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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 541 records · Page 30
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Disorder Dynamics in Battery Nanoparticles During Phase Transitions Revealed by Operando Single-Particle Diffraction

Structural and ion-ordering phase transitions limit the viability of sodium-ion intercalation materials in grid scale battery storage by reducing their lifetime. However, the combination of phenomena in nanoparticulate electrodes creates complex behavior that is difficult to investigate, especially on the single-nanoparticle scale under operating conditions. In this work, operando single-particle X-ray diffraction (oSP-XRD) is used to observe single-particle rotation, interlayer spacing, and layer misorientation in a functional sodium-ion battery. oSP-XRD is applied to Na 2/3 [Ni 1/3 Mn 2/3 ]O 2 , an archetypal P2-type sodium-ion-positive electrode material with the notorious P2-O2 phase transition induced by sodium (de)intercalation. Here, it is found that during sodium extraction, the misorientation of crystalline layers inside individual particles increases before the layers suddenly align just prior to the P2-O2 transition. The increase in the long-range order coincides with an additional voltage plateau signifying a phase transition prior to the P2-O2 transition. To explain the layer alignment, a model for the phase evolution is proposed that includes a transition from localized to correlated Jahn-Teller distortions. The model is anticipated to guide further characterization and engineering of sodium-ion intercalation materials with P2-O2 type transitions. oSP-XRD, therefore, opens a powerful avenue for revealing complex phase behavior in heterogeneous nanoparticulate systems.

25 ENERGY STORAGE↗
DOE OSTI2025

In Situ Diffraction and Ex Situ Transmission X‐Ray Microscopy Studies of Solid‐State Upcycling for NMC Cathodes

Upcycling of recycled LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) cathodes offers an economical route to produce cathode materials with increased energy density (i.e., LiNi 0.8 Mn 0.1 Co 0.1 O 2 , NMC811) that meet the performance needs of present-day electric vehicles. In this work, solid-state upcycling of NMC622 via calcination with Ni(OH) 2 and LiOH was monitored using in situ synchrotron powder X-ray diffraction measurements. Sequential Rietveld refinements indicate that the calcination proceeds by initially converting Ni(OH) 2 to a rocksalt NiO phase followed by lithiation of NiO to form LiNiO 2 (LNO), with both NMC and LNO phases present in nearly equal proportions at the calcination endpoint. Variable-energy transmission X-ray microscopy tomograms of upcycled samples reveal that the NMC and LNO domains are intermixed at sub-micron length scales. Depth-dependent analysis of multi-elemental fitting maps matches the expected NMC811 composition at the secondary particle level and indicates that transition metal diffusion is not limited by the secondary particle size.

cathode upcycling↗
DOE OSTI2024

Accurate and Data‐Efficient Micro X‐ray Diffraction Phase Identification Using Multitask Learning: Application to Hydrothermal Fluids

Traditional analysis of highly distorted micro X‐ray diffraction (μ‐XRD) patterns from hydrothermal fluid environments is a time‐consuming process, often requiring substantial data preprocessing and labeled experimental data. Herein, the potential of deep learning with a multitask learning (MTL) architecture to overcome these limitations is demonstrated. MTL models are trained to identify phase information in μ‐XRD patterns, minimizing the need for labeled experimental data and masking preprocessing steps. Notably, MTL models show superior accuracy compared to binary classification convolutional neural networks. Additionally, introducing a tailored cross‐entropy loss function improves MTL model performance. Most significantly, MTL models tuned to analyze raw and unmasked XRD patterns achieve close performance to models analyzing preprocessed data, with minimal accuracy differences. This work indicates that advanced deep learning architectures like MTL can automate arduous data handling tasks, streamline the analysis of distorted XRD patterns, and reduce the reliance on labor‐intensive experimental datasets.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2022

Simulation of the Impact of Point Defects and Edge Dislocations on X-Ray Diffraction in Hexagonal (Ni,Co) 1+2 x Ti 1– x O 3 Thin Films

In this work, a computer code for simulating high-resolution X-ray diffraction (XRD) data from disordered crystals with arbitrary spatial composition and local lattice parameters is developed. Simulated patterns are compared with the experimental data collected on a single phase, highly crystalline (Ni 0.42 Co 0.58 ) 2.22 Ti 0.39 O 3 solid-solution thin film exhibiting a large number of subsidiary minima. As a case study, the edge dislocations in hexagonal (Ni,Co) 3 O 3 thin films with Burgers vector parallel and perpendicular to the a-axis and c-axis, respectively, are modeled. No peak profiles are assumed and thus issues related to profile fitting are avoided. Both macroscopic features, such as film thickness, and atomic-scale structure, such as dislocations, are simultaneously modeled. Simulations are run on a desktop machine. Commonly applied database-based phase identification routines can result in wrong phase identification, unless intensities are properly modeled. Modeling tools of diffractometer manufacturers are compared with the present approach. An example of how simulated reciprocal lattice patterns can be used to choose relevant measurement geometries in defected thin films is given.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
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 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 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 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↗
DOE OSTI2023

In-situ high energy X-ray diffraction study of deformation behavior in Nb nanoparticle-martensitic NiTi composite wire

Here, this study investigated the deformation behavior in Nb nanoparticle-martensitic NiTi composite wire during tensile loading by means of in-situ high-energy X-ray diffraction. Compared to Nb nanowires, the dispersedly distributed Nb nanoparticles have little effect on the transformation and deformation behaviors of NiTi matrix, causing the absence of R phase transformation and the occurrence of deformation twinning in NiTi matrix. Meanwhile, the occurrence of deformation twinning in NiTi matrix can reduce the shape strain to be coordinated by the unfavorable orientated martensite variants, and thus decreases the internal stress among NiTi martensite variants generated during martensite reorientation process. In addition, TEM result proved that Nb nanoparticles can achieve exceptionally large elastic strain in B19'-NiTi matrix (~4%), just as Nb nanowires. However, this large elastic strain (stress) will be released with the occurrence of NiTi deformation twinning.

36 MATERIALS SCIENCE↗