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NASA NTRS1988

Tension fatigue analysis and life prediction for composite laminates

A tension fatigue life prediction methodology for composite laminates is presented. Tension fatigue tests were conducted on quasi-isotropic and orthotropic glass epoxy, graphite epoxy, and glass/graphite epoxy hybrid laminates. Edge delamination onset data were used to generate plots of strain energy release rate as a function of cycles to delamination onset. These plots were then used along with strain energy release rate analyses of delaminations initiating at matrix cracks to predict local delamination onset. Stiffness loss was measured experimentally to account for the accumulation of matrix cracks and for delamination growth. Fatigue failure was predicted by comparing the increase in global strain resulting from stiffness loss to the decrease in laminate failure strain resulting from delaminations forming at matrix cracks through the laminate thickness. Good agreement between measured and predicted lives indicated that the through-thickness damage accumulation model can accurately describe fatigue failure for laminates where the delamination onset behavior in fatigue is well characterized, and stiffness loss can be monitored in real time to account for damage growth.

Obrien, T. K.↗

NASA NTRS1987

Interlaminar shear fracture toughness and fatigue thresholds for composite materials

Static and cyclic end notched flexure tests were conducted on a graphite epoxy, a glass epoxy, and graphite thermoplastic to determine their interlaminar shear fracture toughness and fatigue thresholds for delamination in terms of limiting values of the mode II strain energy release rate, G-II, for delamination growth. The influence of precracking and data reduction schemes are discussed. Finite element analysis indicated that the beam theory calculation for G-II with the transverse shear contribution included was reasonably accurate over the entire range of crack lengths. Cyclic loading significantly reduced the critical G-II for delamination. A threshold value of the maximum cyclic G-II below which no delamination occurred after one million cycles was identified for each material. Also, residual static toughness tests were conducted on glass epoxy specimens that had undergone one million cycles without delamination. A linear mixed-mode delamination criteria was used to characterize the static toughness of several composite materials; however, a total G threshold criterion appears to characterize the fatigue delamination durability of composite materials with a wide range of static toughness.

Obrien, T. Kevin↗

NASA NTRS1989

A new concept for high-cycle-life LEO: Rechargeable MnO2-hydrogen

The nickel-hydrogen secondary battery system is now the one of choice for use in GEO satellites. It offers superior energy density to that of nickel-cadmium, with a lifetime that is at least comparable in terms of both cycle life and overall operating life. While the number of deep cycles required for GEO use is small, LEO satellites with long lifetimes (5 to 10 years) will require secondary battery systems allowing 30,000 to 60,000 useful cycles which are characterized by an approximately 2C charge rate and C average discharge rate. Recent work has shown that birnessite MnO2 doped with bismuth oxide can be cycled at very high rates (6C) over a very large number of cycles (thousands) at depths-of-discharge in the 85 to 90 percent range, based on two electrons, which discharge at the same potential in a flat plateau. The potential is about 0.7 V vs. hydrogen, with a cut-off at 0.6 V. At first sight, this low voltage would seem to be a disadvantage, since the theoretical energy density will be low. However, it permits the use of lightweight materials that are immune from corrosion at the positive. The high utilization and low equivalent weight of the active material, together with the use of teflon-bonded graphite for current collection, result in very light positives, especially when these are compared with those in a derated nickel-hydrogen system. In addition, the weight of the pressure vessel falls somewhat, since the dead volume is lower. Calculations show that a total system will have 2.5 times the Ah capacity of a derated nickel-hydrogen LEO battery, so that the energy density, based on 1.2 V for nickel-hydrogen and 0.7 V for MnO2-hydrogen, will be 45 percent higher for comparable cycling performance.

Appleby, A. John↗

NASA NTRS1989

Interlaminar shear fracture toughness and fatigue thresholds for composite materials

O'Brien, T. Kevin↗

NASA NTRS1995

Flexure fatigue testing of 90 deg graphite/epoxy composites

A great deal of research has been performed characterizing the in-plane fiber-dominated properties, under both static and fatigue loading, of advanced composite materials. To the author's knowledge, no study has been performed to date investigating fatigue characteristics in the transverse direction. This information is important in the design of bonded composite airframe structure where repeated, cyclic out-of-plane bending may occur. Recent tests characterizing skin/stringer debond failures in reinforced composite panels where the dominant loading in the skin is flexure along the edge of the frame indicate failure initiated either in the skin or else the flange, near the flange tip. When failure initiated in the skin, transverse matrix cracks formed in the surface skin ply closest to the flange and either initiated delaminations or created matrix cracks in the next lower ply, which in turn initiated delaminations. When failure initiated in the flanges, transverse cracks formed in the flange angle ply closest to the skin and initiated delamination. In no configuration did failure propagate through the adhesive bond layer. For the examined skin/flange configurations, the maximum transverse tension stress at failure correlates very well with the transverse tension strength of the composites. Transverse tension strength (static) data of graphite epoxy composites have been shown to vary with the volume of material stressed. As the volume of material stressed increased, the strength decreased. A volumetric scaling law based on Weibull statistics can be used to predict the transverse strength measurements. The volume dependence reflects the presence of inherent flaws in the microstructure of the lamina. A similar approach may be taken to determine a volume scale effect on the transverse tension fatigue behavior of graphite/epoxy composites. The objective of this work is to generate transverse tension strength and fatigue S-N characteristics for composite materials using 3-point flexure tests of 90 deg graphite/epoxy specimens. Investigations will include the volume scale effect as well as frequency and span-to-thickness ratio effects. Prior to the start of the experimental study, an analytical study using finite element modeling will be performed to investigate the span-to-thickness effect. The ratio of transverse flexure stress to shear stress will be monitored and its values predicted by the FEM analysis compared with the value obtained using a 'strength of materials' based approach.

Peck, Ann Nancy W.↗

DOE OSTI2022

Surface analysis insight note: Differentiation methods applicable to noisy data for determination of sp2‐ versus sp3‐hybridization of carbon allotropes and AES signal strengths

The derivatives of the spectra are commonly used for quantification in Auger Electron Spectroscopy (AES) spectra, while the derivative of the KLL C Auger line has proven to be valuable in obtaining a measure of the relative proportions of sp 2 ‐ and sp 3 ‐hybridization using the D‐parameter in both AES and X‐ray Photoelectron Spectroscopy (XPS). Differentiation of X‐ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) spectra by numerical means is presented and illustrated for polymeric, such as PEEK and Nylon, as well as for graphitic materials including highly ordered pyrolytic graphite and graphene oxide. The most commonly available Savitzky–Golay method is explained mathematically and developed through the case of constructing a 5‐point quadratic polynomial convolution kernel suitable for differentiating spectra of adequate signal to noise. The concept of differentiation of spectra where signal to noise is less than adequate is also developed. Two alternative strategies to Savitzky–Golay differentiation are presented, which fit curves to data that allow derivatives to be obtained where Savitzky–Golay would otherwise fail. These alternative methods involve constructing a parametric curve that fits data over the entire energy interval of interest. Derivatives of spectra are then obtained by differentiating these parametric curves directly. A comparison of results for different materials for which specific sp 2 ‐ vs sp 3 ‐hybridized carbon proportions are of interest is used to emphasize the importance of characterizing methods used to differentiate spectra and understanding the characteristics of instrumentation used to measure spectra. The case for using Principal Component Analysis noise reduction with C KLL spectra is made for spectra collected from a heterogeneous graphene oxide sample.

Fairley, Neal↗

NASA NTRS1979

Mechanical and thermophysical properties of graphite/polyimide composite materials

An on-going program to characterize advanced composites for up to 50,000 hours of exposure to simulated supersonic cruise environments is summarized. Results are presented for up to 25,000 hours of thermal exposure and 10,000 hours of flight simulation at temperatures up to 560K (550 F) with emphasis on HTS/710 graphite/polyimide composite material. Results to date indicate that the maximum use temperature for HTS/710 may be reduced to 505K (450 F) for long-time (1000 hours) application such as the supersonic transport. Preliminary thermophysical properties data for HTS/PMR15 graphite/polyimide were generated. These data include thermal conductivity, thermal expansion, and specific heat from 115K (-252 F) to 590K (600 F) and emittance at room temperature and 590K (600 F). The purpose in generating these data was to validate use of state-of-the-art property measurement methods for advanced graphite fiber reinforced resin matrix composites. Based on results to this point, thermal expansion measurements for composites are most difficult to perform. A high degree of caution in conducting thermal expansion tests and analyzing results is required to produce reliable data.

Rummler, D. R.↗

NASA NTRS2008

Evaluation of Vapor Pressure and Ultra-High Vacuum Tribological Properties of Ionic Liquids (2) Mixtures and Additives

Ionic liquids are salts, many of which are typically viscous fluids at room temperature. The fluids are characterized by negligible vapor pressures under ambient conditions. These properties have led us to study the effectiveness of ionic liquids containing both organic cations and anions for use as space lubricants. In the previous paper we have measured the vapor pressure and some tribological properties of two distinct ionic liquids under simulated space conditions. In this paper we will present vapor pressure measurements for two new ionic liquids and friction coefficient data for boundary lubrication conditions in a spiral orbit tribometer using stainless steel tribocouples. In addition we present the first tribological data on mixed ionic liquids and an ionic liquid additive. Post mortem infrared and Raman analysis of the balls and races indicates the major degradation pathway for these two organic ionic liquids is similar to those of other carbon based lubricants, i.e. deterioration of the organic structure into amorphous graphitic carbon. The coefficients of friction and lifetimes of these lubricants are comparable to or exceed these properties for several commonly used space oils.

Morales, Wilfredo↗

DOE OSTI2021

Using In Situ High-Energy X-ray Diffraction to Quantify Electrode Behavior of Li-Ion Batteries from Extreme Fast Charging

Extreme fast charging (XFC, =15 min charging time) of Li-ion batteries (LIBs) has been proposed as an immediate target to increase the commercial appeal of electric vehicles. However, XFC of LIBs is associated with the degradation of battery performance and safety concerns. Quantitative and simultaneous characterization of various components during cell degradation represents a major experimental challenge. In this work, we outline a methodology for the use of spatially resolved, high-energy X-ray diffraction as a quantitative, in situ method of mapping the degradation of LIBs. We use this approach to study the battery cell capacity loss, both locally (mm scale) and globally over the entire cell (cm scale). Specifically, our workflow allows us to quantify the total amount of plated Li on the anode, as well as its spatial correlation to the structural properties of the anode and cathode. The method complements existing optical methods to resolve the spatial heterogeneity of local degradation mechanisms such as Li plating and provides simultaneous insights into concomitant anode state-of-charge variability. We apply it to commercially relevant single-layer pouch cells with the graphite anode and the LiNi 0.5 Mn 0.3 Co 0.2 O 2 cathode. Our results show that Li plating occurs heterogeneously on the graphite anode and that it is spatially correlated to the extent of anode lithiation. In this work, we anticipate that the described workflow will allow for understanding multiscale degradation in energy-storage devices beyond LIBs, where quantitative analysis at a local and global length scale can be performed without the necessity to tear down the device, due to the applicability of high-energy X-rays to probe in situ degradation.

25 ENERGY STORAGE↗

NASA NTRS1998

High Temperature Mechanical Characterization of Ceramic Matrix Composites

A high temperature mechanical characterization laboratory has been assembled at NASA Lewis Research Center. One contribution of this work is to test ceramic matrix composite specimens in tension in environmental extremes. Two high temperature tensile testing systems were assembled. The systems were assembled based on the performance and experience of other laboratories and meeting projected service conditions for the materials in question. The systems use frames with an electric actuator and a center screw. A PC based data acquisition and analysis system is used to collect and analyze the data. Mechanical extensometers are used to measure specimen strain. Thermocouples, placed near the specimen, are used to measure the specimen gage section temperature. The system for testing in air has a resistance element furnace with molybdenum disilicide elements and pneumatic grips with water cooling attached to hydraulic alignment devices. The system for testing in an inert gas has a graphite resistance element furnace in a chamber with rigidly mounted, water cooled, hydraulically actuated grips. Unidirectional SiC fiber reinforced reaction bonded Si3N4 and triaxially woven, two dimensional, SiC fiber reinforced enhanced SiC composites were tested in unidirectional tension. Theories for predicting the Young's modulus, modulus near the ultimate strength, first matrix cracking stress, and ultimate strength were applied and evaluated for suitability in predicting the mechanical behavior of SiC/RBSN and enhanced SiC/SiC composites. The SiC/RBSN composite exhibited pseudo tough behavior (increased area under the stress/strain curve) from 22 C to 1500 C. The rule of mixtures provides a good estimate of the Young's modulus of the SiC/RBSN composite using the constituent properties from room temperature to 1440 C for short term static tensile tests in air or nitrogen. The rule of mixtures significantly overestimates the secondary modulus near the ultimate strength. The ACK theory provides the best approximation of the first matrix cracking stress when residual stresses are ignored. The theory of Cao and Thouless, based on Weibull statistics, gave the best prediction for the composite ultimate strength. The enhanced SiC/SiC composite exhibited nonlinear stress/strain behavior from 24 C to 1370 C in air with increased ultimate strain when compared to monolithic SiC. The theory of Yang and Chou with the assumption of a frictional fiber/matrix interface provided the best estimate of the Young's modulus. The theory of Cao and Thouless gave the best estimate for the ultimate strength.

Gyekenyesi, John Z.↗

NASA NTRS2004

The History of Presolar Grains

Below we summarize the results of our investigations into the history of presolar grains that were conducted in the last year. During this time we have expended much of our effort in the development of experimental techniques and sample preparation methods that are needed to laboratory in December, 2000. Specific information on this instrument is contained in the Full Proposal of PI Ernst Zinner and will not be repeated here. Our general strategy in the past year has been in large measure to explore novel sample handling methods for the very small (sub-micron), but more representative, presolar grains that can now be characterized isotopically in the NanoSIMS. We have developed experimental techniques that will permit NanoSIMS analyses of the very same ultramicrotome sections studied in the TEM, and we have developed grain dispersion, handling and mounting techniques that permit NanoSIMS isotopic analysis as well as field emission SEM, high energy TEM, and atomic force microscopy of pristine presolar grains. Although much of this has been slow and very difficult work that has no immediate payoff in terms of publishable results, we considered it absolutely necessary groundwork for future discoveries, especially in the realm of individual presolar grains that have been inaccessible to past studies due to size constraints. As discussed below, we have been largely successful in these endeavors, and expect to reap the benefits of this work in the next year. We also report on our continued morphologic studies of pristine presolar grains, on our investigations of presolar graphite grains from supernovae as well as on rarer types of presotar SIC, on the search for presolar silicates, and on our efforts to obtain direct size-distribution information on presolar SiC through X-ray mapping techniques.

Bernatowicz, Thomas J.↗

NASA NTRS1981

Ultra-high modulus organic fiber hybrid composites

An experimental organic fiber, designated Fiber D, was characterized, and its performance as a reinforcement for composites was investigated. The fiber has a modulus of 172 GPa, tensile strength of 3.14 GPa, and density of 1.46 gm/cu cm. Unidirectional Fiber D/epoxy laminates containing 60 percent fiber by volume were evaluated in flexure, shear, and compression, at room temperature and 121 C in both the as fabricated condition and after humidity aging for 14 days at 95 percent RH and 82 C. A modulus of 94.1 GPa, flexure strength of 700 MPa, shear strength of 54 MPa, and compressive strength of 232 MPa were observed at room temperature. The as-fabricated composites at elevated temperature and humidity aged material at room temperature had properties 1 to 20 percent below these values. Combined humidity aging plus evaluated temperature testing resulted in even lower mechanical properties. Hybrid composite laminates of Fiber D with Fiber FP alumina or Thornel 300 graphite fiber were also evaluated and significant increases in modulus, flexure, and compressive strengths were observed.

Champion, A. R.↗

DOE OSTI2024

Experimental investigation into coal wettability changes caused by reactions with scCO 2 -H 2 O

Geological CO 2 sequestration (GCS) can help mitigate global warming and enhance methane recovery from coal beds. However, few studies have linked the effects of CO 2 to surface chemistry changes controlling wetting behavior in deep coal beds. Contact angles (CAs) of CO 2 /N 2 -high volatile bituminous coal-water systems were measured under different temperatures and pressures. The surface chemistry and physical structure of coals were characterized to investigate changes in physicochemical properties and their relations with wettability after reactions. For N 2 treatment, the time-dependence of static and dynamic CAs were insignificant, ranging within 4°. For gaseous CO 2 treatment, the static CAs and the average advancing angles increased slightly. With supercritical (sc) CO 2 , both the static and dynamic CAs increased significantly, and θ adv changed to intermediate-wet (92°). Reactions with minerals exposed to scCO 2 resulted in greater surface roughness and heterogeneity, greater contact angle hysteresis and more surface sites occupied by scCO 2 rather than H 2 O. Increases in hydrophobic functional groups and decreases in hydrophilicity were shown by FTIR spectra, reflecting the shedding of polar oxygen-containing functional groups, reduction of hydrogen bonds, and increasing percentage of hydrocarbons. XRD patterns obtained following scCO 2 -treatment showed that crystallite growth and molecular polymerization were higher toward graphite-like. The calculated structural parameters of functional groups and crystallites both showed elevated coal rank. Changes in crystallite structure, notably higher carbon content and decreased negative surface charge, are unfavorable for water-wetting. Finally, this study contributes to understanding surface chemistry changes responsible for decreased wettability during CO 2 -enhanced coal bed methane recovery and GCS in coal reservoirs.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2026

Characterization of runaway electron impact on instrumented sacrificial limiters on DIII-D

Instrumented sacrificial limiter heads, both domed (proud) and flat (flush) are used in DIII-D runaway electron (RE) wall strikes to study the wall impact dynamics with high spatial and time resolution. The approximate structure of the RE wetted area and heating depth on the domed limiter heads were predicted qualitatively using orbit-tracking simulations, although a strong left–right asymmetry (about the magnetic field direction) was not captured well by the simulations. It is hypothesized that this difference is perhaps due to the local 3D magnetic field perturbation of the dome limiter head. The average kinetic energy K and pitch angle θ of REs striking the limiter head were estimated from the spatial distribution of local HXR emission and were estimated to be roughly K ≈ 4 MeV and θ ≈ 0.2 rad. These values are roughly consistent with in-plasma values estimated before the loss event, indicating that RE kinetic energy and pitch angle are not drastically altered when transporting to the wall. Large shot–shot variations (1–10 kJ) in energy deposition into the limiter head were observed and were explained by shot–shot variations in locked magneto-hydrodynamics mode toroidal phase. For the largest deposited energies (10 kJ), graphite material failure and explosive dust release was observed, and the depth of material failure at higher energy deposition was successfully reproduced using modelling of volumetric energy deposition and brittle failure. The presence of energetic (keV) level ion impact during the RE wall strike was confirmed by three different surface analysis techniques. The ratio of energetic ion to RE flux appears to be larger on flat surfaces within the RE wetted area, although the energetic ion flux and total energy flux due to energetic ions have not yet been quantified.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS2012

First Keck Nulling Observations of a Young Stellar Object: Probing the Circumstellar Environment of the Herbig Ae Star MWC325

We present the first N-band nulling plus K- and L-band V(sup 2) observations of a young stellar object, MWC 325, taken with the 85 m baseline Keck Interferometer. The Keck nuller was designed for the study of faint dust signatures associated with debris disks, but it also has a unique capability for studying the temperature and density distribution of denser disks found around young stellar objects. Interferometric observations of MWC 325 at K, L, and N encompass a factor of five in spectral range and thus, especially when spectrally dispersed within each band, enable characterization of the structure of the inner disk regions where planets form. Fitting our observations with . geometric models such as a uniform disk or a Gaussian disk show that the apparent size increases 'monotonically with wavelength in the 2-12/Lm wavelength region, confirming the widely held assumption based on radiative transfer models, now with spatially resolved measurements over a broad wavelength range, that disks are extended with a temperature gradient. The effective size is a factor of about 1.4 and 2.2 larger in the L band and N band, respectively, compared to that in the K band. The existing interferometric measurements and the spectral energy distribution can be reproduced by a flat disk or a weakly shadowed nearly flat disk model, with only slight flaring in the outer regions of the disk, consisting of representative "sub-micron" (0.1 micron) and "micron" (2 micron) grains of a 50:50 ratio of silicate and graphite. This is in marked contrast io the disks previously found in other Herbig Ae/Be stars, suggesting a wide variety in the disk properties among Herbig Ae/Be stars.

Ragland, S.↗

NASA NTRS2012

First Keck Nulling Observations of a Young Stellar Object: Probing the Circumstellar Environment of the Herbig Ae star MWC 325

We present the first N-band nulling plus K- and L-band V(sup 2) observations of a young stellar object, MWC325, taken with the 85 m baseline Keck Interferometer. The Keck nuller was designed for the study of faint dust signatures associated with debris disks, but it also has a unique capability for studying the temperature and density distribution of denser disks found around young stellar objects. Interferometric observations of MWC 325 at K, L and N encompass a factor of five in spectral range and thus, especially when spectrally dispersed within each band, enable characterization of the structure of the inner disk regions where planets form. Fitting our observations with geometric models such as a uniform disk or a Gaussian disk show that the apparent size increases monotonically with wavelength in the 2-12 micrometer wavelength region, confirming the widely held assumption based on radiative transfer models, now with spatially resolved measurements over broad wavelength range, that disks are extended with a temperature gradient. The effective size is a factor of about 1.3 and 2 larger in the Lband and N-band, respectively, compared to that in the K-band. The existing interferometric measurements and the spectral energy distribution can be reproduced by a flat disk or a weakly shadowed nearly flat-disk model, with only slight flaring in the outer regions of the disk, consisting of representative "sub-micron" (0.1 micron) and "micron" (2 micron) grains of a 50:50 ratio of silicate and graphite. This is marked contrast with the disks previously found in other Herbig Ae/Be stars suggesting a wide variety in the disk properties among Herbig Ae/Be stars.

Ragland, S.↗

DOE OSTI2024

Graphitic Carbon Nitride Quantum Dots (g‐C 3 N 4 QDs): From Chemistry to Applications

Since their emergence in 2014, graphitic carbon nitride quantum dots (g-C 3 N 4 QDs) have attracted much interest from the scientific community due to their distinctive physicochemical features, including structural, morphological, electrochemical, and optoelectronic properties. Owing to their desirable characteristics, such as non-zero band gap, ability to be chemically functionalized or doped, possessing tunable properties, outstanding dispersibility in different media, and biocompatibility, g-C 3 N 4 QDs have shown promise for photocatalysis, energy devices, sensing, bioimaging, solar cells, optoelectronics, among other applications. As these fields are rapidly evolving, it is very strenuous to pinpoint the emerging challenges of the g-C 3 N 4 QDs development and application during the last decade, mainly due to the lack of critical reviews of the innovations in the g-C 3 N 4 QDs synthesis pathways and domains of application. Herein, an extensive survey is conducted on the g-C 3 N 4 QDs synthesis, characterization, and applications. Scenarios for the future development of g-C 3 N 4 QDs and their potential applications are highlighted and discussed in detail. In conclusion, the provided critical section suggests a myriad of opportunities for g-C 3 N 4 QDs, especially for their synthesis and functionalization, where a combination of eco-friendly/single step synthesis and chemical modification may be used to prepare g-C 3 N 4 QDs with, for example, enhanced photoluminescence and production yields.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Interpretation of wide-angle x-ray diffraction patterns from mesophase pitch-based carbon fibers – a simulation and experimental study

Carbon fiber is a critical material in a wide range of industries, where it is highly valued for its high specific strength/stiffness, excellent wear resistance, efficient electrical and thermal transport properties, chemical resistance, and low coefficient of thermal expansion. The properties of a specific carbon fiber are closely tied to its structural characteristics at all length scales. Here, in this work, we applied wide-angle x-ray diffraction to a set of heat-treated mesophase pitch-based carbon fibers, with the goal of elucidating the crystalline structures as a function of fiber orientation. To assist with analysis and interpretation of the experimental data, we employed diffraction pattern simulations using the scalar and vector forms of the Debye scattering equation to determine the influence of basal plane orientation, crystalline ordering (turbostratic-graphitic), and basal plane asymmetry on the diffraction patterns. The results presented here suggest that growth of the transverse crystallites in mesophase pitch-based carbon fiber is fixed until graphitization temperatures are reached. The work completed here provides a framework for the analysis of carbon fiber and other oriented carbon-based materials via diffraction.

36 MATERIALS SCIENCE↗