Search NASA⌕ Search

SEARCH · Search NASA

Results for “Microstructure characterization”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 253 records · Page 14

Examining the microtexture evolution in a hole-edge punched into 780 MPa grade hot-rolled steel

The deformation behavior in the hole-edge of 780 MPa grade hot-rolled steel during the punching process was investigated via microstructure characterization and computational simulation. Microstructure characterization was conducted to observe the edges of punched holes through the thickness direction, and electron back-scattered diffraction (EBSD) was used to analyze the heterogeneity of the deformation. Finite element analysis (FEA) that could account for a ductile fracture criterion was conducted to simulate the deformation and fracture behaviors of 780 MPa grade hot-rolled steel during the punching process. Calculation of rotation rate fields at the edges of the punched holes during the punching process revealed that metastable orientations in Euler space were confined to specific orientation groups. Rotation-rate fields effectively explained the stability of the initial texture components in the hole-edge region during the punching process. A visco-plastic self-consistent (VPSC) polycrystal model was used to calculate the microtexture evolution in the hole-edge region during the punching process. FEA revealed that the heterogeneous effective strain was closely related to the heterogeneity of the Kernel average misorientation (KAM) distribution in the hole-edge region. A simulation of the deformation microtexture evolution in the hole-edge region using a VPSC model was in good agreement with the experimental results. - Highlights: •We analyzed the microstructure in a hole-edge punched in HR 780HB steel. •Rotation rate fields revealed the stability of the initial texture components. •Heterogeneous effective stain was closely related to the KAM distribution. •VPSC model successfully simulated the deformation microtexture evolution.

36 MATERIALS SCIENCE↗

Characterizing Copper-Graphene Composites (Abstract)

In this project, Pacific Northwest National Laboratory (PNNL) will measure the electrical and mechanical properties of the metal composite samples provided by MetalKraft Technologies, LLC. PNNL will also use multimodal methods for characterizing the microstructure of MetalKraft Technologies, LLC’s copper graphene composites. PNNL will work with MetalKraft Technologies, LLC as part of the CABLE Manufacturing Prize efforts under a CRADA. The voucher from DOE has a budget of $100,000 over a period of 6 months. PNNL will be the primary place of performance for the property and microstructure characterization efforts.

36 MATERIALS SCIENCE↗

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↗

Scaling up the Single Transducer Thickness-Independent Ultrasonic Imaging Method for Accurate Characterization of Microstructural Gradients in Monolithic and Composite Tubular Structures

Ultrasonic velocity/time-of-flight imaging that uses back surface reflections to gauge 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/time-of-flight 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 time-of-flight-based ultrasonic imaging method that requires using a single transducer in combination with a reflector plate placed behind samples that eliminates the effect of thickness variation in the image. In those studies, this method was successful at isolating ultrasonic variations due to material microstructure 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/curved geometry. The experimental inspection technique and results are described as applied to (1) monolithic mullite ceramic and polymer matrix composite 'proof-of-concept' tubular structures that contain machined patches of various depths and (2) as-manufactured monolithic silicon nitride ceramic and silicon carbide/silicon carbide composite tubular structures that might be used in 'real world' applications.

Roth, Don J.↗

Infrared spectroscopy data- and physics-driven machine learning for characterizing surface microstructure of complex materials

There is a need to characterize complex materials and their dynamics under reaction conditions to accelerate materials design. Adsorbate vibrational excitations are selective to adsorbate/surface interactions and infrared (IR) spectra associated with activating adsorbate vibrational modes are accurate, capture details of most modes, and can be obtained operando. Current interpretation depends on heuristic peak assignments for simple spectra, precluding the possibility of obtaining detailed structural information. Here, we combine data-based approaches with chemistry-dependent problem formulation to develop physics-driven surrogate models that generate synthetic IR spectra from first-principles calculations. Using synthetic IR spectra of carbon monoxide on platinum, we implement multinomial regression via neural network ensembles to learn probability distributions functions (pdfs) that describe adsorption sites and quantify uncertainty. We use these pdfs to infer detailed surface microstructure from experimental spectra and extend this methodology to other systems as a first step towards characterizing complex interfaces and closing the materials gap.

Science & Technology - Other Topics↗

Far-Field High-Energy Diffraction Microscopy: A Non-Destructive Tool for Characterizing the Microstructure and Micromechanical State of Polycrystalline Materials

A suite of non-destructive, three-dimensional X-ray microscopy techniques have recently been developed and used to characterize the microstructures of polycrystalline materials. These techniques utilize high-energy synchrotron radiation and include near-field and far-field diffraction microscopy (NF- and FF-HEDM, respectively) and absorption tomography. Several compatible sample environments have also been developed, enabling a wide range of 3D studies of material evolution. In this article, the FF-HEDM technique is described in detail, including its implementation at the 1-ID beamline of the Advanced Photon Source. Examples of how the information obtained from FF-HEDM can be used to deepen our understanding of structure-property-processing relationships in selected materials are presented.

36 MATERIALS SCIENCE↗

Update on Activities Related to the Library of Graphite Microstructures

This report provides an overview and update of the ongoing efforts to create a comprehensive library of microstructures for nuclear graphite and carbon-based materials under consideration for nuclear applications. The library includes data on microstructural characterization of unirradiated graphite materials, a guide to the techniques used to analyze graphite (which complements the ASME guidelines and ASTM standards), a summary of characterization data for neutron-irradiated or oxidized material, and a compendium of microstructural information for carbon-based materials. These efforts are being conducted at various length scales for the filler and binder phases in graphite to better understand graphite’s local structure and property relationships. This report is a follow-up to the previous milestone report titled Report on initial development of a database of nuclear graphite characteristics based on microstructural characterization, ORNL/TM/-2023/2992, published in July 2023.The effort to develop the library of microstructures supports the US Department of Energy Office of Advanced Reactor Technologies program objectives of aiding the material selection, licensing, management, and core assessments of a graphite core by documenting the unirradiated microstructure of relevant grades or characterizing the microstructure’s evolution under the reactor environment. Additionally, this project aims to provide (1) information and guidelines for the characterizing of graphite and (2) a protocol to assess a nuclear graphite grade.

36 MATERIALS SCIENCE↗

Ultrasonic characterization of microstructure in powder metal alloy

The ultrasonic wave propagation characteristics were measured for IN-100, a powder metallurgy alloy used for aircraft engine components. This material was as a model system for testing the feasibility of characterizing the microstructure of a variety of inhomogeneous media including powder metals, ceramics, castings and components. The data were obtained for a frequency range from about 2 to 20 MHz and were statistically averaged over numerous volume elements of the samples. Micrographical examination provided size and number distributions for grain and pore structure. The results showed that the predominant source for the ultrasonic attenuation and backscatter was a dense (approx. 100/cubic mm) distribution of small micropores (approx. 10 micron radius). Two samples with different micropore densities were studied in detail to test the feasibility of calculating from observed microstructural parameters the frequency dependence of the microstructural backscatter in the regime for which the wavelength is much larger than the size of the individual scattering centers. Excellent agreement was found between predicted and observed values so as to demonstrate the feasibility of solving the forward problem. The results suggest a way towards the nondestructive detection and characterization of anomalous distributions of micropores when conventional ultrasonic imaging is difficult. The findings are potentially significant toward the application of the early detection of porosity during the materials fabrication process and after manufacturing of potential sites for stress induced void coalescence leading to crack initiation and subsequent failure.

Tittmann, B. R.↗

Explicit Backscattering Coefficient for Ultrasonic Wave Propagating in Hexagonal Polycrystals with Fiber Texture

Hexagonal polycrystalline materials such as titanium, zirconium and magnesium are common in engineering structures like car bodies and airplane engines. These components are usually specially designed in microstructure level to guarantee desired mechanical properties, so microstructure characterization is of great importance to the optimization of manufacturing processes. Compared with traditional destructive characterization methods like scanning electron microscopy (SEM), the ultrasonic approach is nondestructive and cost-effective. Although some progress has been made in ultrasonic microstructure characterization of polycrystal aggregates of hexagonal grains, some factors like macro texture and grain size distribution associated with realistic microstructures were not accounted for yet. Targeting one common texture component for hexagonal polycrystalline materials, {0001} basal fiber texture, this paper derived the explicit backscattering coefficient for aggregates of ellipsoidal grains through one texture parameter and obtained an analytical backscattering coefficient for microstructures with various grain size distributions. In this study, the basal fiber texture was quantified by the 1D Gaussian orientation distribution function (ODF), which merely includes one texture parameter, and its relationship with generalized spherical harmonics ODF was also addressed. Moreover, explicit expressions for effective elastic moduli and elastic constant covariances were derived. Furthermore, some computational examples were given to demonstrate the impacts of texture, frequency, grain geometry and grain size distribution on backscattering behavior. The theoretical results in this study will greatly benefit the later ultrasonic microstructure characterization of hexagonal polycrystalline materials.

42 ENGINEERING↗

Characterization of microstructure with low frequency electromagnetic techniques

A new computational method for characterizing the relationship between surface crystallography and electrical conductivity in anisotropic materials with low frequency electromagnetic techniques is presented. The method is discussed from the standpoint of characterizing the orientation of a single grain, as well as characterizing statistical information about grain ensembles in the microstructure. Large-area electron backscatter diffraction (EBSD) data was obtained and used in conjunction with a synthetic aperture approach to simulate the eddy current response of beta annealed Ti-6Al-4V. Experimental eddy current results are compared to the computed eddy current approximations based on electron backscatter diffraction (EBSD) data, demonstrating good agreement. The detectability of notches in the presence of noise from microstructure is analyzed with the described simulation method and advantages and limitations of this method are discussed relative to other NDE techniques for such analysis.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

SEM and TEM characterization of microstructure of stainless steel composites reinforced with TiB{sub 2}

Steel-8TiB{sub 2} composites were produced by two new sintering techniques, i.e. Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT) sintering. This study discusses the impact of these sintering methods on the microstructure of steel composites reinforced with TiB{sub 2} particles. Scanning electron microscopy (SEM), wavelength dispersive spectroscopy (WDS), X-ray diffraction, electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) were used to analyze the microstructure evolution in steel matrix composites. The results of microscopic examinations revealed a close relationship between the composite microstructure and the methods and conditions of sintering. Substantial differences were observed in the grain size of materials sintered by HP-HT and SPS. It has been demonstrated that the composites sintered by HP-HT tend to form a chromium-iron-nickel phase in the steel matrix. In contrast, the microstructure of the composites sintered by SPS is characterized by the presence of complex borides and chromium-iron phase. - Highlights: •The steel-8TiB{sub 2} composites were fabricated by Spark Plasma Sintering (SPS) and High Pressure-High Temperature (HP-HT). •Sintering techniques has an important effect on changes in the microstructure of steel-8TiB{sub 2} composites. •New phases of different size and morphology were identified.

36 MATERIALS SCIENCE↗

Report on the FY20 Characterization of Age Hardened Alloy 709 Materials

This report provides the results on microstructural characterization of the first commercial heat of Alloy 709 plate material undergone additional age hardening treatment. In FY19, through thermodynamic-kinetic modeling and microstructural characterization, it is determined that the 775°C/10 h age-hardening treatment can promote desired precipitation on dislocations and has the potential to further improve the mechanical performance of the material. In FY20, the treatment protocol was applied to the ESR-1150°C condition, and the microstructure was then compared with the ESR-1100°C condition. It was found that the 1150°C solution annealing (SA) dramatically reduced the dislocation density compared to the 1100°C SA, resulting a smaller number density of Nb-rich fine precipitates which grow on dislocations during the age hardening treatment. Other features are very similar between the two. The effect of age hardening on creep performance is discussed. In addition, TEM characterization of a creep-ruptured sample (600°C/330 MPa) was performed. Specimens from the grip region and the gauge region was studied. The grip region specimen was effectively aged at 600°C for extended period, while the gauge region specimen was mechanically deformed at 600°C. The microstructures are very different, implying the importance of a dynamical effect on precipitation.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

STEM imaging of irradiation induced defects in Eurofer97 steel variants irradiated in the EUROfusion collaboration

Ten exploratory variants of Eurofer97 reduced activation ferritic martensitic (RAFM) steel were irradiated in HFIR to ~2.94 – 32.4 dpa, 300±30 °C as a part of the EUROfusion collaboration. The irradiations were performed in rabbit capsules. ES21-22 capsule were used for irradiating SS-J3 tensile samples while M4CVN bend bar samples were irradiated in ES31-35 capsules. The mechanical properties and multi-length scale characterization of the microstructures of these ten steels, designated as H, I, P, J, K, L, M, N, O, P and reference E, in the nonirradiated form was reported in "Mechanical properties and microstructure characterization of unirradiated Eurofer-97 steel variants for the EUROfusion project, ORNL/SPR-2018/882," while their irradiated properties and some microstructure analysis was reported in "Post-irradiation examination of Eurofer97 steel variants irradiated to 2.5 dpa, ~300 °C in HFIR for the EUROfusion program, ORNL/SPR-2020/1440." Here, additional microstructures using TEM/STEM and STEM-EDX of the irradiated steels is presented. Characterization was performed at the Low Activation Materials Development and Analysis (LAMDA) laboratory.

36 MATERIALS SCIENCE↗

Microstructural and Defect Characterization in Ceramic Composites Using an Ultrasonic Guided Wave Scan System

In this study, an ultrasonic guided wave scan system was used to characterize various microstructural and flaw conditions in two types of ceramic matrix composites, SiC/SiC and C/SiC. Rather than attempting to isolate specific lamb wave modes to use for characterization (as is desired for many types of guided wave inspection problems), the guided wave scan system utilizes the total (multi-mode) ultrasonic response in its inspection analysis. Several time and frequency-domain parameters are calculated from the ultrasonic guided wave signal at each scan location to form images. Microstructural and defect conditions examined include delamination, density variation, cracking, and pre/ post-infiltration. Results are compared with thermographic imaging methods. Although the guided wave technique is commonly used so scanning can be eliminated, applying the technique in the scanning mode allows a more precise characterization of defect conditions.

Roth, D. J.↗

Ultra-Fast Laser Fabrication of Alumina Micro-Sample Array and High-Throughput Characterization of Microstructure and Hardness

In the light of recent advances in material informatics, there is a great demand for high-throughput approaches of sample fabrication and property characterization. Currently, no high-throughput approach has been demonstrated for the fast sampling of the microstructure and the correlated properties. In this paper, we demonstrate the ultra-fast fabrication of an alumina sample array and the high-throughput hardness characterization of these sample units. The alumina sample array was fabricated using picosecond (PS) laser micromachining and CO2 laser sintering within a short time (i.e., less than a few minutes). After laser sintering, the hardness of these sample units was characterized using micro-indentation, and the microstructure was observed using scanning electron microscopy (SEM). In each sample unit, the microstructure was uniform for the entire top surface and within about 20 µm depth from the top surface. The relative density (RD) and corresponding micro-hardness of the sample units was found to continuously vary over a wide range from 89% RD with 600 kgf/mm2 hardness to 99% RD with 1609 kgf/mm2 hardness. For these laser-sintered samples, the correlation of hardness and relative density of the alumina matched well with the literature reports on sintered alumina obtained using conventional low-throughput furnace sintering experiments.

36 MATERIALS SCIENCE↗

Characterization of martensite-austenite constituents and micro-hardness in intercritical reheated and coarse-grained heat affected zones of API X70 HSLA steel

Highlights: • The influence of cold wire addition to the tandem submerged arc welding process on the ICRCGHAZ is investigated. • Comprehensive characterization of the microstructure and micro-hardness in the ICRCGHAZ of a HSLA steel is performed. • A lower fraction of finely distributed M-A formed in the ICRCGHAZ of TSAW + cold wire steel, leading to lower micro-hardness. • The aspect ratio and inter-particle spacing of M-A constituents decreased in the ICRCGHAZ through cold wire addition. - Abstract: The thermal cycles that high strength low alloy (HSLA) low carbon steels experience during welding inevitably affect the microstructure and mechanical properties of the weld joints. It is generally agreed that the coarse-grained heat affected zone (CGHAZ) and the intercritical reheated coarse-grained heat affected zone (ICRCGHAZ) in one-pass and multi-pass welding, respectively, have the poorest microstructure and mechanical properties relative to the rest of the steel joint. The martensite-austenite (M-A) constituents formed in the HAZ regions predominantly govern property deterioration in the CGHAZ and the ICRCGHAZ by promoting the initiation and propagation of micro-cracks. However, the characteristics of the M-A constituents, i.e., fraction, size, shape and aspect ratio, are strongly affected by the welding heat input. Accordingly, in this study, the aim was to evaluate the influence of a cold wire addition in conventional tandem submerged arc welding (TSAW + cold-wire) on the microstructure and micro-hardness in the CGHAZ and ICRCGHAZ. Microstructural characterization showed that a lower fraction of finely distributed M-A constituents associated with smaller prior austenite grains (PAGs) formed in the CGHAZ of the steel welded by the TSAW + cold-wire process (CW-OD weld) relative to that welded by the conventional TSAW process (TW-OD weld). Furthermore, the fraction of M-A constituents in the ICRCGHAZ of the CW-OD weld was decreased. A higher fraction of slender shaped M-A constituents in the ICRCGHAZ of the TW-OD weld resulted in an increase in the micro-hardness. The microstructure and micro-hardness changes associated with cold wire addition were attributed to the lower welding heat input and, consequently, the faster cooling rate with a corresponding reduction in the retention time in the austenitic region and ferrite/austenite region in the CGHAZ and ICRCGHAZ regions, respectively.

36 MATERIALS SCIENCE↗

On the toughness scatter in low alloy C-Mn steel samples fabricated using wire arc additive manufacturing

Low alloy carbon manganese (C-Mn) steel builds were fabricated using a wire based additive manufacturing system developed at Oak Ridge National Laboratory. Specimens were fabricated in the X,Y and Z direction and detailed mechanical testing was performed. The mechanical testing results showed a significant scatter in tensile ductility and significant variation in Charpy toughness. Further detailed microstructure characterization showed significant microstructural heterogeneity in builds fabricated in each direction. The scatter in mechanical properties was then rationalized based on the microstructural observations and the underlying changes in the local heat transfer conditions. Lastly, the results indicate that when fabricating parts using C-Mn low alloy steel welds the process parameters and tool path should be chosen such that the cooling rate from 800 °C to 500 °C is greater than 30 s to avoid formation of martensite austenite (MA) phases, which leads to toughness reductions.

36 MATERIALS SCIENCE↗