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NASA NTRS2017

Microstructural Characterization and Modeling of SLM Superalloy 718

Superalloy 718 is an excellent candidate for selective laser melting (SLM) fabrication due to a combination of excellent mechanical properties and workability. Predicting and validating the microstructure of SLM-fabricated Superalloy 718 after potential post heat-treatment paths is an important step towards producing components comparable to those made using conventional methods. At present, obtaining accurate volume fraction and size measurements of gamma-double-prime, gamma-prime and delta precipitates has been challenging due to their size, low volume fractions, and similar chemistries. A technique combining high resolution distortion corrected SEM imaging and with x-ray energy dispersive spectroscopy has been developed to accurately and independently measure the size and volume fractions of the three precipitates. These results were further validated using x-ray diffraction and phase extraction methods and compared to the precipitation kinetics predicted by PANDAT and JMatPro. Discrepancies are discussed in context of materials properties, model assumptions, sampling, and experimental errors.

SEM↗

DOE OSTI2023

Report on initial development of a database of nuclear graphite characteristics based on microstructural characterization

This report outlines the current and future efforts to produce a comprehensive library of microstructures of nuclear graphite and carbon-based materials that are candidate materials for nuclear applications in the United States. This library must contain extensive characterizations of unirradiated graphite materials, a guide to some of the techniques used to characterize graphite, a compendium of characterization data of neutron-irradiated or oxidized material, and a compendium of microstructural information of carbon-based materials. These characterization efforts are being conducted at various length scales to understand these complex materials’ local structure and property relationships. Achieving this goal requires further developing or adapting advanced characterization techniques that capture graphite’s most relevant characteristics. Some of the general objectives of this project are to aid with the material selection, licensing, management, and core assessments of a graphite core by documenting the unirradiated microstructure of relevant grades or by characterizing the evolution of the microstructure under the reactor environment. Moreover, this project aims to provide additional information, guidelines for characterizing graphite, and a protocol to assess a nuclear graphite grade. This report also summarizes some of the initial results and some of the techniques commonly used to characterize nuclear graphite.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Microstructural characterization of U-20Pu-10Zr-4Sb and U-20Pu-10Zr-4Sb-4Ln

Antimony is being investigated as a potential additive to metallic fuel to control fuel-cladding chemical interactions (FCCI). The most detrimental elements involved in FCCI are fission product lanthanides, leading to brittle intermetallics and low melting eutectic phases. Previous investigations of Sb as an additive focused on U-10Zr, in wt. %, as the fuel. The current investigation expands that to include Pu in the fuel. Here, two alloys, U-20Pu-10Zr-4Sb and U-20Pu-10Zr-4Sb-4Ln (wt. %, Ln=53Nd-25Ce-16Pr-6La) have been investigated using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to characterize the fuel as-cast microstructure and the microstructure after introduction of lanthanides. Sb reacts with Zr initially, forming Zr 2 Sb and Zr 5 Sb 3 , with as much as 20 at. % interstitial Pu present. In the presence of lanthanides, Sb forms Ln 4 Sb 3 with the lanthanides, containing ~14 at. % Pu. The Pu is substitutional for the lanthanides in the crystal lattice.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Microstructural Characterization of A709 Commercial Heats with Precipitation Treatment

This report discusses work conducted at Idaho National Laboratory in fiscal year 2022 associated with the precipitates in Alloy 709 (A709). The purpose of this work is to support the development of the A709 Code Cases to qualify A709 in Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code. This would permit the use of A709 for elevated-temperature nuclear construction. This work encompassed two broad goals. The first goal was to understand the microstructure of the second commercial heat of plate A709 purchased through the Advanced Reactors Technologies Program in both the solution-annealed and precipitation-treated conditions. Transmission electron microscopy was utilized to characterize these microstructures. Direct comparisons were then made between the solution-annealed and precipitation-treated conditions as well as between the first and second commercial heats of plate A709. The second goal was to understand the impact of variations in the time and temperature of the precipitation treatment on the properties of A709. The precipitation treatment temperature was varied from 750°C to 800°C for times ranging from 3 hours to 30 hours. The hardness of each precipitation treatment variation was measured. All of the precipitation treatment variations investigated besides a specimen from the second commercial heat of plate A709 precipitation treated at 800? for 9 hours met the room-temperature hardness requirement specified in ASTM A213 and SA-213 for UNS S31025. The hardness measured for the specimen from the second commercial heat of plate A709 that was precipitation treated at 800? for 9 hours is considered an outlier. The next step is to look at the extremes of the precipitation treatment variations investigated and conduct elevated-temperature mechanical testing. The purpose of this testing would be to assess if these time and temperature variations have any impact on the mechanical performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2004

Ultrasonic Guided-Wave Scan System Used to Characterize Microstructure and Defects in Ceramic Composites

Ceramic matrix composites (CMCs) are being developed for advanced aerospace propulsion applications to save weight, improve reuse capability, and increase performance. However, mechanical and environmental loads applied to CMCs can cause discrete flaws and distributed microdamage, significantly reducing desirable physical properties. Such microdamage includes fiber/matrix debonding (interface failure), matrix microcracking, fiber fracture and buckling, oxidation, and second phase formation. A recent study (ref. 1) of the durability of a C/SiC CMC discussed the requirement for improved nondestructive evaluation (NDE) methods for monitoring degradation in these materials. Distributed microdamage in CMCs has proven difficult to characterize nondestructively because of the complex microstructure and macrostructure of these materials. This year, an ultrasonic guided-wave scan system developed at the NASA Glenn Research Center was used to characterize various microstructural and flaw conditions in SiC/SiC (silicon carbide fiber in silicon carbide matrix) and C/SiC (carbon fiber in silicon carbide matrix) CMC samples.

Roth, Don J.↗

NASA NTRS1997

Microstructural Characterization of Polymers with Positrons

Positrons provide a versatile probe for monitoring microstructural features of molecular solids. In this paper, we report on positron lifetime measurements in two different types of polymers. The first group comprises polyacrylates processed on earth and in space. The second group includes fully-compatible and totally-incompatible Semi-Interpenetrating polymer networks of thermosetting and thermoplastic polyimides. On the basis of lifetime measurements, it is concluded that free volumes are a direct reflection of physical/electromagnetic properties of the host polymers.

Singh, Jag J.↗

NASA NTRS1996

Microstructural Characterization of Polymers by Positron Lifetime Spectroscopy

Singh, Jag J.↗

DOE OSTI2025

Microstructural Characterization of AGR-2 TRISO-coated Particle Buffer, IPyC, and Buffer-IPyC Interfaces

Investigating the microstructural, mechanical, and chemical behaviors of Tristructural Isotropic (TRISO) fuel particles is vital for its qualification and use in advanced reactors. Central to the study of TRISO particles is understanding the silicon carbide (SiC) layer's ability to confine fission products, with failure mechanisms linked to chemical degradation following mechanical degradation of the buffer and IPyC layers. Research has been done to quantify the micro-tensile properties of the buffer, inner pyrolytic carbon (IPyC), and buffer-IPyC interlayer regions and their interactions within both irradiated and un-irradiated TRISO particles. Techniques such as atom probe tomography (APT) and transmission electron microscopy (TEM) have also been deployed to examine microstructural defects and fission product distribution in detail. The goal is to understand layer delamination, establish connections between microstructure and mechanical attributes, and inform computational predictions of fuel performance. This work may help refine predictive models of TRISO fuel behavior and facilitating its certification for use in advanced reactors.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRSDate not supplied

Microstructural Characterization of Laser Powder Bed Fusion (L-PBF) Additively Manufactured Inconel 718 for Aerospace Application

Alloy 718 (Inconel 718) is used for aerospace applications because of its excellent corrosion resistance and mechanical properties. This alloy is particularly applicable in manufacturing components subjected to high temperatures in rocket engines, aero-engines, and gas turbines. Properties for this alloy when processing on systems from similar and different Laser Powder Bed Fusion (L-PBF) machines provide subtle differences due to process parameters, feedstock, and machine configurations. A series of sixteen L-PBF AM Inconel 718 geometric feature build plates have been evaluated for microstructure using optical microscopy. This study presents the details of the microstructure analysis concerning geometry and different machine platforms. Microstructural investigations of these samples included average grain width measurement for all the X-Y and Y-Z build layers and are accompanied by process parameters and powder characterization. The present work concludes with a discussion on the importance of captured differences among builds to understand the practical limitations among AM platforms.

Additive Manufacturing↗

DOE OSTI2023

Microstructural Characterizations of Two High Fluence Baffle-Former Bolts Retrieved from a Westinghouse Two-loop Downflow Type PWR

As one of the pressurized water reactor (PWR) internal components, baffle-former bolts (BFBs) are subjected to significant mechanical stress and neutron irradiation from the reactor core during the plant operation. Over the long operation period, these conditions lead to potential degradation and reduced load-carrying capacity of the bolts. In support of evaluating long-term operational performance of materials used in core internal components, the Oak Ridge National Laboratory (ORNL), through the Department of Energy (DOE), Office of Nuclear Energy, Light Water Reactor Sustainability (LWRS) Program, Materials Research Pathway (MRP), has harvested two high fluence BFBs from a commercial Westinghouse two-loop downflow type PWR. The two bolts of interest, i.e. bolts # 4412 and 4416, were withdrawn from service in 2011 as part of a preventative replacement plan. No identification of cracking or potential damage was found for these bolts during their removal in 2011. However, the bolts required a lower torque for removal from the baffle structure than the original torque specified during installation. Irradiation damage levels in the bolts range from 15 to 41 displacements per atom. The goal of this project is to perform detailed microstructural and mechanical property characterization of BFBs following in-service exposures. The information from these bolts will be integral to the LWRS program initiatives in evaluating end of life microstructure and properties. Furthermore, valuable data will be obtained that can be incorporated into model predictions of long term irradiation behavior and compared to results obtained from experimental reactor conditions

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

An Integrated High-Speed Microstructural Characterization Method Using Simultaneous XRD, Stereo-DIC, and PCI

High-speed characterization of the deformation mechanisms in polycrystalline metals requires the quantification of full strain fields and local microstructural evolutions simultaneously. In this paper, we present a novel experimental method to integrate phase-contrast imaging (PCI), stereographic digital image correlation (stereo-DIC), and full-ring X-ray diffraction (XRD) to allow for the simultaneous characterization of polycrystalline metals at 1MHz or higher. A Kolsky bar was integrated into the synchrotron X-ray source in Sector 32 ID-B at the Advance Photon Source (APS) at Argonne National Laboratory. When the sample is dynamically loaded, the diagnostic methods of full-ring XRD, PCI, and stereo-DIC are properly synchronized to record the deformation behavior at both continuum and microstructural scales as a function of the loading history. An advanced high-strength steel (AHSS) is used as a model material to demonstrate the capabilities of this new experimental method.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Microstructural Characterization of Enhanced Conductivity Aluminum Alloys (Abstract)

In this project, Pacific Northwest National Laboratory (PNNL) will perform multimodal imaging to determine the microstructural features of enhanced conductivity aluminum alloys manufactured by NanoAL LLC. In particular, we will perform imaging to identify the basis of the strengthening mechanisms in the custom AA6X alloys provided by NanoAL LLC. These activities will be performed as part of a voucher service provided by the PNNL for the CABLE Manufacturing Prize stewarded by DOE Advanced Manufacturing Office. This 6-month effort will be executed predominantly at PNNL with a budget of $50,000.

36 MATERIALS SCIENCE↗

NASA NTRS2010

Microstructural Characterization of Metal Foams: An Examination of the Applicability of the Theoretical Models for Modeling Foams

Establishing the geometry of foam cells is useful in developing microstructure-based acoustic and structural models. Since experimental data on the geometry of the foam cells are limited, most modeling efforts use the three-dimensional, space-filling Kelvin tetrakaidecahedron. The validity of this assumption is investigated in the present paper. Several FeCrAlY foams with relative densities varying between 3 and 15 percent and cells per mm (c.p.mm.) varying between 0.2 and 3.9 c.p.mm. were microstructurally evaluated. The number of edges per face for each foam specimen was counted by approximating the cell faces by regular polygons, where the number of cell faces measured varied between 207 and 745. The present observations revealed that 50 to 57 percent of the cell faces were pentagonal while 24 to 28 percent were quadrilateral and 15 to 22 percent were hexagonal. The present measurements are shown to be in excellent agreement with literature data. It is demonstrated that the Kelvin model, as well as other proposed theoretical models, cannot accurately describe the FeCrAlY foam cell structure. Instead, it is suggested that the ideal foam cell geometry consists of 11 faces with 3 quadrilateral, 6 pentagonal faces and 2 hexagonal faces consistent with the 3-6-2 cell.

Raj, S. V.↗

NASA NTRS2011

Microstructural Characterization of Metal Foams: An Examination of the Applicability of the Theoretical Models for Modeling Foams

Establishing the geometry of foam cells is useful in developing microstructure-based acoustic and structural models. Since experimental data on the geometry of the foam cells are limited, most modeling efforts use an idealized three-dimensional, space-filling Kelvin tetrakaidecahedron. The validity of this assumption is investigated in the present paper. Several FeCrAlY foams with relative densities varying between 3 and 15 percent and cells per mm (c.p.mm.) varying between 0.2 and 3.9 c.p.mm. were microstructurally evaluated. The number of edges per face for each foam specimen was counted by approximating the cell faces by regular polygons, where the number of cell faces measured varied between 207 and 745. The present observations revealed that 50 to 57 percent of the cell faces were pentagonal while 24 to 28 percent were quadrilateral and 15 to 22 percent were hexagonal. The present measurements are shown to be in excellent agreement with literature data. It is demonstrated that the Kelvin model, as well as other proposed theoretical models, cannot accurately describe the FeCrAlY foam cell structure. Instead, it is suggested that the ideal foam cell geometry consists of 11 faces with three quadrilateral, six pentagonal faces and two hexagonal faces consistent with the 3-6-2 Matzke cell. A compilation of 90 years of experimental data reveals that the average number of cell faces decreases linearly with the increasing ratio of quadrilateral to pentagonal faces. It is concluded that the Kelvin model is not supported by these experimental data.

Raj, S. V.↗

NASA NTRS2011

Corrigendum to "Microstructural Characterization of Metal Foams: An Examination of the Applicability of the Theoretical Models for Modeling Foams"

Establishing the geometry of foam cells is useful in developing microstructure-based acoustic and structural models. Since experimental data on the geometry of the foam cells are limited, most modeling efforts use an idealized three-dimensional, space-filling Kelvin tetrakaidecahedron. The validity of this assumption is investigated in the present paper. Several FeCrAlY foams with relative densities varying between 3 and 15% and cells per mm (c.p.mm.) varying between 0.2 and 3.9 c.p.mm. were microstructurally evaluated. The number of edges per face for each foam specimen was counted by approximating the cell faces by regular polygons, where the number of cell faces measured varied between 207 and 745. The present observations revealed that 50-57% of the cell faces were pentagonal while 24-28% were quadrilateral and 15-22% were hexagonal. The present measurements are shown to be in excellent agreement with literature data. It is demonstrated that the Kelvin model, as well as other proposed theoretical models, cannot accurately describe the FeCrAlY foam cell structure. Instead, it is suggested that the ideal foam cell geometry consists of 11 faces with 3 quadrilateral, 6 pentagonal faces and 2 hexagonal faces consistent with the 3-6-2 Matzke cell

Raj. Sai V.↗

NASA NTRS1998

Tensile Properties and Microstructural Characterization of Hi-Nicalon SiC/RBSN Composites

The room temperature physical and mechanical properties of silicon carbide fiber-reinforced reaction-bonded silicon nitride matrix composites (SiC/RBSN) were measured, and the composite microstructure was analyzed. The composites consist of nearly 24 vol% of aligned Hi-Nicalon SiC fiber yarns in a approx. 30 vol% porous silicon nitride matrix. The fiber yarns were coated by chemical vapor deposition with a 0.8 mm layer of boron nitride (BN) followed by a 0.2 mm layer of SiC. In the as-fabricated condition, both 1-D and 2-D composites exhibited high strength and graceful failure, and showed improved properties w en compared with unreinforced matrix of comparable density. No indication of reaction between the SiC fiber and BN coating was noticed, but the outer SiC layer reacted locally with the nitridation enhancing additive in the RBSN matrix. A comparison is made between the predicted and measured values of matrix cracking strength.

Bhatt, Ramakrishna T.↗

NASA NTRS1998

Tensile Properties and Microstructural Characterization of Hi-Nicalon SiC/RBSN Composites

The room temperature physical and mechanical properties of silicon carbide fiber-reinforced reaction-bonded silicon nitride matrix composites (SiC/RBSN) were measured, and the composite microstructure was analyzed. The composites consist of nearly 24 vol% of aligned Hi-Nicalon SiC fiber yarns in a approx. 30 vo1% porous silicon nitride matrix. The fiber yarns were coated by chemical vapor deposition with a 0.8 micron layer of boron nitride (BN) followed by a 0.2 micron layer of SiC. In the as-fabricated condition, both 1-D and 2-D composites exhibited high strength and graceful failure, and showed improved properties when compared with unreinforced matrix of comparable density. No indication of reaction between the SiC fiber and BN coating was noticed, but the outer SiC layer reacted locally with the nitridation enhancing additive in the RBSN matrix. A comparison is made between the predicted and measured values of matrix cracking strength.

Bhatt, Ramakrishna T.↗

NASA NTRS2001

C-Coupon Studies of CMCS: Fracture Behavior and Microstructural Characterization

A curved beam 'C-coupon' was used to assess fracture behavior in a Sylramic(tm)/melt infiltration (MI) SiC matrix composite. Failure stresses and fracture mechanisms, as determined by optical and scanning electron microstructural analysis, are compared with finite element stress calculations to analyze failure modes. Material microstructure was found to have a strong influence on mechanical behavior. Fracture occurs in interlaminar tension (ILT), provided that the ratio of ILT to tensile strength for the material is less than the ratio of radial to hoop stresses for the C-coupon geometry. Utilization of 3D architectures to improve interlaminar strength requires significant development efforts to incorporate through thickness fibers in regions with high curvatures while maintaining uniform thickness, radius, and microstructure.

Hurwitz, Frances I.↗