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At least 19 records

Microstructure Characterization and Stress Corrosion Evaluation of Autogenous and Hybrid Friction Stir Welded Al-Cu-Li 2195 Alloy

Friction stir welding process is being evaluated for application on the Al-Cu-Li 2195 Super-Light Weight External Tank of the Space Transportation System. In the present investigation Al-Cu-Li 2195 plates were joined by autogenous friction stir welding (FSW) and hybrid FSW (friction stir welding over existing variable polarity plasma arc weld). Optical microscopy and transmission electron microscopy (TEM) were utilized to characterize microstructures of the weldments processed by both welding methods. TEM observations of autogenous FSW coupons in the center section of the dynamically-recrystallized zone showed an equiaxed recrystallized microstructure with an average grain size of approx. 3.8 microns. No T(sub 1), precipitates were present in the above-mentioned zone. Instead, T(sub B) and alpha precipitates were found in this zone with a lower population. Alternate immersion, anodic polarization, constant load, and slow strain tests were carried out to evaluate the general corrosion and stress-corrosion properties of autogenous and hybrid FSW prepared coupons. The experimental results will be discussed.

Li, Zhixian

Microstructural Characterization of Reaction-Formed Silicon Carbide Ceramics

Microstructural characterization of two reaction-formed silicon carbide ceramics has been carried out by interference layering, plasma etching, and microscopy. These specimens contained free silicon and niobium disilicide as minor phases with silicon carbide as the major phase. In conventionally prepared samples, the niobium disilicide cannot be distinguished from silicon in optical micrographs. After interference layering, all phases are clearly distinguishable. Back scattered electron (BSE) imaging and energy dispersive spectrometry (EDS) confirmed the results obtained by interference layering. Plasma etching with CF4 plus 4% O2 selectively attacks silicon in these specimens. It is demonstrated that interference layering and plasma etching are very useful techniques in the phase identification and microstructural characterization of multiphase ceramic materials.

Singh, M.

Microstructural characterization of SiC (SCS) filaments

Microstructural features of SiC('SCS') fibers demonstrating growth properties have been investigated using scanning and transmission electron microscopy. An etchant of fused KOH:KNO3 was developed which adequately brought out previously undetermined features.

Wawner, F. W.

High-Throughput Microstructural Characterization and Process Correlation Using Automated Electron Backscatter Diffraction

The need to optimize the processing conditions of additively manufactured (AM) metals and alloys has driven advances in throughput capabilities for material property measurements such as tensile strength or hardness. High-throughput (HT) characterization of AM metal microstructure has fallen significantly behind the pace of property measurements due to intrinsic bottlenecks associated with the artisan and labor-intensive preparation methods required to produce highly polished surfaces. This inequality in data throughput has led to a reliance on heuristics to connect process to structure or structure to properties for AM structural materials. In this study, we show a transformative approach to achieve laser powder bed fusion (LPBF) printing, HT preparation using dry electropolishing and HT electron backscatter diffraction (EBSD). This approach was used to construct a library of > 600 experimental EBSD sample sets spanning a diverse range of LPBF process conditions for AM Kovar. This vast library is far more expansive in parameter space than most state-of-the-art studies, yet it required only approximately 10 labor hours to acquire. Build geometries, surface preparation methods, and microscopy details, as well as the entire library of >600 EBSD data sets over the two sample design versions, have been shared with intent for the materials community to leverage the data and further advance the approach. Using this library, we investigated process–structure relationships and uncovered an unexpected, strong dependence of microstructure on location within the build, when varied, using otherwise identical laser parameters.

Characterization and Analytical Technique

FFTF HT9 Cladding Microstructure Characterization

The sodium-cooled fast reactor (SFR) is a promising candidate for next generation nuclear reactors, operating at extreme conditions which include high temperatures (>500?C core outlet temperature) and significant neutron damage. High-Cr martensitic HT9 steel is an excellent candidate for SFR cladding and duct material due to its compatibility with liquid sodium, good thermal conductivity, resistance to void swelling, and strong creep rupture strength [1-4].However, the harsh in-core environment of SFRs can cause complex microstructural changes and mechanical property degradation in HT-9. Ensuring the safe use of HT9 cladding for metallic fuel requires both a thorough understanding of its mechanical response to microstructure evolution as well as reliable microstructure-sensitive modeling predictions. Microstructure-sensitive modeling of high temperature creep behavior in HT9 cladding for SFR applications currently lack experimental data to model the phenomena accurately. To fill this need, methods to perform microstructural characterization have been developed and performed on HT9.

36 MATERIALS SCIENCE

Mechanical Properties and Microstructural Characterization of Particulate Reinforced Diboride Composites for High Temperature Leading Edge Applications

Previous work on refractory diboride composites has shown that these systems have the potential for use in high temperature leading edge applications for reusable reentry vehicles. Experiments in reentry environments have shown that these materials have multiple use temperatures greater than 1900 C. The work to be discussed focuses on three compositions: HfB2/SiC, ZrB2/SiC, and ZrB2/C/SiC. These composites have been hot pressed and their mechanical properties measured at room and elevated temperatures. Extensive microstructural characterization has been conducted on polished cross sections and the fracture surfaces have been examined to determine their failure origins.

Ellerby, Donald T.

Mechanical Properties and Microstructural Characterization of Particulate Reinforced Diboride Composites for High Temperature Leading Edge Applications

Previous work on refractory diboride composites has shown that these systems have the potential for use in high temperature leading edge applications for reusable reentry vehicles. Experiments in reentry environments have shown that these materials have multiple use temperatures greater than 1900 C. The work to be discussed focuses on three compositions: HfB2/SiC, ZrB2/SiC, and ZrB2/C/SiC. These composites have been hot pressed and their mechanical properties measured at room and elevated temperatures. Extensive microstructural characterization has been conducted on polished cross sections and the fracture surfaces have been examined to determine their failure origins.

Ellerby, Donald T.

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur

A Novel Ultrasonic Method for Characterizing Microstructural Gradients in Tubular Structures

Ultrasonic velocity and time-of-flight (TOF) imaging that uses back surface reflections to gage volumetric material quality is highly suited for quantitative characterization of microstructural gradients including those due to pore fraction, density, fiber fraction, and chemical composition variations. However, a weakness of conventional pulse echo ultrasonic velocity and TOF imaging is that the image shows the effects of thickness as well as microstructural variations, unless the part is uniformly thick. This limits this imaging method's usefulness in practical applications. Prior studies have described a pulse echo TOF based ultrasonic imaging method that requires using a single transducer in combination with a reflector plate placed behind samples which, eliminates the effect of thickness variation in the image. In those studies, this method was successful at isolating ultrasonic variations due to material in plate like samples of silicon nitride, metal matrix composite, and polymer matrix composite. In this study, the method is engineered for inspection of more complex shaped structures- those having (hollow) tubular or curved geometry. The experimental inspection technique and results are described as applied to a polymer matrix composite "proof of concept" tube that contains machined patches of various depths and an as manufactured monolithic silicon nitride ceramic tube that might be used in "real world" applications.

Roth, Don J.

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

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.

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.

Microstructural Characterization of Polymers by Positron Lifetime Spectroscopy

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.

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

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

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