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DOE OSTI2020

Database development and exploration of process–microstructure relationships using variational autoencoders

The paper demonstrates graphical representation of a large database containing process–microstructure relationships using an unsupervised machine learning algorithm. Correlating microstructural features to processing is an essential first step to answer the difficult problem of process sequence design. Here, a large database of 346,200 orientation distribution functions resulting from a variety of process sequences is constructed, where each sequence comprises up to four stages of tension, compression and rolling along different directions in various permutations. This open-source database is constructed for collaborative development of process design algorithms. The paper demonstrates a novel application of the large database: graphical representation of texture–process relationships. A variational autoencoder is used to reduce the entire database to a two dimensional latent space where variations in processes and properties can be visualized. Using proximity analysis in this latent space, we can quickly unearth multiple process solutions to the problem of texture or property design.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Deformation behavior of metallic glass composites and plasticity accommodation at microstructural length-scales

Bulk metallic glass matrix composites represent a unique microstructural design strategy for overcoming the strength/ductility trade-off in structural alloys. Site-specific mechanical behavior of a Ti-based bulk metallic glass composite was evaluated at microstructural length-scale. The micro-pillars on the amorphous matrix showed on average a yield point of 1.9 GPa followed by serrated plastic deformation characteristic of shear banding. In contrast, micro-pillars on the crystalline dendritic phase showed a much lower yield strength of 0.72 GPa on average for the four different crystallographic orientations chosen, smooth plastic flow with no recognizable load burst, and stable strain-hardening after yield point. A number of micro-pillars were made at the interface between the glassy matrix and the crystalline dendrite. The mixed micro-pillars showed homogeneous deformation and greater plasticity which was attributed to their smaller stored elastic energy. Shear bands initiated in the amorphous matrix were arrested by the crystalline dendrite, which accommodated plasticity through slip bands and dislocations pile-ups. The interface remained intact after plastic deformation, with no observable signs of devitrification in the amorphous phase.

Bulk metallic glass matrix composite, Micro-pillar↗

DOE OSTI2026

Temperature dependent interfacial microstructure in HIP-bonded Al6061/Zr joints

Pressing (HIP) at 450 °C and 560 °C under 103 MPa for 90 minutes to evaluate interfacial diffusion and microstructural evolution. Sound metallurgical bonding was achieved at both temperatures, with Zr serving as an effective diffusion barrier. Microstructural analysis revealed the the formation of a (Al,Si)3Zr intermetallic layer at the Al/Zr interface, whose thickness increased from ~100 nm at 450 °C to ~2100 nm at 560 °C, consistent with temperature-driven diffusion kinetics. The thin and continuous reaction layer observed at 450 °C indicates controlled interdiffusion and minimal reaction zone growth, favorable for maintaining interface stability and ductility. At 560 °C, enhanced atomic mobility led to pronounced intermetallic development, confirming diffusion-controlled growth behavior. These results provide valuable insights for optimizing Al/Zr interface design and diffusion barrier performance in advanced structural and energy systems.

Al/Zr interface↗

DOE OSTI2019

Microstructural characterization of plutonium oxalate and oxide particles by three-dimensional focused ion beam tomography

Focused ion beam (FIB) tomography was used to characterize three-dimensional (3D) internal microstructures of plutonium oxalate and oxide particles. Sequential two-dimensional (2D) sectioning and imaging using FIB and 3D image reconstruction were used to elucidate and distinguish internal pore microstructure and distribution in plutonium oxide particles calcined from plutonium oxalate precipitates. The results show that the plutonium oxide particles have a significant increase in pore volume fraction while retaining the exterior morphological shape of the corresponding oxalate precipitates. This technique enables the examination of the internal structure of radioactive microparticles for nuclear forensics that is not available with conventional microscopy.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Microstructural stability of tantalum-alloyed ferritic-martensitic steel with neutron irradiation to 7.4 dpa at ~490 °C

Specimens of a reduced-activation ferritic-martensitic steel, called CNA1, were irradiated to 7.4 displacements per atom at ~490 °C in the High Flux Isotope Reactor. Vickers hardness and tensile properties revealed consistent softening that is attributed to some recovery during irradiation, with reduced laths and dislocation density. Detailed microstructural characterization by transmission electron microscopy and energy dispersive x-ray spectroscopy showed radiation-induced dislocation loops, few cavities, and slight dissolution of M 23 C 6 and MX precipitates. Partial amorphization was only observed in M 23 C 6 precipitated in matrix. Transmutation somewhat destabilized M 23 C 6 and MX, with a stronger effect on the later one by noticeable depletion of Ta with enriched W, which is consistent with the transmutation calculations. The microstructural evolution and associated strength changes were discussed with the assistance of computational thermodynamics.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Insights into enhanced sodium ion storage mechanism in Fe 3 S 4 : The coupling of surface chemistry, microstructural regulation and 3D electronic transport

Sodium ion batteries (SIBs) are considered a potential energy storage technology due to their low cost and the abundance of sodium resources. Numerous strategies have been made to address the remaining challenges such as low electronic conductivity, huge volume change, and sluggish sodium ions kinetics. In spite of impressive advances, a comprehensive understanding of the microstructure-stability correlation remains elusive. Here, the three-dimensional (3D) Fe 3 S 4 flower-like hierarchical materials constructed from two-dimensional (2D) nanosheet building units were synthesized via a facile and cost-effective method. Instead of materials synthesis and performance evaluation, more attentions have been paid on the underlying coupling mechanism between microstructure design, surface chemistry and 3D electronic/ionic transport pathways. It found that the thin and stable SEI layer generated by ether-based electrolytes contributes to the stable surface chemistry and fast interfacial Na + ion transport, while 3D hierarchical structure enables short diffusion distance, volume change accomodation as well as stabilizing SEI layer. Taking advantage of the inherent high electronic conductivity in Fe 3 S 4 , we have demonstrated the paramount importance of the synergistic strategy to improve the stability of SIBs through X-ray nanotomography. In conclusion, this work explicitly illuminate the electrochemical stability mechanisms of 3D hierarchitectures and resolves new strategies to rational design SIBs anodes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2017

Microstructural, mechanical and optical properties research of a carbon ion-irradiated Y 2 SiO 5 crystal

Ion irradiation has been a popular method to modify properties of different kinds of materials. Ion-irradiated crystals have been studied for years, but the effects on microstructure and optical properties during irradiation process are still controversial. In this study, we used 6 MeV C ions with a fluence of 1 × 10 15 ion/cm 2 irradiated Y 2 SiO 5 (YSO) crystal at room temperature, and discussed the influence of C ion irradiation on the microstructure, mechanical and optical properties of YSO crystal by Rutherford backscattering/channeling analyzes (RBS/C), X-ray diffraction patterns (XRD), Raman, nano-indentation test, transmission and absorption spectroscopy, the prism coupling and the end-facet coupling experiments. We also used the secondary ion mass spectrometry (SIMS) to analyze the elements distribution along sputtering depth. Finally, 6 MeV C ions with a fluence of 1 × 10 15 ion/cm 2 irradiated caused the deformation of YSO structure and also influenced the spectral properties and lattice vibrations.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Annealing influence on the microstructure of irradiated U-Mo monolithic fuel foils

In this study we compared the microstructure evolution of U-Mo fuel foils produced with and without heat treatment at low burn-up via advanced post-irradiation examination. The aim of this study is to observe after irradiation the ways in which the fabrication processes have influenced fuel behavior at early-stage irradiation, as for very low burn up microstructural studies are lacking. In this work it was observed that the larger grain size detected in the heat-treated samples before irradiation led to decreased grain refinement after irradiation. Grain refinement was associated with the presence of small nano-size bubbles and precipitates. This phenomenon is hypothesized to influence early fuel swelling during reactor irradiation. Grain refinement was also observed to increase in regions where γ-U decomposition was present. Thus, it was enhanced in the samples fabricated without heat treatment. The heat treatment also increased the thickness of the U-Mo/Zr interface, namely of the UZr 2 layer. However, the influence of this layer on fuel performance needs further investigation. On one side, it may contribute to better mechanical bonding; on the other, it may influence swelling and blistering in the interaction layer as porosity increases when this layer is increased. This was observed especially in the presence of increased area containing low Mo concentration, and thus containing a higher fraction of the α-U phase, which is highly susceptible to irradiation induced swelling. Strong evidence of reverse transformation under irradiation (α-U + γ'-U2Mo → bcc γ-U) was observed in these samples. While the precipitates (carbides and oxide) seem to be unaffected by the irradiation at these low burnups. However, further analyses are necessary at higher burn-up to assess the exact impact different heat treatments have on fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Effect of hatch spacing and laser power on microstructure, texture, and thermomechanical properties of laser powder bed fusion (L-PBF) additively manufactured NiTi

This study systematically evaluates the effects of laser powder bed fusion additive manufacturing (L-PBF-AM) parameters (hatch spacing and laser power) on the thermomechanical behavior and microstructure of Ni 50.8 Ti 49.2 shape memory alloy. The samples were fabricated with hatch spacings from 40 to 240 µm and laser powers of 50 and 100 W at a constant scanning speed of 125 mm/s, resulting in parts with volumetric energy density levels from 55 to 666 J/mm 3 and two sets of linear energy densities of 0.4 and 0.8 J/mm. The results showed a reduced melt pool size and discontinuity of scan tracks with decreased laser power. Additionally, the porosity level was increased with larger hatch spacing and lower laser power. More notably, the transformation temperatures increased, and the critical stress, recoverable strain, and functional stability of samples improved with lower hatch spacing, where the recovery ratio of up to 90% was observed, regardless of the employed laser power. This study also discussed the relationship between the fabrication process and texture formation in the L-PBF-AM process. In conclusion, the advantage of L-PBF-AM was revealed in tailoring the microstructure from highly textured samples in [1 1 1] or [0 0 1] direction when hatch spacing lower than laser beam focused was employed, to the appearance of equiaxed solidification front with island grains and random orientations.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effect of Microstructure on Chain Flexibility and Glass Transition Temperature of Polybenzofulvene

Polybenzofulvene (PBF) is a polydiene with a very high glass transition temperature (T g ), which makes it a potential candidate for use as the hard block for high-temperature thermoplastic elastomer applications. The T g s of polydienes are known to be related to chain flexibility. However, no studies have been reported that correlate the chain flexibility to the microstructure of PBF. Herein, we present a study of solution properties of linear PBFs with narrow molecular weight dispersity and having 1,2-addition ranging from 23% to 99%. The materials were prepared by living anionic polymerization under different conditions. Specifically, the chain flexibility as defined by the Flory's characteristic ratio, , and dependence of chain flexibility on microstructure by combined measurements of intrinsic viscosity and molecular weight using triple-detector size exclusion chromatography (SEC) is studied. The persistence lengths (l p ) and chain diameters (d B ) were also estimated using the touched-bead wormlike chain model. To the best of our knowledge, the characteristic ratio of PBF is found to be the highest of all polydienes that have been reported so far.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Scaling CFB risers: Beyond the data using microstructure similarity

Scaling circulating fluidized bed risers has been a point of contention for nearly a century. There have been numerous attempts to define various methodologies. These have all fallen short of providing a robust approach, primarily due to a lack of maintaining microstructure dynamics – a key factor in maintaining interphase heat and mass transfer. Recent work by the author put forward an approach based upon preserving dynamic similarity at different scales by ensuring that the microstructure remained similar by maintaining statistical and chaotic parameters across the scale. That work relied on a dimensionless regime map in which the x-axis was defined by the ratio of the solids flux to the saturation carrying capacity. This latter property was only good within the range of the data, and it became evident that extrapolation beyond the limits of the data could induce unrealistic conditions. Therefore, literature was reviewed to develop a better correlation for the saturation carrying capacity. In doing so, a critical riser diameter concept was developed and applied to the correlations for both Geldart Group A and B materials. The critical diameter for Geldart Group A and B materials is 0.2 m and 0.3 m, respectively. Here the paper then gives three examples on how to use the scaling approach to maintain dynamic similarity across the scales.

02 PETROLEUM↗

DOE OSTI2026

Effect of 316 stainless steel powder processing conditions on microstructure

One parameter that has both economic and performance effects in the manufacturing of steel parts is the powder feedstock used. 316 L steel powder can be produced through water atomization or gas atomization, where both the powder size and the atomization process determine the cost of powder feedstock. Gas atomized powder is spherical and has a lower oxygen content than water atomized powder, making it the preferred choice for performance, but comes at a higher financial cost. Here, in this study, various 316 L powder batches are characterized to understand physical properties and microstructural variations. Density and flowability were determined using gas pycnometry and Hall flow tests. Powder morphology and porosity were qualitatively analyzed via optical microscopy and scanning electron microscopy, Finally, transmission electron microscopy was used to determine changes in phases present. Spherical gas atomized powder of 30–100 μm contained Mn$-$Si rich oxides both on the surface and within the matrix. Meanwhile, irregular water atomized powder 30 μm in diameter contained silicon oxides without manganese. All powder particles contained a nickel rich cellular structure which was shown to support the formation of additional phases. While literature has observed general microstructural features across 316 L powder particles, transmission electron microscopy (TEM) in this study has identified variations in precipitation and cell structures. Information regarding morphology, flowability, density, and phase distributions can be applied to understand variations in part consolidation, which will in turn show which powder aspects are significant for production.

Chemical segregation↗

DOE OSTI2022

A boundary-based approach to the multiscale microstructural characterization of a W-Ni-Fe tungsten heavy alloy

Here, a combination electron backscattered diffraction and transmission electron microscopy based approach has been implemented to study the effects of purposefully introduced anisotropy in a tungsten heavy alloy (WHA) through hot-rolling. Particular attention has been paid to changes in number and proportion of various boundary types from a quantitative standpoint; incorporating qualitative behavioral observations from prior analyses to generate experimentally-validated bases for the examination and application of a microstructure which exhibits an optimal balance of strength and ductility. It is asserted that a combination of increased temperatures during rolling and additional isothermal hold time for the post-rolling annealing steps may lead to a reduction in unfavorable textural components due to rolling in the W-phase and a decrease in premature fracture due to W-W microcracking respectively. This is expected to further increase the proportion of interphase boundaries and improve the ductility of these rolled structures, producing a superior rolled WHA microstructure.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Microstructure degradation of YSZ in Ni/YSZ anodes of SOFC operated in phosphine-containing fuels

The interaction of trace (ppm) phosphine with the nickel/yttria stabilized zirconia (YSZ) anode of commercial solid oxide fuel cells has been investigated and evaluated for both synthesis gas and hydrogen fuels in an effort to examine P–Y reactions. The Ni poisoning effects reported in literature were confirmed and degradation was examined by electrochemical methods and post-test microstructural and chemical analyses. The results indicate that P-induced degradation rates and mechanisms are fuel dependent and that degradation of cells operated in synthesis gas (syngas) with phosphine is more severe than that of cells operated in hydrogen with phosphine. As reported in published literature, a cell operated in syngas containing 10 ppm phosphine demonstrated significant microstructural degradation within the Ni phase, including formation of Ni–P phases concentrated on the outer layer of the anode and significant pitting corrosion in the Ni grains. In this research, a previously undetected YPO{sub 4} phase is observed at the YSZ/YSZ/Ni triple grain junctions located at the interface with the YSZ electrolyte. Tetragonal YSZ (t-YSZ) and cubic-YSZ (c-YSZ) domains with sizes of several tens of nanometers are also newly observed along the Ni/YSZ interface. These observations contrast with data obtained for a cell operated in dry hydrogen with phosphine, where no YPO{sub 4} phase is observed and the alternating t-YSZ and c-YSZ domains at the Ni/YSZ interface are smaller with typical sizes of 5–10 nm. The data imply that electrolyte attack by P is a potentially debilitating mode of degradation in SOFC anodes, and that the associated reaction mechanisms and rates are worthy of further examination.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2018

Microstructure and properties of Cu-Sn-Zn-TiO 2 nano-composite coatings on mild steel

Cu-Sn-Zn coatings have been widely used in industry for their unique properties, such as good conductivity, high corrosion resistance and excellent solderability. To further improve the mechanical performance of Cu-Sn-Zn coatings, powder-enhanced method was applied and Cu-Sn-Zn-TiO 2 nano-composite coatings with different TiO 2 concentration were fabricated. The microstructure of Cu-Sn-Zn-TiO 2 nano-composite coatings were investigated by X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The mechanical properties of coatings including microhardness and wear resistance were studied. The results indicate that the incorporation of TiO 2 nanoparticle can significantly influence the properties of Cu-Sn-Zn coatings. The microhardness of Cu-Sn-Zn coating was increased to 383 HV from 330 HV with 1 g/L TiO 2 addition. Also, the corrosion resistance of coating was enhanced. The effects of TiO 2 nanoparticle concentration on the microstructure, mechanical properties and corrosion resistance of Cu-Sn-Zn-TiO 2 nano-composite coatings were discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Microstructural Developments Leading to New Advanced High Strength Sheet Steels: A Historical Assessment of Critical Metallographic Observations

In the past 30+ years significant advancements have been made in the development of higher strength sheet steels with improved combinations of strength and ductility that have enabled important product improvements leading to safer, lighter weight, and more fuel efficient automobiles and in other applications. Properties of the primarily low carbon, low alloy steels are derived through careful control of time-temperature processing histories designed to produce multiphase ferritic based microstructures that include martensite and other constituents including retained austenite. The basis for these developments stems from the early work on dual-phase steels which was the subject of much interest. In response to industry needs, dual-phase steels have evolved as a unique class of advanced high strength sheet steels (AHSS) in which the thermal and mechanical processing histories have been specifically designed to produce constituent combinations for the purpose of simultaneously controlling strength and deformation behavior, i.e. stress-strain curve shapes. Improvements continue as enhanced dual-phase steels have recently been produced with finer microstructures, higher strengths, and better overall formability. Today, dual phase steels are the primary AHSS products used in vehicle manufacture, and several companies have indicated that the steels will remain as important design materials well into the future. In this presentation, fundamental results from the early work on dual-phase steels will be reviewed and assessed in light of recent steel developments. Specific contributions from industry/university cooperative research leading to product improvements will be highlighted. The historical perspective provided in the evolution of dual-phase steels represents a case-study that provides important framework and lessons to be incorporated in next generation AHSS products.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Investigating the Microstructure of Poly(cyclosilane) by 29 Si Solid-State NMR Spectroscopy and DFT Calculations

Using high-resolution magic-angle spinning (MAS) solid-state NMR spectroscopy and density-functional theory (DFT) calculations, we determine the microstructure of the silicon-based functional polymer poly( 1,4Si 6 ) arising from the dehydrocoupling polymerization of cyclosilane 1,4Si 6 . 1 H- 29 Si refocused-INEPT experiments allow the unambiguous determination of the number of attached protons to a silicon atom for each 29 Si signal in 1,4Si 6 and poly( 1,4Si 6 ). One-dimensional 1 H→ 29 Si cross-polarization MAS (CPMAS) spectra of poly( 1,4Si 6 ) show the development of SiH resonances upon polymerization and peak integration indicates an average degree of polymerization of 20. The 1 H→ 29 Si CPMAS spectrum of poly( 1,4Si 6 ) also shows two sets of isotropic signals, suggesting the presence of at least two distinct species. Two-dimensional 29 Si dipolar double-quantum-single-quantum and single-quantum-single-quantum homonuclear correlation spectra reveal similar connectivity in the two species, pointing to stereochemical and/or conformational heterogeneity. DFT calculations on trimer models predict that chair or twist-boat conformations and with cis or trans diastereomers are all energetic minima. 29 Si chemical shift calculations of the lowest energy structures show that conformers and stereoisomers are expected to give rise to distinct 29 Si NMR peaks and likely explain the appearance of multiple sets of 29 Si NMR signals. Finally, the strategy outlined in this article is expected to be widely useful for the microstructural elucidation of silicon-based functional polymers.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Geochemical and Microstructural Characterization of Shale Rock: A Workflow for Site Evaluation for Energy–Fluids Storage

Shales are a central component of petroleum systems, as source, seal, and unconventional reservoir rocks. Unlike traditional unconventional shale, a newly emerging Caney Shale play is regarded as an unconventional of unconventional shales (UUS), due to its high content of fine-grained materials, lower reservoir porosity, dominance of nanopores, and a scarcity of visible natural fractures. Other developed unconventional shales such as the Woodford and Barnett have larger average pore size, higher porosity, and extensive natural fractures at core scale that contribute to reservoir quality. In this work, the Caney Shale was cored in entirety to characterize its interbedded ductile and reservoir intervals and establish criteria for their recognition. Representative ductile and reservoir intervals known as D2 and R3, respectively, were selected for detailed analysis including variations in elemental composition, mineralogy, facies, and the presence of natural fractures at well and core scales using X-ray fluorescence, X-ray diffraction, and thin section and core description. Characteristics of microstructure and microgeochemistry at nano- and microscales are compared using field emission scanning electron microscopy with energy dispersive spectroscopy and lowpressure nitrogen adsorption isotherms with fractal dimension analysis. The ductile (detrital clay-rich) member D2 is characterized by higher concentrations of Ti and Al and lower Si, while the reservoir R3 (possibly biogenic silica-accumulated) is characterized by lower Ti and Al and higher Si. Eight mixed carbonate–siliciclastic facies are recognized, and R3 shows a higher heterogeneity of facies stacking and average fracture abundance than D2. Further, R3 shows a more microscopically heterogeneous fabric/texture of matrix and a higher microporosity than D2 that has a higher pore surface heterogeneity. A fundamental understanding of the compositional and microstructural characteristics of UUS and further ductile/reservoir intervals will allow for a better assessment of reservoir quality, more effective production of hydrocarbons, and optimized selection of safe caprocks in carbon sequestration and subsurface hydrogen storage.

58 GEOSCIENCES↗