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NASA NTRS1988

High temperature tensile testing of ceramic composites

The various components of a high temperature tensile testing system are evaluated. The objective is the high temperature tensile testing of SiC fiber reinforced reaction bonded Si3N4 specimens at test temperatures up to 1650 C (3000 F). Testing is to be conducted in inert gases and air. Gripping fixtures, specimen configurations, furnaces, optical strain measuring systems, and temperature measurement techniques are reviewed. Advantages and disadvantages of the various techniques are also noted.

Gyekenyesi, John Z.↗

NASA NTRS1995

Advanced High-Temperature Engine Materials Technology Progresses

The objective of the Advanced High Temperature Engine Materials Technology Program (HITEMP) is to generate technology for advanced materials and structural analysis that will increase fuel economy, improve reliability, extend life, and reduce operating costs for 21st century civil propulsion systems. The primary focus is on fan and compressor materials (polymer-matrix composites--PMC's), compressor and turbine materials (superalloys, and metal-matrix and intermetallic-matrix composites--MMC's and IMC's) and turbine materials (ceramic-matrix composites--CMC's). These advanced materials are being developed by in-house researchers and on grants and contracts. NASA considers this program to be a focused materials and structures research effort that builds on our base research programs and supports component-development projects. HITEMP is coordinated with the Advanced Subsonic Technology (AST) Program and the Department of Defense/NASA Integrated High-Performance Turbine Engine Technology (IHPTET) Program. Advanced materials and structures technologies from HITEMP may be used in these future applications. Recent technical accomplishments have not only improved the state-of-the-art but have wideranging applications to industry. A high-temperature thin-film strain gage was developed to measure both dynamic and static strain up to 1100 C (2000 F). The gage's unique feature is that it is minimally intrusive. This technology, which received a 1995 R&D 100 Award, has been transferred to AlliedSignal Engines, General Electric Company, and Ford Motor Company. Analytical models developed at the NASA Lewis Research Center were used to study Textron Specialty Materials' manufacturing process for titanium-matrix composite rings. Implementation of our recommendations on tooling and processing conditions resulted in the production of defect free rings. In the Lincoln Composites/AlliedSignal/Lewis cooperative program, a composite compressor case is being manufactured with a Lewis-developed matrix, VCAP. The compressor case, which will reduce weight by 30 percent and costs by 50 percent, is scheduled to be engine tested in the near future.

Source record↗

NASA NTRS2015

On the Recovery Stress of a Ni50.3Ti29.7Hf20 High Temperature Shape Memory Alloy

Recovery stress in shape memory alloys (SMAs), also known as blocking stress, is an important property generally obtained during heating under a dimensional constraint as the material undergoes the martensitic phase transformation. This property has been instinctively utilized in most SMA shape-setting procedures, and has been used in numerous applications such as fastening and joining, rock splitting, safety release mechanisms, reinforced composites, medical devices, and many other applications. The stress generation is also relevant to actuator applications where jamming loads (e.g., in case the actuator gets stuck and is impeded from moving) need to be determined for proper hardware sizing. Recovery stresses in many SMA systems have been shown to reach stresses in the order of 800 MPa, achieved via thermo-mechanical training such as pre-straining, heat treatments or other factors. With the advent of high strength, high temperature SMAs, recovery stress data has been rarely probed, and there is no information pertinent to the magnitudes of these stresses. Thus, the purpose of this work is to investigate the recovery stress capability of a precipitation strengthened, Ni50.3Ti29.7Hf20 (at.) high temperature SMA in uniaxial tension and compression. This material has been shown to exhibit outstanding strength and stability during constant-stress, thermal cycling, but no data exists on constant-strain thermal cycling. Several training routines were implemented as part of this work including isothermal pre-straining, isobaric thermal cycling, and isothermal cyclic training routines. Regardless of the training method used, the recovery stress was characterized using constant-strain (strain-controlled condition) thermal cycling between the upper and lower cycle temperatures. Preliminary results indicate recovery stresses in excess of 1.5 GPa were obtained after a specific training routine. This stress magnitude is significantly higher than conventional NiTi stress generation capability.

Recovery Stress↗

NASA NTRS1986

The role of fiber and matrix in crash energy absorption of composite materials

Static crushing tests were conducted on tube specimens fabricated from graphite/epoxy, Kevlar/epoxy and hybrid combinations of graphite-Kevlar/epoxy to examine the influence the fiber and matrix constitutive properties and laminate architecture have on energy absorption. Fiber and matrix ultimate failure strain were determined to significantly effect energy absorption. The energy absorption capability of high ultimate failure strain materials (AS-6/F185 and AS-6/HST-7) was less than materials having lower ultimate failure strain. Lamina stacking sequence had up to a 300 percent change in energy absorption for the materials tested. Hybridizing with graphite and Kevlar reinforcements resulted in materials with high energy absorption capabilities that have postcrushing integrity.

Farley, G. L.↗

DOE OSTI2020

Mechanical and self-healing behavior of low carbon engineered cementitious composites reinforced with PP-fibers

While the ultrahigh tensile ductility and superior durability of Engineered Cementitious Composites (ECC) have been demonstrated, the relatively high energy and carbon intensity, as well as high material cost present potential impediments to broader ECC applications. The objective of this research is to develop a more sustainable and cost-effective ECC. The ordinary Portland cement (OPC) and the commonly used PVA fiber in conventional ECC were replaced by limestone calcined clay cement (LC3) and polypropylene (PP) fiber, respectively. The ECC compressive strength, tensile stress-strain relationship, and microcrack self-healing behavior were studied at three water to binder ratios (0.3, 0.2, 0.16). The novel LC3-PP-ECC showed a tensile strain capacity of greater than 6% and an intrinsically tight crack width below 82 μm when loaded to 1% tensile strain. Further, the LC3-PP-ECC demonstrated efficient recovery of the composite tensile ductility and ultimate tensile strength through self-healing. Compared to typical ECC made with OPC and PVA fiber, the material cost, embodied energy and carbon footprint of LC3-PP-ECC are reduced by 61%, 45%, and 48%, respectively. Here, the superior mechanical properties and durability combined with the low environmental impact and cost for material production promote LC3-PP-ECC as a sustainable material for structural and non-structural applications.

42 ENGINEERING↗

DOE OSTI2024

Watching a signaling protein function: What has been learned over four decades of time-resolved studies of photoactive yellow protein

Photoactive yellow protein (PYP) is a signaling protein whose internal p-coumaric acid chromophore undergoes reversible, light-induced trans-to-cis isomerization, which triggers a sequence of structural changes that ultimately lead to a signaling state. Since its discovery nearly 40 years ago, PYP has attracted much interest and has become one of the most extensively studied proteins found in nature. The method of time-resolved crystallography, pioneered by Keith Moffat, has successfully characterized intermediates in the PYP photocycle at near atomic resolution over 12 decades of time down to the sub-picosecond time scale, allowing one to stitch together a movie and literally watch a protein as it functions. But how close to reality is this movie? To address this question, results from numerous complementary time-resolved techniques including x-ray crystallography, x-ray scattering, and spectroscopy are discussed. Emerging from spectroscopic studies is a general consensus that three time constants are required to model the excited state relaxation, with a highly strained ground-state cis intermediate formed in less than 2.4 ps. Persistent strain drives the sequence of structural transitions that ultimately produce the signaling state. Crystal packing forces produce a restoring force that slows somewhat the rates of interconversion between the intermediates. Moreover, the solvent composition surrounding PYP can influence the number and structures of intermediates as well as the rates at which they interconvert. When chloride is present, the PYP photocycle in a crystal closely tracks that in solution, which suggests the epic movie of the PYP photocycle is indeed based in reality.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Data-Driven Study of Shape Memory Behavior of Multi-component Ni-Ti Alloys

Ni-Ti based shape memory alloys (SMAs) have found wide-spread use in aerospace, automotive, biomedical, and commercial applications owing to their favorable properties and ease of operation. Especially important for many NASA applications is the ability to tune the martensitic transformation temperature of Ni-Ti alloys by varying the composition and processing conditions. Recently, researchers at NASA have compiled an extensive database of shape memory properties of materials, including over 8,000 multi-component Ni-Ti alloys containing 37 different alloying elements. Using this dataset, machine learning models are trained to predict transformation temperatures, hysteresis, and transformation strain with extremely small errors. These models are used to learn relationships between shape memory behavior and input parameters in the composition and processing space. ML predictions are validated through new experiments. The combination of an extensive dataset and accurate learning models, together, make our approach highly suitable for the rapid discovery of novel SMAs with targeted properties.

Shape Memory Alloys↗

NASA NTRS2018

Bistable Collapsible Tubular Mast Booms

A promising candidate for deployable composite structures is the two-shelled Collapsible Tubular Mast (CTM) boom, which is to be employed on future solar sail and interplanetary small satellite platforms by the National Aeronautics and Space Administration (NASA). This is due to its two omega-shaped shells forming a closed-section which yields large stiffnesses that allowed for high dimensional stability. An inextensional analytical model describing the bending deformation mechanics of CTM booms was used to determine how design variables induce bistability, or the existence of two strain energy wells. Bistable booms were favorable due to low strain energy requirements for the coiled state and had more controllable deployment when compared to monostable booms. The effects of varying lamina material, laminate layup, and shell arc geometries between different inner and outer shell segments on the second strain energy well and stiffness properties were determined for cross-sections formed by circular segments. The full design space for two-shelled composite CTM booms was explored to evaluate the validity of the simple analytical model developed. Optimal CTM boom designs were manufactured and experimentally characterized for comparisons against model results. The model under-predicted the second stable coiled diameter of the complete two-shelled booms by 27-33% and as low as 3-8% for the individual shells wrapped alone.

Fernandez, Juan M.↗

DOE OSTI2023

Three-dimensional atomic structure and local chemical order of medium- and high-entropy nanoalloys

Medium- and high-entropy alloys (M/HEAs) mix several principal elements with near-equiatomic composition and represent a model-shift strategy for designing previously unknown materials in metallurgy, catalysis and other fields. One of the core hypotheses of M/HEAs is lattice distortion, which has been investigated by different numerical and experimental techniques. However, determining the three-dimensional (3D) lattice distortion in M/HEAs remains a challenge. Moreover, the presumed random elemental mixing in M/HEAs has been questioned by X-ray and neutron studies, atomistic simulations, energy dispersive spectroscopy and electron diffraction, which suggest the existence of local chemical order in M/HEAs. However, direct experimental observation of the 3D local chemical order has been difficult because energy dispersive spectroscopy integrates the composition of atomic columns along the zone axes and diffuse electron reflections may originate from planar defects instead of local chemical order. Here, in this work, we determine the 3D atomic positions of M/HEA nanoparticles using atomic electron tomography and quantitatively characterize the local lattice distortion, strain tensor, twin boundaries, dislocation cores and chemical short-range order (CSRO). We find that the high-entropy alloys have larger local lattice distortion and more heterogeneous strain than the medium-entropy alloys and that strain is correlated to CSRO. We also observe CSRO-mediated twinning in the medium-entropy alloys, that is, twinning occurs in energetically unfavoured CSRO regions but not in energetically favoured CSRO ones, which represents, to our knowledge, the first experimental observation of correlating local chemical order with structural defects in any material. We expect that this work will not only expand our fundamental understanding of this important class of materials but also provide the foundation for tailoring M/HEA properties through engineering lattice distortion and local chemical order.

36 MATERIALS SCIENCE↗

NASA NTRS2002

High-Fidelity Generalization Method of Cells for Inelastic Periodic Multiphase Materials

An extension of a recently-developed linear thermoelastic theory for multiphase periodic materials is presented which admits inelastic behavior of the constituent phases. The extended theory is capable of accurately estimating both the effective inelastic response of a periodic multiphase composite and the local stress and strain fields in the individual phases. The model is presently limited to materials characterized by constituent phases that are continuous in one direction, but arbitrarily distributed within the repeating unit cell which characterizes the material's periodic microstructure. The model's analytical framework is based on the homogenization technique for periodic media, but the method of solution for the local displacement and stress fields borrows concepts previously employed by the authors in constructing the higher-order theory for functionally graded materials, in contrast with the standard finite-element solution method typically used in conjunction with the homogenization technique. The present approach produces a closed-form macroscopic constitutive equation for a periodic multiphase material valid for both uniaxial and multiaxial loading. The model's predictive accuracy in generating both the effective inelastic stress-strain response and the local stress said inelastic strain fields is demonstrated by comparison with the results of an analytical inelastic solution for the axisymmetric and axial shear response of a unidirectional composite based on the concentric cylinder model, and with finite-element results for transverse loading.

Aboudi, Jacob↗

DOE OSTI2020

Investigation of the discontinuous precipitation of U-Nb alloys via thermodynamic analysis and phase-field modeling

U-Nb’s discontinuous precipitation, $\gamma^{bcc}_{matrix}$, $\alpha^{orth}_{cellular}$, $\gamma\prime^{bcc}_{cellular}$, is intriguing in the sense that it allows formation and growth of the metastable $\gamma\prime$ phase during the course of its occurrence. Previous attempts to explain the thermodynamic origin of U-Nb’s discontinuous precipitation hypothesized that the energy of $\alpha$ forms an intermediate common tangent with the first potential of the double-well energy of $\gamma$ at the $\gamma\prime$ composition. In this work, we examine different possible mechanisms by which the discontinuous precipitation product in the U-Nb system can be stabilized. We put forward a mechanism by which the bulk free energy of the $\gamma$ can develop a non-monotonic dependency with composition. Additionally we posit that local contributions due to lattice mismatch between the $\alpha$ and $\gamma$ phases may be responsible for the generation of metastable states that may stabilized by thermodynamics as well as by kinetics. Our work suggests that local misfit strain tends to play a crucial role in the growth of the discontinuous precipitation product. Depending on the magnitude of strain developed at the $\alpha$/$\gamma\prime$ interfaces, either an increasing $\gamma\prime$ composition or a random distribution of $\gamma\prime$ compositions around the equiatomic value with respect to increasing temperature could be expected. Moreover, we show how it is possible to stabilize the discontinuous precipitation front through highly anisotropic and fast interface diffusion.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2024

Hydrogen production in microbial electrolysis cells with biocathodes

Electroautotrophic microbes at biocathodes in microbial electrolysis cells (MECs) can catalyze the hydrogen evolution reaction with low energy demand, facilitating long-term stable performance through specific and renewable biocatalysts. However, MECs have not yet reached commercialization due to a lack of understanding of the optimal microbial strains and reactor configurations for achieving high performance. Here, we critically analyze the criteria for the inocula selection, with a focus on the effect of hydrogenase activity and microbe–electrode interactions. We also evaluate the impact of the reactor design and key parameters, such as membrane type, composition, and electrode surface area on internal resistance, mass transport, and pH imbalances within MECs. Furthermore, this analysis paves the way for advancements that could propel biocathode-assisted MECs toward scalable hydrogen gas production.

Biotechnology & Applied Microbiology↗

NASA NTRS1990

Survivability characteristics of composite compression structure

Test and evaluation was performed to determine the compression residual capability of graphite reinforced composite panels following perforation by high-velocity fragments representative of combat threats. Assessments were made of the size of the ballistic damage, the effect of applied compression load at impact, damage growth during cyclic loading and residual static strength. Several fiber/matrix systems were investigated including high-strain fibers, tough epoxies, and APC-2 thermoplastic. Additionally, several laminate configurations were evaluated including hard and soft laminates and the incorporation of buffer strips and stitching for improved damage resistance of tolerance. Both panels (12 x 20-inches) and full scale box-beam components were tested to assure scalability of results. The evaluation generally showed small differences in the responses of the material systems tested. The soft laminate configurations with concentrated reinforcement exhibited the highest residual strength. Ballistic damage did not grow or increase in severity as a result of cyclic loading, and the effects of applied load at impact were not significant under the conditions tested.

Avery, John G.↗

DOE OSTI2023

Characterization of Annealing-Induced Phase Segregation in Composite Silicon Anodes for Li-ion Batteries

Silicon (Si) anodes present a promising alternative to graphite anodes for lithium-ion batteries (LIBs), as Si has a greater specific capacity. However, one major constraint is the volumetric change of Si during lithiation that results in an unstable solid-electrolyte interphase (SEI), so Si-containing electrodes require the use of various strategies to mitigate these effects and improve performance. One such solution is the use of Si nanoparticles (NPs) that maximize the surface area to volume ratio. Here, we discuss electrodes made with Si NPs treated with polyethylene oxide (PEO) (for improving dispersion during processing), conductive carbon NPs, and P84 polyimide binder which shows significant impacts of annealing treatment on improvements of active material utilization, first cycle efficiency, and capacity retention with extensive cycling . We used air-free argon ion polishing to create electrode cross sections and imaged through the electrode thickness using atomic force microscopy (AFM)-based nano-electrical characterization of scanning spreading resistance microscopy (SSRM), nano-mechanical characterizations of contact resonance and force volume (CR-FV), and scanning electron microscopy-based energy dispersive x-ray spectroscopy (SEM-EDS). Results show that the Si and conductive carbon segregate into phases with a distinctive carbon-rich banded morphology that surrounds the Si-rich phase during annealing. In pristine electrodes, the carbon- and SEI-rich bands exhibit a higher electronic conductivity and a lower elastic modulus than the Si active material phase. These structures, as well as distinct electronic and mechanical properties, remain during cycling, suggesting an improvement of electrical conduction pathways and a mechanical strain buffer for active Si material expansion during cycling. This phase separation may be a major factor in the improvement seen in electrochemical performance due to annealing. Additionally, our nm-scale and multi-mode characterizations provide a novel route for understanding and improving energy storage devices, which is advantageous due to the highly inhomogeneous of composite electrodes in nm-mm scales.

ENERGY STORAGE↗

NASA NTRS1979

High temperature dynamic modulus and damping of aluminum and titanium matrix composites

Dynamic modulus and damping capacity property data were measured from 20 to over 500 C for unidirectional B/Al (1100), B/Al (6061), B/SiC/Al (6061), Al2O3/Al, SiC/Ti-6Al-4V, and SiC/Ti composites. The measurements were made under vacuum by the forced vibration of composite bars at free-free flexural resonance near 2000 Hz and at strain application below 0.000001. The damping of B/Al composites was found at all temperatures to be significantly greater than the damping of the Al2O3/Al and SiC/Ti composites, with little variation observed in the dynamic moduli of specimens having almost the same fiber content. It is concluded that on the practical level, the finding of a damping-strength correlation supports the use of composite damping measurements for the nondestructive evaluation of boron fiber strength in as-fabricated and heat-treated B/Al (6061) composites.

Dicarlo, J. A.↗

DOE OSTI2021

Systematic discovery of pseudomonad genetic factors involved in sensitivity to tailocins

Tailocins are bactericidal protein complexes produced by a wide variety of bacteria that kill closely related strains and may play a role in microbial community structure. Thanks to their high specificity, tailocins have been proposed as precision antibacterial agents for therapeutic applications. Compared to tailed phages, with whom they share an evolutionary and morphological relationship, bacterially produced tailocins kill their host upon production but producing strains display resistance to self-intoxication. Though lipopolysaccharide (LPS) has been shown to act as a receptor for tailocins, the breadth of factors involved in tailocin sensitivity, and the mechanisms behind resistance to self-intoxication, remain unclear. Here, we employed genome-wide screens in four non-model pseudomonads to identify mutants with altered fitness in the presence of tailocins produced by closely related pseudomonads. Our mutant screens identified O-antigen composition and display as most important in defining sensitivity to our tailocins. In addition, the screens suggest LPS thinning as a mechanism by which resistant strains can become more sensitive to tailocins. Furthermore, we validate many of these novel findings, and extend these observations of tailocin sensitivity to 130 genome-sequenced pseudomonads. This work offers insights into tailocin–bacteria interactions, informing the potential use of tailocins in microbiome manipulation and antibacterial therapy.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

On the Use of Surfactant-Complexed Chitosan for Toughening 3D Printed Polymethacrylate Composites

This work reports a simple approach to prepare toughened 3D-printed polymethacrylate (PMA) composites using surfactant-modified chitosan (SMCS) particles at loadings between 2–10 wt%. Chitosan (CS) is modified with anionic surfactant, sodium dodecyl sulfate, via ionic complexation to facilitate compatibility and dispersion of CS to PMA matrix by non-covalent interactions between the components. The study successfully demonstrates high-accuracy 3D printing of composites with significant improvements in the overall mechanical properties. The composite with the best loading of 8 wt% SMCS shows a tensile modulus of 1.23 ± 0.05 GPa, a tensile strength at 49.8 ± 0.96 MPa, a yield stress at 33.3 ± 1.48 MPa, and a strain-at-ailure 10.3 ± 0.61%, which are 45%, 40%, 32%, and 68% higher than neat PMA, respectively. This provides a significant improvement in toughness at 4.92 ± 0.55 MJ m -3 for the composite, 184% higher than that of neat PMA. The marked increase in toughness is due to enhanced filler-matrix interactions which improve the ability of the 3D printed composite to absorb energy under tensile load. The results from this work provide new understandings into the strategies for design and preparation of stereolithography 3D printed materials reinforced with toughening fillers from renewable resources.

36 MATERIALS SCIENCE↗

DOE OSTI2025

A deep learning and finite element approach for exploration of inverse structure–property designs of lightweight hybrid composites

Hybrid composites have important applications, such as high-performance and lightweight materials in aerospace and automotive industries. Hybrid composites utilize the synergy of diverse fillers to achieve desired material properties, but usually have more complicated microstructures. While topology optimization can optimize a particular property, designing hybrid composites for customized mechanical performances, e.g. full-range stress–strain curve, remains challenging. Here, a computational framework that integrated finite element analysis (FEA) and artificial intelligence (AI) methods of Conditional Generative Adversarial Networks (cGAN) deep learning and transfer learning was developed to establish inverse structure–property relationships and design tailor-made hybrid composites. Based on FEA-generated datasets of hybrid fiber-particle–matrix microstructures and their corresponding full-range stress–strain curves, a cGAN architecture was trained to generate tailored microstructures and establish structure–property relationships. Similarity in microstructural features and well-matched stress–strain curves based on the AI-generated composites were achieved. In conclusion, transfer learning was used to expand the pre-trained model for designing different materials systems.

Hybrid composites↗