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At least 667 records · Page 37

Design, Fabrication, and Testing of Ceramic Joints for High Temperature SiC/SiC Composites

Various issues associated with the design and mechanical evaluation of joints of ceramic matrix composites are discussed. The specific case of an affordable, robust ceramic joining technology (ARCJoinT) to join silicon carbide (CG-Nicalon(sup TM)) fiber-reinforced-chemically vapor infiltrated (CVI) silicon carbide matrix composites is addressed. Experimental results are presented for the time and temperature dependence of the shear strength of these joints in air up to 1200 C. From compression testing of double-notched joint specimens with a notch separation of 4 mm, it was found that the apparent shear strength of the joints decreased from 92 MPa at room temperature to 71 MPa at 1200 C. From shear stress-rupture testing in air at 1200 C it was found that the shear strength of the joints decreased rapidly with time from an initial shear strength of 71 to 17.5 MPa after 14.3 hr. The implications of these results in relation to the expected long-term service life of these joints in applications at elevated temperatures are discussed.

Singh, Mrityunjay↗

Composite Overwrapped Pressure Vessels (COPV): Developing Flight Rationale for the Space Shuttle Program

Introducing composite vessels into the Space Shuttle Program represented a significant technical achievement. Each Orbiter vehicle contains 24 (nominally) Kevlar tanks for storage of pressurized helium (for propulsion) and nitrogen (for life support). The use of composite cylinders saved 752 pounds per Orbiter vehicle compared with all-metal tanks. The weight savings is significant considering each Shuttle flight can deliver 54,000 pounds of payload to the International Space Station. In the wake of the Columbia accident and the ensuing Return to Flight activities, the Space Shuttle Program, in 2005, re-examined COPV hardware certification. Incorporating COPV data that had been generated over the last 30 years and recognizing differences between initial Shuttle Program requirements and current operation, a new failure mode was identified, as composite stress rupture was deemed credible. The Orbiter Project undertook a comprehensive investigation to quantify and mitigate this risk. First, the engineering team considered and later deemed as unfeasible the option to replace existing all flight tanks. Second, operational improvements to flight procedures were instituted to reduce the flight risk and the danger to personnel. Third, an Orbiter reliability model was developed to quantify flight risk. Laser profilometry inspection of several flight COPVs identified deep (up to 20 mil) depressions on the tank interior. A comprehensive analysis was performed and it confirmed that these observed depressions were far less than the criterion which was established as necessary to lead to liner buckling. Existing fleet vessels were exonerated from this failure mechanism. Because full validation of the Orbiter Reliability Model was not possible given limited hardware resources, an Accelerated Stress Rupture Test of a flown flight vessel was performed to provide increased confidence. A Bayesian statistical approach was developed to evaluate possible test results with respect to the model credibility and thus flight rationale for continued operation of the Space Shuttle with existing flight hardware. A non-destructive evaluation (NDE) technique utilizing Raman Spectroscopy was developed to directly measure the overwrap residual stress state. Preliminary results provide optimistic results that patterns of fluctuation in fiber elastic strains over the outside vessel surface could be directly correlated with increased fiber stress ratios and thus reduced reliability.

Kezirian, Michael T.↗

Flaw growth of 7075, 7475, 7050 and 7049 aluminum alloy plate in stress corrosion environments

Marine atmosphere and laboratory stress corrosion test results on smooth and precracked specimens from 7075, 7475, 7050, and 7049 alloy plates (1.25 and 3.0-in. thick) are presented. It is shown that for a given strength level, alloys 7050-T7X and 7049-T7X have superior short-transverse stress corrosion resistance (SCR) to 7X75-T7X. At typical strength levels above the minimum, for example, SCR of these alloys is considerably better than that of 7075-T76, and approaches that of 7075-T73. Alloy 7475 maintains an advantage in the area of fracture toughness, however, because it can be thermally processed to give particularly clean microstructures. Results from precracked specimens are in good qualitative agreement with those obtained from smooth specimens. Although both specimen types are capable of distinguishing between -T6, -T76 and -T73 tempers in relatively short time periods the precracked specimen provides more information about crack growth rates.

Dorward, R. C.↗

The Evolution of Interfacial Sliding Stresses During Cyclic Push-in Testing of C- and BN-Coated Hi-Nicalon Fiber-Reinforced CMCs

Interfacial debond cracks and fiber/matrix sliding stresses in ceramic matrix composites (CMCs) can evolve under cyclic fatigue conditions as well as with changes in the environment, strongly affecting the crack growth behavior, and therefore, the useful service lifetime of the composite. In this study, room temperature cyclic fiber push-in testing was applied to monitor the evolution of frictional sliding stresses and fiber sliding distances with continued cycling in both C- and BN-coated Hi-Nicalon SiC fiber-reinforced CMCs. A SiC matrix composite reinforced with C-coated Hi-Nical on fibers as well as barium strontium aluminosilicate (BSAS) matrix composites reinforced with BN-coated (four different deposition processes compared) Hi-Nicalon fibers were examined. For failure at a C interface, test results indicated progressive increases in fiber sliding distances during cycling in room air but not in nitrogen. These results suggest the presence of moisture will promote crack growth when interfacial failure occurs at a C interface. While short-term testing environmental effects were not apparent for failure at the BN interfaces, long-term exposure of partially debonded BN-coated fibers to humid air resulted in large increases in fiber sliding distances and decreases in interfacial sliding stresses for all the BN coatings, presumably due to moisture attack. A wide variation was observed in debond and frictional sliding stresses among the different BN coatings.

Eldridge, J. I.↗

Determining the Reaction Kinetics and Thermodynamics of a Diels–Alder Network Using Dynamic Gel Criteria

We undertook a detailed rheological investigation to evaluate the kinetic parameters of the forward and reverse Diels–Alder (DA) reactions of a model network cross-linked using a furan prepolymer and a common aromatic bismaleimide. At high temperature where the Winter–Chambon’s criterion of frequency-independence was more applicable, a multiwave technique permitted van’t Hoff analysis and calculation of the reaction thermodynamic parameters, specifically the enthalpy and entropy of the reaction: ΔH° = –38.3 ± 5.2 kJ mol –1 and ΔS° = –94.3 ± 13.4 J mol –1 . At mild temperatures where the G'–G" crossover point is experimentally convenient to measure gelation, isothermal tests were used to obtain reasonable fDA kinetic parameters from Eyring analysis such as the apparent activation enthalpy and entropy of ΔH$^{‡}_{fDA}$ = 76.8 ± 6.9 kJ mol –1 and ΔS$^{‡}_{fDA}$= –82.8 ± 22.2 J mol –1 K –1 . Comparable rheokinetic methods include cross-linking density measurements and stress relaxation tests to calculate effective kinetics, whereas the critical gel conversion was consistently applied here. As a result, rate data are fitted with the Arrhenius equation for comparison purposes and the Eyring equation to demonstrate its broader utility.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High temperature compounds for turbine vanes

Fabrication and microstructure control studies were conducted on SiC, Si3N4, and composites based on these compounds. Charpy mode impact testing to 2400 F established that beta-spodumene, lithium aluminum silicate, coated Si3N4, Si3N4 derived from alpha-Si3N4 powder, and SiC containing 5-25 v/o chopped C fibers had the most promising strengths. Several other composite systems had excellent microstructures and could prove interesting materials in the future. Stress-rupture testing on Si3N4 established that increasing 2000 F - 100 hour strengths were obtained for increasing grain size to at least 5 micrometers, increasing density and possibly increasing phase purity. These parameters became less important at 2400 F where it is thought a grain boundary phase controls strength.

Rhodes, W. H.↗

Residual Silicone Detection

Both photoelectron emission and ellipsometry proved successful in detecting silicone contamination on unpainted and epoxy painted metal surfaces such as those of the external tank and the solid rocket booster. Great success was achieved using photoelectron emission (PEE). Panels were deliberately contaminated to controlled levels and then mapped with PEE to reveal the areas and levels that were contaminated. The panels were then tested with regard to adhesive properties. Tapes were bonded over the contaminated and uncontaminated regions and the peel force was measured, or the contaminated panels were bonded (with CPR 483 foam) to uncontaminated panels and made into lap shear specimens. Other panels were bonded and made into wedge specimens for hydrothermal stress endurance tests. Strong adhesion resulted if the PEE signal fell within an acceptance window, but was poor outside the acceptance window. A prototype instrument is being prepared which can automatically be scanned over the external liquid hydrogen tank and identify those regions that are contaminated and will cause bond degradation.

Smith, T.↗

Model 9975 O-Ring Fixture Long-Term Leak Performance (FY2022 Status Report)

Leak testing experiments to monitor the aging performance of Viton® GLT and GLT-S O-rings used in the model 9975 shipping package has been ongoing since 2004 at Savannah River National Laboratory. Seventy tests using mock-up 9975 primary containment vessels (PCVs) with GLT O-rings were assembled and heated to temperatures ranging from 200 to 450 °F. Due to material substitution, fourteen tests with GLT-S O-rings were initiated in 2008 and heated to temperatures ranging from 200 to 400 °F. The conditioning temperatures are elevated compared to the calculated maximum O-ring temperature in a 9975 package in storage, 158 °F, to accelerate aging and enable observations of O-ring failures in a reasonable time frame. The fixtures are leak tested periodically and all GLT O-ring fixtures aging at 350 °F or above have failed to maintain a leak-tight seal. Eight GLT O-ring fixtures aging at 300 °F have failed after 2.8 to 5.7 years at temperature while the remaining fixtures at 300 °F were retired from testing following more than five years without failure. There has been one GLT O-ring fixture which failed after 13.4 years aging at 200 °F. However, 20 other GLT O-rings aging at 200 °F have remained leak-tight for over 14 years and remain in test. No failures have yet been observed in GLT O-ring fixtures aging at 270 °F for 10.4 years. All GLT-S O-ring fixtures aging at 300 °F or above have failed their leak test. No failures have yet been observed in GLT-S O-ring fixtures aging at 250 °F for 12.5 years. This year, one GLT-S O-ring fixture failed after 12.4 years aging at 200 °F. Data from the O-ring fixtures are generally consistent with results from compression stress-relaxation testing, and provide confidence in the predictive models based on those results. However, uncertainty exists in extrapolating these elevated temperature results to the lower temperatures of interest for normal storage in K-Area Complex (KAC). Oxygen consumption testing, which includes results from temperatures near KAC normal storage temperatures, is ongoing to provide further confidence and corroborate these extrapolations. The collective data from these test efforts suggest the minimum O-ring service life at KAC normal storage conditions should be at least 34 years for GLT and GLT-S O-rings. Measurement of compression set in O-rings removed from failed fixtures, compared to that from KAC surveillance O-rings, indicate significant margin remains for O-rings still in service in 9975 packages in KAC. Aging and periodic leak testing will continue for the remaining 25 mock-up PCV fixtures.

36 MATERIALS SCIENCE↗

FY2025 Status Report: Model 9975 O Ring Fixture Long-Term Leak Performance

Leak testing experiments to monitor the aging performance of Viton® GLT and GLT-S O-rings used in the model 9975 shipping package have been ongoing since 2004 at Savannah River National Laboratory. Seventy tests using mock-up 9975 primary containment vessels (PCVs) with GLT O-rings were assembled and heated to temperatures ranging from 200 to 450 °F. Due to material substitution, fourteen tests with GLT-S O-rings were initiated in 2008 and heated to temperatures ranging from 200 to 400 °F. The conditioning temperatures are elevated compared to the calculated maximum O-ring temperature in a 9975 package in storage, 158 °F, to accelerate aging and enable observations of O-ring failures in a reasonable time frame. The mock-up PCV fixtures are leak tested periodically, and all GLT O-ring fixtures aged at 350 °F or above have failed to maintain a leak-tight seal. Eight GLT O-ring fixtures aged at 300 °F have failed after 2.8 to 5.7 years at temperature while the remaining fixtures at 300 °F were retired from testing following more than five years of aging without failure. Two of these retired fixtures were returned to testing and heated to 350 °F to evaluate the impact of additional heating at higher temperature for aged O-rings. Fixture #20 failed after 3 months while fixture #18 failed after 9 months at 350 °F. These O-rings demonstrated that aged and in-service O-rings can continue to be used, even at higher temperatures, after being in storage, and their leak performance are consistent with other samples at 350 °F. There has been one GLT O-ring fixture which failed after 13.4 years of aging at 200 °F. However, 20 other GLT O-rings aging at 200 °F have remained leak-tight for over 16.9 years and remain in test. There are two GLT O-ring fixtures at 270 °F; one fixture has failed after 12.9 years while the other fixture remains in test after 12.5 years. All GLT-S O-ring fixtures aged at 300 °F or above have failed their leak test. No failures have yet been observed in GLT-S O-ring fixtures aging at 250 °F for 14.9 years, while one GLT-S O-ring fixture failed after 12.4 years at 200 °F. The leak testing data to date suggest the GLT and GLT-S O-rings aging in the K-Area Complex (KAC) storage at temperatures of 158 °F might maintain a leak-tight seal for up to 59 years. Data from the O-ring fixtures are generally consistent with results from compression stress-relaxation testing and provide confidence in the predictive models based on those results. However, uncertainty exists in extrapolating these elevated temperature results to the lower temperatures of interest for normal storage in KAC. The collective data from these test efforts suggest the minimum O-ring service life at KAC normal storage conditions should be at least 34 years for GLT and GLT-S O-rings. Measurement of compression set in O-rings removed from failed fixtures, compared to that from KAC surveillance O-rings, indicate significant margin remains for O-rings still in service in 9975 packages in KAC. Aging and periodic leak testing will continue for the remaining 24 mock-up PCV fixtures.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Oxidation- and Creep-Enhanced Fatigue of Haynes 188 Alloy-Oxide Scale System Under Simulated Pulse Detonation Engine Conditions

The development of the pulse detonation engine (PDE) requires robust design of the engine components that are capable of enduring harsh detonation environments. In this study, a high cycle thermal fatigue test rig was developed for evaluating candidate PDE combustor materials using a CO2 laser. The high cycle thermal fatigue behavior of Haynes 188 alloy was investigated under an enhanced pulsed laser test condition of 30 Hz cycle frequency (33 ms pulse period, and 10 ms pulse width including 0.2 ms pulse spike). The temperature swings generated by the laser pulses near the specimen surface were characterized by using one-dimensional finite difference modeling combined with experimental measurements. The temperature swings resulted in significant thermal cyclic stresses in the oxide scale/alloy system, and induced extensive surface cracking. Striations of various sizes were observed at the cracked surfaces and oxide/alloy interfaces under the cyclic stresses. The test results indicated that oxidation and creep-enhanced fatigue at the oxide scale/alloy interface was an important mechanism for the surface crack initiation and propagation under the simulated PDE condition.

Zhu, Dongming↗

Viscoelastic properties of addition-cured polyimides used in high temperature polymer matrix composites

The viscoelastic properties of an addition-cured polyimide, PMR-15, were evaluated through dynamic mechanical and stress relaxation testing. Below the glass transition temperature, the dynamic mechanical properties of the composites are strongly affected by the absorbed moisture in the resin. At temperature 20 C and more above the glass transition temperature, the storage modulus increases continuously with time, indicating that additional crosslinking is occurring in the resin. For resin moisture contents less than 2 percent, stress relaxation curves measured at different temperatures can be superimposed using horizontal shifts along the log(time) axis with only small shifts along the vertical axis.

Roberts, Gary D.↗

Effect of reduction of strategic Columbium addition in 718 Alloy on the structure and properties

A series of alloys was developed having a base composition similar to Inconel 718, with reduced Cb levels of 3.00 and 1.10 wt% Cb. Substitutions of 3.0% W, 3.0W + 0.9V or Mo increased from 3.0% to 5.8% were made for the Cb in these alloys. Two additional alloys, one containing 3.49% Cb and 1.10% Ti and another containing 3.89% Cb and 1.29% Ti were also studied. Tensile properties at rooom and elevated temperatures, stress-rupture tests, and an analysis of extracted phases were carried out for each of the alloys. Additions of solid solution elements to a reduced Cb alloy had no significant effect on the properties of the alloys under either process condition. The solution and age alloys with substitutions of 1.27% i at 3.89% Cb had tensile properties similar top hose of the original alloy and stress-rupture properties superior to the original alloy. The improved stress-rupture properties were the result of significant precipitation of Ni3Ti-gamma prime in the alloy, which is more stable than gamma' at the elevated temperatures. At lower temperatures, the new alloy benefits from gamma' strengthening. With more precise control and proper processing, the reduced Cb direct-age alloy could substitute for Alloy 718 in high strength applications.

Ziegler, K. R.↗

Fabrication of Pop-up Detector Arrays on Si Wafers

High sensitivity is a basic requirement for a new generation of thermal detectors. To meet the requirement, close-packed, two-dimensional silicon detector arrays have been developed in NASA Goddard Space Flight Center. The goal of the task is to fabricate detector arrays configured with thermal detectors such as infrared bolometers and x-ray calorimeters to use in space fliGht missions. This paper focuses on the fabrication and the mechanical testing of detector arrays in a 0.2 mm pixel size, the smallest pop-up detectors being developed so far. These array structures, nicknamed "PUDS" for "Pop-Up Detectors", are fabricated on I pm thick, single-crystal, silicon membranes. Their designs have been refined so we can utilize the flexibility of thin silicon films by actually folding the silicon membranes to 90 degrees in order to obtain close-packed two-dimensional arrays. The PUD elements consist of a detector platform and two legs for mechanical support while also serving as electrical and thermal paths. Torsion bars and cantilevers connecting the detector platform to the legs provide additional flexures for strain relief. Using micro-electromechanical structure (MEMS) fabrication techniques, including photolithography, anisotropic chemical etching, reactive-ion etching, and laser dicing, we have fabricated PLTD detector arrays of fourteen designs with a variation of four parameters including cantilever length, torsion bar length and width, and leg length. Folding tests were conducted to test mechanical stress distribution for the array structures. We obtained folding yields and selected optimum design parameters to reach minimal stress levels. Computer simulation was also employed to verify mechanical behaviors of PUDs in the folding process. In addition, scanning electron microscopy was utilized to examine the flatness of detectors and the alignment of detector pixels in arrays. The fabrication of thermistors and heaters on the pop-up detectors is under way, preparing us for the next step of the experiment, the thermal test.

Li, Mary J.↗

Integrated flow and structural modeling for rocket engine component test facility propellant systems

A set of PC-based computational Dynamic Fluid Flow Simulation models is presented for modeling facility gas and cryogenic systems. Data obtained provide important information regarding performance envelope parameters for the facility using different engine components; time-dependent valve setting for controlling steady-state, quasi-steady state, and transient profiles; optimum facility pipe and pipe component sizes and parameters; momentum transfer loads; and fluid conditions at critical points. A set of COSMIC NASTRAN-based finite element models is also presented to evaluate the loads and stresses on test facility piping systems from fluid and gaseous effects, thermal chill down, and occasional wind loads. The models are based on Apple Macintosh software which makes it possible to change numerous parameters.

Dequay, L.↗

Structural analysis of an NDE-inspected carbon-carbon component

In this research, it is demonstrated that the integration of nondestructive evaluation with the finite element method (a quantitative NDE/FEM approach) can be used for analysis and behavior prediction of advanced materials, such as fiber composites, after processing and during in-service testing. First, stress, strain, and energy data were calculated by the finite element method for square plates with a 10 percent difference in the material properties between specified segments, i.e., between the center and the outside section or between two halves of the plate. This demonstrated the efficiency of the method in predicting variations in the structural behavior based on small material property differences. Then, finite element analyses and actual axial compression tests were performed on a Space Shuttle brake stator made from woven carbon-carbon composites. The material properties used in the numerical modeling of the stator were previously characterized at a large number of points on the component by quantitative NDE-procedures, i.e., ultrasonics and radiography. The results from the experimental compressive loading tests were used to verify the NDE/FEM results. Good agreement was found for most parameters.

Striz, A. G.↗

Flaw growth of 7075, 7475, 7050 and 7049 aluminum alloy plate in stress corrosion environments: 4-year marine atmosphere results

After nearly 53 months of exposure to marine atmosphere, crack growth in SL DCB specimens from 7075, 7475, 7050, and 7049-T7X plate has slowed to the arbitrary 10 to the -10 power m/sec used to define threshold stress intensity. Because some specimens appear to be approaching crack arrest, the importance of self-loading from corrosion product wedging as a significant driving force for crack propagation in overaged materials is questioned. Crack length-time data were analyzed using a computer curve fitting program which minimized the effects of normal data scatter, and provided a clearer picture of material performance. Precracked specimen data are supported by the results of smooth specimen tests. Transgranular stress corrosion cracking was observed in TL DCB specimens from all four alloys. This process is extremely slow and is characterized by a striated surface morphology.

Hasse, K. R.↗

Strain shift measured from stress-controlled oscillatory shear: Evidence for a continuous yielding transition and new techniques to determine recovery rheology measures

Understanding the yielding of complex fluids is an important rheological challenge that affects our ability to engineer and process materials for a wide variety of applications. Common theoretical understandings of yield stress fluids follow the Oldroyd–Prager formalism in which the material behavior below the yield stress is treated as solidlike, and above the yield stress as liquidlike, with an instantaneous transition between the two states. This formalism was built on a quasi-static approach to the yield stress, while most applications, ranging from material processing to end user applications, involve a transient approach to yielding over a finite timescale. Using stress-controlled oscillatory shear experiments, we show that yield stress fluids flow below their yield stresses. This is quantified through measuring the strain shift, which is the value about which the strain oscillates during a stress-controlled test and is a function of only the unrecoverable strain. Measurements of the strain shift are, therefore, measurements of flow having taken place. These experimental results are compared to the Herschel–Bulkley form of the Saramito model, which utilizes the Oldroyd–Prager formalism, and the recently published Kamani–Donley–Rogers (KDR) model, in which one constitutive equation represents the entire range of material responses. Scaling relationships are derived, which allow us to show why yield stress fluids will flow across all stresses, above and below their yield stress. Finally, derivations are presented that show strain shift can be used to determine average metrics previously attainable only through recovery rheology, and these are experimentally verified.

Mechanics↗