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At least 451 records · Page 25

Mechanical Performance of Additively Manufactured ODS 316L and 316H Stainless Steels

This work package within the Advanced Materials and Manufacturing Technologies (AMMT) program focused on the mechanical and microstructural characterization of oxide dispersion strengthened (ODS) stainless steels produced using advanced manufacturing techniques. The research aimed to identify an accelerated development path for ODS alloys by integrating additive manufacturing (AM) technologies with recent advancements in ODS materials and traditional manufacturing methods. For FY 24, the research specifically targeted exploring an accelerated development path for ODS alloys by combining AM technologies with these advancements. Novel AM and post-build processing routes were developed for ODS austenitic alloys, including Fe-Cr-Ni alloys such as 316L and 316H. Electron microscopy and mechanical characterizations were conducted to evaluate the impact of process variables on microstructure and properties, with the goal of optimizing these properties economically. Traditionally, producing ODS alloys involves multi-day, high-energy mechanical milling of alloy powder with yttria powder, followed by milled-powder consolidation through extrusion or other methods, and additional thermomechanical processing (TMP) for property control. To overcome the challenges associated with this complex and costly approach, we propose exploring alternative, cost-effective processing routes that emphasize AM and traditional TMP methods. The new processing routes for ODS alloys have achieved significantly higher strengths—several times greater than those of wrought stainless steels—while maintaining substantial ductility and fracture toughness. This report outlines the novel and economical AM-based processing routes for ODS austenitic alloys, combined with post-build TMPs, and discusses the mechanical and microstructural characteristics of the developed materials.

36 MATERIALS SCIENCE↗

Out-of-plane properties

This paper summarizes three areas of research which were performed to characterize out-of-plane properties of composite materials. In the first investigation, a series of tests was run to characterize the through-the-thickness tensile strength for a variety of composites that included 2D braids, 2D and 3D weaves, and prepreg tapes. A new test method based on a curved beam was evaluated. Failures were significantly different between the 2D materials and the 3D weaves. The 2D materials delaminated between layers due to out-of-plane tensile stresses while the 3D weaves failed due to the formation of radial cracks between the surface plies caused by high circumferential stresses along the inner radius. The strength of the 2D textile composites did not increase relative to the tapes. Final failure in the 3D weaves was caused by a circumferential crack similar to the 2D materials and occurred at a lower bending moment than in other materials. The early failures in the 3D weaves were caused by radial crack formation rather than a low through-the-thickness strength. The second investigation focused on the development of a standard impact test method to measure impact damage resistance. The only impact tests that currently exist are compression after impact (CAI) tests which incorporate elements of both damage resistance and damage tolerance. A new impact test method is under development which uses a quasi-static indentation (QSI) test to directly measure damage resistance. Damage resistance is quantified in terms of the contact force to produce a unit of damage where a metric for damage may be area in C-scan, depth of residual dent , penetration, damage growth, etc. A final draft of an impact standard that uses a QSI test method will be presented to the ASTM Impact Task Group on impact. In the third investigation, the impact damage resistance behavior of a variety of textile materials was studied using the QSI test method. In this study, the force where large damage initiates was measured and the delamination size as a function of force was determined. The force to initiate large damage was significantly lower in braids and weaves. The delamination diameter - impact forace relationship was quanitfied using a damage resistance parameter, Q(*), which related delamination diameter to imapct force over a range of delamination sizes. Using this Q(*) parameter to rate the materials, the stitched uniweaves, toughened epoxy tapes, and through-the-thickness orthogonal interlock weave were the most damage resistant.

Jackson, Wade C.↗

EBIC spectroscopy - A new approach to microscale characterization of deep levels in semi-insulating GaAs

The microscale characterization of electronic defects in (SI) GaAs has been a challenging issue in connection with materials problems encountered in GaAs IC technology. The main obstacle which limits the applicability of high resolution electron beam methods such as Electron Beam-Induced Current (EBIC) and cathodoluminescence (CL) is the low concentration of free carriers in semiinsulating (SI) GaAs. The present paper provides a new photo-EBIC characterization approach which combines the spectroscopic advantages of optical methods with the high spatial resolution and scanning capability of EBIC. A scanning electron microscope modified for electronic characterization studies is shown schematically. The instrument can operate in the standard SEM mode, in the EBIC modes (including photo-EBIC and thermally stimulated EBIC /TS-EBIC/), and in the cathodo-luminescence (CL) and scanning modes. Attention is given to the use of CL, Photo-EBIC, and TS-EBIC techniques.

Li, C.-J.↗

Spatially Resolved Raman Spectroscopy of Thin Carbon Interphase in SiC Ceramic Matrix Composites

A dedicated analysis method is presented to extract the Raman spectrum of an interphase layer thinner than the laser spot size. We focused on spatial correlations between the contrast of optical micrographs and Raman hyperspectral data to predict the constituents of the mixed spectra measured near the interphase. By employing a mapping step size of 0.1 μm, the Raman spectrum of approximately 0.3-μm-thick carbon interphase in a SiC fiber-reinforced SiC matrix composite was extracted from data acquired with a theoretical spot size of about 0.7 μm. Notably, conventional chemometrics procedures were unable to isolate the interphase signal, instead producing a spectrum representing a mixture of interphase and matrix. This study used another composite with approximately 0.9-μm-thick interphase to validate the analysis method, enabling direct measurement of the interphase spectrum. The proposed Raman analysis method has advantages in specimen volume and turnaround time compared to traditional characterization methods, such as transmission electron microscopy. In conclusion, this study also evaluates the applicability of the analysis method to different composite materials and identifies key requirements of the measurements, including the ratio of interphase thickness to spot size and the homogeneity of the surrounding matrix.

ceramic matrix composite↗

Advancements in NbTiN based circuits for Superconducting Digital Logic

Superconducting (SC) electronics have emerged as a promising platform for high-speed, energy-efficient computing and quantum information processing. This work, centered on NbTiN, presents recent advances in material science and fabrication methods leading to significant improvements in performance, scalability and vertical integration. We specifically report on fabrication and characterization of key components, including Josephson junctions (JJs), flux trapping structures and SC interconnects. Together, these efforts represent critical steps towards realizing practical, complex, dense and large-scale SC integrated circuits.

Pokhrel, A. [Imec,Heverlee,Belgium]↗

Impact of Annealing on the Chemical and Superconducting Properties of Ta Thin Films

Tantalum thin films are annealed to dissolve the surface oxide. The effect of annealing is studied using material characterization tools, XPS and TOF-SIMS, and electrical transport measurements of the annealed films are taken using standard PPMS methods to correlate with the surface chemistry. Annealing dissociates the surface oxide, and the oxygen produced diffuses into the thin film. The introduction of oxygen reduces the quality of the thin film, as shown by the suppression of Tc and a reduction in RRR.

Shinde, Maithilee [IIT, Chicago]↗

High purity silica reflective heat shield development

A hyperpure vitreous silica material is being developed for use as a reflective and ablative heat shield for planetary entry. Various purity grades and forms of raw materials were evaluated along with various processing methods. Slip casting of high purity grain was selected as the best processing method, resulting in a highly reflective material in the wavelength bands of interest (the visible and ultraviolet regions). The selected material was characterized with respect to optical, mechanical and physical properties using a limited number of specimens. The process has been scaled up to produce a one-half scale heat shield (18 in. dia.) (45.72 cm) for a Jupiter entry vehicle. This work is now being extended to improve the structural safety factor of the heat shield by making hyperpure silica material tougher through the addition of silica fibers.

Nachtscheim, P. R.↗

Research in nonlinear structural and solid mechanics

Nonlinear analysis of building structures and numerical solution of nonlinear algebraic equations and Newton's method are discussed. Other topics include: nonlinear interaction problems; solution procedures for nonlinear problems; crash dynamics and advanced nonlinear applications; material characterization, contact problems, and inelastic response; and formulation aspects and special software for nonlinear analysis.

Mccomb, H. G., Jr.↗

Lamb wave characterization of the effects of long-term thermal-mechanical aging on composite stiffness

Lamb waves offer a promising method of evaluating damage in composite materials. The Lamb wave velocity is directly related to the material parameters, so an effective tool exists to monitor damage in composites by measuring the velocity of these waves. The Lamb Wave Imager (LWI) uses a pulse/receive technique that excites an antisymmetric Lamb mode and measures the time-of-flight over a wide frequency range. Given the material density and plate thickness, the bending and out-of-plane shear stiffnesses are calculated from a reconstruction of the dispersion curve. In this study, the time-of-flight as well as the elastic stiffnesses D11, D22, A44, and A55 for composite samples which have undergone combined thermal and mechanical aging are obtained. The samples examined include a baseline specimen with 0 cycles, specimens which have been aged 2350 and 3530 cycles at high strain levels, and one specimen aged 3530 cycles at low strain levels.

Aircraft↗

PETI-298 Prepared by Microwave Synthesis: Neat Resin and Composite Properties

PETI-298 is a high temperature/high performance matrix resin that is processable into composites by resin transfer molding (RTM), resin infusion and vacuum assisted RTM techniques. It is typically synthesized in a polar aprotic solvent from the reaction of an aromatic anhydride and a combination of diamines and endcapped with phenylethynylphthalic anhydride. Microwave synthesis of PETI-298 was investigated as a means to eliminate solvent and decrease reaction time. The monomers were manually mixed and placed in a microwave oven for various times to determine optimum reaction conditions. The synthetic process was subsequently scaled-up to 330g. Three batches were synthesized and combined to give 1 kg of material that was characterized for thermal and rheological properties and compared to PETI-298 prepared by the classic solution based synthetic method. The microwave synthesized PETI-298 was subsequently used to fabricate flat laminates on T650 carbon fabric by RTM. The composite panels were analyzed and mechanical properties determined and compared with those fabricated from PETI-298 prepared by the classic solution method. The microwave synthesis process and characterization of neat resin and carbon fiber reinforced composites fabricated by RTM will be presented. KEY WORDS: Resin Transfer Molding, High Temperature Polymers, Phenylethynyl Terminated Imides, Microwave Synthesis

Smith, Joseph G.↗

Location-Specific Microstructure Characterization Within AM Bench 2022 Nickel Alloy 718 3D Builds

Abstract The Additive Manufacturing Benchmark Test Series (AM Bench) is a broad effort to produce rigorous measurement datasets for validating AM computer simulations across the range of processing, structure, and properties, for many additive manufacturing (AM) build methods and material classes. Here, the microstructures of nickel alloy 718 AM Bench 2022 test artifacts produced using laser-based powder bed fusion (PBF-LB), in both as-built and fully heat-treated conditions, are examined. Cross sections are primarily characterized using large area scanning electron microscopy (SEM) electron backscatter diffraction (EBSD) and example analyses of the crystallographic textures are described. These data are part of a large set of in situ and ex situ measurements from both three-dimensional builds and laser tracks on bare plates. All the measurement data are available online with download links at www.nist.gov/ambench .

Levine, L. E. (ORCID:0000000334484229)↗

A study of degradation of plates for nickel-cadmium spacecraft cells

The relative merits of coining and not coining of sintered nickel oxide and cadmium plates was investigated. Sample plate materials from most commercial cell suppliers were obtained and characterized for properties that may correlate with the tendency toward physical disintegration during handling and over long periods of time in the cell. Special test methods were developed to obtain comparative data in a short time. A wide range of physical properties and coining thickness was observed, resulting in a range of responses. The stronger materials resisted loss of sinter better than weaker materials whether or not coined. Coining improved handling and resistance to electrochemical cycling of weaker materials. The mechanism of break-down of positive plate edges under cycling appears to be the same as that of thickening and blistering. Brittle, nonadherent sinter, resulting from certain impregnation processes, is the most vulnerable to degradation. It is concluded that the latter type of materials should be coined, but coining of strong materials is optional.

Scott, W. R.↗

Spinel high-entropy oxides (FeNiCrMnZnX) 3 O 4 (X = Al, mg) as anode materials for high-performance lithium-ion batteries

To address the high cost, cobalt dependency, and resource constraints typical of conventional high-entropy oxide (HEO) anodes, this study reports the successful synthesis of two Co-free, six-component spinel-type HEOs(FeNiCrMnZnAl) 3 O 4 (HEO-Al) and (FeNiCrMnZnMg) 3 O 4 (HEO-Mg), via a sol-gel method. The distinct effects of Al 3+ and Mg 2+ incorporation on the electrochemical performance and lithium storage kinetics were systematically investigated. XRD, Raman, and TEM characterizations confirm that both materials possess a pure spinel phase, uniform particle size, and homogeneous elemental distribution. Notably, electrochemical evaluations reveal that HEO-Al delivers a superior reversible capacity of 480.7 mAh g −1 after 100 cycles at 0.1 A g −1 , and maintains 354.5 mAh g −1 after 1000 long-term cycles at 1 A g −1 , significantly outperforming HEO-Mg. Kinetic analysis indicates that HEO-Al exhibits lower charge transfer resistance, a higher Li + diffusion coefficient, and a pseudocapacitive contribution of up to 82%. Furthermore, these findings demonstrate that Al substitution effectively optimizes the structural stability and lithium storage kinetics of Co-free HEOs, providing a viable strategy for designing low-cost, highly stable HEO anode systems.

Anode materials↗

A study of degradation of plates for nickel-cadmium spacecraft cells

The relative merits of coining and not coining of sintered nickel-oxide and cadmium plates was investigated. A survey of the industry including cell manufactures and users was made and results summarized. Sample plate materials from most commercial cell suppliers were obtained and characterized for properties that may correlate with the tendency toward physical disintegration during handling and over long periods of time in the cell. Special test methods were developed to obtain comparative data in a short time. A wide range of physical properties and coining thicknesses was observed, resulting in a range of responses. The stronger, less brittle materials resisted loss of sinter better than weaker materials whether or not coined. Coining improved handling and resistance to electrochemical cycling in all materials tested. An apparent exception was found to be due to improper coining of a tapered edge.

Scott, W. R.↗

The mechanics of delamination in fiber-reinforced composite materials. Part 2: Delamination behavior and fracture mechanics parameters

Based on theories of laminate anisotropic elasticity and interlaminar fracture, the complete solution structure associated with a composite delamination is determined. Fracture mechanics parameters characterizing the interlaminar crack behavior are defined from asymptotic stress solutions for delaminations with different crack-tip deformation configurations. A numerical method employing singular finite elements is developed to study delaminations in fiber composites with any arbitrary combinations of lamination, material, geometric, and crack variables. The special finite elements include the exact delamination stress singularity in its formulation. The method is shown to be computationally accurate and efficient, and operationally simple. To illustrate the basic nature of composite delamination, solutions are shown for edge-delaminated (0/-0/-0/0) and (+ or - 0/+ or - 0/90/90 deg) graphite-epoxy systems under uniform axial extenstion. Three-dimensional crack-tip stress intensity factors, associated energy release rates, and delamination crack-closure are determined for each individual case. The basic mechanics and mechanisms of composite delamination are studied, and fundamental characteristics unique to recently proposed tests for interlaminar fracture toughness of fiber composite laminates are examined.

Wang, S. S.↗

The mechanics of delamination in fiber-reinforced composite materials. II - The delamination behavior and fracture mechanics parameters

Based on theories of laminate anisotropic elasticity and interlaminar fracture, the complete solution structure associated with a composite delamination is determined. Fracture mechanics parameters characterizing the interlaminar crack behavior are defined from asymptotic stress solutions for delaminations with different crack-tip deformation configurations. A numerical method employing singular finite elements is developed to study delaminations in fiber composites with any arbitrary combinations of lamination, material, geometric, and crack variables. The special finite elements include the exact delamination stress singularity in its formulation. The method is shown to be computationally accurate and efficient, and operationally simple. To illustrate the basic nature of composite delamination, solutions are shown for edge-delaminated (0/-0/-0/0) and (+ or - 0/+ or - 0/90/90 deg) graphite-epoxy systems under uniform axial extension. Three-dimensional crack-tip stress intensity factors, associated energy release rates, and delamination crack-closure are determined for each individual case. The basic mechanics and mechanisms of composite delamination are studied, and fundamental characteristics unique to recently proposed tests for interlaminar fracture toughness of fiber composite laminates are examined. Previously announced in STAR as N84-13222

Wang, S. S.↗

Mode I Cohesive Law Characterization of Through-Crack Propagation in a Multidirectional Laminate

A method is proposed and assessed for the experimental characterization of through-the-thickness crack propagation in multidirectional composite laminates with a cohesive law. The fracture toughness and crack opening displacement are measured and used to determine a cohesive law. Two methods of computing fracture toughness are assessed and compared. While previously proposed cohesive characterizations based on the R-curve exhibit size effects, the proposed approach results in a cohesive law that is a material property. The compact tension specimen configuration is used to propagate damage while load and full-field displacements are recorded. These measurements are used to compute the fracture toughness and crack opening displacement from which the cohesive law is characterized. The experimental results show that a steady-state fracture toughness is not reached. However, the proposed method extrapolates to steady-state and is demonstrated capable of predicting the structural behavior of geometrically-scaled specimens.

Bergan, Andrew C.↗