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DOE OSTI2022

Microsized Pore Structure Determination in EPDM Rubbers Using High-Pressure 129 Xe NMR Techniques

Microsized pore parameters, such as pore size and distance between pores in a series of model EPDM rubbers, were determined in situ under the pressure of 500 psi using 129 Xe nuclear magnetic resonance (NMR) techniques: spin–lattice (T 1 ) and spin–spin (T 2 ) relaxation measurements, pulsed-field gradient (PFG) NMR, and two-dimensional exchange spectroscopy (2D EXSY). The T 1 /T 2 (>>1) ratio for the xenon confined in the pores is larger than that for nonconfined free xenon. This suggests that almost the entire pore surface interacts with xenon atoms like a closed pore. While these pores still connect each other through very narrow diffusion/exchange channels, it is possible to observe the echo decay in PFG-NMR and cross-peaks in 2D EXSY. The results show that both diffusion (D pore ≈ 2.1 × 10 –10 m 2 /s) and exchange (exchange rate, τ exch = a few tens of milliseconds) of xenon between a pore within the material and outer surface are prolonged. The exchange distances (l), which correspond to the xenon gas penetration depth, were estimated to be 70–100 μm based on the measured diffusion coefficients and exchange rate (1/τ exch ). NMR diffraction analysis reveals that pore size (a) and pore distance (b) are on the order of magnitude of micrometers and tens of micrometers, while the diffusion coefficients of xenon gas in the diffusion channels (D eff ) are about 10 –8 m 2 /s. Overall, this study suggests that the pores with a few micrometers connected through very narrow flowing channels with the length of several tens of micrometers are developed 70 to 100 μm below the rubber surface. Furthermore, the overall steady-state diffusion of xenon is slower, approximately 2 orders of magnitudes, than the diffusion in the channel between the pores. Finally, the pore and exchange distances correlated with the composition of rubbers showed that the properties of EPDM rubber as a high-pressure gas barrier could be improved by reducing the size of cracks and the depth of gas penetration by the addition of both carbon black and silica fillers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Impact of Thermal Stress on Attachment and Stability of High Temperature Strain Sensors

Static and dynamic strain sensing is required in high-temperature (HT), harsh-environments (HE) for industrial, aerospace, and energy sector applications to ensure equipment and process safety, reduce the cost of operation and maintenance, and increase process efficiency. Challenges that arise in HT HE sensing applications include device mounting, packaging, integrity, and stability to HT HE conditions. In previously reported work, static and dynamic strain surface acoustic wave resonator (SAWR) sensors were fabricated on langasite (LGS) and mounted on Inconel 625 strain beams for wireless testing up to 400°C. In this work, it has been identified that after subjecting the mounted SAWR strain sensor to thermal cycling between 100°C and 425°C, the measured sensitivity to dynamic strain decreased by 73% due to cracking at the adhesive/LGS interface, further deteriorating after additional thermal cycles. Strain modeling of the mounted LGS sensor chip up to 400°C revealed the existence of concentrated strain at the borders of the LGS chip. Microcracks caused by dicing make the chip boarders the most susceptible location for cracks to initiate when the sensor is subjected to thermal stress. In an attempt to mitigate the high strain at the LGS chip borders due to heating, adhesive shaping is proposed in this work. Simulations indicate a strain reduction of 50% at the border is achieved using both circular and triangular adhesive shapes, while also reducing the maximum strain over the entire adhesive/LGS interface by around 30%. Furthermore, the technique is thus promising for improving the integrity, reliability, and stability of static and dynamic strain sensors, particularly while operating under HT HE with several hundreddegree Celsius temperature excursions.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

Mechanisms for the Generation of Complex Fracture Networks: Observations From Slant Core, Analog Models, and Outcrop

We use observations of hydraulic fractures in core, outcrop attributes of natural hydraulic fractures, and analogue models, to address how hydraulic fracture networks evolve. A slant core from the Wolfcamp Formation—an unconventional shale hydrocarbon reservoir in the Permian Basin of West Texas—collected within 18 m and 30 m of two hydraulically stimulated horizontal wells, provided an opportunity to examine hydraulic fractures directly. In approximately 183 m of core, 309 calcite-sealed natural opening-mode fractures and 375 hydraulic fractures were identified. Many hydraulic fractures in the core show complex morphology, including twist-hackle segmentation, diversion, and bifurcation; these structures most commonly develop at lithological bed boundaries and mechanical heterogeneities such as natural fractures and concretions. An outcrop of bed-parallel pavements in the Cretaceous Boquillas Formation in West Texas contains opening-mode fractures that likely formed by natural hydraulic fracturing. Fracture traces provide evidence of twist-hackle segmentation, and are typically associated with bed boundaries and preexisting bed-parallel stylolites. A laboratory study of hydraulic fracturing of 33 synthetic blocks of gypsum and hydrostone revealed fracture steps, diversions, twist hackles, and multiple overlapping fractures together with information on fracture growth directions. These complexities in the fracture network were dominantly nucleated at inclusions used to simulate pre-existing fractures, and as a result of mechanical heterogeneity introduced by the wellbore and perforations. Collectively, our results show that complex fracture networks are produced in hydraulic fracturing of self-sourced reservoir strata. Mechanical stratigraphic boundaries and other heterogeneities are likely to enhance fracture network complexity through the processes of segmentation, diversion, and bifurcation. These processes create multiple fracture strands, resulting in an increased number of hydraulic fractures over those initiated, thereby increasing total fracture surface area. Our study provides insight into hydraulic fracture network propagation, and has applications for evaluation, completion, production, and fracture modeling of unconventional reservoirs.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1987

A micrographic study of bending failure in five thermoplastic/carbon fiber composite laminates

The local deformation and failure sequences of five thermoplastic matrix composites were microscopically observed while bending the samples in a small fixture attached to a microscope stage. The themoplastics are polycarbonate, polysulfone, polyphenylsulfide, polyethersulfone, and polyetheretherketone. Comparison was made to an epoxy matrix composite, 5208/T-300. Laminates tested are (0/90) sub 2S, with outer ply fibers parallel to the beam axis. Four point bending was used at a typical span-to-thickness ratio of 39:1. It was found that all of the thermoplastic composites failed by abrupt longitudinal compression buckling of the outer ply. Very little precursory damage was observed. Micrographs reveal typical fiber kinking associated with longitudinal compression failure. Curved fracture surfaces on the fibers suggest they failed in bending rather than direct compression. Delamination was suppressed in the thermoplastic composites, and the delamination that did occur was found to be the result of compression buckling, rather than visa-versa. Microbuckling also caused other subsequent damage such as ply splitting, transverse ply shear failure, fiber tensile failure, and transverse ply cracking.

Yurgartis, S. W.↗

NASA NTRS1988

A micrographic study of bending failure in five thermoplastic-carbon fibre composite laminates

The local deformation and failure sequences of five thermoplastic matrix composites were microscopically observed while bending the samples in a small fixture attached to a microscope stage. The thermoplastics are polycarbonate, polysulfane, polyphenylsulfide, polyethersulfane, and polyetheretherketone. Comparison was made to an epoxy matrix composite, 5208/T-300. Laminates tested are (0/90) sub 2S, with outer ply fibers parallel to the beam axis. Four point bending was used at a typical span-to-thickness ratio of 39:1. It was found that all of the thermoplastic composites failed by abrupt longitudinal compression buckling of the outer ply. Very little precursory damage was observed. Micrographs reveal typical fiber kinking associated with longitudinal compression failure. Curved fracture surfaces on the fibers suggest they failed in bending rather than direct compression. Delamination was suppressed in the thermoplastic composites, and the delamination that did occur was found to be the result of compression buckling, rather than vice-versa. Microbuckling also caused other subsequent damage such as ply splitting, transverse ply shear failure, fiber tensile failure, and transverse ply cracking.

Yurgartis, S. W.↗

NASA NTRS1988

Catastrophic volcanism as a cause of shocked features found at the K/T boundary and in cryptoexplosion structures

The presence of quartz grains containing shock lamellae at the Cretaceous/Tertiary (K/T) boundary is viewed by many as the single most compelling evidence of meteoritic or cometary impact because there is no known endogenous mechanism for producing these features. Similarly the presence of shocked quartz, shatter cones, coesite and stishovite at cryptoexplosion structures is comonly taken as conclusive evidence of impact. However, several recent studies have cast doubt on this interpretation. It is argued that basaltic volcanism, although not normally explosive, can under exceptional circumstances produce overpressures sufficiently high to produce shock features. The exceptional circumstances include a high content of volatiles, usually CO2, and no preestablished pathway to the surface. Rapid cooling of the saturated basaltic magma can occur if it underlies a cooler more evolved magma in a chamber. Initial slow cooling and partial exsolution of the volatiles will cause the density of the basaltic magma to become less than that of the overlying magma, leading to overturning and mixing. Gas will escape the magma chamber along planar cracks once the pressure becomes sufficiently high. In the vicinity of the crack tip there is a smallscale deviatoric stress pattern which is thought to be sufficiently high to produce transient cracks along secondary axes in the quartz crystals, causing the planar features. The CO2-rich fluid inclusions which have been found along planar elements of quartz in basement rocks of the Vredefort Dome were likely to have been emplaced by such a process. If the mechanism described is capable of producing shocked features as above, it would require a reassessment of the origin of many cryptoexplosion structures as well as seriously weakening the case for an impact origin of the K/T event.

Loper, D. E.↗

NASA NTRS1991

Correlation of mechanical properties with metallurgical structure for 18Ni 200 grade maraging steel at room and cryogenic temperatures

An extensive metallurgical study is presented which is intended to explain variations in the mechanical properties of Ni18 200 grade maraging steel in various product forms and orientations. Fracture toughness and Charpy impact values are found to decrease with decreasing temperature and be dependent on product form, specimen orientation, and metallurgical condition. Fatigue crack growth rates are dependent on temperature only. Fractographic analysis reveals that the decrease in toughness at -170 C is not associated with cleavage-type fracture morphology. Those specimens exhibiting low fracture toughness at room temperature or -170 C are found to have a significantly larger number of titanium-rich particles associated with dimple formation on the fracture surface.

Wagner, J. A.↗

NASA NTRS2011

Material Gradients in Oxygen System Components Improve Safety

Oxygen system components fabricated by Laser Engineered Net Shaping (TradeMark) (LENS(TradeMark)) could result in improved safety and performance. LENS(TradeMark) is a near-net shape manufacturing process fusing powdered materials injected into a laser beam. Parts can be fabricated with a variety of elemental metals, alloys, and nonmetallic materials without the use of a mold. The LENS(TradeMark) process allows the injected materials to be varied throughout a single workpiece. Hence, surfaces exposed to oxygen could be constructed of an oxygen-compatible material while the remainder of the part could be one chosen for strength or reduced weight. Unlike conventional coating applications, a compositional gradient would exist between the two materials, so no abrupt material boundary exists. Without an interface between dissimilar materials, there is less tendency for chipping or cracking associated with thermal-expansion mismatches.

Forsyth, Bradley S.↗

DOE OSTI2022

Compatibility of Medium Density Polyethylene (MDPE) for Distribution of Gaseous Hydrogen

Hydrogen has emerged as a convenient energy storage medium and is being considered as an alternative for reducing the use of carbon-based fuels. Numerous projects are looking into distributing blends of natural gas and different amounts of gaseous hydrogen through the existing natural gas distribution system, which is widely composed of medium density polyethylene (MDPE) line pipes. The mechanical behavior of MDPE with hydrogen is not well understood; therefore, the effect of gaseous hydrogen on the mechanical properties of MDPE needs to be examined. In the current study, we investigate the effects of gaseous hydrogen on fatigue crack growth rate, fracture resistance, and fatigue life of MDPE in the presence of 3.4 MPa gaseous hydrogen. Fatigue crack growth behavior and fracture resistance are measured using compact tension specimens, while the fatigue life tests are carried out using circumferential notched tensile specimens. In addition, fatigue and fracture tests were conducted in air to determine the baseline properties of MDPE, which was then compared with the ones observed in gaseous hydrogen environment. After the completion of mechanical testing, fracture surfaces are also analyzed using optical and scanning electron microscopes to understand salient fracture features of MDPE with and without the presence of gaseous hydrogen.

Shrestha, Rakish↗

DOE OSTI2022

X-ray Computed Tomography as a Metrology Technique for the Analysis of Additively Manufactured Material

X-ray computed tomography (X-ray CT) is an analytical technique used in materials science to non-destructively characterize features in a variety materials like polymer, metals, composites, and explosives. It also has the capability of imaging additively manufacture, machine and assembled parts. The non-destructive imaging allows for the analysis of features (voids and cracks), which give a fundamental understanding of the material characteristics. Additionally, X-ray CT can obtain accurate measurements of dimensional and topographic variations due to different stimuli and assess the accuracy of material production. This study focuses on parts manufactured via metal additive manufacturing (AM). Although AM produces parts faster and easier, the printing process can produce defects (pores and surface roughness) that undermine the part’s mechanical properties and performance. The analysis of 3D printed objects has an asset in that the material has an STL file from which the item was printed, which is not available in many manufactured materials (i.e., foams) due to stochastic structures. For this study, the print accuracy of four additively manufactured cylinders will be assessed via X-ray CTto approximate the surface roughness and visualize any major morphological changes to assess the dimensional accuracy of complex additively manufactured parts. It was concluded that using X-ray CT to measure surface roughness was affective because reasonable surface roughness values were measured. Additionally, itwas determined that small-scale features can be produced via additive manufacturing with strong dimensional accuracy so long as the features are highly complex with sharp grooves.

36 MATERIALS SCIENCE↗

NASA NTRS1973

Mars - The intermediate between earth and moon

The present work represents a summary of the state of our knowledge concerning the chief physical characteristics of Mars as deduced from existing observational and theoretical evidence. Two main geological provinces are distinguished on Mars: areas of rough terrain and dense cratering, and smooth areas comparable to lunar maria. A thermal model for the Martian poles which takes into account convective transport would indicate that the CO2 frost over the north pole is not permanent, lasting about 420 days with the water frost lasting the remaining 267 days of the Martian year. The meandering appearance of Martian rift valleys are cracks probably produced, as also in the case of lunar rilles, by stresses, perhaps in solidifying lava of impact origin, and not by erosional river beds. Data indicate a strong absorption in the thin Martian atmosphere. The atmospheric blue and violet cap around a Martian pole in winter is interpreted as a 'blue clearing' of the atmosphere increasing transparency so that surface detail of higher albedo shines through in the blue.

Opik, E. J.↗

NASA NTRS1984

Methods for assessing the structural reliability of brittle materials

Failure from contact-induced surface flaws is considered along with controlled indentation flaws for construction of toughness and fatigue master maps, fatigue properties of ceramics with natural and controlled flaws, and a statistical analysis of size and stress state effects on the strength of an alumina ceramic. Attention is also given to dynamic and static fatigue of a machinable glass ceramic, the effect of multiregion crack growth on proof testing, and a fracture mechanics analysis of defect sizes. Other topics explored are related to the effect of temperature and humidity on delayed failure of optical glass fibers, subthreshold indentation flaws in the study of fatigue properties of ultrahigh-strength glass, the lifetime prediction for hot-pressed silicon nitride at high temperatures, static fatigue in high-performance ceramics, and requirements for flexure testing of brittle materials.

Freiman, S. W.↗

NASA NTRSDate not supplied

History of Structural Stitching Development for Aerospace Applications

Layered composite structures are a commonly used, lightweight option for aerospace vehicles today. However, these structures are prone to delamination between plies as well as separation between co-cured sections such as skins and flanges. In addition, delamination can easily be induced by impact damage from events such as tool drops and hailstones. Since such delaminations are often not visible from the external surface of the structure, additional material or fasteners must be included in the design to ensure the structure will maintain the required load-carrying ability through its lifetime. However, adding extra material increases weight and reduces structural efficiency and adding fasteners and their associated holes reduces manufacturing efficiency and adds the requirement to inspect the holes since they could become crack initiation points. Alternate means to reduce delaminations could be beneficial. An alternative to these options is to build the structure with through-thickness reinforcement, such as using stitching threads, to limit delamination, increase out-of-plane strength, and provide a method to join structural elements together without fasteners. The history of through-thickness stitching as it could be applied to aerospace vehicles is described in this paper.

carbon-epoxy↗

NASA NTRS1983

Morphology of ductile metals eroded by a jet of spherical particles impinging at normal incidence

Scanning electron microscopy and energy-dispersive X-ray spectroscopy are used, together with surface profile measurements, in the present morphological study of the erosion of an aluminum alloy and copper by the normal impact of spherical glass erodent particles. The morphology of the damage pattern is a manifestation of the flow pattern of erodent particles, and yields insight into the mechanisms that may be active at different stages of erosion. The simultaneous appearance of radial cracks and concentric rings is reported, together with wave crests which contain an accumulation of metallic flakes. A preliminary analysis is advanced to explain the formation of the various damage patterns observed.

Veerabhadra Rao, P.↗

NASA NTRS1999

Turbomachinery Design Quality Checks to Avoid Friction Induced Structural Failure

A unique configuration of the P&W SSME Alternate Fuel Turbopump turbine disk/blade assembly, combined with a severe thermal environment, resulted in several structural anomalies that were driven by frictional contact forces. Understanding the mechanics of these problems provides new quality checks for future turbo machinery designs. During development testing in 1997 of the SSME alternate fuel turbopump at Stennis Space Center, several potentially serious problems surfaced with the turbine disk/blade assembly that had not been experienced in extensive earlier testing. Changes to the operational thermal environment were noted based on analytical prediction of modifications that affected performance and on stationary thermal measurements adjacent to the rotor assembly. A detailed structural investigation was required to reveal the mechanism of distress induced by the change. The turbine disk experienced cracking in several locations due to increased thermal gradient induced stress during start and shutdown transients. This was easily predictable using standard analysis procedures and expected once the thermal environment was characterized. What was not expected was the curling of a piston ring used for blade axial retention in the disk, indentation of the axial face of the blade attachment by a spacer separating the first and second stage blades, and most significantly, galling and cracking of the blade root attachment that could have resulted in blade release. Past experience, in gas turbine environments, set a precedent of never relying on friction for help and to evaluate it only in specific instances where it was obvious that it would degrade capability. In each of the three cases above, friction proved to be a determining factor that pushed the components into an unsatisfactory mode of operation. The higher than expected temperatures and rapid thermal transients combined with friction to move beyond past experience. The turbine disk/blade assembly configuration contributed to the potential for these problems to occur by limiting the radial deflection from thermals and centrifugal loading. The cooled solid bore configuration was chosen to improve rotordynamic stability by limiting the length of rotor overhang while still protecting the roller bearing by maintaining zero slope under the inner race. During a start transient, the rim area of the disk heats rapidly and expands axially and circumferentially and requires corresponding radial and axial growth of the disk to maintain relative positioning of the disk, blades, spacers and retainer rings. The stiffness, large thermal mass, and bore cooling flow combine to severely limit the disk rim radial growth which results in the potential for relative movement between these parts. Friction then becomes a player in the determination of component stress.

Moore, Jerry H.↗

NASA NTRS2015

Plume Collection Strategies for Icy World Sample Return

Three icy worlds in the solar system display evidence of pluming activity. Water vapor and ice particles emanate from cracks near the south pole of Saturn's moon Enceladus. The plume gas contains simple hydrocarbons that could be fragments of larger, more complex organics. More recently, observations using the Hubble and Herschel space telescopes have hinted at transient water vapor plumes at Jupiter's moon Europa and the dwarf planet Ceres. Plume materials may be ejected directly from possible sub-surface oceans, at least on Enceladus. In such oceans, liquid water, organics, and energy may co-exist, making these environments habitable. The venting of habitable ocean material into space provides a unique opportunity to capture this material during a relatively simple flyby mission and return it to Earth. Plume collection strategies should enable investigations of evidence for life in the returned samples via laboratory analyses of the structure, distribution, isotopic composition, and chirality of the chemical components (including biomolecules) of plume materials. Here, we discuss approaches for the collection of dust and volatiles during flybys through Enceladus' plume, based on Cassini results and lessons learned from the Stardust comet sample return mission. We also highlight areas where sample collector and containment technology development and testing may be needed for future plume sample return missions.

Stardust Collector↗

NASA NTRS2024

Considerations for Qualifying Reliable Eddy Current Array Technique for Detection of Backwall Cracks

A reliable nondestructive evaluation (NDE) technique provides minimum 90% probability of detection(POD) with 95% confidence for detection of cracklike flaws of a qualified size. In this case, the flaws are on backside of material. Eddy current array (ECA) probe or a single sensor eddy current probe in c-scanning mode is used for the flaw detection. Here, two geometries are considered for the test specimens. The two geometries are, a flat plate, and tube or pipe. The probe is assumed to be on outer diameter (OD)surface and the flaw is assumed to be at the inner diameter (ID) surface for tube inspection. The flaw and probe are on opposite side of wall thickness for inspection of plate material. The application may be used for acreage inspection or just for inspection of butt weld and heat affected zone (HAZ) in a tube, cylinder, or plate. The proposed approach is based on developing an instrument standardization or calibration procedure. Decision threshold of inspection procedure is determined using empirical qualification and noise data. The work explores essential parameters that are required to meet certain conditions to ensure reliable flaw detection. Physics-based simulation of eddy current array flaw detection is used to understand effect of essential parameters on signal response (amplitude and phase),and therefore flaw detectability. Simulation data is used to justify choice of calibration reference standard requirements and the qualification approach. An ECA technique qualification model is provided. The paper gives brief description of tasks to be completed for qualifying ECA technique for reliable detection of cracklike flaws.

Eddy current array inspection, nondestructive eval↗

NASA NTRS1980

Stress corrosion cracking in the earth

Two fundamental concepts of fracture mechanics are used to develop a theory of the earthquake mechanism which specifically predicts observed time-dependent rupture phenomena such as slow earthquakes, postseismic rupture growth and afterslip, multiple events, foreshocks, and aftershocks. The theory also predicts that there must be a nucleation stage prior to an earthquake, and suggests a physical mechanism by which one earthquake may trigger another. Investigations show that all earthquakes must be preceded by a quasi-static slip over a portion of the rupture surfaces, although it may be difficult to detect in practice, and a study of delayed multiple events characterizes the strength of some barriers in the earth as having a stress corrosion index of about 24.

Das, S.↗