (PAN)-based CFs dominate the market due to their high tensile strength, rendering them suitable for structural applications in a wide variety of applications ranging from sporting goods to aerospace. Over five decades of commercial development of PAN-based CF has resulted in a range of varieties with different tensile moduli and tensile strengths. The microstructures, nanostructures, and crystal structures of PAN-based CF play pivotal roles in the macroscale properties of this material. In particular, the crystal structure and crystallite orientation in CF is closely related to the mechanical properties. The crystal structure of PAN-based CF generally consists of turbostratic carbon, which is a disordered form of graphite, the characteristics of which can be effectively characterized in a bulk format through wide-angle x-ray diffraction (WAXD). In this work, we employed a three-part approach to the analysis of WAXD patterns collected from four intermediate modulus PAN-based CFs. The approach incorporates a Scherrer analysis, a Debye analysis, and an orientational analysis to provide precise estimates of crystallite sizes, crystallite distributions, and crystallite orientations with the fiber axis. Furthermore, the results presented here suggest that intermediate modulus PAN-based CF mostly consists of small turbostratic crystallites (<4 nm), with larger crystallites having increased orientation with the fiber axis. The results here imply the presence of curvature and/or wrinkling of the turbostratic layers within the CF structure.

36 MATERIALS SCIENCE↗