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NASA NTRS2023

Handbook for Additively Manufactured Materials: Microstructure, Properties, and Fractography

As the additive manufacturing (AM) industry has grown and the processes have matured more alloys have been adapted to the various AM processes. Understanding the microstructure and properties of these AM alloys is important in designing parts that perform appropriately in application. For decades materials handbooks have been informative references for designers and engineers alike to know what properties and microstructures to expect in alloys produced by other forms of manufacturing. AM alloy references for properties and microstructures have been largely limited to literature that may not be subject to the same industry standard heat treatments or in standard process parameters. NASA has worked with partners to characterize various commercially available AM alloys with a high degree of traceability. This work aims utilize industry-relevant, traceable datasets to develop a new handbook for AM alloys to better inform designers and engineers of the microstructures, fractures, and first order properties from over 30 AM alloys produced across the industry.

Additive Manufacturing↗

DOE OSTI2022

A Novel Approach to Simulate Realistic Concrete Microstructures under Irradiation

The concrete biological shield of light water reactors is exposed to high neutron and gamma irradiation doses in the long term. Irradiation deteriorates the physical and mechanical properties of concrete. Such effects need to be investigated to predict the concrete’s performance in the event of a lifetime extension of a nuclear power plant. This work combines high-resolution characterization techniques with fast-Fourier transform (FFT)-based 2-D simulations to evaluate the radiation-induced volumetric expansion (RIVE) and damage in concrete microstructures under neutron irradiation. Two concrete microstructures from samples provided by the Japan Concrete Aging Management Program (JCAMP) were characterized using micro x-ray fluorescence (mXRF) to obtain elemental intensity maps, and energy-dispersive x-ray spectroscopy to complement mXRF with local elemental information for Na. Minerals and cement paste are then identified based on the elemental composition to produce high-resolution phase maps, resulting in a more accurate representation of the microstructures compared to previous work. Simulations of radiation-induced volumetric expansion (RIVE), creep, and damage in JCAMP concrete use the fast Fourier transform (FFT)-based code Microstructure Oriented Scientific Analysis of Irradiated Concrete (MOSAIC) combined with the irradiated minerals, aggregates, and concrete (IMAC) database, which contains mineral-specific RIVE models. Overall, the simulation results are in fair agreement with experimental data.

Cheniour, Amani↗

DOE OSTI2022

Mechanical response and microstructure evolution from multiaxial stress relaxation in textured zircaloy nuclear cladding

Modern energy markets provide motivation for nuclear reactors to increase operational flexibility and load following capacity of existing reactor designs. The operational power changes result in fuel pellet expansion and contraction resulting in pellet-cladding mechanical interaction (PCMI) and high cladding stresses that are strongly related to stressed corrosion cracking (SCC) which can lead to fuel rod failure. This work aims to quantify the stress fields in cladding with a focus on multiaxial stress relaxation response from an imposed strain and the resulting microstructure changes in textured zircaloy claddings. Stress relaxation tests resulting in multiaxial stress fields are performed to measure the material response of Zircaloy-4 nuclear cladding. Multiple experiments using samples from the same piece of cladding are performed so samples with the same processing history may be removed at strategic points throughout mechanical testing for microstructure characterization. The microstructure evolution is analyzed with mechanical response to evaluate the static recovery impact on crystallographic texture and grain morphology. Experiments are performed at Idaho National Laboratory using an experimental device capable of applying internal pressure and independent axial load to commercial nuclear cladding at elevated temperatures with stress- or strain-controlled experimental capability. X-ray diffraction and electron backscatter diffraction are used for microstructure analysis. Rheological models are used to visualize the multiaxial stress-strain relationships and isolate elastic, plastic, and viscoplastic material properties for analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Microstructural characterization of the oxidation of nuclear graphite under chronic and accident conditions via XCT and synchrotron XCT

Graphite is a candidate material to moderate fast neutrons and for structural components in the US next-generation graphite-moderated reactors. A graphite core is conceived as a large formation of interconnected bricks that primarily serves as the moderator of fast neutrons, holds instrumentation, fuel elements, control rods, and is a receptacle for molten salts for Molten Salt Reactors (MSRs) designs. During the operation of a graphite-moderated power plant, graphite components might be subjected to chronic oxidation during normal operating conditions or aggressive oxidation as a result of accidental ingress of air that reacts vigorously with the graphite core. Using synchrotron, x-ray computed tomography (XCT), this research systematically characterized microstructural changes that accompanied these two oxidation scenarios. Chronic oxidation was studied by characterizing IG-110, PCEA, and NBG-18 specimens that were gradually oxidized in air at a low temperature (520°C). The accidental ingress of air into the graphite reactor was simulated by subjecting the grades mentioned above to high-temperature oxidation at approximately 750°C. This research is the first, in situ, systematic characterization of nuclear graphite microstructural evolution that can be associated with the two possible oxidation scenarios and provide insight into related repercussions. The results show that the microstructure and pore connectivity influence the rate of oxidation and evolution of the microstructure under the two oxidation regimes. These results are crucial to understanding which grades are more resilient to each type of oxidation and documenting the damage created in the graphite.

Arregui Mena, Jose'↗

DOE OSTI2024

Assessment of effective elastic constants of U-10Mo fuel microstructures

Monolithic U-10Mo fuel undergoes significant microstructural changes during fuel burnup which degrades its mechanical properties. In this talk, we present results form a numerical method to assess the impact of the various microstructural features--grains, intragranular and intergranular Xe gas bubbles--on the elastic stiffness tensor. Using the Multiphysics Object-Oriented Simulation Environment (MOOSE), phase-field-based microstructures are combined with asymptotic expansion homogenization method to obtain effective elastic constants as a function of porosity and fission density. The results are verified and compared against analytical homogenization models. With this approach, elastic degradation in operating nuclear fuels can be quantified when the distributions of microstructural features are known from experimental characterization or rate-theory based models. We further develop an evolution model based on the virial equation of state for Xe gas and investigate the effect of growth and coalescence of the bubbles at the grain boundary faces and triple junctions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Python codes for the paper - "Trade-offs in the latent representation of microstructure evolution"

SAND2024-00946O Python codes used in "Trade-offs in the latent representation of microstructure evolution," a manuscript accepted for publication in Acta Materialia, are part of a repository. The code was developed to perform analysis of microstructure evolution. The repository consists of two main directories: models, which train and test models such as autoencoders and diffusion maps, and analysis, which analyzes microstructures. Source code is used to perform dimensionality reduction of microstructure data for analysis of its evolution in time. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-NA0003525.

Dingreville, Remi↗

DOE OSTI2024

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Process–structure–property relationships in bimodal machined microstructures using robust structure descriptors

Machining is a severe plastic deformation process that subjects materials to high rates of deformation and elevated temperatures. Dynamic recrystallization during severe plastic deformation drives grain refinement into the sub-micron range but the ductility and thermal stability of these structures is poor. In contrast, bimodal microstructures consisting of both fine and coarse grains have been shown to exhibit attractive strength and ductility properties at these temperatures. In this paper, we study the process–structure–property relationships for pure copper subject to a machining process where the cutting speeds are varied. Further, we investigate the role of thermal effects by varying the post-deformation cooling rates. Microstructures generated under these deformation conditions are quantified using angularly resolved chord length statistics. The derived metrics are found to be robust descriptors of the studied microstructures as they automatically capture complex features such as unimodal and bimodal distributions of grain structure, grain constituent length scales, and morphological anisotropy induced by shear deformation. The uniaxial equivalent yield strength of the generated structures are estimated using spherical nanoindentation and inverse modeling techniques. Lastly, we present a methodology for identifying the constrained property-process inverse mapping for machining using a Bayesian framework and the established forward process–structure–property mapping.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Laser‐Powder Melt Pool Solidification Dynamics and Microstructural Engineering of Ti‐5553 Microlattices

The fine geometric and topological control afforded by additive manufacturing technologies has enabled the manufacture of architected materials across length scales, and enabling tunable mechanical performance as a function of local and global design. Progress has been made to tune the mechanical response of architected materials through geometry, but understanding how the geometry and processing conditions will inform the microstructure remains a challenge due to the rapid solidification in laser powder bed fusion. This study uses in situ X-ray imaging and electron backscatter diffraction microscopy to demonstrate that the melt pool size, microstructure morphology, and elastic strain distribution is influenced by a combination of lattice geometry and laser processing conditions. These results indicate that within larger melt pools the local thermal gradients are sufficient to enable a columnar-to-equiaxed transition across the melt pool. Furthermore, the solidification mechanisms producing these microstructures are examined across the first 5 ms of melting and solidification, described via in situ high-speed X-ray imaging and mirrored via multiphysics simulation.

additive manufacturing↗

DOE OSTI2022

Overcoming Anode Instability in Solid‐State Batteries through Control of the Lithium Metal Microstructure

Abstract Enabling the lithium metal anode (LMA) in solid‐state batteries (SSBs) is the key to developing high energy density battery technologies. However, maintaining a stable electrode–electrolyte interface presents a critical challenge to high cycling rate and prolonged cycle life. One such issue is the interfacial pore formation in LMA during stripping. To overcome this, either higher stack pressure or binary lithium alloy anodes are used. Herein, it is shown that fine‐grained ( d = 20 µm) polycrystalline LMA can avoid pore formation by exploiting the microstructural dependence of the creep rates. In a symmetric cell set‐up, i.e., LiǀLi 6.25 Al 0.25 La 3 Zr 2 O 12 (LLZO)ǀLi, fine‐grained LMA achieves > 11.0 mAh cm −2 compared to ≈ 3.6 mAh cm −2 for coarse‐grained LMA ( d = 295 µm) at 0.1 mA cm −2 and at moderate stress of 2.0 MPa. Smaller diffusion lengths (≈ 20 µm) and higher diffusivity pathway along dislocations ( D d ≈ 10 −7 cm 2 s −1 ), generated during cell fabrication, result in enhanced viscoplastic deformation in fine‐grained polycrystalline LMA. The electrochemical performances corroborate well with estimated creep rates. Thus, microstructural control of LMA can significantly reduce the required stack pressure during stripping. These results are particularly relevant for “anode‐free” SSBs wherein both the microstructure and the mechanical state of the lithium are critical parameters.

25 ENERGY STORAGE↗

DOE OSTI2025

Reactive Carbide‐Based Synthesis and Microstructure of NASICON Sodium Metal All Solid‐State Electrolyte

Reactive carbide precursor-based synthesis of NASICON-type NZSP (Na 1+x Zr 2 Si x P 3-x O 12 ) solid-state electrolyte (SSE) is demonstrated, in contrast to the established oxide-based approach. Exothermic decomposition of ZrC and SiC in air homogenizes microstructure, yielding 98% compact density after conventional sintering at 1200 °C. Quantitative stereology demonstrates that significant microstructural differences are present. Compacts of carbide-derived Carb-NZSP are 98% dense with a secondary zirconium oxide (ZrO 2 ) volume fraction of 0.2% ± 0.3%, versus 93% dense and 3% ± 1% for oxide-derived baseline. For Carb-NZSP, the secondary glassy phosphate phase is agglomerated, while for baseline, it is dispersed and percolated. Electrochemical testing combined with post-mortem analysis demonstrates how microstructural control of secondary phases is critical for dendrite suppression: Carb-NZSP critical current density (CCD) is 3.1 ± 0.8 mA cm −2 at 0.1 mAh cm −2 , versus 1.0 ± 0.7 mA cm −2 at 0.1 mAh cm −2 . Cryogenic focused ion beam (cryo-FIB) analysis demonstrates that in both materials, the porous 2D sheet-like sodium metal dendrites propagate around and subsume NZSP grains, likely following a path enriched with glassy phase and with porosity. Dendrites also flow around isolated zirconia particles. Phase field simulation reveals deflection of dendrites by mechanically tough zirconia, while brittle glassy phase accelerates dendrite growth, especially when finely distributed.

36 MATERIALS SCIENCE↗

DOE OSTI2019

A Review on Friction Stir Processing of Titanium Alloy: Characterization, Method, Microstructure, Properties

In the past two decades, friction stir processing (FSP) technology has received considerable attention. FSP can be used to adjust and control the microstructure of materials, including eliminating defects, destroying dendrites and controlling fractions in the second stage, and is therefore widely used in titanium and its alloys for biomedical, aerospace and automotive applications. This article comprehensively reviews the methods of studying FSP, the microstructure evolution of materials and the summary of material properties. It begins with the introduction of the FSW system, characterization, structure and elemental analysis, and simulation and performance testing methods, and then introduces the microstructure evolution mechanism of various titanium materials and discusses in detail the material properties of titanium alloy, namely hardness and wear resistance, elasticity and plasticity, corrosion resistance and biocompatibility. Finally, this review presents unresolved issues and outstanding challenges in FSP technology and reveals the direction of this emerging field of research.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructural Characterization, Mechanical Properties, and Corrosion Resistance of Dental Co-Cr-Mo-W Alloys Manufactured by Selective Laser Melting

In this paper, the microstructure, mechanical properties, and corrosion resistance of the dental Co-Cr-Mo-W alloys fabricated by selective laser melting (SLM) were systematically investigated and correlated. The microstructure of the SLM group (SG) specimens is composed of extremely fine columnar crystals, exhibiting supersaturated and homogeneous character. The matrix mainly consists of face-centered-cubic (FCC) cobalt solid solutions, and minimal hexagonal-close-packed (HCP) cobalt solid solutions. Mechanical test results showed that the 0.2% yield strength of SG was 775 ± 7 MPa, and the ultimate tensile strength was 1118 ± 25 MPa. The elongation of SG was 8.28 ± 0.4%, and the microhardness of SG was 476 ± 10 HV. All of these values largely exceeded the cast group (CG) specimens. The high strength is attributed to their fine columnar crystals and supersaturated matrices. The fewer content from the HCP phase and a lack of intermetallic compounds or eutectic contribute to the high ductility. Furthermore, a higher E{sub corr}, lower I{sub corr} were acquired for better corrosion resistance compared to cast specimens, due to even less composition segregation and more microstructural homogeneity.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructure and Mechanical Properties of Al-Mg-Sc-Zr Alloy Variable Polarity Plasma Arc Welding Joint

Al-Mg-Sc-Zr alloy plates were welded by variable polarity plasma arc welding (VPPAW) with Sc-containing filler wire. The microstructure and mechanical properties were investigated. Results show that the weld zone and heat-affected zone (HAZ) are narrow due to the high concentrated heat input of VPPAW. Primary Al{sub 3}(Sc,Zr) particles are nice nucleating sites for α-Al, which can significantly refine the grains of α-Al, helping the weld zone maintain an outstanding strength. The unmelted Al{sub 3}(Sc,Zr) precipitates of the base metal aggregated near the fusion boundary result in the formation of a fine equiaxed grains zone, which improves the bonding degree between the weld zone and the base metal. The Al{sub 3}(Sc,Zr) precipitates in the HAZ have excellent inhibition effect on recrystallization. According to the observed microhardness distribution and microstructure characteristics, the microstructure model of welded joint is obtained. The fractured position of welded joint locates in the weld zone. The tensile strength of the welded joint without reinforcing rib is 330 MPa. The welding coefficient reaches 74%.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of Ni Addition to Sn0.7Cu Solder Alloy on Thermal Behavior, Microstructure, and Mechanical Properties

The addition of Ni on lead-free solder alloys Sn0.7Cu was tested in this study. A small amount of Ni was added to the solder alloys to evaluate the thermal behavior, microstructure, and mechanical properties of the composite solders after sintering and isothermal aging for 3 days and then compared with the results of the binary Sn0.7Cu solder. The results indicated that the ultimate tensile strength and yield tensile strength changed when adding 0.25 wt.% of Ni. The tested results of the differential scanning calorimeter showed that the addition of Ni (such as 0.5 and 1 wt.%) could obviously increase the solidification temperature of Sn0.7Cu alloys in the cooling process. When the Ni content was increased to 0.25 wt.% in the ternary condition, which includes the Sn0.7Cu-xNi (x = 0, 0.1, 0.25, 0.5, and 1 wt.%) solder alloys for the indentation creep test, the minimum creep rate reached the maximum; however, the trend was reversed as the Ni content was higher than this level. In addition, the microstructure of Sn-0.7Cu-xNi solder alloys was obviously different with the eutectic Sn-0.7Cu solder, such that the Ni gradually accumulated in the (Cu, Ni){sub 6}Sn{sub 5} IMCs within the Ni-containing solder alloys. Additionally, this process refined the microstructure of the Sn-0.7Cu solder. The fracture surface of the eutectic Sn-0.7Cu solder revealed ductile fracture modes; however, there was no mixed ductile–brittle fracture mode occurred when the Ni content was in the range of 0-1 wt.%.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Processing, As-Cast Microstructure and Wear Characteristics of a Monotectic Al-Bi-Cu Alloy

Ternary Al-based monotectic alloys have a good combination of wear resistance and mechanical strength. While self-lubricating soft elements guarantee an adequate wear resistance, the modification with third elements can increase the ability to support load. In the present investigation, a collection of microstructures is generated through transient directional solidification of the Al-3.2wt.%Bi-3.0wt.%Cu alloy. Samples with different Bi spacing have been subjected to micro-adhesive wear ball tests. A relationship linking the wear volume, V, the microstructural spacing and the test time is proposed for Bi spacing higher than 16 μm, according to which V decreases with the decrease in Bi spacing. It is observed that wider and deeper grooves emerged on the surface of the samples related to more refined Bi and Al{sub 2}Cu phases, that is, associated with Bi spacing and Bi diameter lower than 16 and 2.4 μm, respectively. A reverse trend is noted for these finer microstructures, for which V increases with further decrease in Bi spacing. This can be caused by the detachment of the very fine and less cohesive Al{sub 2}Cu lamellas as the Al{sub 2}O{sub 3} oxide breaks up forming debris, with the presence of these lamellas as loose debris at the interface acting as third-body abrasives.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Study on the Hot Deformation Behavior and Microstructure Evolution of Cu-Cr-In Alloy

Based on the hot compressive tests in the temperature range of 700-900 °C and strain rate range of 0.01-10 s{sup −1}, the hot deformation behavior of a Cu-Cr-In alloy was investigated. The true stress–strain curves of the alloy were obtained, and a constitutive equation for the alloy was established by the method of equivalent stress. The processing maps were constructed based on the constitutive equation, and the microstructural evolutions were analyzed and correlated with the processing maps. The results show that the true stress of the alloy increased with decreasing strain rate and decreased with increasing temperature. The microstructures of the alloy deformed under different conditions were in good accordance with the processing maps results. According to the processing maps and the microstructures of the alloy with true strains of 0.4 and 0.8, the optimal hot deformation conditions lie in the range of 850-900 °C and strain rate range of 0.01-0.1 s{sup −1}.

36 MATERIALS SCIENCE↗

DOE OSTI2019

A Study of Microstructure Evolution During Creep of 9Cr-1Mo Steel Using Ultrasonic and Hardness Measurements

In this work, microstructural changes during creep of 9Cr-1Mo steel were characterized using ultrasonic and hardness measurements. The creep testing of this steel was firstly performed at 873 K under the initial stresses of 160 and 175 MPa, respectively. Then, eight specimens under each stress level were prepared by the interrupted tests to simulate various creep states. Subsequently, two parameters of ultrasonic attenuation and velocity were introduced by the ultrasonic testing. Experiment results showed that regardless of the stresses, the ultrasonic attenuation experiences a peak at about 20% of the creep rupture time and a minimum value at about 50%, showing a strong correlation between ultrasonic attenuation and the creep life fraction. In addition to a slight increase during the primary creep, the ultrasonic velocity exhibits a significant change during the tertiary creep. Based on the analysis of microstructure changes, it indicated that the ultrasonic attenuation is significantly sensitive to the dynamic changes of the dislocation. In contrast, the velocity is mainly related to the evolution of precipitates. The Vickers hardness decreases monotonously during the creep process and presents a linear relation with the inverse of average diameter of M{sub 23}C{sub 6} carbides during the secondary and tertiary creep. Accordingly, it suggested that the present ultrasonic and hardness measurements provided a convenient tool to evaluate the microstructure evolution during creep degradation of heat-resistant steels.

36 MATERIALS SCIENCE↗