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NASA NTRS1993

Double Cantilever Beam and End Notched Flexure Fracture Toughness Testing of Two Composite Materials

Two different unidirectional composite materials were provided by NASA Langley Research Center and tested by the Composite Materials Research Group within the Department of Mechanical Engineering at the University of Wyoming. Double cantilever beam and end notched flexure tests were performed to measure the mode I (crack opening) and mode II (sliding or shear) interlaminar fracture toughness of the two materials. The two composites consisted of IM7 carbon fiber combined with either RP46 resin toughened with special formulation of LaRC IA resin, known as JJS1356; or PES chain extended thermoplastic resin known as JJS1361. Double Cantilever Beam Specimen Configuration and Test Methods As received from NASA, the test specimens were nominally 0.5 inch wide, 6 inches long, and 0.2 inch thick. A 1 inch long Kapton insert at the midplane of one end of the specimen (placed during laminate fabrication) facilitated crack initiation and extension. It was noted that the specimens provided were smaller than the nominal 1.5 inch wide, 9.0 inch long configuration specified. Similarly, the Kapton inserts were of greater length than those in the present specimens. Hence, the data below should not be compared directly to those generated with the referenced methods. No preconditioning was performed on the specimens prior to testing. In general, the methodology was used for the present work. Crack opening loads were introduced to the specimens via piano hinges attached to the main specimen faces at a single end of each specimen. Hinges were bolted to the specimens using the technique presented. The cracks were extended a small distance from the end of the Kapton insert prior to testing. Just before precracking, the sides of the specimens were coated with water-soluble typewriter correction fluid to aid in crack visualization. Scribe marks were then made in the coating at half-inch intervals.

Kessler, Jeff A.↗

NASA NTRS1999

Composite Materials Research and Technology at NASA/MSFC

The utilization of composite materials in the Space Shuttle and Advanced Space Transportation Programs is reviewed. Topics include goals and challenges, descriptions of multi-generational launch vehicles, and an overview of composite materials research and technologies that support program objectives. A brief discussion of planned composite materials research and technology concludes the presentation.

Ledbetter, Frank E., III↗

NASA NTRS1988

Composite Materials

Langley Research Center researchers invented an advanced polymer, a chemical compound formed by uniting many small molecules to create a complex molecule with different chemical properties. The material is a thermoplastic polyimide that resists solvents. Other polymers of this generic type are soluble in solvents, thus cannot be used where solvents are present. High Technology Services (HTS), Inc. licensed technology and is engaged in development and manufacture of high performance plastics, resins and composite materials. Techimer Materials Division is using technology for composite matrix resins that offer heat resistance and protection from radiation, electrical and chemical degradation. Applications of new polymer include molding resins, adhesives and matrix resins for fiber reinforced composites.

Source record↗

NASA NTRS2003

Facesheet Delamination of Composite Sandwich Materials at Cryogenic Temperatures

The next generation of space transportation vehicles will require advances in lightweight structural materials and related design concepts to meet the increased demands on performance. One potential source for significant structural weight reduction is the replacement of traditional metallic cryogenic fuel tanks with new designs for polymeric matrix composite tanks. These new tank designs may take the form of thin-walled sandwich constructed with lightweight core and composite facesheets. Life-time durability requirements imply the materials must safely carry pressure loads, external structural loads, resist leakage and operate over an extremely wide temperature range. Aside from catastrophic events like tank wall penetration, one of the most likely scenarios for failure of a tank wall of sandwich construction is the permeation of cryogenic fluid into the sandwich core and the subsequent delamination of the sandwich facesheet due to the build-up of excessive internal pressure. The research presented in this paper was undertaken to help understand this specific problem of core to facesheet delamination in cryogenic environments and relate this data to basic mechanical properties. The experimental results presented herein provide data on the strain energy release rate (toughness) of the interface between the facesheet and the core of a composite sandwich subjected to simulated internal pressure. A unique test apparatus and associated test methods are described and the results are presented to highlight the effects of cryogenic temperature on the measured material properties.

Gates, Thomas S.↗

NASA NTRS2004

The Abundance and Isotopic Composition of Hg in Extraterrestrial Materials

During the past three year grant period we made excellent progress in our study of the abundances and isotopic compositions of Hg and other volatile trace elements in extraterrestrial materials. As part of my startup package I received funds to construct a state-of-the-art experimental facility to study gas-solid reaction kinetics. Much of our effort was spent developing the methodology to measure the abundance and isotopic composition of Hg at ultratrace levels in solid materials. In our first study, the abundance and isotopic composition of Hg was determined in bulk samples of the Murchison (CM) and Allende (CV) carbonaceous chondrites. We have continued our study of mercury in primitive meteorites and expanded the suite of meteorites to include other members of the CM and CV chondrite group as well as CI and CO chondrites. Samples of the CI chondrite Orgueil, the CM chondrites Murray, Nogoya, and Cold Bokkeveld, the CO chondrites Kainsaz, Omans, and Isna, and the CV chondrites Vigarano, Mokoia, and Grosnaja were tested. We have developed a thermal analysis ICP-MS technique and applied it to the study of a suite of thermally labile elements (Zn, As, Se, Cd, In, Sn, Sb, Te, Hg, Au, Tl, Pb, and Bi) in geologic materials as well.

Lauretta, D. S.↗

NASA NTRS2005

Fiber Reinforced Composite Materials Used for Tankage

The Nonmetallic Materials and Processes Group is presently working on several projects to optimize cost while providing effect materials for the space program. One factor that must be considered is that these materials must meet certain weight requirements. Composites contribute greatly to this effort. Through the use of composites the cost of launching payloads into orbit will be reduced to one-tenth of the current cost. This research project involved composites used for aluminum pressure vessels. These tanks are used to store cryogenic liquids during flight. The tanks need some type of reinforcement. Steel was considered, but added too much weight. As a result, fiber was chosen. Presently, only carbon fibers with epoxy resin are wrapped around the vessels as a primary source of reinforcement. Carbon fibers are lightweight, yet high strength. The carbon fibers are wet wound onto the pressure vessels. This was done using the ENTEC Filament Winding Machine. It was thought that an additional layer of fiber would aid in reinforcement as well as containment and impact reduction. Kevlar was selected because it is light weight, but five times stronger that steel. This is the same fiber that is used to make bullet-proof vests trampolines, and tennis rackets.

Cunningham, Christy↗

NASA NTRS2009

Characterization of Triaxial Braided Composite Material Properties for Impact Simulation

The reliability of impact simulations for aircraft components made with triaxial braided carbon fiber composites is currently limited by inadequate material property data and lack of validated material models for analysis. Improvements to standard quasi-static test methods are needed to account for the large unit cell size and localized damage within the unit cell. The deformation and damage of a triaxial braided composite material was examined using standard quasi-static in-plane tension, compression, and shear tests. Some modifications to standard test specimen geometries are suggested, and methods for measuring the local strain at the onset of failure within the braid unit cell are presented. Deformation and damage at higher strain rates is examined using ballistic impact tests on 61- by 61- by 3.2-mm (24- by 24- by 0.125-in.) composite panels. Digital image correlation techniques were used to examine full-field deformation and damage during both quasi-static and impact tests. An impact analysis method is presented that utilizes both local and global deformation and failure information from the quasi-static tests as input for impact simulations. Improvements that are needed in test and analysis methods for better predictive capability are examined.

Roberts, Gary D.↗

NASA NTRS2003

Flexible Composite-Material Pressure Vessel

A proposed lightweight pressure vessel would be made of a composite of high-tenacity continuous fibers and a flexible matrix material. The flexibility of this pressure vessel would render it (1) compactly stowable for transport and (2) more able to withstand impacts, relative to lightweight pressure vessels made of rigid composite materials. The vessel would be designed as a structural shell wherein the fibers would be predominantly bias-oriented, the orientations being optimized to make the fibers bear the tensile loads in the structure. Such efficient use of tension-bearing fibers would minimize or eliminate the need for stitching and fill (weft) fibers for strength. The vessel could be fabricated by techniques adapted from filament winding of prior composite-material vessels, perhaps in conjunction with the use of dry film adhesives. In addition to the high-bias main-body substructure described above, the vessel would include a low-bias end substructure to complete coverage and react peak loads. Axial elements would be overlaid to contain damage and to control fiber orientation around side openings. Fiber ring structures would be used as interfaces for connection to ancillary hardware.

Brown, Glen↗

NASA NTRS2012

Investigation of Effects of Material Architecture on the Elastic Response of a Woven Ceramic Matrix Composite

To develop methods for quantifying the effects of the microstructural variations of woven ceramic matrix composites on the effective properties and response of the material, a research program has been undertaken which is described in this paper. In order to characterize and quantify the variations in the microstructure of a five harness satin weave, CVI SiC/SiC, composite material, specimens were serially sectioned and polished to capture images that detailed the fiber tows, matrix, and porosity. Open source quantitative image analysis tools were then used to isolate the constituents and collect relevant statistics such as within ply tow spacing. This information was then used to build two dimensional finite element models that approximated the observed section geometry. With the aid of geometrical models generated by the microstructural characterization process, finite element models were generated and analyses were performed to quantify the effects of the microstructure and its variation on the effective stiffness and areas of stress concentration of the material. The results indicated that the geometry and distribution of the porosity appear to have significant effects on the through-thickness modulus. Similarly, stress concentrations on the outer surface of the composite appear to correlate to regions where the transverse tows are separated by a critical amount.

Goldberg, Robert K.↗

DOE OSTI2021

Evaluating Effects of Shear Processing on 2D Crystalline Materials in 3D Metal Matrices: Atomistic Understanding of High Shear Deformation of Copper Graphene Composites

Composites made of copper and graphene demonstrate high strength, lubricity and enhanced electrical and thermal conductivity compared pure copper. However, manufacturing these composites at bulk volumes for industrial applications has been a big challenge. Shear deformation assisted processing is an effective method for manufacturing materials such as copper-graphene composites demonstrating ultra-fine grain structures and compositional homogeneity. Nevertheless, microstructural evolution of the composites and their property development under such conditions is not clearly understood currently. To rectify this gap in literature, high strain shear deformation of copper coated graphene foils was performed using a tribometer pin in this study. Changes in microstructure of the composite as well as the constituent components under shear deformation was correlated to process conditions. A sharp increase in the coefficient of friction attributed to rupture and smearing of graphene layer into copper substrate was observed during the shear processing. The coefficient of friction of the sheared copper/graphene composite was lower than that of pure copper, suggesting that partially worn graphene is effectively lubricious at the macroscale. A multimodal characterization of the processed region further revealed a shear deformation-induced ultrafine two-phase grain-structure consisting of copper and graphitic domains. Shear deformation reduced the copper grain size from around 50 – 100 µm to ~200 nm on an average and ~2 – 5 nm in some locations. The semicrystalline graphene films were observed to fracture into 10 – 50 µm size flakes. Oxygen enrichment was observed in the processed region. Finally, graphitic domain were identified for the first time in the copper matrix and not just at the grain boundaries providing evidence for a metastable composite microstructure as a result of solid phase processing at room temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2023

High-Throughput Electric-Field-Assisted Sintering and Characterization Techniques for Materials Discovery

Despite improvements in computing and modeling capabilities, the performance of new materials, particularly those which deviate greatly in composition from well-studied materials (e.g., high-entropy alloys), can be difficult to simulate given the lack of available experimental property data. While some modeling techniques may attempt to predict the properties of these exotic materials, most are forced to make extrapolations from more traditional materials. To fulfill the need for accelerated material synthesis and property measurement, a high-throughput methodology has been developed. Utilizing electric-field-assisted sintering (EFAS), also known as spark plasma sintering (SPS), equipped with custom tooling, samples of differing alloy compositions can be produced simultaneously as a single alloy array. Several arrays have been produced with compositions spanning the Co-Cr-Fe-Mn-Ni alloy family, including many high-entropy alloys, while the novel array geometry has enabled the samples to be polished and characterized in parallel, using X-ray diffraction, scanning-electron microscopy, and laser-based thermal diffusivity measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Solid Phase Gradient Alloying Method via ShAPE

Alloying has been used to confer desirable properties to various metallic systems since the bronze age. For example, Ni, Mn, and Cr are alloyed into an Fe matrix to make steel, which has improved strength and corrosion resistance (as displayed in Fig. 1). In addition to the type of alloying elements, the amount of alloying elements added into a matrix is also very critical for a material’s mechanical property, physical property, machinability, and cost. Conventionally, new alloys are discovered by combining alloy precursors and elemental constituents into a mixture and melting them together. The solidified product or ingot represents a usually non-homogeneous combination of the chemistry with a microstructure dictated by the physics of solidification. It is time and energy intensive to optimize the alloying amounts via the casting process and hence, economically not conducive to rapid alloy discovery. In addition, the cast microstructure seen in the as-cast ingot is often not the ideal, nor even desired structure for optimized performance. Cast materials often need further processing such as homogenization, annealing, and deformation work put in through rolling, forging, extruding, etc. to have favorable microstructures and properties. A faster method to discover new alloy combinations and evaluate them in their worked or processed form is needed. Recently, Laser Engineered Net Shaping was applied to fabricate gradient compositional material for alloy designing. However, the mechanical properties of this gradient alloy were poor due to the existence of impurities, oxidation and cracks that are inherent in the melt-solidification process. Because of these limitations, we propose to use a solid-phase process (ShAPE) to create bulk materials (extrudates) that vary in composition from one end of the extruded solid to the other. Various manufacturing methods for alloy design including conventional casting method, laser based combinatorial method and current solid phase gradient alloying method are displayed and compared in Fig. 2. ShAPE machine and a schematic of ShAPE process are displayed in Fig. 3. Starting material is processed by a rotating and plunging die to form an extrudate. We are proposing through this methodology to invent a new, bulk-scale combinatorial technique. With this novel technique, alloying element can be dissolved into the matrix with a continued gradient without bulk melting. Formation of inter-metallics and defects originating from melt processing can be avoided. In addition, the ShAPE process creates the mixed alloy chemistry, and meanwhile subjects the material to severe plastic strain, which induces the favorable “worked” microstructure. Products from the ShAPE process can be tested in hardness directly providing a path to rapid evaluation of mechanical properties. The ability to create graded structures using friction stir processing (FSP) has been demonstrated, however using the ShAPE process we believe will lead to much faster and higher fidelity results. When combined with high throughput screening methods of physical, mechanical and microstructural property characterization, efficiency and accuracy of alloy design can be significantly improved.

36 MATERIALS SCIENCE↗

DOE OSTI2022

The oxygen stable isotope composition of CRM 125-A UO 2 standard reference material

While there is a clear need for standardized reference materials for analytical calibrations and for inter-laboratory comparisons, there are not currently any for the oxygen stable isotopic composition of uranium oxides. In this paper we summarize the results from four laboratories by seven different methods of oxygen stable isotope analyses using fluorination techniques of CRM 125-A UO 2 Standard Reference Material. We synthesize these data and methods to arrive at a consensus oxygen stable isotope composition for CRM 125-A $δ$ 18 O = -9.63‰ (±0.29‰) VSMOW. We discuss methodological differences between analytical approaches, including furnace vs laser heating, fluorination using BrF 5 or ClF 3 , as well as calibration strategies. We highlight the potential effects of calibration scale compression from single-point calibrations using reference material with $δ$ 18 O values having a large relative difference from the sample being analyzed. We demonstrate how calibration scale compression can yield differences in calibrated $δ$ 18 O values up to ~2‰ for samples with ~20‰ difference from a single reference material, if the calibration slope of different analytical systems differs by 0.1. In conclusion, we suggest the use of liquid water calibration standards sealed in silver capillary tubes for multi-point calibrations of fluorination analysis systems.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2023

Exploring pressure-dependent inelastic deformation and failure in bonded granular composites: An energetic materials perspective

In polymer-filled granular composites, damage may develop in mechanical loading prior to material failure. Damage mechanisms such as microcracking or plastic deformation in the binder phase can substantially alter the material’s mesostructure. For energetic materials, such as solid propellants and plastic bonded explosives, these mesostructural changes can have far reaching effects including degraded mechanical properties, potentially increased sensitivity to further insults, and changes in expected performance. Unfortunately, predicting damage is nontrivial due to the complex nature of these composites and the entangled interactions between inelastic mechanisms. In this work, we assess the current literature of experimental knowledge, focusing on the pressure-dependent shear response, and propose a simple simulation framework of bonded particles to study four limiting-case material formulations at both meso- and macro-scales. Further, to construct the four cases, we systematically vary the relative interfacial strength between the polymer binder and granular filler phase and also vary the polymer’s glass transition temperature relative to operating temperature which determines how much the binder can plastically deform. These simulations identify key trends in global mechanical response, such as the emergence of strain hardening or softening regimes with increasing pressure which qualitatively resemble experimental results. By quantifying the activation of different inelastic mechanisms, such as bonds breaking and plastically straining, we identify when each mechanism becomes relevant and provide insight into potential origins for changes in mechanical responses. The locations of broken bonds are also used to define larger, mesoscopic cracks to test various metrics of damage. We primarily focus on triaxial compression, but also test the opposite case of triaxial extension to highlight the impact of Lode angle on mechanical behavior.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Effects of alloy composition in alleviating embrittlement problems associated with the tantalum alloy T-111

The causes of aging embrittlement in T-111 (Ta-8W-2Hf) and the effect of alloy modification were investigated. Results show that T-111 possesses a critical combination of tungsten and hafnium that leads to loss in ductility at -196 C after aging near 1040 C. It was found that this occurs because tungsten enhances hafnium segregation to grain boundaries, which also leads to increased susceptibility to hydrogen embrittlement. Aging embrittlement was not observed in tantalum alloys with reduced tungsten or hafnium contents; most of the alloys studied have lower strengths than T-111 and exhibit susceptibility to hydrogen embrittlement.

Stephens, J. R.↗

NASA NTRS1977

Effects of alloy composition in alleviating embrittlement problems associated with the tantalum alloy T-111

The causes of aging embrittlement in T-111 (Ta-8W-2Hf) and the effects of alloy modification were investigated. Results showed that T-111 contains a critical combination of tungsten and hafnium that leads to loss of ductility at -196 C after aging near 1040 C. This appears to occur because tungsten enhances hafnium segregation to grain boundaries and this also leads to increased susceptibility to hydrogen embrittlement. Aging embrittlement was not observed in tantalum alloys with reduced tungsten or hafnium contents; however, most of the alloys studied have lower strengths than T-111 and exhibit susceptibility to hydrogen embrittlement.

Stephens, J. R.↗

NASA NTRS1996

Effects of Material Degradation on the Structural Integrity of Composite Materials: Experimental Investigation and Modeling of High Temperature Degradation Mechanisms

It has previously been demonstrated that simple coupled reaction-diffusion models can approximate the aging behavior of PMR-15 resin subjected to different oxidative environments. Based on empirically observed phenomena, a model coupling chemical reactions, both thermal and oxidative, with diffusion of oxygen into the material bulk should allow simulation of the aging process. Through preliminary modeling techniques such as this it has become apparent that accurate analytical models cannot be created until the phenomena which cause the aging of these materials are quantified. An experimental program is currently underway to quantify all of the reaction/diffusion related mechanisms involved. The following contains a summary of the experimental data which has been collected through thermogravimetric analyses of neat PMR-15 resin, along with analytical predictions from models based on the empirical data. Thermogravimetric analyses were carried out in a number of different environments - nitrogen, air and oxygen. The nitrogen provides data for the purely thermal degradation mechanisms while those in air provide data for the coupled oxidative-thermal process. The intent here is to effectively subtract the nitrogen atmosphere data (assumed to represent only thermal reactions) from the air and oxygen atmosphere data to back-figure the purely oxidative reactions. Once purely oxidative (concentration dependent) reactions have been quantified it should then be possible to quantify the diffusion of oxygen into the material bulk.

Cunningham, Ronan A.↗

NASA NTRSDate not supplied

Composition-property correlations in NiTi-based shape memory alloys from the first principles

Development of shape memory alloys (SMA) has been traditionally accomplished by means of extensive empirical efforts, with a very limited support from phenomenological models and related tools. We present a theoretical framework based on the Hamiltonian formalism, which connects important thermodynamic properties directly to the relative energies (the eigenvalues of the Hamiltonian), computed from the first principles using density functional theory. The estimates based on this formalism allow to establish correlations between composition and physical properties, such as relative energies, phase transition temperatures, hysteresis, thermal expansion, and other thermodynamic information. Importantly, estimates and correlations not only provide a fast answer, but also elucidate underpinning of thermodynamic features in terms of the electronic structure. Using this framework, we consider phase transformations and correlations between the selected properties and composition in the NiTi-based ternary and multicomponent shape memory alloys. Our theoretical guidance facilitates design and development of future alloys.

shape memory alloys↗