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NASA NTRS2010

Probabilistic Simulation for Combined Cycle Fatigue in Composites

A methodology to compute probabilistic fatigue life of polymer matrix laminated composites has been developed and demonstrated. Matrix degradation effects caused by long term environmental exposure and mechanical/thermal cyclic loads are accounted for in the simulation process. A unified time-temperature-stress dependent multifactor interaction relationship developed at NASA Glenn Research Center has been used to model the degradation/aging of material properties due to cyclic loads. The fast probability integration method is used to compute probabilistic distribution of response. Sensitivities of fatigue life reliability to uncertainties in the primitive random variables (e.g., constituent properties, fiber volume ratio, void volume ratio, ply thickness, etc.) computed and their significance in the reliability-based design for maximum life is discussed. The effect of variation in the thermal cyclic loads on the fatigue reliability for a (0/+/- 45/90)s graphite/epoxy laminate with a ply thickness of 0.127 mm, with respect to impending failure modes has been studied. The results show that, at low mechanical cyclic loads and low thermal cyclic amplitudes, fatigue life for 0.999 reliability is most sensitive to matrix compressive strength, matrix modulus, thermal expansion coefficient, and ply thickness. Whereas at high mechanical cyclic loads and high thermal cyclic amplitudes, fatigue life at 0.999 reliability is more sensitive to the shear strength of matrix, longitudinal fiber modulus, matrix modulus, and ply thickness.

Chamis, Christos C.↗

DOE OSTI2025

Additively manufacturing high-temperature aluminum alloy for automotive engine pistons

The purpose of the project was to evaluate DuAlumin-3D, an ORNL designed Al alloy, for additive manufacturing of high-performance automotive components. The project consisted of additively manufacturing a cylindrical block of representative material which was then heat treated before machining into test coupons. Testing included tensile tests as a function of temperature, high-cycle fatigue testing as a function of temperature, density and elastic modulus measurements, and thermophysical property measurements. Fractography was also performed on failed high-cycle fatigue specimens. The results were compared against benchmark AM Al alloys and current high-performance conventionally manufactured alloys. Overall, the DuAlumin-3D material outperformed the incumbent materials in mechanical properties, especially at elevated temperatures, while maintaining broadly similar thermophysical properties. The results of this study support further maturation of the material for additive manufacturing of high-performance automotive components.

36 MATERIALS SCIENCE↗

NASA NTRS1982

Mechanical properties of the Shuttle Orbiter thermal protection system strain isolator pad

An experimental investigation conducted to determine the static and fatigue properties of the Strain Isolator Pad (SIP) used on the Shuttle Orbiter Thermal protection system is described. Static tension-compression and shear test results show that the SIP is highly nonlinear and that it possesses a large hysteresis, a large low modulus region for low stress levels, and stress-strain properties that are highly sensitive to strain rate and previous load history. In addition, the shear properties are also found to be sensitive to forces applied normal to the plane of the pad and to the orientation of the material. For the undensified tile/SIP system, static and fatigue failure takes place at the SIP/tile interface at low stress levels and for a small number of cycles.

Sawyer, J. W.↗

NASA NTRS2010

Probabilistic Simulation of Combined Thermo-Mechanical Cyclic Fatigue in Composites

A methodology to compute probabilistically-combined thermo-mechanical fatigue life of polymer matrix laminated composites has been developed and is demonstrated. Matrix degradation effects caused by long-term environmental exposure and mechanical/thermal cyclic loads are accounted for in the simulation process. A unified time-temperature-stress-dependent multifactor-interaction relationship developed at NASA Glenn Research Center has been used to model the degradation/aging of material properties due to cyclic loads. The fast probability-integration method is used to compute probabilistic distribution of response. Sensitivities of fatigue life reliability to uncertainties in the primitive random variables (e.g., constituent properties, fiber volume ratio, void volume ratio, ply thickness, etc.) computed and their significance in the reliability-based design for maximum life is discussed. The effect of variation in the thermal cyclic loads on the fatigue reliability for a (0/+/-45/90)s graphite/epoxy laminate with a ply thickness of 0.127 mm, with respect to impending failure modes has been studied. The results show that, at low mechanical-cyclic loads and low thermal-cyclic amplitudes, fatigue life for 0.999 reliability is most sensitive to matrix compressive strength, matrix modulus, thermal expansion coefficient, and ply thickness. Whereas at high mechanical-cyclic loads and high thermal-cyclic amplitudes, fatigue life at 0.999 reliability is more sensitive to the shear strength of matrix, longitudinal fiber modulus, matrix modulus, and ply thickness.

Chamis, Christos C.↗

NASA NTRS2011

Probabilistic Simulation of Combined Thermo-Mechanical Cyclic Fatigue in Composites

Chamis, Christos C.↗

NASA NTRS1979

Anorthite: Thermal equation of state to high pressures

The shock wave (Hugoniot) data on single crystal and porous anorthite (CaAl2Si208) to pressures of 120 GPa are presented. These data are inverted to yield high pressure values of the Grueneisen parameter, adiabatic bulk modulus, and coefficient of thermal expansion over a broad range of pressures and temperatures which in turn are used to reduce the raw Hugoniot data and construct an experimentally based, high pressure thermal equation of state for anorthite. The hypothesis that higher order anharmonic contributions to the thermal properties decrease more rapidly upon compression than the lowest order anharmonicities is supported. The properties of anorthite corrected to lower mantle conditions show that although the density of anorthite is comparable to that of the lower most mantle, its bulk modulus is considerably less, hence making enrichment in the mantle implausible except perhaps near its base.

Jeanloz, R.↗

NASA NTRS1992

Discontinuously reinforced intermetallic matrix composites via XD synthesis

A review is given of recent results obtained for discontinuously reinforced intermetallic matrix composites produced using the XD process. Intermetallic matrices investigated include NiAl, multiphase NiAl + Ni2AlTi, CoAl, near-gamma titanium aluminides, and Ll2 trialuminides containing minor amounts of second phase. Such mechanical properties as low and high temperature strength, compressive and tensile creep, elastic modulus, ambient ductility, and fracture toughness are discussed as functions of reinforcement size, shape, and volume fraction. Microstructures before and after deformation are examined and correlated with measured properties. An observation of interest in many of the systems examined is 'dispersion weakening' at high temperatures and high strain rates. This behavior is not specific to the XD process; rather similar observations have been reported in other discontinuous composites. Proposed mechanisms for this behavior are presented.

Kumar, K. S.↗

DOE OSTI2025

Pultrusion and Vitrimer Composites: Emerging Pathways for Sustainable Structural Materials

Pultrusion is a manufacturing process used to produce fiber-reinforced polymer composites with excellent mechanical, thermal, and chemical properties. The resulting materials are lightweight, durable, and corrosion-resistant, making them valuable in aerospace, automotive, construction, and energy sectors. However, conventional thermoset composites remain difficult to recycle due to their infusible and insoluble cross-linked structure. This review explores integrating vitrimer technology a novel class of recyclable thermosets with dynamic covalent adaptive networks into the pultrusion process. As only limited studies have directly reported vitrimer pultrusion to date, this review provides a forward-looking perspective, highlighting fundamental principles, challenges, and opportunities that can guide future development of recyclable high-performance composites. Vitrimers combine the mechanical strength (tensile strength and modulus) of thermosets with the reprocessability and reshaping of thermoplastics through dynamic bond exchange mechanisms. These polymers offer high-temperature reprocessability, self-healing, and closed-loop recyclability, where recycling efficiency can be evaluated by the recovery yield retention of mechanical properties and reuse cycles meeting the demand for sustainable manufacturing. Key aspects discussed include resin formulation, fiber impregnation, curing cycles, and die design for vitrimer systems. The temperature-dependent bond exchange reactions present challenges in achieving optimal curing and strong fiber–matrix adhesion. Recent studies indicate that vitrimer-based composites can maintain structural integrity while enabling recycling and repair, with mechanical performance such as flexural and tensile strength comparable to conventional composites. Incorporating vitrimer materials into pultrusion could enable high-performance, lightweight products for a circular economy. The remaining challenges include optimizing curing kinetics, improving interfacial adhesion, and scaling production for widespread industrial adoption.

Fiber composites↗

DOE OSTI2022

Graphene nanoplatelets reinforced cement as a solution to leaky wellbores reinforcing weak points in hydrated Portland cement with graphene nanoparticles improves mechanical and chemical durability of wellbore cements

In this work, to improve the performance of wellbore cement under subsurface environments, graphene nanoplatelets (GNPs) were added in various percentages to Class-H cement slurry. Microstructural characterization of cement slurries cured at 90 °C and 95% RH indicates that GNP modifies the microstructure of hydrated cement by reinforcing pore spaces. As a result, the mechanical properties, such as Young's modulus and axial peak stress, obtained from high temperature triaxial compression tests are significantly improved based on different percentages of added GNPs. Furthermore, the hydrated 1 × 2 inch GNP- Portland cement cores tested under simulated deep wellbore conditions of high-temperature and high pressure (HTHP), appear to have a ductile-like behavior, when compared to a typical brittle nature of Portland cement pastes. From our observations and published data on graphene resistance to fracture, GNP addition to cement is evidently enhancing the flexibility of cement. These improvements would reduce the risks associated with wellbore cement deterioration and a consequent leakage in fossil fuel production, geothermal energy production, CO 2 storage as well as long-term sealing materials in plugging and abandonment of all wellbores at the end of their service life.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Polyester-based epoxy vitrimer integrating spent coffee ground as a natural filler

Coffee is a widely consumed beverage, but approximately 80% mass of coffee cherry is discarded as waste. Here, in this study, spent coffee grounds (SCG) were recycled and used as a natural filler in a polyester-based epoxy matrix made from reactions of diglycidyl ethers of Bisphenol A and polyethylene glycol with methyl nadic anhydride. The properties of SCG/epoxy composites with various SCG contents up to 40% w/w were evaluated using various techniques such as FT-IR spectroscopy, tensile testing, optical microscopy, differential scanning calorimetry, and rheology. The SCG filled polyester-based epoxy matrix demonstrated excellent dimensional stability and retained a permanently crosslinked network, but re-shaping was possible at ~150 °C through transesterification, which occurred due to a dynamic chain exchange reaction between the ester group of the epoxy matrix and the hydroxyl group of the SCG fillers. The transesterification also improved the interfacial adhesion between the matrix and SCG fillers, resulting in tensile strength of over 20 MPa and a modulus of around 2.5 GPa, even with high SCG contents up to 40% w/w. While neat, cured epoxy shows thermoset behavior, filling the matrix with SCG enables reforming and origami-inspired spontaneous change in shape.

42 ENGINEERING↗

DOE OSTI2022

Investigating dry room compatibility of sulfide solid-state electrolytes for scalable manufacturing

All-solid-state batteries (ASSBs) are viewed as promising next-generation energy storage devices, due to their enhanced safety by replacing organic liquid electrolytes with non-flammable solid-state electrolytes (SSEs). The high ionic conductivity and low Young's modulus of sulfide SSEs make them suitable candidates for commercial ASSBs. Nevertheless, sulfide SSEs are generally reported to be unstable in ambient air. Moreover, instead of gloveboxes used for laboratory scale studies, large scale production of batteries is usually conducted in dry rooms. Thus, this study aims to elucidate the chemical evolution of a sulfide electrolyte, Li 6 PS 5 Cl (LPSCl), during air exposure and to evaluate its dry room compatibility. When LPSCl is exposed to ambient air, hydrolysis, hydration, and carbonate formation can occur. Moreover, hydrolysis can lead to irreversible sulfur loss and therefore LPSCl cannot be fully recovered in the subsequent heat treatment. During heat treatment, exposed LPSCl undergoes dehydration, decomposition of carbonate species, and reformation of the LPSCl phase. Lastly, LPSCl was found to exhibit good stability in a dry room environment and was subject to only minor conductivity loss due to carbonate formation. The dry room exposed LPSCl sample was tested in a LiNi 0.8 Co 0.1 Mn 0.1 O 2 |LiIn half-cell, exhibiting no significant loss of electrochemical performance compared with the pristine LPSCl, proving it to be compatible with dry room manufacturing processes.

36 MATERIALS SCIENCE↗

DOE OSTI2023

An Investigation of Nanoindentation as Quality Control [Slides]

Nanoindentation Continuous Stiffness Measurement (CSM) mapping, and Strain Rate Jump Testing (SRJT) proved effective to highlight and visualize the extent of property differences between the samples. From the analysis, Lot A has a significant dead zone at its center, especially when compared with the cross section of Lot B. Quick identification of property issues from one of the two feed stocks, both of which fit the specification. Mechanical performance was connected to the microstructure. Thus, using the structure-property results, it is noted that the processing of Lot A may have been insufficient. Nanoindentation allows for the sampling of quality control variables such as hardness and modulus in a short time span at high resolution, which is cheaper and faster than traditional strength experiments (tension and compression tests).

36 MATERIALS SCIENCE↗

NASA NTRS1978

Thermal shock and erosion resistant tantalum carbide ceramic material

Ceramic tantalum carbide artifacts with high thermal shock and mechanical erosion resistance are provided by incorporating tungsten-rhenium and carbon particles in a tantalum carbide matrix. The mix is sintered by hot pressing to form the ceramic article which has a high fracture strength relative to its elastic modulus and thus has an improved thermal shock and mechanical erosion resistance. The tantalum carbide is preferable less than minus 100 mesh, the carbon particles are preferable less than minus 100 mesh, and the tungsten-rhenium particles are preferable elongate, having a length to thickness ratio of at least 2/1. Tungsten-rhenium wire pieces are suitable as well as graphite particles.

Honeycutt, L., III↗

NASA NTRS1995

Mechanical properties of high-temperature superconducting wires

Bending strength, fracture toughness, and elastic modulus data were acquired for YBa2Cu3O(x), Bi2Sr2CaCu2O(x) (Bi,Pb)2Sr2Ca2Cu3O(x), and Tl2Ba2Ca2Cu3O(x) bars. These data and thermal expansion coefficients strongly suggest that the maximum possible tensile strain without fracture of bulk tapes or wires is approximately equals 0.2%. In Ag-clad conductors, residual stresses will be of limited benefit, but fractures produced by larger strains can be accommodated by shunting current through the Ag.

Goretta, K. C.↗

NASA NTRS1998

Hi-Nicalon Fiber-Reinforced Celsian Matrix Composites: Influence of Interface Modification

Unidirectional celsian matrix composites having 42-45 vol % of uncoated or BN-SIC coated Hi-Nicalon fibers were tested in three-point bend at room temperature. The uncoated fiber-reinforced composites showed catastrophic failure with strength of 210 35 MPa and a flat fracture surface. In contrast, composites reinforced with coated fibers exhibited graceful failure with extensive fiber pullout. Values of first matrix cracking stress and strain were 435 +/- 35 MPa and 0.27 +/- 0.01%, respectively, with ultimate strength as high as 960 MPa. The elastic Young modulus of the uncoated and coated fiber-reinforced composites were 184 +/- 4 GPa and 165 +/- 5 GPa, respectively. Fiber push-through tests and microscopic examination indicated no chemical reaction at the uncoated or coated fiber-matrix interface. The low strength of composite with uncoated fibers is due to degradation of the fiber strength from mechanical damage during processing. Because both the coated- and uncoated-fiber-reinforced composites exhibited weak interfaces, the beneficial effect of the BN-SIC dual layer is primarily the protection of fibers from mechanical damage during processing.

Bansal, Narottam P.↗

DOE OSTI2024

Effect of Zn Addition on Phase Evolution in AlCrFeCoNiZn High–Entropy Alloy

The addition of Zn to AlCrFeCoNi high-entropy alloy (HEA) poses intriguing questions as to how it would affect phase evolution. Herein, the phase evolution in AlCrFeCoNiZn is studied using a combination of experimental techniques (X-ray diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and differential scanning calorimetry) and computational (density-functional theory [DFT], calculation of phase diagrams, and machine-learning) methods. Mechanically alloyed and spark-plasma-sintered AlCrFeCoNiZn assumes a metastable single-phase, body-centered-cubic (BCC) structure that undergoes diffusion-controlled phase separation upon subsequent heat treatment to form separate (Al, Cr)-rich, (Fe, Co)-rich, and (Zn, Ni)-rich phases. The formation of (Al, Cr)-rich phase, not reported previously in AlCrFeCoNi-based HEAs, is attributed to strong clustering tendency of Cr–Zn and Cr–Ni pairs, combined with the strong ordering of Zn–Ni pair, driving out Cr that in turn combines with Al to form a (Al, Cr)-rich phase. In the DFT results, the formation of thermodynamically stable L1 2 phase is shown wherein Cr–Fe–Zn [Al–Ni-Co] preferably occupy1a (000) [3c (0 ½ ½)] positions. Furthermore, the sluggish diffusional transformation to L1 2 phase from BCC precursors is attributed to the small stacking-fault energy of AlCrFeCoNiZn. The equilibrated HEA exhibits a high microhardness of 8.24 GPa with an elastic modulus of 184 GPa.

36 MATERIALS SCIENCE↗

NASA NTRS2019

Quantifying the Influence of Redox Conditions on the Seismic Properties of Olivine

A series of eight olivine specimens were fabricated by hot-pressing at 1200 degrees Celsius and 300 megapascals (MPa). Each hot-pressed specimen was then wrapped in Pt, Ni or NiFe foil to vary oxygen fugacity (fO2), and interrogated via forced torsional oscillation. Mechanical testing was conducted at 10 oscillation periods between 1 and 1000 seconds, at a confining pressure of 200 MPa, during a slow staged-cooling from a maximum temperature of 1200 degrees Celsius to room temperature. After mechanical testing, each specimen was axially sectioned and EBSD (Electron BackScatter Diffraction) was used for the determination of the representative grain size, and grain size distribution of each sample. In addition, each longitudinal section was mapped via FTIR (Fourier Transform InfraRed spectroscopy) to determine the spatial distribution and concentrations of chemically bound and molecular water. Amongst these specimens, chemically bound ‘water’ contents were observed to vary between 0 and 1150 atom ppm (parts per million) H/Si, and molecular water concentrations varied between 0 and 245 atom ppm H/Si. Our forced-oscillation results demonstrate that the measured magnitude of anelastic relaxation within the experimental ‘window’ of oscillation periods is unrelated to the water content. Rather, a relationship was observed between the magnitude of anelastic relaxation and the prevailing redox conditions, which is influenced by the choice of metal sleeving used during the mechanical test. Further, regardless of water content or metal sleeving, each specimen exhibits coupled variations in shear modulus and dissipation within the observational window, indicative of ‘high-temperature background’ behavior, that can be described by a Burgers-type model. During initial fitting of the Burgers models, the unrelaxed shear modulus at a reference temperature of 900 degrees Celsius (G (sub UR)) and the temperature derivative of the unrelaxed shear modulus (dG (sub U)/dT), were treated as adjustable parameters. For all Fe-bearing olivine samples (but not a hydrous and oxidized Fe-free sample) we observe deficits of G (sub UR), and increased values of dG (sub U)/dT, relative to the expected elastic (anharmonic) behavior of Fo90 olivine. This behavior is indicative of anelastic relaxation occurring at shorter periods than observable within the ‘window’ of oscillation periods used in the mechanical test. Moving towards a comprehensive seismologically applicable Burgers model, which includes this newly observed effect of redox conditions on anelastic relaxation, we will present our progress in reconciling truly anharmonic and elastic behavior of Fo (sub 90) olivine with our observed forced-oscillation data.

Cline, Christopher, II↗

NASA NTRS2019

The Influence of Redox Conditions on the Seismic Properties of Polycrystalline Olivine

Eight olivine specimens were fabricated by use of a solgel method and hot-pressing at 1200 degrees Centigrade and 300 megapascals (MPa) inside of welded Pt capsules. Each hot-pressed specimen was then recovered, precision ground, and wrapped in Pt, Ni or NiFe foil to vary oxygen fugacity (fO2) during the subsequent forced torsional oscillation measurements. Mechanical testing was conducted at 10 oscillation periods between 1 and 1000 seconds, at a confining pressure of 200 MPa, during a slow staged-cooling from a maximum temperature of 1200 degrees Centigrade down to room temperature. After mechanical testing, each specimen was axially sectioned and EBSD (Electron BackScatter Diffraction) was used for the determination of the representative grain size, and grain size distribution of each sample. In addition, each longitudinal section was mapped via FTIR (Fourier Transform Infrared Spectroscopy) to determine the spatial distribution and concentrations of chemically bound and molecular water. Amongst these eight specimens, chemically bound ‘water’ contents were observed to vary between 0 and 1150 atom parts per million (ppm) H/Si, and molecular water concentrations varied between 0 and 245 atom ppm H/Si. Our forced-oscillation results demonstrate that the measured magnitude of anelastic relaxation within the experimental ‘window’ of oscillation periods is unrelated to the water content. Rather, a relationship was observed between the magnitude of anelastic relaxation and the prevailing redox conditions, which is influenced by the choice of metal sleeving used during the mechanical test. Further, regardless of water content or metal sleeving, each specimen exhibits coupled variations in shear modulus and dissipation within the observational window, indicative of ‘high-temperature background’ behavior, that can be described by a Burgers-type model. During initial fitting of the Burgers models, the unrelaxed shear modulus at a reference temperature of 900°C (elastic unloading/reloading shear modulus G (sub UR)) and the temperature derivative of the unrelaxed shear modulus (dGU/dT), were treated as adjustable parameters. For all Fe-bearing olivine samples we observe deficits of G (sub UR) and increased values of dGU/dT, relative to the expected elastic (anharmonic) behavior for Fo (Forsterite content percentage) (sub 90) olivine. This behavior is indicative of anelastic relaxation occurring at shorter periods than observable within the ‘window’ of oscillation periods used in the mechanical test. Moving towards a comprehensive and seismologically applicable Burgers model, which includes this newly observed effect of redox conditions on anelastic relaxation, we will present our progress on reconciling truly anharmonic and elastic behavior of Fo (sub 90) olivine with our observed forced-oscillation data.

Cline, C. J., II↗