Search NASA⌕ Search

SEARCH · Search NASA

Results for “microstructural analysis”

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 109 records · Page 6

High-throughput experimentation for microstructural design in additively manufactured 316L stainless steel

In the present study, a combination of high-throughput (HT) and low-throughput (LT) techniques was used to rapidly determine the processing window and generate processing maps for Selective Laser Melting (SLM) of 316L stainless steel. The HT method includes the fabrication of hundreds of hex nut-shaped specimens, each processed with a unique combination of laser power, scanning speed, and hatch spacing. An easily removable scaffolding permitted rapid sample extraction from the base plate, thus saving machining cost and time. Hardness and immersion density measurements were used for HT characterization to identify a processing window for maximum strength and density. Within the defined processing window, a low-throughput (LT) microstructural interrogation of specimens were performed. The microstructural analysis included quantification at various length scales (i.e., grains size and morphology, texture, primary dendrite arm spacing, and melt pool geometry analysis). Microstructure-based processing maps as a function of volumetric energy density were generated. The combination of HT and LT methods produced a predictive relationship between hardness and primary dendrite arm spacing using a Hall-Petch relationship. A model is proposed to explain the dependence of microstructure on the melt pool geometry. Here, the HT method can be applied for the microstructural design of SLM-fabricated components in other alloys.

316L stainless steel↗

Materials design of all-cellulose composite using microstructure based finite element analysis

A microstructure based finite element analysis (FEA) model was developed to predict the effective elastic property of cellulose nanowhisker reinforced all-cellulose composite. Analysis was based on microstructure synthesized with assumption on volume fraction, size and orientation distribution of cellulose nanowhiskers. Simulation results demonstrated some interesting discovery: With the increase of aspect ratio, the effective elastic modulus increase. The elastic property anisotropy increases with the narrowing of nanowhisker orientation distribution and increase of aspect ratio. Simulation results from microstructure based FEA agree well with experimental results, comparing with other homogenization methods: upper bound, lower bound and self consistent models. Capturing the anisotropic elastic property, microstructure based FEA demonstrated the capability in guiding microstructure tailor to improve effective properties.

36 MATERIALS SCIENCE↗

Manufacturing of magnesium/aluminum bimetallic ring components by friction stir assisted simultaneous forging and solid-state joining

Here, a bimetallic ring component is forged by a friction stir assisted forging (FS-forging). A cylindrical bimetallic blank, magnesium AZ31 cylinder (Mg core) tightly fitted inside an aluminum 6061-T6 tube (Al skin), is used. In the FS-forging, the frictional heat and stirring of rotating tool forge the blank into a desired shape, while simultaneously generate a solid-state joint between the Mg core and the Al skin, without additional external heating, as confirmed by the microstructural analysis and mechanical tests. The microstructural analysis also shows that the characteristics of the solid-state joint can be different depending on the process parameters.

42 ENGINEERING↗

Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals was followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Status of Joining Thin Sheet and Thin Wall Tubes of 14YWT

Beginning this fiscal year, the FCRD research project initiated an investigation on joining thin sections of the advanced ODS 14YWT ferritic alloy. Friction stir welding (FSW) was investigated as a method to join thin plate and tubing of 14YWT since it is a solid state joining method that has been shown in past studies to be a promising method for joining plates of ODS alloys, such as 14YWT. However, this study will attempt to be the first to demonstrate if FSW can successfully join thin plates and thin wall tubing of 14YWT. In the first FSW attempt, a 1.06 cm thick plate of 14YWT (SM13 heat) was successfully rolled at 1000ºC to the target thickness of 0.1 cm with no edge cracking. This achievement is a highlight since previous attempts to roll 14YWT plates have resulted in extensive cracking. For the FSW run, a pin tool being developed by the ORNL FSW Process Development effort was used. The first FSW run successfully produced a bead-on-plate weld in the 0.1 cm thick plate. The quality of the weld zone appears very good with no evidence of large defects such as cavities. The microstructural characterization study of the bead-on-plate weld zone has been initiated to compare the results of the microstructure analysis with those obtained in the reference microstructural analysis of the 14YWT (SM13 heat) that showed ultra-fine grain size of 0.43 μm and a high number density of ~2-5 nm sizes oxygen-enriched nanoclusters.

42 ENGINEERING↗

Proton irradiation damage of an annealed Alloy 718 beam window

Mechanical testing and microstructural analysis was performed on an Alloy 718 window that was in use at the Los Alamos Neutron Science Center (LANSCE) Isotope Production Facility (IPF) for approximately 5 years. It was replaced as part of the IPF preventive maintenance program. The window was transported to the Wing 9 hot cells at the Chemical and Metallurgical Research (CMR) LANL facility, visually inspected and 3-mm diameter samples were trepanned from the window for mechanical testing and microstructural analysis. Shear punch testing and optical metallography was performed at the CMR hot cells. The 1-mm diameter shear punch disks were cut into smaller samples to further reduce radiation exposure dose rate using Focus Ion Beam (FIB) and microstructure changes were analyzed using a Transmission Electron Microscopy (TEM). Irradiation doses were determined to be ~0.2–0.7 dpa (edge) to 11.3 dpa (peak of beam intensity) using autoradiography and MCNPX calculations. The corresponding irradiation temperatures were calculated to be ~34–120 °C with short excursion to be ~47–220 °C using ANSYS. Mechanical properties and microstructure analysis results with respect to calculated dpa and temperatures show that significant work hardening occurs but useful ductility still remains. The hardening in the lowest dose region (~0.2–0.7 dpa) was the highest and attributed to the formation of γ" precipitates and irradiation defect clusters/bubbles whereas the hardening in the highest dose region (~11.3 dpa) was lower and attributed mainly to irradiation defect clusters and some thermal annealing.

36 MATERIALS SCIENCE↗

Thermal Simulation Analysis of Microstructure and Hardness for CrMoV with PWHT in Type IV Region

Welded components of CrMoV steam pipe exhibit a pernicious form of type IV cracking after long-term service at elevated temperature. To investigate the cracking mechanism, the type IV microstructure and hardness were characterized after thermal simulation of post-weld heat treatment. Below 1098 K (825 °C), loss of carbon from the pearlite region was apparent, and the work zone exhibited a slightly lower hardness than the parent material because of a minor amount of austenite transformation. In addition, for peak temperatures above 1133 K (860 °C), additional transformation into austenite occurred and was followed by retransformation into ferrite upon further increasing the temperature. The pearlite formed at 1173 K to 1223 K (900 °C to 950 °C) resulted in an increase of the volume fraction of pearlite and microstructural refinement, which yielded a remarkable increase of hardness in the work zone. For the peak temperature of 1573 K (1300 °C), previous austenite grains were coarsened and alloy carbides were dissolved in the austenite, which significantly hardened the work zone.

36 MATERIALS SCIENCE↗

Revealing the microstructure of materials

The objectives are to demonstrate how the microstructure of materials may be revealed by abrasive polishing and chemical etching, and to illustrate how microstructural information is used to monitor manufacturing processes, provide in-depth inspection, and perform failure analysis. Microstructural analysis is the procedure used to reveal the internal microstructural details of a material or part by sectioning and polishing the cut surface so that it may be examined under a suitable microscope. A printed wiring board was selected as the test material because it contains both metals and nonmetals that have distinctive microstructures, and because this technique is used throughout the electronic industry as a key quality control tool. The three principle component materials in printed circuit boards are glass/epoxy laminates faced with copper foil; copper, deposited by both electroless and electrolytic plating; and tin/lead solder. Sample preparation, mounting, grinding, polishing, and examination and analysis are discussed.

Nelson, James A.↗

Mechanical Properties and Interfacial Bonding of Overmolded Polymer Composite Lattice Structures

This study investigates the mechanical properties and interfacial bonding of Polyamide 12 filled with Glass Fiber (PA12/GF) lattice structures overmolded with Nylon 66 (PA66) and Thermoplastic Polyurethane (TPU). The PA12/GF lattices, designed in Gyroid, Isotruss, and Octahedral geometries, were produced using the Selective Laser Sintering (SLS) technique. The thermal characteristics of both the lattice and overmolding materials were analyzed using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). The mechanical performance and interfacial bonding were evaluated through mechanical testing and microstructural analysis. The results indicate that overmolding improved flexural strength and impact resistance of the PA12/GF lattices. For instance, the plain PA12/GF Isotruss lattice exhibited a flexural strength of 15.5 MPa. By overmolding it with TPU the flexural strength increased by up to 137%, while PA66-overmolding resulted in an increase of 371%, achieving a flexural strength of 73 MPa. In terms of impact resistance, TPU-overmolding improved performance significantly, with an increase of 1800% (Gyroid) compared to the plain lattice. Microstructural analysis revealed good adhesion at the interface, especially when both the lattice and overmolding materials were thoroughly dried prior to the overmolding process to minimize interfacial porosity. This study highlights the potential of using overmolding to enhance lattice structures performance, offering lightweight and cost-efficient solutions for automotive applications.

Talabi, Isaac [ORNL] (ORCID:0000000340215594)↗

Microstructure of In-Core Molten Salt Corrosion Hastelloy N{sup R} and 316 Stainless Steel

Since 2011, many materials have been discussed for potential application in Fluoride salt-cooled High-temperature nuclear Reactors (FHRs), which are emerging as leading reactor concept for the next generation of nuclear reactors thanks to the benefits of a high degree of passive safety, high thermal efficiency, and low spent fuel volume. Among these discussed materials, Hastelloy N{sup R} and 316L stainless steel have been selected as the most likely candidate alloys for FHRs. To provide direct experience in integrating a real system using molten FLiBe salt for reactor operation, these two candidate alloys were experimentally tested in Li-7 enriched Li{sub 2}BeF{sub 4} (FLiBe) molten salt in the core of MIT Research Reactor (MITR) at 700 deg. C for 1000 hours. After in-core corrosion testing, some basic post-irradiation examinations (PIE) including weight change per unit area and surface profile as well as surface morphology were conducted in the MIT Nuclear Reactor Laboratory (NRL) and compared with out-of-reactor corrosion samples. The deep understanding of these alloys in high-temperature molten salt with strong neutron irradiation requires further microstructural analysis such as electron microscopy and energy dispersive spectroscopy on the surface and cross-section of the in-core corrosion tested samples. The challenge in the microstructural analysis is due to the high radioactivity from the gamma emitting isotopes formed in alloys during neutron irradiation. Additionally, the facilities that are authorized for radioactive materials are very limited on campus. In this study, the microstructure of the in-core corrosion tested Hastelloy N{sup R} and 316L stainless steel specimen was analyzed by using the facilities at the Center for Advanced Energy Studies (CAES) at Idaho National Laboratory (INL) through the Nuclear Science User Facilities (NSUF) Rapid Turnaround Experiment (RTE) program.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Inelastic Deformation of Metal Matrix Composites: Plasticity and Damage Mechanisms - Part 1

The deformation mechanisms of a Ti 15-3/SCS6 (SiC fiber) metal matrix composite (MMC) were investigated using a combination of mechanical measurements and microstructural analysis. The objectives were to evaluate the contributions of plasticity and damage to the overall inelastic response, and to confirm the mechanisms by rigorous microstructural evaluations. The results of room temperature experiments performed on 0 degree and 90 degree systems primarily are reported in this report. Results of experiments performed on other laminate systems and at high temperatures will be provided in a forthcoming report. Inelastic deformation of the 0 degree MMC (fibers parallel to load direction) was dominated by the plasticity of the matrix. In contrast, inelastic deformations of the 90 degree composite (fibers perpendicular to loading direction) occurred by both damage and plasticity. The predictions of a continuum elastic plastic model were compared with experimental data. The model was adequate for predicting the 0 degree response; however, it was inadequate for predicting the 90 degree response largely because it neglected damage. The importance of validating constitutive models using a combination of mechanical measurements and microstructural analysis is pointed out. The deformation mechanisms, and the likely sequence of events associated with the inelastic deformation of MMCs, are indicated in this paper.

Majumdar, B. S.↗

Mechanistic Analysis of Microstructural Attributes to Lithium Plating in Fast Charging

Metallic lithium deposition on graphite anodes is a critical degradation mode in lithium-ion batteries, which limits safety and fast charge capability. A conclusive strategy to mitigate lithium deposition under fast charging yet remains elusive. Herein, we examine the role of electrode microstructure in mitigating lithium plating behavior under various operating conditions, including fast charging. The multilength scale characteristics of the electrode microstructure lead to a complex interaction of transport and kinetic limitations that significantly governs the cell performance and the occurrence of Li plating. We demonstrate, based on a comprehensive mesoscale analysis, that the performance and degradation can be significantly modulated via systematic design improvements at the hierarchy of length scales. It is found that the improvement in kinetic and transport characteristics achievable at disparate scales can dramatically affect Li plating propensity.

25 ENERGY STORAGE↗

Thermomechanical analysis and microstructural characterization of high performance concretes

Ultra-high performance concrete (UHPC) is a family of emerging materials for buildings and constructions. Behaviors of UHPCs at high temperatures are very important to their reliability and safety. In the current study, two UHPC materials were studied using the thermomechanical analysis (TMA) technique between room temperature and 800oC. Both reversible and irreversible phase transformations were observed from the TMA results, which were likely due to the - quartz transformation, and the decarburization and the dehydroxylation transitions, respectively. Thermal expansion coefficients exhibited significant variations in different temperature regimes. Postmortem SEM examinations revealed extensive cracking in the heated samples. In addition, micro-porosities were observed in the C-S-H phase as a result of phase changes during heating.

Ren, Fei↗

Geometry and size dependent microstructure and crack formation in Rene 41 superalloy fabricated by laser powder bed fusion

This study provides a systematic investigation into the size and geometry-dependent microstructural evolution and cracking susceptibility of LPBF-fabricated Rene 41. By coupling experimental microstructural analysis with thermal modeling, this research uniquely identifies the relationship between geometry-specific thermal histories, carbide coarsening, and liquation cracking. Four different geometries with varying thickness were fabricated with the identical process parameters. It was found that the grain size and morphology are not affected by the part size. However, the thinner parts exhibited coarser sub-grain structures compared to the thicker ones. The crack formation was observed for the parts with cross-sections smaller than 1 mm, whereas thicker parts had high density without any defects. Further, the cracks were observed in the interdendritic regions, suggesting that liquation cracking was the active micro-crack formation mechanism. The detailed microstructural analysis combined with a thermal finite element analysis proved that the heat extraction efficiency was lower for thinner parts causing a lower cooling rate and coarser carbides, making them more susceptible to constitutional liquation. Microhardness measurements were conducted for each geometry and correlated with the observed microstructural variations. The findings highlight the critical need for geometry-specific optimization of LPBF process parameters to mitigate cracking and achieve microstructural uniformity, offering valuable insights into the fabrication of complex, high-performance aerospace components.

36 MATERIALS SCIENCE↗

A laboratory nanoseismological study on deep-focus earthquake micromechanics

Global earthquake occurring rate displays an exponential decay down to ~300 km and then peaks around 550 to 600 km before terminating abruptly near 700 km. How fractures initiate, nucleate, and propagate at these depths remains one of the greatest puzzles in earth science, as increasing pressure inhibits fracture propagation. We report nanoseismological analysis on high-resolution acoustic emission (AE) records obtained during ruptures triggered by partial transformation from olivine to spinel in Mg 2 GeO 4 , an analog to the dominant mineral (Mg,Fe) 2 SiO 4 olivine in the upper mantle, using state-of-the-art seismological techniques, in the laboratory. AEs’ focal mechanisms, as well as their distribution in both space and time during deformation, are carefully analyzed. Microstructure analysis shows that AEs are produced by the dynamic propagation of shear bands consisting of nanograined spinel. These nanoshear bands have a near constant thickness (~100 nm) but varying lengths and self-organize during deformation. This precursory seismic process leads to ultimate macroscopic failure of the samples. Several source parameters of AE events were extracted from the recorded waveforms, allowing close tracking of event initiation, clustering, and propagation throughout the deformation/transformation process. AEs follow the Gutenberg-Richter statistics with a well-defined b value of 1.5 over three orders of moment magnitudes, suggesting that laboratory failure processes are self-affine. The seismic relation between magnitude and rupture area correctly predicts AE magnitude at millimeter scales. A rupture propagation model based on strain localization theory is proposed. Future numerical analyses may help resolve scaling issues between laboratory AE events and deep-focus earthquakes.

58 GEOSCIENCES↗

Interface-Driven Plasticity: The Presence of an Interface Affected Zone in Metallic Lamellar Composites: The Presence of an Interface Affected Zone…

Large strain deformation is used to make fine nanolayered two-phase composites from stacks of conventional polycrystalline sheets. The final materials made by this technique possess a crystallographically highly oriented structure containing nearly atomically perfect interfaces prevailing ubiquitously throughout the material. How this ordered structure evolves with strain from the coarser, more disordered state is not known. Here, using microstructural analysis and computational modeling, we discover a local interface-affected zone (IAZ) possessing the same crystallographically sharp structure in coarse layered composites as the final nanolayered composites. This means that this strongly oriented interface “zone” survives the mechanical work and overtakes the structure as it refines to the nanoscale. In essence, through the formation of this interface zone, the crossover to a highly oriented nanostructure occurs. Using microstructural analysis and crystal plasticity simulations, we show that the IAZ is a consequence of slip accommodation at the interface. This insight is valuable for developing processing strategies for superior interface-dominated materials.

36 MATERIALS SCIENCE↗

Comparative analysis of microstructure and reactive sites for nuclear graphite IG-110 and graphite matrix A3

Nuclear graphite and graphite matrix are both high-purity, fine-grain, graphitized materials designed for use in Fluoride-Salt Cooled High Temperature Reactors (FHRs), High Temperature Gas Cooled Reactors (HTGRs), and Molten Salt Reactors (MSRs). Their ability to chemisorb radioisotopes (such as tritium) and their chemical stability is dependent upon the density of reactive carbon sites (RCS), which varies among grades of graphite and changes with neutron irradiation. While nuclear graphites have been extensively characterized, much less data is available for graphite matrix. The current study performs a comparative analysis of IG-110 nuclear graphite and A3 graphite matrix, by X-ray Diffraction (XRD), Raman, and H 2 uptake at 700 °C with H 2 partial pressure range of 300 Pa and 22 kPa. At 10 kPa, the RCS occupied by H 2 uptake per number of carbon atoms at the edge of a crystallite, H/C edge , is 600(300) appm for IG-110 and 2300(200) appm for A3. Prior empirical studies for nuclear graphite establish a linear relationship between H/C and C edge /C and degree of graphitization. The present study shows that these correlations no longer hold when extrapolating to graphite matrix; the type of defects and the defect density at the crystallite surface are different between IG-110 and A3 due to differences in raw materials and manufacturing method.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗