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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 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Investigation of grain-boundary geometry and pores morphology in dense and porous cubic zirconia polycrystals

Highlights: • Cubic zirconia sinters were investigated in three dimensions using dual-beam FEGSEM. • The 3D-EBSD technique was successfully applied to non-conductive ceramics. • New sample preparation approach to automated 3D-EBSD was proposed. • Grain boundary microstructures were reconstructed from inverse pole figure maps. • Pore microstructures were reconstructed from image quality maps. - Abstract: Three-dimensional electron backscatter diffraction technique was used for the visualization of grain boundary geometry and pore morphology in cubic zirconia. A set of four samples sintered under different conditions was investigated. Specimens which were characterized by energy dispersive spectroscopy and X-ray diffraction were entirely composed of cubic phase. Investigations of boundaries and pore structures were carried out in a dual-beam scanning electron microscope. For each sample, a volume of 1000 μm{sup 3} was investigated. The analysis of grain boundary networks reconstructed from inverse pole figure maps revealed a strong dependence between grain boundary density and sample preparation parameters. Sintering also affects the size and distribution of pores. The total number of grains analyzed varied from 17 to 357 and the calculated volume of cavities from 0.01% to 21%. This paper shows the application of three-dimensional crystallographic orientation analysis to characterize the microstructure of yttria stabilized zirconia ceramics.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evaluation of LPBF Steels for Nuclear Applications

This report provides an update on the prioritization of existing reactor materials for advanced manufacturing. This report is a Milestone 3 deliverable in FY2023, under work package CT-23AN130401 to support research and qualification activities supported by the Advanced Materials and Manufacturing Technologies (AMMT) program here at Argonne National Laboratory (ANL). The focus of FY23 for ANL included the determination of a decision criteria matrix for the prioritization of existing materials, the literature review of a select few Fe-based alloys, and working with vendors to obtain customized powders. The work package also includes fabricating test samples in a Renishaw AM400 Laser Powder Bed Fusion (LPBF) system and optimizing the process parameters. The major outcomes of this work package are: With collaborations from PNNL, ORNL, and INL, we were able to establish a decision criteria matrix containing a total of 6 categories and 31 different criteria. These will be used to downselect alloys for further evaluation; As part of that, 6 different Fe-based alloys were selected, 3 austenitic stainless steels (A709, D9, AFA) and 3 ferritic/martensitic steels (HT9, Grade 91, Grade 92). Customized powders were obtained from vendors in small quantities to fabricate initial prints to check printability of these specific alloys; A total of 72 single track experiments were performed on two alloy systems, 1 austenitic stainless steel (A709) and 1 ferritic/martensitic steel (Grade 91) in order to optimize the process parameters for the full 3d prints. The optimization led to the selection of 20 different processing conditions, 10 for each class of alloys; D9 and AFA alloys showed extensive cracking and porosity in the samples. This was due to less-than-ideal conditions present in the chamber during the deposition. A709 printed using the same process parameters showed almost fully dense samples with no noticeable porosity or any other defects. SEM and EBSD analysis revealed single phase FCC microstructure with cellular structure within the grains; HT9, Grade 91, Grade 92 alloys also showed no noticeable signs of cracking and ImageJ analysis showed porosity <0.5% in all conditions. While Grade 91 and Grade 92 showed single phase BCC microstructures, the presence of martensite laths was noted in HT9 alloy; Future work will include further characterization of these alloys to better understand the microstructural evolution during the 3d printing process.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2018

Stochastic reconstruction and microstructure modeling of SMC chopped fiber composites

Here, to establish an integrated Processing-Microstructure-Property workflow for the prediction of material behaviors, this paper presents a new stochastic pseudo-3D microstructure reconstruction method for Sheet Molding Compounds (SMC) chopped fiber composites. The proposed method captures the bi-level microstructural features of SMC composites. At the higher level, a Voronoi diagram-based algorithm is developed to reconstruct the unique substructure features of SMC fiber tows. The geometry of Voronoi cells is adjusted by a Simulated Annealing (SA) algorithm to match the geometrical statistics of the real fiber tows. At the lower level, the algorithm assigns fiber orientation to each Voronoi cell (which represents a fiber tow). The fiber orientation angles are recovered from a statistical fiber orientation tensor. The proposed method is employed to establish a multi-layer pseudo-3D SMC Representative Volume Element (RVE) model for Finite Element Analysis (FEA) of SMC microstructure. This model enables the prediction of mechanical properties based on the material processing information (e.g. fiber orientation tensor obtained from compression molding simulation), and the microstructure information obtained from microscopic imaging for an SMC composite. Lastly, the predicted properties are successfully validated by experimental tensile tests.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Process Integration and Optimization of ICME Carbon Fiber Composites for Vehicle Lightweighting: A Preliminary Development

Process integration and optimization is the key enabler of the Integrated Computational Materials Engineering (ICME) of carbon fiber composites. In this paper, automated workflows are developed for two types of composites: Sheet Molding Compounds (SMC) short fiber composites, and multi-layer unidirectional (UD) composites. For SMC, the proposed workflow integrates material processing simulation, microstructure representation volume element (RVE) models, material property prediction and structure preformation simulation to enable multiscale, multidisciplinary analysis and design. Processing parameters, microstructure parameters and vehicle subframe geometry parameters are defined as the design variables; the stiffness and weight of the structure are defined as the responses. For multi-layer UD structure, this work focuses on the discussion of different design representation methods and their impacts on the optimization performance. Challenges in ICME process integration and optimization are also summarized and highlighted. Two case studies are conducted to demonstrate the integrated process and its application in optimization.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructural creep, fatigue and creep-fatigue modeling of Nickel-based superalloy Inconel 617 at high temperature - 18506

Inconel 617 is a solution strengthened nickel-based alloy which has been considered as one of the leading structural material for the intermediate heat exchangers (IHX) in very high temperature reactor (VHTR). In order to gain understanding of the creep and fatigue deformation mechanisms and their interactions in alloy 617 operating in the VHTR environment, a computational model that operates at the microstructural scale has been developed for creep, fatigue and creep-fatigue modeling of alloy 617. This model is based on an isothermal, large deformation crystal plasticity finite element (CPFE) formulation and idealizes the deformation in the crystal lattice as collective glide and climb of dislocations. A recently developed glide resistance evolution equation by the authors that can capture the intermediate softening observed in both fatigue and creep-fatigue cycles of Inconel 617 at high temperature is adopted for the dislocation glide formulation. Dislocation climb is incorporated to account for the interactions between dislocations and local point defects at high temperature. The CP equations are solved incrementally as the constitutive relationship in the context of FE analysis on fully resolved microstructure reconstructed from experiment data. Model parameters are calibrated and verified using experimental tests. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2018

Quantification of complex-phase steel microstructure by using combined EBSD and EPMA measurements

Highlights: • In CP800 steel, bainite is the dominant phase with a typical lath (width 300 nm) structure and cementite precipitates. • Martensite is dispersed as small islands and only a few narrowed martensite bands are observed which has been induced by annealing process of cold rolled sheet. • The precise carbon content is measured in bainite and martensite utilizing EPMA line scans, which is around 0.2 wt% and 0.4 wt%, respectively. • Digitalization of the microstructure for CP800 is achieved by combining EBSD and EPMA techniques. • The final constituent map consists of plenty of microstructural features including topography, crystal structures, orientations and elemental distribution. - Abstract: We combined electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) techniques to characterize the microstructure of industrial produced complex-phase CP800 steel. First, three major constituents (ferrite, martensite and bainite) are characterized. Then, transformation-induced dislocation zones in ferrite and bainitic regions consisting of different sub-structures are quantified and segmented. A final digitalized component map including plenty of microstructural features including crystal structures, orientations and elemental distribution are successfully achieved. The precise carbon content is measured in bainite and martensite utilizing EPMA line scans, which is around 0.2 wt% and 0.4 wt%, respectively. In the bainite phase of CP800, a typical Bagaryatski orientation relationship between cementite and lath-like bainitic ferrite is revealed based on the select diffraction patterns of transmission electron microscopy measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Formation of gradient microstructure and mechanical properties of hot-pressed W-20 wt% Cu composites after sliding friction severe deformation

Highlights: • W particles of composites were refined during sliding friction treatment (SFD). • Dislocation, dislocation tangles and boundary clearly exist in deformed W particle. • YS and UTS of SFDed sample are 308.74 MPa and 553.60 MPa owing to the refinement. • Electrical conductivity of SFDed sample decreased from 33 IACS% to 28.5 IACS%. • Fracture mode changing from inter-granular mode to trans-granular. - Abstract: W-based alloys are currently considered promising candidates for high heat flux components in future fusion reactors. In this paper, hot pressed W-20 wt%Cu composites were treated at room temperature using a sliding friction severe deformation (SFD) process, with a moving speed of 0.2 m/s and an applied load of 500 N. Microstructural evolution of composites after the SFD treatment was evaluated and compared with that of the untreated composites. Results showed that there was a gradient structure generated and an obvious refinement in tungsten particles size in the surface layer after the SFD process. The average particle size of tungsten in the SFD treated composites was 2.60 μm, whereas it was 4.5 μm for tungsten in the untreated composites. Fracture surfaces of the composites indicated that the SFD treatment destroyed the W skeleton and changed fracture mode from predominant inter-granular one to trans-granular one due to the decrease in contact area of W-W inter-particles. Yield strength and ultimate tensile strength of composites after the SFD treatment were 308 MPa and 553 MPa, respectively. The treated composites exhibited micro-hardness values with an average reading of about 308 HV. Analysis of the facture microstructures clearly suggested that the tungsten particles in the treated composites are consisted of dislocations and boundaries as well as dislocation tangles. The electrical conductivity of the composites was decreased from 33 IACS% to 28.5 IACS% after the SFD treatment, mainly due to loss or squeezing of copper into the inner surface.

36 MATERIALS SCIENCE↗
DOE OSTI2021

edxia: Microstructure characterisation from quantified SEM-EDS hypermaps

The characterisation of cement paste microstructure is an important step towards understanding durability mechanisms in cementitious materials. Scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS) is a widely used technique to analyse the microstructure at the micron-scale. However, it is challenging, notably because the characteristic size of many phases is found on a scale smaller than the EDS interaction volume. This work presents a new image analysis framework to identify phases and quantify the microstructure of cementitious materials from SEM-EDS hypermaps. By leveraging domain knowledge, representative points are attributed to phases and mixtures of phases based on ratio plots. Then, quantitative analysis of the microstructure can be carried out (chemical composition, particle size distributions, volume fractions, …). We demonstrate the abilities of the framework, and we present possible applications and extensions of the method. The framework is available as both a graphical interface and a Python code.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Experimental Study on Microstructure and Hardness of Pure Titanium Subjected to Torsion Deformation at Different Temperatures

The studies of mechanical property, microstructure evolution and fracture analysis in pure titanium processed by torsion deformation at 298, 673 and 1073 K are conducted systematically. The variations of mechanical property of deformed pure titanium are shown through Vickers hardness evaluation. During torsion at 298 K, the grains are refined and elongated, but the α phase with different shapes precipitates for twisted samples at 673 and 1073 K. The fracture appearance indicates that the elongated dimples occur on fracture surface at 298 K. Besides, a large number of shear facets are arranged. However, typical intergranular fracture appearance with lots of blocks in polyhedral shape covers the fracture surface at 673 and 1073 K, respectively.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Post-irradiation characterization of a high burnup mixed oxide fuel rod with minor actinides

The Advanced Fuels Campaign performed a series of irradiation tests of minor actinide-bearing mixed oxide fuel (MA-MOX), the so-called AFC-2C&D experiments, to investigate the transmutation of long-lived transuranic actinide isotopes contained in spent nuclear fuel via fast reactor technology at burnups exceeding 10 % fission of initial metallic atoms. This manuscript reports the test results derived from one of the five MA-MOX rodlets taken to higher burnup in the AFC-2D irradiation. This includes both non-destructive investigations, such as gamma and neutron spectrometry, and destructive investigations, such as fission gas release, ceramography, and chemical burnup analysis. In addition, the microstructure of the fuel was investigated using advanced electron microscopy techniques including electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Here, it was observed with EBSD that the pellet had subdivision of the grains and the TEM observed migration of cladding material into the 5 metal precipitates in the fuel which could have been from the higher than desired oxygen/metal ratio. The TEM also showed an enrichment of Cr in fuel clad chemical interaction (FCCI) layer.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Single-component-at-a-time variation study for glass-ceramic waste forms

Here, a 51-sample composition variation study was performed on glass-ceramic waste forms for a raffinate waste stream from aqueous reprocessing of used nuclear fuel containing high fractions of Mo, alkalis, alkaline earths (AEs), and rare earths (REs). The study was designed with a single-component-at-a-time variation approach off a centroid composition. The components that were varied included Al, B, Ca, Li, Mo, Na, REs, Si, Zr, and Others (containing minor components). Data analysis included crystallization curves, microstructure, and phase compositions. A number of components (i.e., Li 2 O, B 2 O 3 , REO x , MoO 3 , Na 2 O, and ZrO 2 ) significantly impacted the concentration and chemistry of phases, especially the primary phases of oxyapatite [i.e., Ca 2 RE 8 (SiO 4 ) 6 O 2 ] and powellite (i.e., AEMoO 4 ), precipitated in the slow-cool heat-treated waste forms; minor phases included cerianite [i.e., Ce x Zr (1-x) O 2 ], Ba-molybdate [i.e., Ba(Gd 0.67 Mo 0.33 O 3 ], noble metals, pollucite (i.e., CsAlSiO 4 ), and RE-borosilicate (i.e., RE 3 BSi 2 O 10 ).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

How Microstructure and Pore Moisture Affect Strength Gain in Portlandite-Enriched Composites That Mineralize CO 2

Binders containing portlandite (Ca(OH) 2 ) can take up carbon dioxide (CO 2 ) from dilute flue gas streams (<15% CO 2 , v/v), thereby forming carbonate compounds with binding attributes. While the carbonation of portlandite particulates is straightforward, it remains unclear how CO 2 transport into monoliths is affected by microstructure and pore moisture content. Therefore, this study elucidates the influences of pore saturation and CO 2 diffusivity on the carbonation kinetics and strength evolution of portlanditeenriched composites (“mortars”). To assess the influences of microstructure, composites hydrated to different extents and conditioned to different pore saturation levels (S w ) were exposed to dilute CO 2 . First, reducing saturation increases the gas diffusivity and carbonation kinetics so long as saturation exceeds a critical value (S w,c ≈ 0.10) independent of microstructural attributes. Second, careful analysis reveals that both traditional cement hydration and carbonation offer similar levels of strengthening, the magnitude of which can be estimated from the extent of each reaction. As a result, portlandite-enriched binders offer cementation performance that is similar to traditional materials while offering an embodied CO 2 footprint that is more than 50 % smaller. Furthermore, these insights are foundational to create new “low-CO 2 ” cementation agents via in situ CO 2 mineralization (utilization) using dilute CO 2 waste streams.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

On the Cutting of Metals: A Mechanics Viewpoint

The mechanics of large-strain deformation in cutting of metals is discussed, primarily from viewpoint of recent developments in in situ analysis of plastic flow and microstructure characterization. It is shown that a broad range of deformation parameters can be accessed in chip formation—strains of 1–10, strain rates of 10–10 5 /s, and temperatures up to 0.7T m —and controlled. This range is far wider than achievable by any other single-stage, severe plastic deformation (SPD) process. The resulting extreme deformation conditions produce a rich variety of microstructures in the chip. Four principal types of chip formation—continuous, shear-localized, segmented, and mushroom-type—as elucidated first by Nakayama (1974, “The Formation of ‘Saw-Toothed Chip’ in Metal Cutting,” Proceedings of International Conference on Production Engineering, Tokyo, pp. 572–577) are utilized to emphasize the diverse plastic flow phenomena, especially unsteady deformation modes that prevail in cutting. These chip types are intimately connected with the underlying flow, each arising from a distinct mode and triggered by an instability phenomenon. The role of plastic flow instabilities such as shear banding, buckling, and fracture in mediating unsteady flow modes is expounded, along with consequences of the flow modes and chip types for the cutting. Sinuous flow is shown to be the reason why gummy (highly strain-hardening) metals, although relatively soft, are so difficult to cut. Synthesizing the various observations, a hypothesis is put forth that it is the stability of flow modes that determines the mechanics of cutting. Furthermore, this leads to a flow-stability phase diagram that could provide a framework for predicting chip types and process attributes.

42 ENGINEERING↗
DOE OSTI2019

Characterization of Solidification Microstructures in Vacuum Arc Remelted Nickel Alloy 718

Digital image analysis techniques were developed to autonomously characterize dendritic solidification features in microstructures of a nickel alloy 718 ingot produced by vacuum arc remelting (VAR). Automated macrophotography was implemented to image microstructures and produce large image montages of etched ingot cross sections. Two image analysis techniques, particle identification and two-point correlation, were applied to autonomously measure primary dendrite arm orientation and secondary dendrite arm spacing from the image montages. Particle identification measured individual dendritic features. The two-point correlation technique measured averaged feature values over defined image areas. These methods are described and compared. Melt pool profile and solidification time histories were reconstructed from primary dendrite arm orientation and secondary dendrite arm spacing measurements, respectively. These characterization techniques provide two new methods of reconstructing melt pool profiles and solidification times in cast ingots. The information produced is expected to be useful in the validation of computational models for solidification during VAR, similar remelting processes, and general casting processes that produce dendritic solidification features.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Simulation and analysis of small angle scattering (SAS) patterns of Ni-based superalloy microstructures generated by a phase-field model

This paper investigates the relationship between microstructural features and small-angle scattering (SAS) patterns in Ni-based superalloys using a combined phase-field and SAS simulation approach coupled with microstructure analyses. The simulated SAS patterns accurately capture key experimental observations previously reported in the literature, including the time-dependent transition from circular to square-shaped precipitates and the development of anisotropic SAS patterns. Importantly, our analysis reveals the correlations between characteristic length scales extracted from SAS profiles and microstructural descriptors, such as precipitate size and inter-precipitate distance. These findings provide a comprehensive understanding of the link between SAS profiles and microstructure evolution in Ni-based superalloys, offering valuable insights for materials characterization and design.

Microstructure↗
DOE OSTI2017

Effect of cold rolling on the microstructural evolution of new β-typed Ti–6Mo–6V–5Cr–3Sn–2.5Zr alloys

A Ti–6Mo–6V–5Cr–3Sn–2.5Zr (wt.%) alloy was designed as a new metastable β-Ti alloy. The effect that cold rolling had on the microstructural evolution of the material was investigated via optical microscopy (OM), X-ray diffraction (XRD), electron back-scattered diffraction (EBSD) and transmission electron microscopy (TEM) measurements. A single β phase formed in the alloy after solution treatment at 780 °C for 30 min followed by water quenching. The solution-treated alloy was cold rolled with thickness reductions of 10%, 30%, 50% and 70%, and the hardness values increased as the thickness of the specimen decreased. The textures of the cold rolled specimen were characterized according to the 〈110〉 partial parallel to the rolling direction as the rolling reduction increased. The crystallographic orientation showed principal α-fiber textures for (111)〈110〉 and (112)〈110〉. The cold deformation led to the appearance of martensite α″ phases, particularly stress-induced martensite (SIM) α″ phases. - Highlights: • Effect of cold rolling on new β-typed Ti-6Mo-6V-5Cr-3Sn-2.5Zr alloy was studied. • A single β phase was obtained after solution treatment at 780 °C for 30 min. • α-Fiber textures became dominated with the increase in cold rolling reduction. • A stress-induced α″ martensite was caused by cold rolling.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Microstructure of a-C:H films prepared on a microtrench and analysis of ions and radicals behavior

Amorphous carbon films (a-C:H) were prepared on a microtrench (4-μm pitch and 4-μm depth), and the uniformity of film thickness and microstructure of the films on the top, sidewall, and bottom surfaces of the microtrench were evaluated by scanning electron microscopy and Raman spectroscopy. The a-C:H films were prepared by bipolar-type plasma based ion implantation and deposition (bipolar PBII&D), and the negative pulse voltage, which is the main parameter dominating the film structure, was changed from −1.0 to −15 kV. Moreover, the behavior of ions and radicals was analyzed simultaneously by combining the calculation methods of Particle-In-Cell/Monte Carlo Collision (PIC-MCC) and Direct Simulation Monte Carlo (DSMC) to investigate the coating mechanism for the microtrench. The results reveal that the thickness uniformity of a-C:H films improves with decreasing negative pulse voltage due to the decreasing inertia of incoming ions from the trench mouth, although the film thickness on the sidewall tends to be much smaller than that on the top and bottom surfaces of the trench. The normalized flux and the film thickness show similar behavior, i.e., the normalized flux or thickness at the bottom surface increases at low negative pulse voltages and then saturates at a certain value, whereas at the sidewall it monotonically decreases with increasing negative voltage. The microstructure of a-C:H films on the sidewall surface is very different from that on the top and bottom surfaces. The film structure at a low negative pulse voltage shifts to more of a polymer-like carbon (PLC) structure due to the lower incident energy of ions. Although the radical flux on the sidewall increases slightly, the overall film structure is not significantly changed because this film formation at a low negative voltage is originally dominated by radicals. On the other hand, the flux of radicals is dominant on the sidewall in the case of high negative pulse voltage, resulting in a deviation from the Raman behavior of a-C:H films deposited by bipolar PBII&D. This tendency intensifies as the negative voltage becomes greater. Also, the energy of incident ions on the sidewall of the trench increases with increasing negative voltage, which causes a shift in the Raman data of the sidewall to the bottom right corner on the figure depicting the relationship of the FWHM(G) and the G-peak position, indicating increased graphitization of a-C:H film.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2016

Determination of dislocation density by electron backscatter diffraction and X-ray line profile analysis in ferrous lath martensite

The microstructure and the dislocation density in as-quenched ferrous lath martensite were studied by different methods. The blocks, packets and variants formed due to martensitic transformation were identified and their sizes were determined by electron backscatter diffraction (EBSD). Concomitant transmission electron microscopy (TEM) investigation revealed that the laths contain subgrains with the size between 50 and 100 nm. A novel evaluation procedure of EBSD images was elaborated for the determination of the density and the space distribution of geometrically necessary dislocations from the misorientation distribution. The total dislocation density obtained by X-ray diffraction line profile analysis was in good agreement with the value determined by EBSD, indicating that the majority of dislocations formed due to martensitic transformation during quenching are geometrically necessary dislocations.

36 MATERIALS SCIENCE↗