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Effects of Electrons, Protons, and Ultraviolet Radiation on Thermophysical Properties of Polymeric Films

The response of coated thin polymer films to ultraviolet (UV), electron and proton radiation simultaneously has been evaluated, with selected measurements in situ. Exposure was intended to simulate the electron and proton radiation environment near the Earth-Sun Lagrangian points (LI and L2) for five years and approximately 1000 equivalent solar hours (ESH) UV. These orbital environments are relevant to several potential missions such as the Next Generation Space Telescope and Geomagnetic Storm Warning, both of which may use thin film based structures for a sunshade and solar sail, respectively. The thin film candidates (12.5 micrometers thick) consisted of commercially available materials (Kapton(R) E, HN, Upilex(R) S, CP-1, CP-2, TOR-RC, and TOR-LMBP) that were metalized on one side with vapor deposited aluminum. All of the films are aromatic polyimides, with the exception of TORLMBP, which is a copoly(arylene ether benzimidazole). The films were exposed as second surface mirrors and the effects of the exposure on solar absorptance, thermal emittance, and tensile properties were determined. The in situ changes in solar absorptance from Kapton(R) and Upilex(R) were less than 0. 1, whereas the solar absorptance of TOR and CP films increased by more than 0.3 without saturating. The thermal emittance measurements also showed that the Kapton(R) and Upilex(R) materials increased only 1-2%, but the remaining materials increased 5-8%. Based on tensile property measurements made in air following the test, the failure stress of every type of polymer film decreased as a result of irradiation. The polymers most stable in reflectance, namely Upilex(R) and Kapton(R), were also the strongest in tension before irradiation, and they retained the greatest percentage of tensile strength. The films less stable in reflectance were also weaker in tension, and lost more tensile strength as a result of irradiation. The apparent failure strain (as a percent of original gage length) of every type of polymer film except TOR-RC, decreased as a result of irradiation.

Russell, Dennis A.↗

High Temperature Si-doped BN Interphases for Woven SiC/SiC Composites

The hydrolytic stability of high-temperature deposited Si-doped BN has been shown in the past to be superior in comparison to "pure" BN processed at similar or even higher temperatures. This type of material would be very desirable as a SiC/SiC composite interphase that is formed by chemical infiltration into multi-ply woven preform. However, due to rapid deposition on the preform outer surface at the high processing temperature, this has proven very difficult. To overcome this issue, single plies of woven fabric were infiltrated with Si-doped BN. Three composite panels of different SiC fiber types were fabricated with Si-doped BN interphases including Sylramic, Hi-Nicalon Type S and Sylramic-iBN fiber-types. The latter fiber-type possesses a thin in-situ grown BN layer on the fiber surface. High Si contents (approx. 7 to 10 a/o) and low oxygen contents (less than 1 a/o) were achieved. All three composite systems demonstrated reasonable debonding and sliding properties. The coated Sylramic fabric and composites were weak due to fiber degradation apparently caused during interphase processing by the formation of TiN crystals on the fiber surface. The Hi-Nicalon Type S composites with Si-doped BN interphase were only slightly weaker than Hi-Nicalon Type S composites with conventional BN when the strength on the load-bearing fibers at failure was compared. On the other hand, the Sylramic-iBN fabric and composites with Si-doped BN showed excellent composite and intermediate temperature stress-rupture properties. Most impressive was the lack of any significant interphase oxidation on the fracture surface of stress-ruptured specimens tested well above matrix cracking at 815C.

Morscher, Gregory N.↗

NASA NCC2-1290 "Summary of Research" Report

Testing techniques for measuring the mechanical properties of SIRCA were refined and validated. These included tensile and compressive tests and stress-strain response. Analytic models were developed in order to explain initial experimental results.

Milstein, Fred↗

Multidisciplinary Probabilistic Heat Transfer/Structural Analysis Code Developed: NESTEM

High-Speed Civil Transport (HSCT) engine combustor liners are subjected to complex thermal environments and have to endure these for thousands of hours with assured reliability. In the past, several deterministic analyses have been performed, including detailed heat transfer analyses to obtain thermal profiles and deterministic stress analyses to identify critical locations of high stresses. Actual rig tests also have been performed for segments by simulating these loading situations as closely as possible. However, it is well known that many uncertainties exist in loading (primarily thermal loads due to heat transfer), boundary conditions (end fixity unknowns), and material properties (moduli, thermal-expansion coefficients, and conductivities). The present in-house effort at the NASA Lewis Research Center is directed toward accounting for these in a formal way to assess the performance of liner components under complex and uncertain loading conditions as well as subject to other geometry- and material-related uncertainties.

Murthy, Pappu L. N.↗

New Oxide Ceramic Developed for Superior High-Temperature Wear Resistance

Ceramics, for the most part, do not have inherently good tribological properties. For example friction coefficients in excess of 0.7 have been reported for silicon nitride sliding on silicon nitride or on bearing steel (ref. 1). High friction is always accompanied by considerable wear. Despite their inherently poor tribological properties, the high strength and high toughness of silicon nitride (Si3N4) ceramics has led to their successful use in tribological applications (refs. 1 to 4). The upper temperature limit for the application of Si3N4 as wear-resistant material is limited by reaction with the tribological environment (ref. 3). Silicon nitride is known to produce a thin silicon dioxide film with easy shear capability that results in low friction and low wear in a moist environment (ref. 5). At elevated temperatures, the removal of the reaction product that acts as lubricant causes the friction coefficient to increase and, consequently, the wear performance to become poor. New materials are sought that will have wear resistance superior to that of Si3N4 at elevated temperatures and in harsh environments. A new class of oxide ceramic materials has been developed with potential for excellent high-temperature wear resistance. The new material consists of a multicomponent oxide with a two-phase microstructure, in which the wear resistance of the mixed oxide is significantly higher than that of the individual constituents. This is attributed to the strong constraining effects provided by the interlocking microstructures at different length scales, to the large aspect ratio of the phases, to the strong interphase bonding, and to the residual stresses. Fretting wear tests were conducted by rubbing the new ceramic material against boron carbide (B4C). The new ceramic material produced a wear track groove on B4C, suggesting significantly higher wear resistance for the oxide ceramic. The new material did not suffer from any microstructural degradation after the wear test. The wear rate of the new ceramic material at 600 C was determined to be on the order of 10-10 mm3/N-m, which is 3 to 5 orders of magnitude lower than that for the current state-of-theart wear-resistant materials (Si3N4and B4C). The friction coefficient of the new ceramic materials is on the order of 0.4, which is significantly lower than that of silicon nitride. This new class of oxide materials has shown considerable potential for applications requiring high wear resistance at high temperatures and in harsh environments. New understanding of the wear behavior of ceramic materials is emerging as a result of the surprisingly high wear resistance of two-phase oxide ceramics. There is excellent potential for further improvements in the wear resistance of oxide ceramics through optimizing the microstructure and altering the crystallographic properties of specific oxide materials as a second phase to reduce the coefficient of friction at elevated temperatures.

Sayir, Ali↗

Distribution of Inclusion-Initiated Fatigue Cracking in Powder Metallurgy Udimet 720 Characterized

In the absence of extrinsic surface damage, the fatigue life of metals is often dictated by the distribution of intrinsic defects. In powder metallurgy (PM) alloys, relatively large defects occur rarely enough that a typical characterization with a limited number of small volume fatigue test specimens will not adequately sample inclusion-initiated damage. Counterintuitively, inclusion-initiated failure has a greater impact on the distribution in PM alloy fatigue lives because they tend to have fewer defects than their cast and wrought counterparts. Although the relative paucity of defects in PM alloys leads to higher mean fatigue lives, the distribution in observed lives tends to be broader. In order to study this important failure initiation mechanism without expending an inordinate number of specimens, a study was undertaken at the NASA Glenn Research Center where known populations of artificial inclusions (seeds) were introduced to production powder. Fatigue specimens were machined from forgings produced from the seeded powder. Considerable effort has been expended in characterizing the crack growth rate from inclusion-initiated cracks in seeded PM alloys. A rotating and translating positioning system, with associated software, was devised to map the surface inclusions in low-cycle fatigue (LCF) test bars and to monitor the crack growth from these inclusions. The preceding graph illustrates the measured extension in fatigue cracks from inclusions on a seeded LCF test bar subjected to cyclic loading at a strain range of 0.8 percent and a strain ratio (max/min) of zero. Notice that the observed inclusions fall into three categories: some do not propagate at all (arrest), some propagate with a decreasing crack growth rate, and a few propagate at increasing rates that can be modeled by fracture mechanics. The following graph shows the measured inclusion-initiated crack growth rates from 10 interrupted LCF tests plotted against stress intensities calculated for semi-elliptical cracks with the observed surface lengths. The expected scatter in the crack growth rates for stress intensity ranges near threshold is observed. These data will be used to help determine the distribution in growth rates of cracks emanating from inclusions as well as the proportion of cracks that arrest under various loading conditions.

Bonacuse, Peter J.↗

Fracture Mechanics Analysis of LH2 Feed Line Flow Liners

Inspections of the Space Shuttle Main Engine revealed fatigue cracks growing from slots in the flow liner of the liquid hydrogen (LH2) feed lines. During flight, the flow liners experience complex loading induced by flow of LH2 and the resonance characteristics of the structure. The flow liners are made of Inconel 718 and had previously not been considered a fracture critical component. However, fatigue failure of a flow liner could have catastrophic effect on the Shuttle engines. A fracture mechanics study was performed to determine if a damage tolerance approach to life management was possible and to determine the sensitivity to the load spectra, material properties, and crack size. The load spectra were derived separately from ground tests and material properties were obtained from coupon tests. The stress-intensity factors for the fatigue cracks were determined from a shell-dynamics approach that simulated the dominant resonant frequencies. Life predictions were obtained using the NASGRO life prediction code. The results indicated that adequate life could not be demonstrated for initial crack lengths of the size that could be detected by traditional NDE techniques.

James, Mark A.↗

Strain Measurement during Stress Rupture of Composite Over-Wrapped Pressure Vessel with Fiber Bragg Gratings Sensors

Fiber optic Bragg gratings were used to measure strain fields during Stress Rupture (SSM) test of Kevlar Composite Over-Wrapped Pressure Vessels (COPV). The sensors were embedded under the over-wrapped attached to the liner released from the Kevlar and attached to the Kevlar released from the liner. Additional sensors (foil gages and fiber bragg gratings) were surface mounted on the COPY liner.

Banks, Curtis E.↗

Probabilistic Analysis for Comparing Fatigue Data Based on Johnson-Weibull Parameters

Leonard Johnson published a methodology for establishing the confidence that two populations of data are different. Johnson's methodology is dependent on limited combinations of test parameters (Weibull slope, mean life ratio, and degrees of freedom) and a set of complex mathematical equations. In this report, a simplified algebraic equation for confidence numbers is derived based on the original work of Johnson. The confidence numbers calculated with this equation are compared to those obtained graphically by Johnson. Using the ratios of mean life, the resultant values of confidence numbers at the 99 percent level deviate less than 1 percent from those of Johnson. At a 90 percent confidence level, the calculated values differ between +2 and 4 percent. The simplified equation is used to rank the experimental lives of three aluminum alloys (AL 2024, AL 6061, and AL 7075), each tested at three stress levels in rotating beam fatigue, analyzed using the Johnson- Weibull method, and compared to the ASTM Standard (E739 91) method of comparison. The ASTM Standard did not statistically distinguish between AL 6061 and AL 7075. However, it is possible to rank the fatigue lives of different materials with a reasonable degree of statistical certainty based on combined confidence numbers using the Johnson- Weibull analysis. AL 2024 was found to have the longest fatigue life, followed by AL 7075, and then AL 6061. The ASTM Standard and the Johnson-Weibull analysis result in the same stress-life exponent p for each of the three aluminum alloys at the median, or L(sub 50), lives

Vlcek, Brian L.↗

NASA Physics of Failure (PoF) for Reliability

An item’s reliability or longevity is dependent not only on its design but also on how it is used, manufactured, tested, and the stresses it has or will experience. Stresses include operational and environmental exposures to thermal, voltage, current, age/exposure, mechanical, and radiation mechanisms. Therefore, in reliability analysis, it is important to consider the contributions of all of these factors when predicting the failure rates of components. Historically, there has been a reliance on handbook data (e.g., MIL-HDBK-217), but experience has shown that these values and distributions are not representative of actual performance (1,2). Therefore, to make more credible reliability and risk assessments for its missions, NASA must transition to estimating likelihoods of failure based on an item’s reliability/longevity factors (or the physical susceptibilities and strengths impacting the design’s performance) has or will experience, whenever possible. To facilitate this transition a “Handbook on Methodology for Physics of Failure Based Reliability Assessments” has been developed by NASA to assist in applying physics experiences or experiment physics for empirical analysis and conceptualized physics exposures or theoretical physics for deterministic analysis, to develop and aggregate realistic likelihoods of failure leading to more credible forecasts of item performance and longevity. In addition, since it is NASA’s intention that this document continues to evolve based on community lessons learned and the introduction of new assessment methodologies, NASA is encouraging and appreciates the contributions of current and future authors to maintain and enhance this handbook and its supporting case studies.

Physics of Failure↗

NASA Physics of Failure (PoF) for Reliability

An item’s reliability or longevity is dependent not only on its design but also on how it is used, manufactured, tested, and the stresses it has or will experience. Stresses include operational and environmental exposures to thermal, voltage, current, age/exposure, mechanical, and radiation mechanisms. Therefore, in reliability analysis, it is important to consider the contributions of all these factors when predicting the failure rates of components. Historically, there has been a reliance on handbook data (e.g., MIL-HDBK-217), but experience has shown that these values and distributions are not representative of actual performance. Therefore, to make more credible reliability and risk assessments for its missions, NASA must transition to estimating likelihoods of failure based on an item’s reliability or longevity factors (or the physical susceptibilities and strengths impacting the design’s performance) has or will experience, whenever possible. To facilitate this transition, a Handbook on Methodology for Physics of Failure Based Reliability Assessments has been developed by NASA to assist in applying physics experiences or experimental physics for empirical analysis and conceptualized physics exposures or theoretical physics for deterministic analysis, to develop and aggregate realistic likelihoods of failure leading to more credible forecasts of item performance and longevity. In addition, since it is NASA’s intention that this document continues to evolve based on community lessons learned and the introduction of new assessment methodologies, NASA is encouraging and appreciates the contributions of current and future authors to maintain and enhance this handbook and its supporting case studies.

PoF↗

Big Sky Regional Carbon Sequestration Partnership (Phase III Final Scientific/Technical Report)

The Big Sky Carbon Sequestration Partnership (BSCSP) pursued a Phase III demonstration project at Kevin Dome in north central Montana. Kevin Dome covers approximately 700 square miles and is a naturally occurring CO 2 reservoir that is flanked by oil and gas fields. The carbon dioxide (CO 2 ) is in the upper Devonian Duperow (carbonate) formation and does not reach the spill point of the dome; therefore, the dome has potential as a CO 2 sequestration reservoir, a CO 2 supply, or as both if anthropogenic sources and enhanced oil recovery (EOR) operations are associated with the dome. Kevin Dome could potentially act as a buffer to continue accepting anthropogenic CO 2 when EOR flooding operations are interrupted or completed. The project objective was to produce one million tonnes of CO 2 from the gas cap of Kevin Dome, pipe it laterally, inject, and re-store it in the brine leg of the same formation to test the hub / buffer storage concept. This was to be accomplished by drilling up to five production wells, building a short pipeline and compression facilities, and drilling an injection well and several monitoring wells. BSCSP commenced outreach and site characterization activities including acquiring baseline data for near-surface insurance monitoring, acquiring 3-dimensional, 9-component surface seismic over the project area, drilling two test wells (one in the production area and one in the injection area), coring key intervals, and performing comprehensive logging. Well tests of those wells revealed two barriers to the project. The production (Danielson 33-17) well was perforated in multiple zones but failed to produce any significant CO 2 . This was despite being drilled in the near vicinity of a historic well that had produced 3700 MCF per day in a drill stem test. Modeling indicated that this was likely due to a phase change during production causing a temperature drop resulting in hydrate and/or water ice formation that clogged the formation. Tests of the injection zone (Wallewein 22-1) well indicated total dissolved solids (TDS) slightly below the EPA required 10,000 parts per million (ppm) for a Class VI underground injection control permit. While the project was initiated before Class VI rules were promulgated, and this was an experimental project (seemingly qualified for a Class V permit), the Environmental Protection Agency (EPA) indicated that injection would require a Class VI permit. The low salinity result was unexpected as contours plotted based on regional formation water quality data indicated an expected TDS above 20,000 ppm, and wells between the recharge zone and the Wallewein well tested above 10,000 ppm. Faced with the inability to obtain an injection permit, the demonstration project could not proceed. However, the project had generated valuable samples and data on a large natural analog including 32 sq. mi. of 3-D, 9-C seismic, 430 ft. of carbonate core covering seven different depositional environments taken from areas with, and without the presence of CO 2 , 30 ft. of core of two caprocks, a tight carbonate and an anhydrite, a full set of modern logs on both wells, and well tests. DOE decided to re-scope the project around completing studies utilizing this data. This report covers both the initial scope and the re-scope (Task / Section numbers preceded with an R). While the report covers a wide range of project activities, highlights of this work include: Development of a geostatic model using neural nets to match well logs to facies and using multi-waveform seismic to inform reservoir heterogeneity; Unique mechanical testing of permeability – stress relationship in two caprock materials; Development of full waveform inversion to generate a high resolution velocity model; Model development for dual permeability (fracture and matrix) systems to better account for matrix-matrix interactions; Joint seismic wave inversion (including the first quadr-joint inversion) exhibiting better imaging of a challenging reservoir zone in stiff rock; Core flow and core flood results on a reactive carbonate; and Innovative laboratory measurements of seismic response of fractured core as a function of fluid fill.

54 ENVIRONMENTAL SCIENCES↗

Environmentally Assisted Cracking Research for Current and Advanced Nuclear Structural Materials

Understanding environmentally assisted cracking is an important aspect of nuclear materials research, as it provides information about failure mechanisms that lead to safety concerns or shutdowns. Idaho National Laboratory has ongoing research to understand how materials behave in the harsh nuclear environments for both the current fleet of light water reactors, as well as advanced reactors, where materials are exposed to more extreme environments. Corrosion and cracking of current materials, advanced materials, and materials formed through advanced manufacturing techniques are being examined, with particular interest in irradiation effects on corrosion and cracking, as well as the effects of environmental impurities. Testing, such as stress corrosion cracking, corrosion fatigue, and in-situ crack growth measurements, as well as a suite of characterization tools, including electron microscopy techniques and x-ray computed tomography, are being utilized to better understand the material response, limitations, and cracking mechanisms to ensure safe and reliable nuclear plants.

36 MATERIALS SCIENCE↗

Preliminary fatigue tests on short-crack specimens

The objective of the preliminary fatigue tests was to determine the stress levels to be used by the participants in the Cooperative Test Program. As previously mentioned, the United States Air Force Wright-Patterson Aeronautical Laboratory machined about 700 single-edge-notched tension (SENT) specimens from material supplied by the NASA Langley Research Center. In addition, NASA Langley machined about 50 SENT specimens from the same material. Comparison of fatigue tests conducted on the two sets of specimens indicated a large difference in fatigue behavior under constant-amplitude loading. A recovery program was initiated to resolve this difference before the specimens were distributed to participants. The following sections describe the recovery program and the preliminary fatigue tests and analyses conducted to determine stress levels for constant-amplitude, FALSTAFF, and Gaussian loading.

Newman, J. C., Jr.↗

Direct Shear Stress Sensor Characterization in the NASA 13” Flow Facility

This paper describes the testing of a commercially available shear stress sensor with emphasis on an examination of the output data and how variations in the output characteristics impacted the data analysis. The sensor itself is 0.625” in diameter with a length of 2” with a 0.375” diameter floating element and the sensor and housing constructed of stainless steel and aluminum. Shear stress was measured/calculated real time and compared to the output of the shear stress sensor. The range of testing was up to 15 Pa compared to the maximum calibrated range of 300 Pa for the sensor. The resultant sensitives of this device are within the expected range.

Shear Stress↗

Dynamic Breaking Tests of Airplane Parts

The static stresses of airplane parts, the magnitude of which can be determined with the aid of static load assumptions, are mostly superposed by dynamic stresses, the magnitude of which has been but little explored. The object of the present investigation is to show how the strength of airplane parts can best be tested with respect to dynamic stresses with and without superposed static loading, and to what extent the dynamic strength of the parts depends on their structural design. Experimental apparatus and evaluation methods were developed and tried for the execution of vibration-strength tests with entire structural parts both with and without superposed static loading. Altogether ten metal spars and spar pieces and two wooden spars were subjected to vibration breaking tests.

Hertel, Heinrich↗

Development of Methods for In-line Monitoring of Yield Stress During the Transfer of Radioactive Waste - 20435

Radioactive waste slurries at the Savannah River Site (SRS) and Hanford often behave as non-Newtonian fluids with a yield stress. The yield stress increases the size of equipment needed to transport or mix these slurries and can increase the risk of process upsets. This property is often measured by collection of samples and transportation to a laboratory, which can increase the risk of personnel exposure and even change the rheology. In addition, slurry rheology has been observed to change with time. Real-time in-line monitoring (RTIM) of rheological properties of slurries can have substantial benefits to critical processes which are currently in operation or will be part of future plans in Department of Energy (DOE) complex processes. The need for an appropriate RTIM technology that can potentially minimize or eliminate numerous sampling operations was recently identified. This research at Florida International University focuses on addressing the need for a reliable RTIM technology at US Department of Energy sites. The objective of this work is to investigate and develop appropriate and reliable technologies that can perform accurate and easy measurements of yield stress with minimal changes to the flow conditions at US Department of Energy sites. Use of ultrasound in longitudinal and shear modes was considered as a method for monitoring of yield stress variations with no disturbance to the flow. Measurement of shear wave velocity (in shear mode) and monitoring of sound velocity variations with start of flow from rest (longitudinal mode) are the underlying principles. Measurement of pressure loss and liquid rise (due to static differential pressure) during flow of slurries were two other methods that were considered and investigated. In addition, analysis of stability depth of a penetrometer in slurry medium (penetrometer method) revealed a potential suitability. This paper presents efforts associated with investigation of different methods mentioned earlier for kaolin-water mixtures at different concentrations. Theoretical analysis showed that all methods under investigation were capable of monitoring yield stress in a desirable range of 0 to 70 pascal. A bench scale test setup was constructed for investigation of pressure loss and liquid rise methods. Simulants at different concentrations were created for initial testing campaigns. For ultrasonic testing, effects of yield stress on sound propagation speed in longitudinal and shear modes were investigated for simulants placed inside PVC pipes. Parameters such as simulant concentration and pipe diameter were varied to find optimal values. It was found that spacing (or medium thickness) of 1/8 inch or less was necessary to observe echoes with sufficient strength. In addition, a significant effect of yield stress on sound propagation velocity was observed. For the liquid rise method, kaolin-water simulant at 1.17 specific gravity was pumped through a 1/4 inch pipe and liquid height was measured in a vertical riser branching off a three-way connection. Static gauge pressure was varied within [0.3 to 1.1] psi range by increase of pumping pressure and flow. Results showed consistent yield stress data within 10% deviation from values reported by a rheometer. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗