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DOE OSTI2022

Unusual electronic transport in (1 - x )Cu 2 Se-( x )CuInSe 2 hierarchical composites

The ability to control the relative density of electronic point defects as well as their energy distribution in semiconductors could afford a systematic modulation of their electronic, optical, and optoelectronic properties. Using a model binary hybrid system Cu 2 Se–CuInSe 2 , we have investigated the correlation between phase composition, microstructure, and electronic transport behavior in the synthesized composites. We found that both Cu 2 Se and CuInSe 2 phases coexist at multiple length scales, ranging from sub-ten nanometer to several micrometers, leading to the formation of a hybrid hierarchical microstructure. Astonishingly, the electronic phase diagram of the (1 - x)Cu 2 Se–(x)CuInSe 2 (15% ≤ x ≤ 100%) hierarchical composites remarkably deviates from the trend normally expected for composites between a heavily doped semiconductor (Cu 2 Se) and a poorly conducting phase (CuInSe 2 ). A sudden 3-fold increase in the electrical conductivity and carrier concentration along with a marginal increase in the carrier mobility is observed for composites at the vicinity of equimolar composition (48% ≤ x ≤ 52%). The carrier concentration increases from ~1.5 × 10 20 cm -3 for the composites with x ≤ 45% to 5.0 × 10 20 cm -3 for x = 50%, and remains constant at 4.5 × 10 20 cm -3 with x value in the range of 52% < x ≤ 90%, then quickly drops to 8 × 10 18 cm -3 for pristine CuInSe 2 phase (x = 100%). The atypical electronic behavior was rationalized in the light of the formation of an inter-band (IB) within the band gap, which arises from the hybridization of native electronic point defects from both Cu 2 Se and CuInSe 2 phases in the resulting hierarchical composites. The result points to a new strategy to modulate the electronic structure of semiconductor composites to maximize interaction and coupling between two fundamentally contrasting properties enabling access to electronic hybrid systems with potential applications as interactive and stimuli-responsive multifunctional materials.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Bamboo Bio-composite Truck/Trailer Decking

Bamboo is one of the fastest growing plants in the world. Massively productive, bamboo will maintain that productivity with limited inputs and minimal management resulting in predictable volume and operating margins and with low overhead. The goal of this project was to develop a bamboo bio-composite trailer decking product that replaces apitong, is lighter weight, stronger and luminescent. The collaboration partners, Fontaine, Resource Fiber and IACMI, worked closely to develop the bamboo bio-composite decking to Fontaine Trailer’s (end-user) specifications. The various technological objectives were (a) To conduct a comprehensive Design of Experiments study for bamboo composites to understand the structure-property relationships for different resin composites and bamboo forms (strips, woven, bulk etc); (b) To establish the nail pull out characteristics of trailer deck geometry bamboo composite form. The nail pull out is a critical test in trailer decks; (c) To design, process and prototype select number of trailer decking planks for Fontaine evaluation; and (d) To conduct life cycle analysis to conduct energy calculations from the various conversion steps of the bamboo from crop to product. The project meets DOE/IACMI metrics of reduced embodied energy, lightweighting and lowering the cost of the end product. It also offers a green solution to a value-added application, i.e. trailer decking. The development goals and benefits of bamboo composite decking included: A. Decreased weight when compared to Apitong and Gen 1, thereby reducing operating costs and petroleum usage due to increased miles per gallon. B. Flexibility to allow camber design into trailers. C. Luminescence to increase safety during low light and dark conditions. D. Composite material to maximize use of bamboo bio-composites as substitute for petroleum-based composites. E. Embedded layer(s) of conditioned bamboo for added strength and stability. F. Improved safety over Apitong by temporary cargo indentation in planks for better stability. G. Cradle-to-cradle design so end-of-life becomes beginning-of-life for other products. Resource Fiber’s bamboo biocomposite trailer decking passed nail pullout tests as compared to apitong (incumbent), was lighter weight than apitong, and used less embodied energy particularly when bamboo is sourced domestically. The planks were optimized in the lab setting to the extent possible and successfully installed on the trailer at Fontaine for field testing. Despite the process not being fully optimized due to through-heat and tooling limitations within the budget constraints, the prototype decking withstood 400 cycles of reverse fatigue loading of a 107,000 lb Caterpillar 349F which was extreme conditions of field testing by Fontaine Trailer. Resource Fiber plans to outsource production of a next round of planks with a commercial pultrusion processor, then to do a re-test with Fontaine Trailers. Tooling specific to the part is required. Long-term commercial plans are to continue outsourcing production while supplying bamboo fiber and mats. Commercial markets include heavy haul trailers, military trailers, and decking for marine, industrial and residential use.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Thermogravimetric Analysis (TGA) for Carbon Fiber and Glass Fiber Epoxy Composites and their Constituents

In this work, thermogravimetric analysis (TGA) was performed on samples of a carbon fiber epoxy composite, a glass fiber epoxy composite, and a mixed carbon fiber/glass fiber epoxy composite, as well on each constituent material (polymer epoxy, carbon fibers and glass fibers). TGA was conducted for heating rates from 1-20 C/min with purified purge gases of nitrogen and dry air. For the fiberglass composite, we find that ~70% of the material remains after heating in air to 1200 C. For the carbon fiber epoxy composite, we observe greater mass loss as the carbon fibers can oxidize, leaving little material by the end of the test. The mixed composite, which has a 2:1 ratio of glass fibers to carbon fibers, experienced a total mass loss between the two other composites. By determining the relationship between the thermal decomposition of a composite material and its constituent materials, we can predict the fire behavior of novel composites during the material design phase.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Technical Considerations on MURR Control Blade Design Change and Testing using a New Metal Matrix Composite

The University of Missouri Research Reactor (MURR) is one of six research reactors, including a critical facility, that are pursuing conversion as part of a collaboration with the U.S. Department of Energy National Nuclear Security Administration Material Management and Minimization Office of Reactor Conversion and Uranium Supply, under the U.S. High Performance Research Reactors (USHPRR) conversion project. Five of the six USHPRR are planned to convert from highly enriched uranium (HEU) fuel using a low-enriched uranium (LEU) high assay monolithic alloy of uranium-10 wt% molybdenum (U-10Mo). As part of the conversion safety analysis, it is necessary to demonstrate the safety performance of the proposed core fueled with LEU as compared to the current HEU cores. The MURR reactor is planning to switch to a new control blade design that uses a metal matrix composite of boron carbide (B 4 C) and aluminum as the absorber in place of Boral®. Since MURR is expected to adopt the new metal matrix composite control blade design prior to conversion, the impact of the new blade design on the neutronics characteristics of the MURR cores for conversion are analyzed in this work through updates to incorporate the changes to the blade design in conversion models as they directly impact the LEU conversion safety analysis. The quantitative comparison shows that the neutronics and thermal hydraulic behavior of one metal matrix composite blade replacing a Boral blade is comparable for the two example MURR LEU and HEU cores states considered. Geometrical changes in the metal matrix composite blade design, combined with a 4% increase in areal boron density, showed local heating effects up to 20% higher than the Boral design. As expected, the metal matrix composite showed slightly lower heat depositions and absorber region temperatures for the LEU cases compared to HEU. Although this analysis was comparative for a single blade, maximum control blade temperatures for both Boral, metal matrix composite, and HEU/LEU remained below 100 °C, though additional analysis at a core level could differ. A qualitative irradiation behavior assessment concludes that the mechanisms that may drive swelling and blistering in the current Boral design are eased by the adoption of the metal matrix composite design. The work concludes that the two blade designs are essentially equivalent with regards to neutronics, thermal hydraulics, and expected material behavior under irradiation. However, due to the geometrical changes to the blades including redesigned and thinner cladding, new testing and increased surveillance for distortion and swelling are recommended to confirm the performance of the metal matrix composite control blade design. Where testing is completed prior to conversion, the only anticipated impacts on conversion to LEU U-10Mo fuel would be the need for models and safety analysis incorporating the metal matrix composite control blades.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

Characterization of Mechanical Performance of Composites Fabricated Using Innovative Carbon Fiber Wet Laid Process

Recent innovation in production of optimized nonwoven wet laid (WL) carbon fiber (CF) mats raised the question of optimal translation of the performance and isotropy into composites formed through these dry preforms. This work explores the mechanical behavior of composites produced from WL-CF mats in conjunction with the microstructure predicted through Object Oriented Finite Element Analysis (OOF). The mats used for the composites were prepared in two dispersion regimes using 25.4 mm long CF. The mixing regimes discussed in the author’s previous work, are identified as Method 1 for the traditional processing regime and Method 2 for the innovative regime that provided optimal nonwoven WL-CF mats. Composite panels from Method 2 mats showed a normalized tensile strength increase of 52% over those from Method 1 panels. Reproducibility analysis of composites made from Method 2 mats demonstrated a standard deviation of 2% in fiber weight content, 2% in tensile modulus and 9% in tensile strength, while composites made from Method 1 mats demonstrated a standard deviation of 5% in fiber weight content, 5% in tensile modulus and 17% in tensile strength. Systematic study of the microstructure and its analysis through OOF confirmed the isotropy translation of mats produced through method 2 to the composites. This study validated the hypothesis that optimal nonwoven mats lead to a well-balanced composite with optimal performance and that non-optimal nonwoven mats do not pack into a well-balanced composite.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Mechanical Properties of High-Temperature Fiber-Reinforced Thermoset Composites with Plain Weave and Unidirectional Carbon Fiber Fillers

Fiber-reinforced thermoset composites are a class of materials that address the arising needs from the aerospace and hypersonic industries for high specific strength, temperature-resistant structural materials. Among the high-temperature resistant thermoset categories, phenolic triazine (PT) cyanate esters stand out thanks to their inherent high degradation temperature, glass transition temperature, and mechanical strength. Despite the outstanding properties of these thermosets, the performance of carbon fiber composites using PT cyanate esters as matrices has not been thoroughly characterized. This work evaluated PT and carbon fiber composites’ compressive properties and failure mechanisms with different fiber arrangements. A PT resin with both plain weave (PW) and non-crimped unidirectional (UD) carbon fiber mats was analyzed in this research. Highly loaded thermoset composites were obtained using process temperatures not exceeding 260 °C, and the composites proved to retain compressive strength at temperatures beyond 300 °C. Compressive testing revealed that PT composites retained compressive strength values of 50.4% of room temperature for UD composites and 61.4% for PW composites. Post-compressive failure observations of the gage section revealed that the mechanisms for failure evolved with temperature from brittle, delamination-dominant failure to shear-like failure promoted by the plastic failure of the matrix. This study demonstrated that PT composites are a good candidate for structural applications in harsh environments.

Hall, Samuel Ernesto↗

NASA NTRS1974

Some metal-graphite and metal-ceramic composites for use as high energy brake lining materials

Materials were studied as candidates for development as potential new aircraft brake lining materials. These families were (1) copper-graphite composites; (2) nickel-graphite composites; (3) copper - rare-earth-oxide (gadolinium oxide (Gd2O3) or lanthanum oxide (La2O3)) composites and copper - rare-earth-oxide (La2O3) - rare-earth-fluoride (lanthanum fluoride (LaF3)) composites; (4) nickel - rare-earth-oxide composites and nickel - rare-earth-oxide - rare-earth-fluoride composites. For comparison purposes, a currently used metal-ceramic composite was also studied. Results showed that the nickel-Gd2O3 and nickel-La2O3-LaF3 composites were comparable or superior in friction and wear performance to the currently used composite and therefore deserve to be considered for further development.

Bill, R. C.↗

NASA NTRS1986

A heater made from graphite composite material for potential deicing application

A surface heater was developed using a graphite fiber-epoxy composite as the heating element. This heater can be thin, highly electrically and thermally conductive, and can conform to an irregular surface. Therefore it may be used in an aircraft's thermal deicing system to quickly and uniformly heat the aircraft surface. One-ply of unidirectional graphite fiber-epoxy composite was laminated between two plies of fiber glass-epoxy composite, with nickel foil contacting the end portions of the composite and partly exposed beyond the composites for electrical contact. The model heater used brominated P-100 fibers from Amoco. The fiber's electrical resistivity, thermal conductivity and density were 50 micro ohms per centimeter, 270 W/m-K and 2.30 gm/cubic cm, respectively. The electricity was found to penetrate through the composite in the transverse direction to make an acceptably low foil-composite contact resistance. When conducting current, the heater temperature increase reached 50 percent of the steady state value within 20 sec. There was no overheating at the ends of the heater provided there was no water corrosion. If the foil-composite bonding failed during storage, liquid water exposure was found to oxidize the foil. Such bonding failure may be avoided if perforated nickel foil is used, so that the composite plies can bond to each other through the perforated holes and therefore lock the foil in place.

Hung, C. C.↗

NASA NTRS1987

A heater made from graphite composite material for potential deicing application

A surface heater was developed using a graphite fiber-epoxy composite as the heating element. This heater can be thin, highly electrically and thermally conductive, and can conform to an irregular surface. Therefore it may be used in an aircraft's thermal deicing system to quickly and uniformly heat the aircraft surface. One-ply of unidirectional graphite fiber-epoxy composite was laminated between two plies of fiber glass-epoxy composite, with nickel foil contacting the end portions of the composite and partly exposed beyond the composites for electrical contact. The model heater used brominated P-100 fibers from Amoco. The fiber's electrical resistivity, thermal conductivity and density were 50 micro ohms per centimenter, 270 W/m-K and 2.30 gm/cubic cm, respectively. The electricity was found to penetrate through the composite in the transverse direction to make an acceptably low foil-composite contact resistance. When conducting current, the heater temperature increase reached 50 percent of the steady state value within 20 sec. There was no overheating at the ends of the heater provided there was no water corrosion. If the foil-composite bonding failed during storage, liquid water exposure was found to oxidize the foil. Such bonding failure may be avoided if perforated nickel foil is used, so that the composite plies can bond to each other through the perforated holes and therefore lock the foil in place.

Hung, Ching-Cheh↗

NASA NTRS1986

SiC fiber reinforced reaction-bonded Si3N4 composites

A technique for fabricating strong and tough SiC fiber reinforced reaction bonded Si3N4 matrix composites (SiC/RBSN) was developed. Using this technique, composites containing approximately 23, 30, and 40 volume fractions of aligned 140 micron diameter, chemically vapor deposited SiC fibers were fabricated. The room temperature physical and mechanical properties were evaluated. The results for composite tensile strength, bend strength, and fracture strain indicate that the composite displays excellent properties when compared with the unreinforced matrix of comparable porosity. The composite stress at which the matrix first cracks and the ultimate composite fracture strength increase with increasing volume fraction of fibers, and the composite fails gracefully. The mechanical property data of this ceramic composite are compared with similar data for unreinforced commercially available Si3N4 materials and for SEP SiC/SiC composites.

Bhatt, Ramakrishna T.↗

NASA NTRS1989

The role of rapid solidification processing in the fabrication of fiber reinforced metal matrix composites

Advanced composite processing techniques for fiber reinforced metal matrix composites require the flexibility to meet several widespread objectives. The development of uniquely desired matrix microstructures and uniformly arrayed fiber spacing with sufficient bonding between fiber and matrix to transmit load between them without degradation to the fiber or matrix are the minimum requirements necessary of any fabrication process. For most applications these criteria can be met by fabricating composite monotapes which are then consolidated into composite panels or more complicated components such as fiber reinforced turbine blades. Regardless of the end component, composite monotapes are the building blocks from which near net shape composite structures can be formed. The most common methods for forming composite monotapes are the powder cloth, foil/fiber, plasma spray, and arc spray processes. These practices, however, employ rapid solidification techniques in processing of the composite matrix phase. Consequently, rapid solidification processes play a vital and yet generally overlooked role in composite fabrication. The future potential of rapid solidification processing is discussed.

Locci, Ivan E.↗

NASA NTRS1990

Open hole and post-impact compression fatigue of stitched and unstitched carbon/epoxy composites

The performance is studied of a stitched uniweave fabric composite and that of a toughened tape composite. The effects of stitching on compression fatigue life are addressed. Post impact compression fatigue and open hole fatigue tests were run on an AS4/3501-6 uniweave with stitching and a toughened IM7/8551-7 tape without stitching. Stitching was found to increase the thickness and consequently the weight of the composite material. The two materials were compared on an equal carbon content basis as well as on an equal weight basis. The excess thickness in the stitched uniweave composite was responsible for the lower fatigue life, on an equal carbon basis, compared to the toughened resin tape composite. Comparison of fatigue lives on an equal carbon content basis indicated that puncture or crimp type damage from stitching has very little effect on compression failure. Post impact fatigue test showed that although the damage area in the stitched uniweave composite was twice that of the toughened tape composite, the fatigue lives of the stitched composite were significantly longer than those of the toughened composite. Thus, it appears that the increase in thickness from stitching is much more of a penalty than crimped fibers or puncture type damage from stitching.

Portanova, M. A.↗

NASA NTRS1992

Flight-vehicle materials, structures, and dynamics - Assessment and future directions. Vol. 3 - Ceramics and ceramic-matrix composites

The present volume discusses ceramics and ceramic-matrix composites in prospective aerospace systems, monolithic ceramics, transformation-toughened and whisker-reinforced ceramic composites, glass-ceramic matrix composites, reaction-bonded Si3N4 and SiC composites, and chemical vapor-infiltrated composites. Also discussed are the sol-gel-processing of ceramic composites, the fabrication and properties of fiber-reinforced ceramic composites with directed metal oxidation, the fracture behavior of ceramic-matrix composites (CMCs), the fatigue of fiber-reinforced CMCs, creep and rupture of CMCs, structural design methodologies for ceramic-based materials systems, the joining of ceramics and CMCs, and carbon-carbon composites.

Levine, Stanley R.↗

NASA NTRS1992

Open hole and postimpact compressive fatigue of stitched and unstitched carbon-epoxy composites

Portanova, Marc A.↗

NASA NTRS1990

Intermetallic matrix composites; Proceedings of the MRS Symposium, San Francisco, CA, Apr. 18-20, 1990

The present volume on intermetallic matrix composites discusses the modeling, processing, microstructure/property relationships, and compatibility of intermetallic matrix composites. Attention is given to models for the strength of ductile matrix composites, innovative processing techniques for intermetallic matrix composites, ductile phase toughening of brittle intermetallics, and reactive synthesis of NbAl3 matrix composites. Topics addressed include solidification processing of NbCr2 alloys, Ta and Nb reinforced MoSi2, the microstructure and mechanical behavior of Ni3Al-matrix composites, and ductile-phase toughening of Cr3Si with chromium. Also discussed are dislocation morphologies in TiB2/NiAl, the development of highly impact resistant NiAl matrix composites, the effect of notches on the fatigue life of the SCS-6Ti3Al composite, and the chemical stability of fiber-metal matrix composites.

Anton, D. L.↗

NASA NTRS1993

An overview of the NASA textile composites program

The NASA Langley Research Center is conducting and sponsoring research to explore the benefits of textile reinforced composites for civil transport aircraft primary structures. The objective of this program is to develop and demonstrate the potential of affordable textile reinforced composite materials to meet design properties and damage tolerance requirements of advanced aircraft structures. In addition to in-house research, the program includes major participation by the aircraft industry and aerospace textile companies. The major program elements include development of textile preforms, processing science, mechanics of materials, experimental characterization of materials, and development and evaluation of textile reinforced composite structural elements and subcomponents. The NASA Langley in-house research is focused on science-based understanding of resin transfer molding (RTM), development of powder-coated towpreg processes, analysis methodology, and development of a performance database on textile reinforced composites. The focus of the textile industry participation is on development of multidirectional, damage-tolerant preforms, and the aircraft industry participation is in the areas of innovative design concepts, cost-effective fabrication, and testing of textile reinforced composite structural elements and subcomponents. Textile processes such as 3-D weaving, 2-D and 3-D braiding, and knitting/stitching are being compared with conventional laminated tape processes for improved damage tolerance. Through-the-thickness reinforcements offer significant damage tolerance improvements. However, these gains must be weighed against potential loss in in-plane properties such as strength and stiffness. Analytical trade studies are underway to establish design guidelines for the application of textile material forms to meet specific loading requirements. Fabrication and testing of large structural components are required to establish the full potential of textile reinforced composite materials. The goals of the NASA Langley-sponsored research program are to demonstrate technology readiness with subscale composite components by 1995 and to verify the performance of full-scale composite primary aircraft structural components by 1997. The status of textile reinforced composite structural elements under development by Boeing, Douglas, Lockheed, and Grumman are presented. Included are braided frames and woven/stitched wing and fuselage panels.

Dexter, H. Benson↗

NASA NTRS1992

Properties of Graphite Fiber Reinforced Copper Matrix Composites for Space Power Applications

The thermal and mechanical properties of pitch-based graphite fiber reinforced copper matrix (Gr/Cu) composites usable for space applications such as radiator fins were investigated. Thermal conductivity was measured as a function of fiber volume fraction and architecture. Results showed for unidirectional P-100 Gr/Cu composites, the longitudinal thermal conductivity was nearly independent of fiber volume fraction. Transverse thermal conductivities (perpendicular to the fibers) were strongly affected by the fiber volume fraction with higher volume fractions resulting in lower thermal conductivities. The effect of architecture on thermal conductivity followed the cosine squared law for simple architectures. Insufficient data are available currently to model more complex architectures, but adding fibers in the direction of the heat flow increases the thermal conductivity as low conductivity plies are supplemented by high conductivity plies. Thermal expansion tests were conducted on the Gr fibers and Gr/Cu composites. The results show a considerable thermal expansion mismatch between the fibers and the Cu matrix. The longitudinal thermal expansion showed a strong dependence on the architecture of the Gr/Cu composites. The composites also show a thermal expansion hysteresis. The hysteresis was eliminated by an engineered interface. Mechanical testing concentrated on the dynamic modulus and strength of the composites. The dynamic modulus of the Gr/Cu composites was 305 GPa up to 400 C, a value equivalent to Be. The strengths of the composites were less than expected, but this is attributed to the poor bond across the interface between the Gr fibers and Cu matrix. Testing of composites with an engineered interface is expected to yield strengths nearer the values predicted by the rule of mixtures.

Ellis, David L.↗

NASA NTRS1993

IPACS (Integrated Probabilistic Assessment of Composite Structures): Code development and applications

A methodology and attendant computer code have been developed and are described to computationally simulate the uncertain behavior of composite structures. The uncertain behavior includes buckling loads, stress concentration factors, displacements, stress/strain etc., which are the consequences of the inherent uncertainties (scatter) in the primitive (independent random) variables (constituent, ply, laminate and structural) that describe the composite structures. The computer code, IPACS (Integrated Probabilistic Assessment of Composite Structures), can handle both composite mechanics and composite structures. Application to probabilistic composite mechanics is illustrated by its uses to evaluate the uncertainties in the major Poisson's ratio and in laminate stiffness and strength. IPACS application to probabilistic structural analysis is illustrated by its use to evaluate the uncertainties in the buckling of a composite plate, in the stress concentration factor in a composite panel and in the vertical displacement and ply stress in a composite aircraft wing segment.

Chamis, C. C.↗