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DOE OSTI2021

Perovskite-Derived Cs 2 SnCl 6 –Silica Composites as Advanced Waste Forms for Chloride Salt Wastes

Advanced materials and processes are required to separate halides and fission products from complex salt waste streams associated with the chemical reprocessing of used nuclear fuels and molten salt reactor technologies for immobilization into chemically durable waste forms. Here, in this work, we explore an innovative concept using metal-halide perovskites as advanced host phases to incorporate Cs and Cl with very high waste loadings. Wet chemistry-synthesized Cs 2 SnCl 6 powders from CsCl salt solutions are successfully encapsulated into a silica matrix to form a composite using low-temperature spark plasma sintering with tunable Cs and Cl loadings up to 31 wt.% and 26 wt.%, respectively. Chemical durability testing of the composite waste forms by semi-dynamic leaching experiments demonstrates that incongruent leaching mechanism dominated. The metal-halide perovskite-silica composite waste forms display exceptional chemical durability with the long-term release rates of Cs and Cl comparable to or outperforming the state-of-the-art waste form materials but with significantly higher waste loadings. The scalable synthesis of the metal-halide perovskite from wet-chemistry processes opens up new opportunities in designing perovskite-glass composite waste forms for salt wastes with very high waste loadings and exceptional chemical durability for the sustainable development of advanced fuel cycles and next-generation reactor technologies.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1992

Indentation flaw formation and strength response of silicon nitride ceramics at low indentation loads

The configuration and the strength response of indentation flaws in silicon nitrides are described as a function of indentation loads primarily near the threshold level. Test materials under consideration include 30 vol percent SiC whisker-reinforced composite silicon nitride and similar monolithic silicon nitride. The results of strength testing show that, at indentation loads less than or equal to 1.96, a number of the specimens fail from the intrinsic flaws of the materials rather than from the indent sites, causing a distinct trend to reach a plateau, at a level corresponding to the as-received strength of the material. The ratio of the mirror constant to the fracture toughness for the composite and monolithic materials is found to be 1.44 and 1.51, respectively.

Choi, Sung R.↗

NASA NTRS2003

Mechanical Behaviour of Woven Graphite/Polyimide Composites with Medium and High Modulus Graphite Fibers Subjected to Biaxial Shear Dominated Loads

A major limitation of woven fiber/polymer matrix composite systems is the inability of these materials to resist intralaminar and interlaminar damage initiation and propagation under shear-dominated biaxial loading conditions. There are numerous shear test methods for woven fabric composites, each with its own advantages and disadvantages. Two techniques, which show much potential, are the Iosipescu shear and +/- 45 deg tensile tests. In this paper, the application of these two tests for the room and high temperature failure analyses of woven graphite/polyimide composites is briefly evaluated. In particular, visco-elastic micro, meso, and macro-stress distributions in a woven eight harness satin (8HS) T650/PMR-15 composite subjected to these two tests are presented and their effect on the failure process of the composite is evaluated. Subsequently, the application of the Iosipescu tests to the failure analysis of woven composites with medium (T650) and high (M40J and M60J) modulus graphite fibers and PMR-15 and PMR-II-50 polyimide resins is discussed. The composites were tested as-supplied and after thermal conditioning. The effect of temperature and thermal conditioning on the initiation of intralaminar damage and the shear strength of the composites was established.

Kumose, M.↗

NASA NTRS1991

The effect of matrix mechanical properties on (0)8 unidirectional SiC/Ti composite fatigue resistance

The relationship between constituent and MMC properties in fatigue loading is investigated with low-cycle fatigue-resistance testing of an alloy Ti-15-3 matrix reinforced with SiC SCS-6 fibers. The fabrication of the composite is described, and specimens are generated that are weak and ductile (WD), strong and moderately ductile (SM), or strong and brittle (SB). Strain is measured during MMC fatigue tests at a constant load amplitude with a load-controlled waveform and during matrix-alloy fatigue tests at a constant strain amplitude using a strain-controlled waveform. The fatigue resistance of the (0)8 SiC/Ti-15-3 composite is found to be slightly influenced by matrix mechanical properties, and the composite- and matrix-alloy fatigue lives are not correlated. This finding is suggested to relate to the different crack-initiation and -growth processes in MMCs and matrix alloys.

Gabb, T. P.↗

NASA NTRS1997

Damage Initiation and Ultimate Tensile Strength of Scaled [0 deg n/90 deg n/0 deg n]sub T Graphite-Epoxy Coupons

Previous research on scaling effects in composite materials has demonstrated that the stress levels at first ply failure and ultimate failure of composite laminates are dependent on the size of the laminate. In particular, the thickness dimension has been shown to be the most influential parameter in strength scaling of composite coupons loaded in tension. Geometrically and constitutively scaled laminates exhibit decreasing strength with increasing specimen size, and the magnitude of the strength-size effect is a function of both material properties and laminate stacking sequence. Some of the commonly used failure criteria for composite materials such as maximum stress, maximum strain, and tensor polynomial (e.g., Tsai-Wu) cannot account for the strength-size effect. In this paper, three concepts are developed and evaluated for incorporating size dependency into failure criteria for composite materials. An experimental program of limited scope was performed to determine the first ply failure stress in scaled cross-ply laminates loaded in tension. Test specimens were fabricated of AS-4/3502 graphite-epoxy composite material with laminate stacking sequences of [0 deg n/90 deg n/o deg n]subT where n=1-6. Two experimental techniques were used to determine first ply failure, defined as a transverse matrix crack in the 90 deg ply: (1) step loading with dye penetrant x-ray of the specimen at each load interval, and (2) acoustic emission. The best correlation between first ply failure analysis and experimental data was obtained using a modified Weibull approach which incorporated the residual thermal stress and the outer ply constraint, as well as the ply thickness effect. Finally, a second set of experiments was performed to determine the tensile response and ultimate failure of the scaled cross-ply laminates. The results of these experiments indicated no influence of specimen size on tensile response or ultimate strength.

Jackson, Karen E.↗

NASA NTRS1980

Proof test and fatigue of unnotched composite laminates

A comprehensive fatigue and residual strength degradation model has been used to predict the effect of proof loads (or high load) on the statistical fatigue behavior of composite laminates. The validity of the theoretical model is confirmed by the experimental test results. The correlation between the test results and the theoretical distributions of the fatigue life and the residual strength for composite specimens with or without the effect of proof loads is shown to be very good.

Yang, J. N.↗

NASA NTRSDate not supplied

Critical Progressive Damage Analysis Model Features for Low-Velocity Impact on Thermoset and Thermoplastic Panels

A previous verification and validation framework evaluated the ability of various progressive damage analysis (PDA) tools to predict the mechanical response and damage state in post-buckled stiffened aerospace structures composed of fiber-reinforced thermoset composite materials. Herein, the ability of PDA tools to predict damage in thermoplastic composite materials subject to low-velocity impact (LVI) loading has been assessed. LVI tests and analyses have been conducted for similar panels, comprising thermoset or thermoplastic composite materials. Preliminary test/analysis correlations revealed that using the same combination of PDA model features and finite element model-building guidelines for the thermoset and thermoplastic LVI specimens resulted in underprediction of matrix crack lengths and delaminated area in the thermoplastic analyses despite yielding good correlations for the thermoset specimens. In this paper, the quality of the test/analysis correlations for analyses of thermoplastic LVI specimens performed with different combinations of PDA model features using the NASA CompDam material model are presented. Model features that were assessed in terms of effect on the quality of the test/analysis correlation include the representation of damageable interfaces, residual thermal stresses, and fiber damage.

Frank Leone↗

NASA NTRSDate not supplied

Critical Progressive Damage Analysis Model Features for Low-Velocity Impact on Thermoset and Thermoplastic Panels

Frank Leone↗

NASA NTRS1998

An Experimental Investigation of Transverse Tension Fatigue Characterization of IM6/3501-6 Composite Materials Using a Three-Point Bend Test

As composites are introduced into more complex structures with out-of-plane loadings, a better understanding is needed of the out-of-plane, matrix-dominated failure mechanisms. This work investigates the transverse tension fatigue characteristics of IM6/3501 composite materials. To test the 90 degree laminae, a three-point bend test was chosen, potentially minimizing handling and gripping issues associated with tension tests. A finite element analysis was performed of a particular specimen configuration to investigate the influence of specimen size on the stress distribution for a three-point bend test. Static testing of 50 specimens of 9 different sized configurations produced a mean transverse tensile strength of 61.3 Mpa (8.0 ksi). The smallest configuration (10.2 mm wide, Span-to-thickness ratio of 3) consistently exhibited transverse tensile failures. A volume scale effect was difficult to discern due to the large scatter of the data. Static testing of 10 different specimens taken from a second panel produced a mean transverse tensile strength of 82.7 Mpa (12.0 ksi). Weibull parameterization of the data was possible, but due to variability in raw material and/or manufacturing, more replicates are needed for greater confidence. Three-point flex fatigue testing of the smallest configuration was performed on 59 specimens at various levels of the mean static transverse tensile strength using an R ratio of 0.1 and a frequency of 20 Hz. A great deal of scatter was seen in the data. The majority of specimens failed near the center loading roller. To determine whether the scatter in the fatigue data is due to variability in raw material and/or the manufacturing process, additional testing should be performed on panels manufactured from different sources.

Peck, Ann W.↗

NASA NTRS1972

Graphite fiber polyimide composites for spherical bearings to 340 C (650 F)

Journal bearings with self-alining spherical elements of graphite-fiber-reinforced-polyimide composites were tested from 24 to 340 C (75 to 650 F) at unit loads up to 3.5 times 10 to the 7th power N/sq m (5000 psi). The journal oscillated in the cylindrical bore of the composite element + or - 15 deg at 1 hertz. Outer races and journals were metal hardened of Rockwell C-32 and finished to 10 to the minus 7th power m. A 45 wt. percent graphite-fiber composite gave low friction (0.08 to 0.13), low wear, and almost no plastic deformation under any of the test conditions. Composites with 15 and 25 wt. percent graphite fiber failed by plastic deformation at 315 C (600 F) and 3.5 times 10 to the 7th power N/sq m (5000 psi). A composite with 60 wt. percent graphite fiber failed by brittle fracture under the same conditions, but had very low friction coefficients (0.05 to 0.10) and may be a good bearing material at lighter loads.

Sliney, H. E.↗

NASA NTRS1998

Mechanical Behavior and Analytical Modeling of Melt-Infiltrated SiC/SiC Woven Composite

The desirable properties in ceramic matrix composites (CMCs), such as high temperature strength, corrosion resistance, high toughness, low density, or good creep resistance have led to increased use of CMCs in high-speed engine structural components and structures that operate in extreme temperature and hostile aero-thermo-chemical environments. Ceramic matrix composites have been chosen for turbine material in the design of 21st century civil propulsion systems to achieve high fuel economy, improved reliability, extended life, and reduced cost. Most commercial CMCs are manufactured using a chemical vapor infiltration (CVI) process. However, a lower cost fabrication known as melt-infiltration process is also providing CMCs marked for use in hot sections of high-speed civil transports. Limited samples of a SiC/SiC melt-infiltrated woven composites are being investigated at room and elevated temperature below and above matrix cracking. These samples show graceful failure and toughness at room temperature with a reduction in strength and modulus at elevated temperatures. A generic finite element model is also being developed to predict monotonic and cyclic loading behavior of the woven composite. Use of the initial test data from the woven composite is being used for the development of the analytical model. This model is the first of a iterative process leading towards the development the model's capability to predict behavior at room and elevated temperature for monotonic and cyclic loading. The purpose of this paper is to report on the material and mechanical findings of the SiC/SiC melt-infiltrated woven composite and progress on the development of the finite element model.

Lang, J.↗

NASA NTRS1993

Flexure Test For Off-Axis Unidirectional Composites

Improved flexure test yields data on ply strength of off-axis unidirectional composite material. Rotatable end supports allow ends of specimen to twist freely. End supports apply only vertical loads, making simple three-point bending test. Ply-strength data provide basis for predicting onset of damage in composite structures and serve as measure of fiber-matrix adhesion.

Crews, John H., Jr.↗

NASA NTRS2015

Nonlinear Analysis and Preliminary Testing Results of a Hybrid Wing Body Center Section Test Article

A large test article was recently designed, analyzed, fabricated, and successfully tested up to the representative design ultimate loads to demonstrate that stiffened composite panels with through-the-thickness reinforcement are a viable option for the next generation large transport category aircraft, including non-conventional configurations such as the hybrid wing body. This paper focuses on finite element analysis and test data correlation of the hybrid wing body center section test article under mechanical, pressure and combined load conditions. Good agreement between predictive nonlinear finite element analysis and test data is found. Results indicate that a geometrically nonlinear analysis is needed to accurately capture the behavior of the non-circular pressurized and highly-stressed structure when the design approach permits local buckling.

Przekop, Adam↗

NASA NTRS2018

Freeze Casting of LAGP for 3D Textured Solid-State Structural Electrolytes

In this study, all-solid-state structural lithium-ion batteries, a type of load bearing electrochemical energy storage that provides systems-level weight savings is being pursued for the realization of inherently safe next generation hybrid-electric and all-electric green aerospace propulsion systems. Currently investigated all-solid-state batteries do not meet the requirements for specific power and mechanical stability. To address these issues, freeze casting of lithium aluminum germanium phosphate (LAGP) electrolyte material has been explored for the creation of a textured 3D electrolyte scaffold with large interfacial surface area for high power discharge and hierarchical porosity for accommodation of active material volume changes during electrochemical cycling. We report the effects of freeze casting processing parameters on the microstructural development and mechanical performance of the scaffolds, characterized through scanning electron microscopy and ring-on-ring mechanical testing. Slurry composition and casting parameters such as solids loading, casting speed, tape angle, and temperature gradients have been modified to determine the impact on density, lamellar morphology, and final load-bearing performance.

ceramics↗

NASA NTRS1989

Crashworthy design of helicopter composite airframe structures

The crashworthy behavior of composite materials and generic structural elements is investigated. Cruciform structural elements are crushed in order to determine their energy absorption capability to rotorcraft crash-type loads, and quasi-static compression tests are conducted on a series of aluminum and composite cruciform elements. These elements are representative of keel beam and bulkhead intersections in the subfloor of rotorcraft. Various designs of 'trigger mechanisms' reducing initial peak failure loads and initiating stable crushing failure modes are considered. It is shown that a carbon-fiber-composite/aramid-fiber-composite hybrid element with a columnlike midsection behaves more like a well-designed tubular composite element. Specimens which fail primarily in bending are typical of structural components used in the upper and lower portions of rotorcraft airframes.

Boitnott, Richard L.↗

NASA NTRS1981

Low-velocity impact tests on fibrous composite sandwich structures

The effect of low-velocity projectile impact on the load-carrying ability of the composite sandwich structural components is investigated experimentally, the impact simulating the damage caused by runway debris and the accidental dropping of hand tools during servicing on secondary aircraft structures made with composites. The sandwich-type beam specimens were fabricated with graphite/epoxy face sheets, aluminum honeycomb core, and a steel (back) plate. A four-point beam-loading apparatus was used, and the ultimate strength, ultimate strain, and residual strength of the composites were determined. A faired curve is presented indicating the lower bound of the failure threshold for each of the laminate configurations tested in compression and tension as a function of the projectile impact energy. It is shown that strength degradation due to impact is dependent on the laminate configuration and the fiber/matrix combination. The laminates having more angle plies near the impact surface and unidirectional plies elsewhere seem to show extensive interply and intraply fiber delaminations at failure relative to the laminates with a cross-ply on the impact surface.

Sharma, A. V.↗

NASA NTRS1985

Impact wear of iron rich superalloys

The impact-sliding wear resistance of chill cast and aligned eutectic Fe-base superalloys against M42 and 17-4 PH steel counterface materials is examined. The aligned material tests were run with carbide fibers perpendicular to the counterface contact surface and the characterization focused on fracture processes as observed in the subsurface microstructure of the worn materials. Metallographic analyses were performed on specimens exposed to various numbers of repetitive impact load cycles, and for comparison, two other aligned composites were tested with the same fiber orientation under identical test conditions against hardened M42 tool steel. A strong improvement was found in wear resistance of an aligned eutectic structure as compared to the corresponding randomized chill cast structure. Experiments with the softer 17-4 counterface were characterized by transfer onto the Fe-base superalloy, and the cracks formed were oriented transverse to the relative sliding direction and occurred in a periodic fashion. Observations in subsurface regions of the worn materials indicated crack intergranularity with an occasional transgranular fracture of the M7C3 carbide phase.

Wayne, S. F.↗

NASA NTRS1997

Ultrasonic Studies of Composites Undergoing Thermal and Fatigue Loading

New composite materials possess attractive properties for use in advanced aircraft. A necessary requirement for their introduction into aeronautic use is an accurate understanding of their long term aging processes so that proper design criteria can be established. In order to understand those properties, these composites must be exposed to thermal and load cycles that are characteristic of flight conditions. Additionally, airline companies will require nondestructive evaluation (NDE) methods that can be used in the field to assess the condition of these new materials as they age. As part of an effort to obtain the required information about new composites for aviation use, we are performing ultrasonic measurements both in the NDE laboratory and in the materials testing laboratory at NASA. The materials testing laboratory is equipped with environmental chambers mounted on load frames so that composite samples can be exposed to thermal and loading cycles representative of flight protocols. Applying both temperature and load simultaneously will help to highlight temperature and load interactions during the aging of these composite materials. This study reports on our initial ultrasonic attenuation results from thermoset and thermoplastic composite samples. Ultrasonic attenuation measurements have been used reliably to assess the effects of material degradation. For example, recently, researchers have shown that by using frequencies of ultrasound on the order of 24 MHz, they could obtain adequate contrast in the evaluation of thermal degradation in these composites. This paper will present data that shows results at a lower frequency range. In addition, we report results on the frequency dependence of attenuation as the slope of attenuation with respect to frequency, beta = delta alpha (f) / delta f. The slope of attenuation is an attractive parameter since it is quantitative, yet does not require interface corrections like conventional quantitative attenuation measurements. This is a consequence of the assumption that interface correction terms are frequently independent. Uncertainty in those corrections terms compromises the value of conventional quantitative attenuation data.

Madaras, Eric I.↗