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Fracture of composite-adhesive-composite systems

This program was undertaken to initiate the development of a test method for testing adhesive joints in metal-adhesive-composite systems. The uniform double cantilever beam (UDCB) and the width tapered beam (WTB) specimen geometries were evaluated for measuring Mode I fracture toughness in these systems. The WTB specimen is the preferred geometry in spite of the fact that it is more costly to machine than the UDCB specimen. The use of loading tabs attached to thin sheets of composites proved to be experimentally unsatisfactory. Consequently, a new system was developed to load thin sheets of adherends. This system allows for the direct measurement of displacement along the load line. In well made joints separation occurred between the plies rather than in the adhesive.

Ripling, E. J.↗

High Volume Fraction Carbon Nanotube Composites for Aerospace Applications

Reported mechanical properties of carbon nanotubes (CNTs) at the nanoscale suggest their potential to enable significantly lighter structures of interest for space applications. However, their utility depends on the retention of these properties in bulk material formats that permit practical fabrication of large structures. This presentation summarizes recent progress made to produce carbon nanotube composites with specific tensile properties that begin to rival those of carbon fiber reinforced polymer composites. CNT content in these nanocomposites was greater than 70% by weight. Tested nanocomposite specimens were fabricated from kilometers or tens of square meters of CNT, depending on the starting material format. Processing methods to yield these results, and characterization and testing to evaluate the performance of these composites will be discussed. The final objective is the demonstration of a CNT composite overwrapped pressure vessel to be flight tested in the Fall of 2016.

Siochi, E. J.↗

Large-scale additive manufacturing of self-heating molds

Large-scale material extrusion additive manufacturing technology is becoming the new mainstream technology for scaled-up composite mold and die applications. This paradigm shift in composite processing technology is primarily driven by out-of-autoclave tooling applications, in which fiber reinforced composite molds with scaled-up sizes and embedded heating elements are attractive. The present research describes the design, manufacturing, and testing of self-heating composite molds fabricated via a large-scale pellet extrusion 3D printing machine with an integrated wire co-extrusion tool. Polycarbonate (PC) composites reinforced with carbon fiber (PC/CF; 20 wt.%) and glass fiber (PC/GF; 20 wt.%) were used to fabricate mold parts. Joule heating thermal test results showed that uniform temperatures (~100 °C) were achieved for both PC/CF and PC/GF mold surfaces, using a custom-made feedback control power supply and infrared thermography. Mechanical characterizations, including tensile and flexural testing were performed on the wire-embedded and un-wired PC/CF and PC/GF base specimens to investigate the impact of the fiber reinforcement as well as the embedded wires. In the direction of extrusion, the ultimate tensile stress of PC/CF was 105 MPa, and that of PC/GF was 73 MPa, while the neat PC value was 64 MPa. Inner-bead voids and interfacial gaps were observed and characterized via optical and scanning electron microscopy. The embedded wires and inner bead impacted the mechanical properties of the composites. Furthermore, the stiffness of the wire-embedded mold was still satisfactory, proving that the technology can be used to fabricate additively manufactured out-of-oven/autoclave molds.

36 MATERIALS SCIENCE↗

Designing and Validating Ternary Pd Alloys for Optimum Sulfur/Carbon Resistance in Hydrogen Separation and Carbon Capture Membrane Systems Using High-Throughput Combinatorial Methods

This report summarizes the work completed under the U.S. Department of Energy Project Award No.: DE-FE0001181 titled “Designing and Validating Ternary Pd Alloys for Optimum Sulfur/Carbon Resistance in Hydrogen Separation and Carbon Capture Membrane Systems Using High-Throughput Combinatorial Methods.” The project started in October 1, 2009 and was finished September 30, 2014. Pall Corporation worked with Cornell University to sputter and test palladium-based ternary alloys onto silicon wafers to examine many alloys at once. With the specialized equipment at Georgia Institute of Technology that analyzed the wafers for adsorbed carbon and sulfur species six compositions were identified to have resistance to carbon and sulfur species. These compositions were deposited on Pall AccuSep® supports by Colorado School of Mines and then tested in simulated synthetic coal gas at the Pall Corporation. Two of the six alloys were chosen for further investigations based on their performance. Alloy reproducibility and long-term testing of PdAuAg and PdZrAu provided insight to the ability to manufacture these compositions for testing. PdAuAg is the most promising alloy found in this work based on the fabrication reproducibility and resistance to carbon and sulfur. Although PdZrAu had great initial resistance to carbon and sulfur species, the alloy composition has a very narrow range that hindered testing reproducibility.

36 MATERIALS SCIENCE↗

Synthesis of improved phenolic resins

Twenty seven addition cured phenolic resin compositions were prepared and tested for their ability to give char residues comparable to state-of-the-art phenolic resins. Cyanate, epoxy, allyl, acrylate, methacrylate and ethynyl derivatized phenolic oligomers were investigated. The novolac-cyanate and propargyl-novolac resins provided anaerobic char yields at 800 C of 58 percent. A 59 percent char yield was obtained from modified epoxy novolacs. A phosphonitrilic derivative was found to be effective as an additive for increasing char yields. The novolac-cyanate, epoxy-novolac and methacrylate-epoxy-novolac systems were investigated as composite matrices with Thornel 300 graphite fiber. All three resins showed good potential as composite matrices. The free radical cured methacrylate-epoxy-novolac graphite composite provided short beam shear strengths at room temperature of 93.3 MPa (13.5 ksi). The novolac-cyanate graphite composite produced a short beam shear strength of 74 MPa (10.7 ksi) and flexural strength of 1302 MPa (189 ksi) at 177 C. Air heat aging of the novolac-cyanate and epoxy novolac based composites for 12 weeks at 204 C showed good property retention.

Delano, C. B.↗

Material property characterization of 3D printed polypropylene wood plastic composites

Abstract Wood flour (WF) at 10 wt.% and 20 wt.% loadings was used as a reinforcing filler to enhance the applicability of polypropylene (PP) for 3D printing. After performing printability tests of PP wood plastic composites (WPCs), the mechanical properties of both injection‐molded and 3D‐printed PP WPC specimens were explored. Test specimens were prepared from 3D printed hexagons for analyzing the mechanical properties. Adding WF to neat PP increased the storage modulus and the glass transition temperature while decreasing the degree of crystallinity and the coefficient of thermal expansion, while enhancing the printability of neat PP. The tensile strength, tensile modulus of elasticity, flexural strength, and flexural modulus of elasticity of injection‐molded neat PP improved by up to 21%, 59%, 30%, and 56%, respectively, with 20 wt.% WF. However, the impact strength of injection‐molded neat PP decreased by 85%, with 20 wt.% WF. After 3D printing, the tensile strength and tensile modulus of elasticity of printed neat PP increased by up to 84% and 60%, respectively, with 20 wt.% WF. The flexural strength and flexural modulus of elasticity of neat printed PP remained unchanged compared to those of PP filled with 20 wt.% WF, while the impact strength decreased by 87%. Highlights WF was used as a reinforcement in polypropylene designed for 3D printing A pilot‐scale, pellet‐fed 3D printer was used to print hollow hexagons, and then test specimens were fabricated from these hexagons for mechanical properties The tensile and flexural properties of 3D printed neat polypropylene improved, while the impact strength decreased after adding 20 wt.% WF to the neat PP.

Hwang, Sungjun↗

Macro Scale Independently Homogenized Subcells for Modeling Braided Composites

An analytical method has been developed to analyze the impact response of triaxially braided carbon fiber composites, including the penetration velocity and impact damage patterns. In the analytical model, the triaxial braid architecture is simulated by using four parallel shell elements, each of which is modeled as a laminated composite. Currently, each shell element is considered to be a smeared homogeneous material. The commercial transient dynamic finite element code LS-DYNA is used to conduct the simulations, and a continuum damage mechanics model internal to LS-DYNA is used as the material constitutive model. To determine the stiffness and strength properties required for the constitutive model, a top-down approach for determining the strength properties is merged with a bottom-up approach for determining the stiffness properties. The top-down portion uses global strengths obtained from macro-scale coupon level testing to characterize the material strengths for each subcell. The bottom-up portion uses micro-scale fiber and matrix stiffness properties to characterize the material stiffness for each subcell. Simulations of quasi-static coupon level tests for several representative composites are conducted along with impact simulations.

Blinzler, Brina J.↗

Distilling physical origins of hardness in multi-principal element alloys directly from ensemble neural network models

Abstract Despite a plethora of data being generated on the mechanical behavior of multi-principal element alloys, a systematic assessment remains inaccessible via Edisonian approaches. We approach this challenge by considering the specific case of alloy hardness, and present a machine-learning framework that captures the essential physical features contributing to hardness and allows high-throughput exploration of multi-dimensional compositional space. The model, tested on diverse datasets, was used to explore and successfully predict hardness in Al x Ti y (CrFeNi) 1- x - y , Hf x Co y (CrFeNi) 1- x - y and Al x (TiZrHf) 1- x systems supported by data from density-functional theory predicted phase stability and ordering behavior. The experimental validation of hardness was done on TiZrHfAl x . The selected systems pose diverse challenges due to the presence of ordering and clustering pairs, as well as vacancy-stabilized novel structures. We also present a detailed model analysis that integrates local partial-dependencies with a compositional-stimulus and model-response study to derive material-specific insights from the decision-making process.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Atmospheric Corrosion Behavior and Mechanism of a Ni-Advanced Weathering Steel in Simulated Tropical Marine Environment

Corrosion behavior of Ni-advanced weathering steel, as well as carbon steel and conventional weathering steel, in a simulated tropical marine atmosphere was studied by field exposure and indoor simulation tests. Meanwhile, morphology and composition of corrosion products formed on the exposed steels were surveyed through scanning electron microscopy, energy-dispersive x-ray spectroscopy and x-ray diffraction. Results indicated that the additive Ni in weathering steel played an important role during the corrosion process, which took part in the formation of corrosion products, enriched in the inner rust layer and promoted the transformation from loose γ-FeOOH to dense α-FeOOH. As a result, the main aggressive ion, i.e., Cl{sup −}, was effectively separated in the outer rust layer which leads to the lowest corrosion rate among these tested steels. Thus, the resistance of Ni-advanced weathering steel to atmospheric corrosion was significantly improved in a simulated tropical marine environment.

36 MATERIALS SCIENCE↗

Evaluation of oxide-coated iridium-rhenium chambers

Iridium-coated rhenium (Ir-Re) provides long life operation of radiation-cooled rockets at temperatures up to 2200 C. Ceramic oxide coatings could be used to increase Ir-Re rocket lifetimes and allow operation in highly oxidizing environments. Ceramic oxide coatings promise to serve as both thermal and diffusion barriers for the iridium layer. Seven ceramic oxide-coated Ir-Re, 22-N rocket chambers were tested with gaseous hydrogen/gaseous oxygen (GHz/G02) propellants. Five chambers had thick (over 10 mils), monolithic coatings of either hafnia (HfO2) or zirconia (ZrO2). Two chambers had coatings with thicknesses less than 5 mils. One of these chambers had a thin-walled coating of ZrO2 infiltrated with sol gel HfO2. The other chamber had a coating composed of an Ir-oxide composite. The purpose of this test program was to assess the ability of the oxide coatings to withstand the thermal shock of combustion initiation, adhere under repeated thermal cycling, and operate in aggressively oxidizing environments. All of the coatings survived the thermal shock of combustion and demonstrated operation at mixture ratios up to 11. Testing the Ir-oxide composite-coated chamber included over 29 min at mixture ratio 16. The thicker walled coatings provided the larger temperature drops across the oxide layer (up to 570 C), but were susceptible to macrocracking and eventual chipping at a stress concentrator. The cracks apparently resealed during firing, under compression of the oxide layer. The thinner walled coatings did not experience the macrocracking and chipping of the chambers that was seen with the thick, monolithic coatings. However, burn-throughs in the throat region did occur in both of the thin-walled chambers at mixture ratios well above stoichiometric. The burn-throughs were probably the result of oxygen diffusion through the oxide coating that allowed the underlying Ir and Re layers to be oxidized. The results of this test program indicated that the thin-walled oxide coatings are better suited for repeated thermal cycling than the thick-walled coating, while thicker coatings may be required for operation in aggressively oxidizing environments.

Reed, Brian D.↗

Experimental clean combustor program, phase 2

The alternate fuels investigation objective was to experimentally determine the impacts, if any, on exhaust emissions, performance, and durability characteristics of the hybrid and vorbix low pollution combustor concepts when operated on test fuels which simulate composition and property changes which might result from future broadened aviation turbine fuel specifications or use of synthetically derived crude feedstocks. Results of the program indicate a significant increase in CO and small NOX increase in emissions at idle for both combustor concepts, and an increase in THC for the vorbix concept. Minimal impact was observed on gaseous emissions at high power. The vorbix concept exhibited significant increase in exhaust smoke with increasing fuel aromatic content. Altitude stability was not affected for the vorbix combustor, but was substantially reduced for the hybrid concept. Severe carbon deposition was observed in both combustors following limited endurance testing with No. 2 home heat fuel. Liner temperature levels were insensitive to variations in aromatic content over the range of conditions investigated.

Roberts, R.↗

Synthesis of MgCo 2 O 4 -coated Li 4 Ti 5 O 12 composite anodes using co-precipitation method for lithium-ion batteries

In the present work, we report synthesis of MgCo 2 O 4 (MCO)/Li 4 Ti 5 O 12 (LTO) composites for Li-ion battery anodes by a co-precipitation method. The objective here is to replace expensive Co with Mg and also to exploit advantages of both MCO and LTO. Three samples of MCO/LTO particles with different MCO proportion have various average particle sizes of 38.1, 56.9, and 58.5 nm, confirmed by scanning electron microscopy. Electrochemical studies show that a MCO/LTO anode offers a discharge capacity of ca. 300 mAh g -1 , which is two times higher than that achieved by pristine LTO. The MCO/LTO anode also retains 75% of its initial capacity, even if the discharge rate is increased to 5 C. Cyclic stability test reveals that the composite anode still maintains nearly 85.5% of its initial capacity after 150 cycles. Electrochemical impedance spectroscopy indicates that the equivalent series resistance of MCO/LTO electrodes is significantly lower than that of LTO, i.e., from 35.5 to 9.9 Ω. The enhanced performance of the composite electrodes can be attributed to its improved conductivity as well as to the surface modification of LTO particles by MCO nanoparticle deposition which leads to increased number of active sites on the former.

25 ENERGY STORAGE↗

Satellite Broadcast of Graphical Weather Data Flight Tested

NASA Glenn Research Center at Lewis Field's aviation Weather Information Communications (WINCOMM) and NASA Langley Research Center's Aviation Weather Information (AWIN) programs collaborated in a flight test and evaluation of a worldwide weather data-link capability using satellites. This successful flight testing moves NASA closer to its goal of developing advanced communications and information technologies to enable high-quality and timely dissemination of aviation weather information to all relevant users on the aviation information network. Recognized as a major contributing factor in aviation accidents and incidents, weather contributes directly or indirectly to nearly 80 percent of fatal general aviation (small private aircraft) accidents. In 1997, the Aeronautics Safety Investment Strategy Team s weather team produced a prioritized list of investment areas under weather accident prevention. Weather data dissemination is the most critical and highest ranked priority on the list. NASA's Aviation Safety Program founded the Aviation Weather Information initiative to focus efforts on significantly reducing the number of weather-related aviation fatalities. Access to accurate and timely weather data could contribute to a major reduction of weather-related incidents and accidents. However, a cost-effective solution has eluded most general aviation pilots because of the high cost of onboard weather radar equipment. Rockwell Collins, through a contract with NASA and in cooperation with WorldSpace Corporation, successfully completed ground and flight testing of a receiver and antenna in Johannesburg, South Africa. This NASA/Rockwell Collins project is an evaluation of worldwide weather data-link capability using transmissions from the Satellite Digital Audio Radio Services (S DARS) AfriStar satellite. Owned and operated by WorldSpace, AfriStar is a geostationary satellite that broadcasts commercial digital audio services to stationary and mobile platforms. S DARS satellites are the most powerful communications satellites produced to date, allowing users to receive signals using simple, low-cost patch antennas instead of more expensive, beam-steered antenna arrays. Engineers connected an inexpensive, commercially available radio receiver to a laptop computer and an antenna designed and built by Rockwell Collins, enabling them to receive WorldSpace signals from the AfriStar satellite during flight tests. WorldSpace broadcast their composite color graphical weather data files, which were multiplexed with normal audio streams, to the flat patch antenna mounted on a single-engine aircraft. The aircraft was equipped with a modified commercial S-DARS receiver, a Global Positioning Satellite (GPS) receiver, and a laptop computer with color display. Continuous data reception occurred during normal aircraft maneuvers performed throughout takeoff, cruise, and landing operations. In addition, engineers monitored receiver power levels during steep turns and banks. In most instances, the receiver was able to maintain acceptable power levels during all phases of flight and to obtain weather data with little or with the successful completion of ground and flight testing of a receiver and antenna in Johannesburg, South Africa, the team has started to prepare for experiments using highspeed aircraft in areas of the world with limited access to timely weather data. NASA plans to provide a more advanced antenna design and consultation support. This successful test of real-time aviation-related weather data is a positive step toward solving communications-specific issues associated with the dissemination of weather data directly to the cockpit.

Mallasch, Paul G.↗

Imide modified epoxy matrix resins

Results of a program designed to develop tough imide modified epoxy (IME) resins cured by bisimide amine (BIA) hardeners are presented. State of the art epoxy resin, MY720, was used. Three aromatic bisimide amines and one aromatic aliphatic BIA were evaluated. BIA's derived from 6F anhydride (3,3 prime 4,4 prime-(hexafluoro isopropyl idene) bis (phthalic anhydride) and diamines, 3,3 prime-diam nodiphenyl sulfone (3,3 prime-DDS), 4,4 prime-diamino diphenyl sulfone (4,4 prime-DDS), 1.12-dodecane diamine (1,12-DDA) were used. BIA's were abbreviated 6F-3,3 prime-DDS, 6F-4,4 prime-DDS, 6F-3,3 prime-DDS-4,4 prime DDS, and 6F-3,3 prime-DDS-1,12-DDA corresponding to 6F anhydride and diamines mentioned. Epoxy resin and BIA's (MY720/6F-3,3 prime-DDS, MY720/6F-3,3 prime-DDS-4,4 prime-DDS, MY720/6F-3,3 prime-DDS-1,12-DDA and a 50:50 mixture of a BIA and parent diamine, MY720/6F-3,3 prime-DDS/3,3 prime-DDS, MY720/6F-3,3 prime-DDS-4,4 prime-DDS/3,3 prime-DDS, MY720/6F-3,3 prime-DDS-1,12-DDA/3,3 prime-DDS were studied to determine effect of structure and composition. Effect of the addition of two commercial epoxies, glyamine 200 and glyamine 100 on the properties of several formulations was evaluated. Bisimide amine cured epoxies were designated IME's (imide modified epoxy). Physical, thermal and mechanical properties of these resins were determined. Moisture absorption in boiling water exhibited by several of the IME's was considerably lower than the state of the art epoxies (from 3.2% for the control and state of the art to 2.0 wt% moisture absorption). Char yields are increased from 20% for control and state of the art epoxies to 40% for IME resins. Relative toughness characteristics of IME resins were measured by 10 deg off axis tensile tests of Celion 6000/IME composites. Results show that IME's containing 6F-3,3 prime-DDS or 6F-3,3 prime-DDS-1,12-DDA improved the "toughness" characteristics of composites by about 35% (tensile strength), about 35% (intralaminar shear strength), and about 78% (shear strain to failure) relative to the control composite.

Scola, D. A.↗

Post-irradiation Examinations of High Burnup PWR Rods - 18456

The High Burnup Spent Fuel Data Project (herein referred to as the 'project'), sponsored by the US Department of Energy (DOE) Office of Nuclear Energy (NE), is focused on experimentally evaluating the effects of long-term storage and transportation on high burnup (HBU) (defined as >45 gigawatt days per metric ton uranium) pressurized water reactor (PWR) spent nuclear fuel (SNF) [1]. To support this project, in the fall of 2017, an instrumented bolted-lid cask (project cask) at the North Anna reactor site was loaded with intact, HBU PWR fuel assemblies (project assemblies) having four different kinds of cladding and will be reopened in approximately 10-years for inspection. To support pre- and post-storage SNF rod characterization, 25 'sister rods' that are similar to the rods being stored in the project cask were extracted from seven different fuel assemblies at the North Anna nuclear power plant for post-irradiation examination (PIE). The sister rod testing program has multiple objectives, including: 1) Baseline testing to provide essential information on the physical condition and properties of the cladding and the fuel in the cladding prior to the loading, drying, and long-term dry storage process (analogous to an experiment control group). Similar tests are expected to be performed at the end of the 10-year storage period on rods extracted from the cask to identify any changes in the properties of the fuel rods that may have occurred during the dry storage period; and 2) Tests to provide material property and physical data using accelerated separate effects tests (SETs) and small-scale tests (SSTs) to explore a wide range of conditions that may occur for other dry storage systems and/or while the fuel is being transported after aging. Testing will be focused on understanding overall SNF rod strength and durability, and be comprised of both composite fuel and defueled clad testing with a focus on measuring cladding material and mechanical properties. Nondestructive testing is currently underway and plans are being updated to support the initial set of destructive tests that are expected to begin by early 2018. While the data generated can be used for multiple purposes, a primary goal of the sister rod PIE data and associated measured mechanical properties are expected to support existing fuel storage licensing and relicensing activities by addressing identified knowledge gaps, and enhance the technical bases for post-storage transportation, handling, and consolidation activities [1]. This paper presents results obtained from the sister rod testing to date, and describes some of the planned measurements, equipment, and procedures that will be implemented for the initial set of destructive examinations. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization and manufacture of braided composites for large commercial aircraft structures

Braided composite materials, one of the advanced material forms which is under investigation in Boeing's ATCAS program, have been recognized as a potential cost-effective material form for fuselage structural elements. Consequently, there is a strong need for more knowledge in the design, manufacture, test, and analysis of textile structural composites. The overall objective of this work is to advance braided composite technology towards applications to a large commercial transport fuselage. This paper summarizes the mechanics of materials and manufacturing demonstration results which have been obtained in order to acquire an understanding of how braided composites can be applied to a commercial fuselage. Textile composites consisting of 1D, 2D triaxial, and 3D braid patterns with thermoplastic and two RTM resin systems were investigated. The structural performance of braided composites was evaluated through an extensive mechanical test program. Analytical methods were also developed and applied to predict the following: internal fiber architectures, stiffnesses, fiber stresses, failure mechanisms, notch effects, and the entire history of failure of the braided composites specimens. The applicability of braided composites to a commercial transport fuselage was further assessed through a manufacturing demonstration. Three foot fuselage circumferential hoop frames were manufactured to demonstrate the feasibility of consistently producing high quality braided/RTM composite primary structures. The manufacturing issues (tooling requirements, processing requirements, and process/quality control) addressed during the demonstration are summarized. The manufacturing demonstration in conjunction with the mechanical test results and developed analytical methods increased the confidence in the ATCAS approach to the design, manufacture, test, and analysis of braided composites.

Fedro, Mark J.↗

Absorptive Weak Plume Detection on Gaussian and Non-Gaussian Background Clutter

For additive signals on Gaussian clutter, the optimal detector is a linear matched filter that is adapted to the known signal and the covariance of the background. This adaptive matched filter is widely used for gas-phase plume detection, even though the effect of the plume on the background is not strictly additive. Here, a derivation of the matched filter for a strictly absorptive plume produces, in the weak plume limit, a quadratic filter. This quadratic matched filter is extended in two ways: an elliptically-contoured multivariate t distribution is used to generalize the Gaussian background clutter, and a generalized likelihood ratio test detector is derived to extend applicability to stronger plumes. In addition to detectors whose purpose is to identify presence versus absence of a plume, expressions are also derived for estimating plume strength. The performance of these various detectors is evaluated by implanting simulated plume into background images that are either real hyperspectral images or simulated images based on different (Gaussian, multivariate t, and lognormal) clutter distributions.

79 ASTRONOMY AND ASTROPHYSICS↗