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DOE OSTI2024

Use of carbonyldiimidazole as a derivatization agent for the detection of pinacolyl alcohol, a forensic marker for Soman, by EI-GC–MS and LC-HRMS in official OPCW proficiency test matrices

Pinacolyl alcohol (PA), a key forensic marker for the nerve agent Soman (GD), is a particularly difficult analyte to detect by various analytical methods. In this work, we have explored the reaction between PA and 1,1'-carbonyldiimidazole (CDI) to yield pinacolyl 1H-imidazole-1-carboxylate (PIC), a product that can be conveniently detected by gas chromatography–mass spectrometry (GC–MS) and liquid chromatography-high-resolution mass spectrometry (LC-HRMS). Regarding its GC–MS profile, this new carbamate derivative of PA possesses favorable chromatographic features such as a sharp peak and a longer retention time (RT = 16.62 min) relative to PA (broad peak and short retention time, RT = 4.1 min). Additionally, the derivative can also be detected by LC-HRMS, providing an avenue for the analysis of this chemical using this technique where PA is virtually undetectable unless present in large concentrations. From a forensic science standpoint, detection of this low molecular weight alcohol signals the past or latent presence of the nerve agent Soman (GD) in a given matrix (i.e., environmental or biological). The efficiency of the protocol was tested separately in the analysis and detection of PA by EI-GC–MS and LC-HRMS when present at a 10 μg/mL in a soil matrix featured in the 44th PT and in a glycerol-rich liquid matrix featured in the 48th Official Organization for the Prohibition of Chemical Weapons (OPCW) Proficiency Test when present at a 5 μg/mL concentration. In both scenarios, PA was successfully transformed into PIC, establishing the protocol as an additional tool for the analysis of this unnatural and unique nerve agent marker by GC–MS and LC-HRMS.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Meteorite Ablation at the HYMETS ARC-JET Facility

One of the primary goals of the Asteroid Threat Assessment Program (ATAP) is to understand the ablation phenomena of meteors (e.g., spallation, evaporation, melt flow, etc.). Therefore, a test campaign was executed at the Hypersonic Material Test System (HYMETS) facility on samples of an ordinary chondrite (e.g., Tamdakht) and samples of basalt from the Columbia plateau. High melt viscosities and low ablation rates are predicted for basalt due to higher concentrations of silica and alumina in the matrix phase. However, high-speed video and post-test analysis reveal that basalt experiences greater rates of ablation than Tamdakht. Post-test analysis of emission spectra reveals the presence of volatile species that may explain the discrepancy between model predictions and observed phenomena.

Meteor↗

NASA NTRS1976

Improved impact-resistant boron/aluminum composites for use as turbine engine fan blades

Thin-sheet Charpy and Izod impact tests and standard full-size Charpy impact tests were conducted on unidirectional and angleply composites containing 4, 5.6 and 8 mil boron in 1100, 2024, 5052 and 6061 Al matrices. Impact failure modes of B/Al are proposed to describe the mechanisms involved and to provide insight for maximizing impact resistance. The impact strength of B/Al was significantly increased by proper selection of materials and processing. The use of more ductile matrices and larger diameter boron fibers gave the highest impact strengths by allowing matrix shear deformation and multiple fiber breakage. Pendulum impact test results of improved B/Al were higher than notched titanium and indicate sufficient foreign object damage protection to warrant consideration of B/Al for application to fan blades in aircraft gas turbine engines.

Mcdanels, D. L.↗

NASA NTRS2005

Damage Accumulation in SiC/SiC Composites with 3D Architecture

Matrix cracking in Sic fiber reinforced, melt-infiltrated Sic composites with 3D orthogonal architectures was determined for specimens tested in tension at room temperature. Acoustic emission (AE) was used to monitor the matrix cracking activity and was later confirmed by microscopic examination of specimens that had failed. Exact location of AE demonstrated that initial cracking occurred in the matrix rich regions when a large z-direction fiber bundle was used. For specimens with large z-direction fiber tows, the earliest matrix cracking could occur at half the stress for standard 2D woven composites with similar constituents.

Yun, Hee-Mann↗

NASA NTRS1994

Interlaminar shear test method development for long term durability testing of composites

The high speed civil transport is a commercial aircraft that is expected to carry 300 passengers at Mach 2.4 over a range of more than 6000 nautical miles. With the existing commercial structural material technology (i.e., aluminum) the performance characteristics of the high speed civil transport would not be realized. Therefore there has been a concerted effort in the development of light weight materials capable of withstanding elevated temperatures for long duration. Thermoplastic composite materials are such candidate materials and the understanding of how these materials perform over the long term under harsh environments is essential to safe and effective design. The matrix dominated properties of thermoplastic composites are most affected by both time and temperature. There is currently an effort to perform short term testing to predict long term behavior of in-plane mechanical properties E22 (transverse modulus of elasticity) and G12 (shear modulus). Out-of-plane properties such as E33, G13, and G23 are inherently more difficult to characterize. This is especially true for the out-of-plane shear modulus G23 and hence there is no existing acceptable standard test method. Since G23 is the most matrix dominated property, it is essential that a test method be developed. A shear test methodology is developed to do just that. The test method, called the double notched specimen, along with the previously developed shear gage was tested at room temperature. Mechanical testing confirmed the attributes of the methodology. A finite element parametric study was conducted for specimen optimization. Moire interferometry, a high sensitivity laser optical method, was used for full-field analysis of the specimen. From this work, material parameters will be determined and thus enable the prediction of long term material behavior of laminates subjected to general loading states.

Ifju, Peter G.↗

NASA NTRS2015

A Fully Non-Metallic Gas Turbine Engine Enabled by Additive Manufacturing Part I: System Analysis, Component Identification, Additive Manufacturing, and Testing of Polymer Composites

The research and development activities reported in this publication were carried out under NASA Aeronautics Research Institute (NARI) funded project entitled "A Fully Nonmetallic Gas Turbine Engine Enabled by Additive Manufacturing." The objective of the project was to conduct evaluation of emerging materials and manufacturing technologies that will enable fully nonmetallic gas turbine engines. The results of the activities are described in three part report. The first part of the report contains the data and analysis of engine system trade studies, which were carried out to estimate reduction in engine emissions and fuel burn enabled due to advanced materials and manufacturing processes. A number of key engine components were identified in which advanced materials and additive manufacturing processes would provide the most significant benefits to engine operation. The technical scope of activities included an assessment of the feasibility of using additive manufacturing technologies to fabricate gas turbine engine components from polymer and ceramic matrix composites, which were accomplished by fabricating prototype engine components and testing them in simulated engine operating conditions. The manufacturing process parameters were developed and optimized for polymer and ceramic composites (described in detail in the second and third part of the report). A number of prototype components (inlet guide vane (IGV), acoustic liners, engine access door) were additively manufactured using high temperature polymer materials. Ceramic matrix composite components included turbine nozzle components. In addition, IGVs and acoustic liners were tested in simulated engine conditions in test rigs. The test results are reported and discussed in detail.

acoustic liners↗

NASA NTRS1991

Local delamination in laminates with angle ply matrix cracks. Part 2: Delamination fracture analysis and fatigue characterization

Constant amplitude tension-tension fatigue tests were conducted on AS4/3501-6 graphite/epoxy (02/ theta sub 2/ -(theta sub 2))sub s laminates, where theta was 15, 20, 25, or 30 degrees. Fatigue tests were conducted at a frequency of 5 Hz and an R-ratio of 0.1. Dye penetrant enhanced x-radiography was used to document the onset of matrix cracking in the central -(theta) degree plies, and the subsequent onset of local delaminations in the theta/ -(theta) interface at the intersection of the matrix cracks and the free edge, as a function of the number of fatigue cycles. Two strain energy release rate solutions for local delamination from matrix cracks were derived: one for a local delamination growing from an angle ply matrix crack with a uniform delamination growing from an angle ply matrix crack with a triangular shaped delamination area that extended only partially into the laminate width from the free edge. Plots of G(max) vs. N were generated to assess the accuracy of these G solutions. The influence of residual thermal and moisture stresses on G were also quantified. However, a detailed analysis of the G components and a mixed-mode fatigue failure criterion for this material may be needed to predict the fatigue behavior of these laminates.

Obrien, T. Kevin↗

NASA NTRS1985

Long-life high performance fuel cell program

A multihundred kilowatt Regenerative Fuel Cell for use in a space station is envisioned. Three 0.508 sq ft (471.9 cm) active area multicell stacks were assembled and endurance tested. The long term performance stability of the platinum on carbon catalyst configuration suitability of the lightweight graphite electrolyte reservoir plate, the stability of the free standing butyl bonded potassium titanate matrix structure, and the long life potential of a hybrid polysulfone cell edge frame construction were demonstrated. A 18,000 hour demonstration test of multicell stack to a continuous cyclical load profile was conducted. A total of 12,000 cycles was completed, confirming the ability of the alkaline fuel cell to operate to a load profile simulating Regenerative Fuel Cell operation. An orbiter production hydrogen recirculation pump employed in support of the cyclical load profile test completed 13,000 hours of maintenance free operation. Laboratory endurance tests demonstrated the suitability of the butyl bonded potassium matrix, perforated nickel foil electrode substrates, and carbon ribbed substrate anode for use in the alkaline fuel cell. Corrosion testing of materials at 250 F (121.1 C) in 42% wgt. potassium identified ceria, zirconia, strontium titanate, strontium zirconate and lithium cobaltate as candidate matrix materials.

Martin, R. E.↗

DOE OSTI2022

Cs 3 Bi 2 I 9 -hydroxyapatite composite waste forms for cesium and iodine immobilization

Perovskite-based ceramic composites were developed as potential waste form materials for immobilizing cesium (Cs) and iodine (I) with high waste loadings and chemical durability. The perovskite Cs 3 Bi 2 I 9 has high Cs (22 wt%) and I (58 wt%) content, and thus can be used as a potential host phase to immobilize these critical radionuclides. In this work, the perovskite Cs 3 Bi 2 I 9 phase was synthesized by a cost effective solution-based approach, and was embedded into a highly durable hydroxyapatite matrix by spark plasma sintering to form dense ceramic composite waste forms. The chemical durabilities of the monolithic Cs 3 Bi 2 I 9 and Cs 3 Bi 2 I 9 -hydroxyapatite composite pellets were investigated by static and semi-dynamic leaching tests, respectively. Cs and I are incongruently released from the matrix for both pure Cs 3 Bi 2 I 9 and composite structures. The normalized Cs release rate is faster than that of I, which can be explained by the difference in the strengths between Cs-I and Bi-I bonds as well as the formation of insoluble micrometer-sized BiOI precipitates. The activation energies of elemental releases based on dissolution and diffusion-controlled mechanisms are determined with significantly higher energy barriers for dissolution from the composite versus that of the monolithic Cs 3 Bi 2 I 9 . The ceramic-based composite waste forms exhibit excellent chemical durabilities and waste loadings, commensurate with the state-of-the-art glass-bonded perovskite composites for I and Cs immobilization.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1992

Transverse flexural tests as a tool for assessing damage to PMR-15 composites from isothermal aging in air at elevated temperatures

To date, the effect of thermo-oxidative aging on unidirectional composite mechanical properties has been monitored by the measurement of interlaminar shear strength (ILSS) and either three or four point longitudinal flexural strength (LFS) of the composites being tested. Both results are affected by the fiber-to-matrix bonding, the former being dependent on the shear resistance of the interface and the latter on the degree of load sharing by the fibers through the fiber/matrix interface. Recently, fiber/matrix interfacial bond strengths have been monitored using a transverse flexural strength (TFS) test method. This test method was used to evaluate the effect of fiber surface treatment on the fiber/matrix bond. The interface bonding was varied in these tests using Hercules A-fibers with three-types of surfaces that produce bonds of poor, better, and good quality. The TFS was found not only to be sensitive to the bonding, but also to the aging time of unidirectional A-fiber/PMR-15 composites. This relationship reflects the mechanism by which the PMR-15 degrades during thermal aging.

Bowles, Kenneth J.↗

NASA NTRS1993

Transverse flexural tests as a tool for assessing damage to PMR-15 composites from isothermal aging in air at elevated temperatures

Bowles, Kenneth J.↗

NASA NTRS1986

Electrically conductive, black thermal control coatings for space craft application. II - Silicone matrix formulation

Five black electrically conductive thermal-control coatings have been formulated and tested for application on the Galileo spacecraft. The coatings consisted of organic and inorganic systems applied on titanium and aluminum surfaces. The coatings were tested under simulated space environment conditions. Coated specimens were subjected to thermal radiation and convective and conductive heating from -196 to 538 C. Mechanical, physical, thermal, electrical, and optical characteristics, formulation, mixing, application, surface preparation of substrates, and a method of determining electrical resistance are presented for the silicone matrix formulation designated as GF-580.

Hribar, V. F.↗

NASA NTRS1995

Mechanical Properties of Aerogels

Aerogels are extremely low density solids that are characterized by a high porosity and pore sizes on the order of nanometers. Their low thermal conductivity and sometimes transparent appearance make them desirable for applications such as insulation in cryogenic vessels and between double paned glass in solar architecture. An understanding of the mechanical properties of aerogels is necessary before aerogels can be used in load bearing applications. In the present study, the mechanical behavior of various types of fiber-reinforced silica aerogels was investigated with hardness, compression, tension and shear tests. Particular attention was paid to the effects of processing parameters, testing conditions, storage environment, and age on the aerogels' mechanical response. The results indicate that the addition of fibers to the aerogel matrix generally resulted in softer, weaker materials with smaller elastic moduli. Furthermore, the testing environment significantly affected compression results. Tests in ethanol show an appreciable amount of scatter, and are not consistent with results for tests in air. In fact, the compression specimens appeared to crack and begin to dissolve upon exposure to the ethanol solution. This is consistent with the inherent hydrophobic nature of these aerogels. In addition, the aging process affected the aerogels' mechanical behavior by increasing their compressive strength and elastic moduli while decreasing their strain at fracture. However, desiccation of the specimens did not appreciably affect the mechanical properties, even though it reduced the aerogel density by removing trapped moisture. Finally, tension and shear test results indicate that the shear strength of the aerogels exceeds the tensile strength. This is consistent with the response of brittle materials. Future work should concentrate on mechanical testing at cryogenic temperatures, and should involve more extensive tensile tests. Moreover, before the mechanical response of reinforced aerogels can be fully understood, more tests of unreinforced aerogels are necessary. Unreinforced aerogels are of particular use because their birefringent nature allows for visual determination of stress fields during mechanical testing. The success of any future tests depends on the availability of a large supply of quality specimens with well-documented preparation and storage histories.

Parmenter, Kelly E.↗

NASA NTRS1992

International SAMPE Symposium and Exhibition, 37th, Anaheim, CA, Mar. 9-12, 1992, Proceedings

The present conference discusses the industrial and transportation markets for advanced composites, novel NASA and military applications of advanced materials, composite space structures, sandwich structures, composite tooling and processing, advanced epoxy compositions, composites repair, commercial applications of advanced resins, metal-matrix composites, adhesive compositions, ultrahigh-temperature composites, failure analyses, testing methods for composites, and bismaleimides and polyimides. Also discussed are composite structures design, innovations in composite reinforcement, nonautoclave-processed composites, molecular composites, design and manufacture processes with thermoplastics, automation in manufacturing, technologies for large component fabrication, damage-limitation design practices, thermoplastic-matrix composites, industrial applications of composites, and process controls in composites manufacturing.

Grimes, Glenn C.↗

NASA NTRS1997

Alternative Processing Method Leads to Stronger Sapphire-Reinforced Alumina Composites

The development of advanced engines for aerospace applications depends on the availability of strong, tough materials that can withstand increasingly higher temperatures under oxidizing conditions. The need for such materials led to the study of an oxide-based composite composed of an alumina matrix reinforced with zirconia-coated sapphire fibers. Because the nonbrittle behavior of this system depends on the interface and its ability to prevent fiber-to-matrix bonding and reduce interfacial shear stress, the microstructure of the zirconia must be carefully controlled during both coating application and composite processing. When it was both porous and unstabilized, zirconia (which does not react easily with alumina) was found to be the most effective material tested in reducing interfacial shear strength between the fiber and matrix.

Jaskowiak, Martha H.↗

NASA NTRS2002

Thermal Cyclic Behavior of Thermal and Environmental Barrier Coatings Investigated Under High-Heat-Flux Conditions

Environmental barrier coatings (EBC's) have been developed to protect silicon-carbide- (SiC) based ceramic components in gas turbine engines from high-temperature environmental attack. With continuously increasing demands for significantly higher engine operating temperature, future EBC systems must be designed for both thermal and environmental protection of the engine components in combustion gases. In particular, the thermal barrier functions of EBC's become a necessity for reducing the engine-component thermal loads and chemical reaction rates, thus maintaining the required mechanical properties and durability of these components. Advances in the development of thermal and environmental barrier coatings (TBC's and EBC's, respectively) will directly impact the successful use of ceramic components in advanced engines. To develop high-performance coating systems, researchers must establish advanced test approaches. In this study, a laser high-heat-flux technique was employed to investigate the thermal cyclic behavior of TBC's and EBC's on SiC-reinforced SiC ceramic matrix composite substrates (SiC/SiC) under high thermal gradient and thermal cycling conditions. Because the laser heat flux test approach can monitor the coating's real-time thermal conductivity variations at high temperature, the coating thermal insulation performance, sintering, and delamination can all be obtained during thermal cycling tests. Plasma-sprayed yttria-stabilized zirconia (ZrO2-8 wt% Y2O3) thermal barrier and barium strontium aluminosilicate-based environmental barrier coatings (BSAS/BSAS+mullite/Si) on SiC/SiC ceramic matrix composites were investigated in this study. These coatings were laser tested in air under thermal gradients (the surface and interface temperatures were approximately 1482 and 1300 C, respectively). Some coating specimens were also subject to alternating furnace cycling (in a 90-percent water vapor environment at 1300 C) and laser thermal gradient cycling tests (in air), to investigate the water vapor effect. All cyclic tests were conducted using a 60-min hot-time temperature.

Zhu, Dongming↗

NASA NTRS2003

Damage Accumulation in SiC/SiC Composites with 3D Architectures

The formation and propagation of multiple matrix cracks in relatively dense ceramic matrix composites when subjected to increasing tensile stress is necessary for high strength and tough composites. However, the occurrence of matrix cracks at low stresses may limit the usefulness of some non-oxide composite systems when subjected to oxidizing environments for long times at stresses sufficient to cause matrix cracking. For SiC fiber-reinforced composites with two-dimensional woven architectures and chemically vapor infiltrated (CVI) SiC matrix and melt-infiltrated (MI) Si/SiC matrix composites, the matrix cracking behavior has been fairly well characterized for different fiber-types and woven architectures. It was found that the occurrence, degree, and growth of matrix cracks depends on the material properties of the composite constituents as well as other physical properties of the composite or architecture, e.g., matrix porosity and size of the fiber bundle. In this study, matrix cracking in SiC fiber reinforced, melt-infiltrated SiC composites with a 3D orthogonal architecture was determined for specimens tested in tension at room temperature. Acoustic emission (AE) was used to monitor the matrix cracking activity, which was later confirmed by microscopic examination of specimens that had failed. The determination of the exact location of AE demonstrated that initial cracking occurred in the matrix rich regions when a large z-direction fiber bundle was used. For specimens with large z-direction fiber tows, the earliest matrix cracking could occur at half the stress for standard 2D woven composites with similar constituents. Damage accumulation in 3D architecture composites will be compared to damage accumulation in 2D architecture composites and discussed with respect to modeling composite stress-strain behavior and use of these composites at elevated temperatures.

Morscher, Gregory N.↗

NASA NTRS1974

Effect of rolling on the high temperature tensile and stress-rupture properties of tungsten fiber-superalloy composites

An investigation was conducted to determine the effects of mechanical working on the 1093 C tensile and stress-rupture strength of tungsten alloy/superalloy composites. Hot pressed composites containing either conventional tungsten lamp filament wire or tungsten-1% ThO2 wire and a nickel base alloy matrix were hot rolled at 1093 C. The hot pressed and rolled composite specimens were then tested in tension and stress-rupture at 1093 C. Rolling decreased the degree of fiber-matrix reaction as a function of time of exposure at 1093 C. The stress-rupture properties of the rolled composites were superior to hot pressed composites containing equivalent diameter fibers. Rolling did not appreciably affect the 1093 C ultimate tensile strength of the composites.

Petrasek, D. W.↗