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Polyimide Fibers

A polyimide fiber having textile physical property characteristics and the process of melt extruding same from a polyimide powder. Polyimide powder formed as the reaction product of the monomers 3.4'-ODA and ODPA, and endcapped with phthalic anhydride to control the molecular weight thereof, is melt extruded in the temperature range of 340? C. to 360? C. and at heights of 100.5 inches, 209 inches and 364.5 inches. The fibers obtained have a diameter in the range of 0.0068 inch to 0.0147 inch; a mean tensile strength in the range of 15.6 to 23.1 ksi; a mean modulus of 406 to 465 ksi; and a mean elongation in the range of 14 to 103%.

St.Clair, Terry L.↗

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.↗

Effect of Decarburization on Notch Sensitivity and Fatigue-Crack-Propagation Rates in 12 MoV Stainless-Steel Sheet

Tests were conducted in order to determine the effect of surface decarburization on the notch sensitivity and rate of fatigue crack propagation in 12 MoV stainless-steel sheet at room temperature. Three specimen configurations were utilized in the course of the investigation: standard tensile specimen, 9-inch-wide specimens containing fatigue cracks or thread-cut notches of 0.005-inch radius, and 2-inch-wide specimens containing fatigue cracks. The 12 MoV stainless-steel sheet in the normal condition was found to have an ultimate tensile strength of 251 ksi and to be extremely notch sensitive. The material in the decarburized condition was found to have an ultimate tensile strength of 210 ksi and to be considerably stronger than the normal material in the presence of fatigue cracks. Decarburization did not appear to have any significant influence on the rate of fatigue crack propagation in the 2-inch-wide specimens at the stress levels considered. In addition to the tests, two methods for predicting residual static strength and their application to the material are discussed.

Herrnstein, William H., III↗

Polyimide Fibers

A polyimide fiber having textile physical property characteristics and the process of melt extruding same from a polyimide powder. Polyimide powder formed as the reaction product of the monomers 3.4'-ODA and ODPA, and end- capped with phthalic anhydride to control the molecular weight thereof, is melt extruded in the temperature range of 340 C. to 360 C. and at heights of 100.5 inches. 209 inches and 364.5 inches. The fibers obtained have a diameter in the range of 0.0068 inch to 0.0147 inch; a mean tensile strength in the range of 15.6 to 23.1 ksi; a mean modulus of 406 to 465 ksi, and a mean elongation in the range of 14 to 103%.

St.Clair, Terry L.↗

Dimensionally Stable Poyimide Copolymers for Microelectronics Applications

Polyimides are finding increased applications in microelectronics due to their high thermal stability, good chemical resistance, good adhesion, low moisture absorption, good mechanical properties, and low coefficient of thermal expansion (CTE). Four series of random copolyimides were synthesized and characterized for potential application as encapsulants, stress-relief layers, and interlevel dielectrics. Several candidates exhibited good combinations of physical and mechanical properties with inherent viscosities from 1.21 to 1.42 dL/g, T(sub g)'s ranging from 251 to 277 C, 10% weight loss temperatures between 503 and 527 C, and CTEs ranging from 33 to 39 ppm/deg C. Mechanical properties at room temperature for the best candidates included tensile strengths of 17.8-21.3 ksi, moduli between 388 and 506 ksi, and elongations of 11-43%. Moisture absorption for these copolyimides ranged between 0.85 and 1.38 wt %.

Fay, Catherine C.↗

One-step Tape Casting of Composites via Slurry on Fiber

A process by which metal matrix composites can be made was presented. The process involves putting a powder slurry on fibers to make a precursor green tape. These green tapes are cut, stacked and hot pressed to form the fully dense composite. A computer program was presented which enables complete quantification and control of the process. Once some easily obtained properties of the slurry and its behavior are determined (such as the shrinkage from the wet to green state, and the density of the green tape) modification of the fiber spacing and blade height give the maker precise control of fiber volume fraction, and fiber architecture in the composite. The process was shown to be accurate and flexible through the production of a wide variety of volume fraction fiber composites made from a wide variety of fibers and powders. The most time consuming step of the tape casting process (other than hot pressing) was winding the fiber on the drum. The tape casting techniques developed resulted in high quality metal matrix composites, with ultimate tensile strength in the range of 215 ksi (1477 MPa), a strain at failure of 1.15 percent, and in fatigue at room temperature 0 to 120 ksi, n = 0.3 Hz, a 4-ply Ti-24Al-11Nb/SCS-6, 32 vol% fiber tape cast composite lasted 202,205 cycles with a maximum strain on the 100th cycle of 0.43 percent.

deGroh, Henry C., III↗

High Strength Discontinuously Reinforced Aluminum For Rocket Applications

This study presents results on the development of a new aluminum alloy with very high strength and ductility. Five compositions of Al-Mg-Sc-Gd-Zr alloy were selected for this purpose. These alloys were also reinforced with 15 volume percent silicon-carbide and boron-carbide particles to produce Discontinuously Reinforced Aluminum (DRA) materials. Matrix alloys and DRA were processed using a powder metallurgy process. The helium gas atomization produced very fine powder with cellular-dentritic microstructure. The microstructure of matrix alloys showed fine Al3Sc based precipitate which provides significant strengthening in these alloys. DRA showed uniform distribution of reinforcement in aluminum matrix. DRA materials were tested at -320 F, 75 F in air and 7S F in gaseous hydrogen environments and matrix alloys were tested at 75 F in air. DRA showed high strengths in the range of 89-111 ksi (614-697 MPa) depending on alloy compositions and test environments. Matrix alloys had a good combination of strength, 84-89 ksi (579-621 MPa) and ductility, 4.5-6.5%. The properties of these materials can further be improved by proper control of processing parameters.

Pandey, A. B.↗

Interference Fit Life Factors for Roller Bearings

The effect of hoop stresses in reducing cylindrical roller bearing fatigue life was determined for various classes of inner ring interference fit. Calculations were performed for up to seven interference fit classes for each of ten bearing sizes. Each fit was taken at tightest, average and loosest values within the fit class for RBEC-5 tolerance, thus requiring 486 separate analyses. The hoop stresses were superimposed on the Hertzian principal stresses created by the applied radial load to calculate roller bearing fatigue life. The method was developed through a series of equations to calculate the life reduction for cylindrical roller bearings based on interference fit. All calculated lives are for zero initial bearing internal clearance. Any reduction in bearing clearance due to interference fit was compensated by increasing the initial (unmounted) clearance. Results are presented as tables and charts of life factors for bearings with light, moderate and heavy loads and interference fits ranging from extremely light to extremely heavy and for bearing accuracy class RBEC 5 (ISO class 5). Interference fits on the inner bearing ring of a cylindrical roller bearing can significantly reduce bearing fatigue life. In general, life factors are smaller (lower life) for bearings running under light load where the unfactored life is highest. The various bearing series within a particular bore size had almost identical interference fit life factors for a particular fit. The tightest fit at the high end of the RBEC-5 tolerance band defined in ANSI/ABMA shaft fit tables produces a life factor of approximately 0.40 for an inner-race maximum Hertz stress of 1200 MPa (175 ksi) and a life factor of 0.60 for an inner-race maximum Hertz stress of 2200 MPa (320 ksi). Interference fits also impact the maximum Hertz stress-life relation.

Oswald, Fred B.↗

Probabilistic Estimation of Critical Flaw Sizes in the Primary Structure Welds of the Ares I-X Launch Vehicle

The primary structure of the Ares I-X Upper Stage Simulator (USS) launch vehicle is constructed of welded mild steel plates. There is some concern over the possibility of structural failure due to welding flaws. It was considered critical to quantify the impact of uncertainties in residual stress, material porosity, applied loads, and material and crack growth properties on the reliability of the welds during its pre-flight and flight. A criterion--an existing maximum size crack at the weld toe must be smaller than the maximum allowable flaw size--was established to estimate the reliability of the welds. A spectrum of maximum allowable flaw sizes was developed for different possible combinations of all of the above listed variables by performing probabilistic crack growth analyses using the ANSYS finite element analysis code in conjunction with the NASGRO crack growth code. Two alternative methods were used to account for residual stresses: (1) The mean residual stress was assumed to be 41 ksi and a limit was set on the net section flow stress during crack propagation. The critical flaw size was determined by parametrically increasing the initial flaw size and detecting if this limit was exceeded during four complete flight cycles, and (2) The mean residual stress was assumed to be 49.6 ksi (the parent material s yield strength) and the net section flow stress limit was ignored. The critical flaw size was determined by parametrically increasing the initial flaw size and detecting if catastrophic crack growth occurred during four complete flight cycles. Both surface-crack models and through-crack models were utilized to characterize cracks in the weld toe.

Pai, Shantaram S.↗

Empirical Method to Estimate Hydrogen Embrittlement of Metals as a Function of Hydrogen Gas Pressure at Constant Temperature

High pressure Hydrogen (H) gas has been known to have a deleterious effect on the mechanical properties of certain metals, particularly, the notched tensile strength, fracture toughness and ductility. The ratio of these properties in Hydrogen as compared to Helium or Air is called the Hydrogen Environment Embrittlement (HEE) Index, which is a useful method to classify the severity of H embrittlement and to aid in the material screening and selection for safety usage H gas environment. A comprehensive world-wide database compilation, in the past 50 years, has shown that the HEE index is mostly collected at two conveniently high H pressure points of 5 ksi and 10 ksi near room temperature. Since H embrittlement is directly related to pressure, the lack of HEE index at other pressure points has posed a technical problem for the designers to select appropriate materials at a specific H pressure for various applications in aerospace, alternate and renewable energy sectors for an emerging hydrogen economy. Based on the Power-Law mathematical relationship, an empirical method to accurately predict the HEE index, as a function of H pressure at constant temperature, is presented with a brief review on Sievert's law for gas-metal absorption.

Lee, Jonathan A.↗

2014/2219 Tri-Point Crack Analysis

Friction stir welding (FSW) is a solid state welding process with potential advantages for aerospace and automotive industries dealing with light alloys. Self-reacting friction stir welding (SR-FSW) is one variation of the FSW process being developed at the National Aeronautics and Space Administration (NASA) for use in the fabrication of propellant tanks. Friction plug welding is used to seal the exit hole that remains in a circumferential SR-FSW. The objective of this study was to evaluate the deformation response at the tips of cracks located in the heat affected zone of friction plug welds and to study the fracture behavior of welds with defects in the form of fatigue cracks. The study used existing 2014-T6 to 2219-T87 self-reacting friction stir weld panels with 2219-T87 friction plug welds. Electro-discharge machined (EDM) notches were machined into the heat affected zone of the plug at the plug-to-base metal interface. Samples were then cycled to generate a fatigue crack emanating from the notch. After the fatigue crack reached a pre-defined length, a speckle pattern was applied and the ARAMIS system (a three dimensional imaging correlation system) was used to measure the deformations at the crack tip under a sequence of loads. Testing was conducted at ambient laboratory conditions. Fracture data from the testing was analyzed to evaluate residual strength capability of the panel as a function of flaw size. ARAMIS strain data was evaluated to examine strain and deformation patterns that develop around the crack tip and at the plug/weld interfaces. Four samples were used in this study, with three samples in a post-weld heat treated condition. Three samples contained large diameter plugs (M5) and one sample contained a small diameter plug (M3). Two samples were 4 inches in width and two samples were 8.5 inches in width. All samples failed through the precrack with residual strengths ranging from 37 ksi to 42 ksi.

Horton, Karla Renee↗

Interference-Fit Life Factors for Roller Bearings

The effect of hoop stresses in reducing cylindrical roller bearing fatigue life was determined for various classes of inner-ring interference fit. Calculations were performed for up to 7 fit classes for each of 10 bearing sizes. The hoop stresses were superimposed on the Hertzian principal stresses created by the applied radial load to calculate roller bearing fatigue life. A method was developed through a series of equations to calculate the life reduction for cylindrical roller bearings. All calculated lives are for zero initial internal clearance. Any reduction in bearing clearance due to interference fit would be compensated by increasing the initial (unmounted) clearance. Results are presented as tables and charts of life factors for bearings with light, moderate, and heavy loads and interference fits ranging from extremely light to extremely heavy for bearing accuracy class RBEC-5 (ISO class 5). Interference fits on the inner ring of a cylindrical roller bearing can significantly reduce bearing fatigue life. In general, life factors are smaller (lower life) for bearings running under light load where the unfactored life is highest. The various bearing series within a particular bore size had almost identical interference-fit life factors for a particular fit. The tightest fit at the high end of the tolerance band produces a life factor of approximately 0.40 for an inner-race maximum Hertz stress of 1200 MPa (175 ksi) and a life factor of 0.60 for an inner-race maximum Hertz stress of 2200 MPa (320 ksi). Interference fits also impact the maximum Hertz stress-life relation.

Oswald, Fred B.↗

Development of Long-Lifetime Pulsed Gas Valves for Pulsed Electric Thrusters

It is advantageous for gas-fed pulsed electric thrusters to employ pulsed valves so propellant is only flowing to the device during operation. The propellant utilization of the thruster will be maximized when all the gas injected into the thruster is acted upon by the fields produced by the electrical pulse. Gas that is injected too early will diffuse away from the thruster before the electrical pulse can act to accelerate the propellant. Gas that is injected too late will miss being accelerated by the already-completed electrical pulse. As a consequence, the valve must open quickly and close equally quickly, only remaining open for a short duration. In addition, the valve must have only a small amount of volume between the sealing body and the thruster so the front and back ends of the pulse are as coincident as possible with the valve cycling, with very little latent propellant remaining in the feed lines after the valve is closed. For a real mission of interest, a pulsed thruster can be expected to pulse at least 10(exp 10) - 10(exp 11) times, setting the range for the number of times a valve must open and close. The valves described in this paper have been fabricated and tested for operation in an inductive pulsed plasma thruster (IPPT) for in-space propulsion. In general, an IPPT is an electrodeless space propulsion device where a capacitor is charged to an initial voltage and then discharged, producing a high-current pulse through a coil. The field produced by this pulse ionizes propellant, inductively driving current in a plasma located near the face of the coil. Once the plasma is formed, it can be accelerated and expelled at a high exhaust velocity by the electromagnetic Lorentz body force arising from the interaction of the induced plasma current and the magnetic field produced by the current in the coil. The valve characteristics needed for the IPPT application require a fast-acting valve capable of a minimum of 10(exp 10) valve actuation cycles. Since even 10(exp 9) cycles is well above anything demonstrated, this lower value was selected as the design point for the present work. The valve seal must remain leak-tight throughout operation, and the body must maintain a low internal leakage at relatively high operating temperatures. The full set of design requirements used for this program are summarized in Table 1. In this work, we describe two pulsed gas valves that have been fabricated to have long lifetime and demonstrate the characteristics listed above. The first is a miniaturized, conventional electromagnet-based valve while the second is a piezoelectric-based valve design. The conventional valve, shown in Fig. 1, is opened by use of a solenoid electromagnetic actuator. When current is applied to the solenoid coil, magnetic forces pull the plunger away from the valve seat, allowing fluid to flow through the valve. Removal of electrical current permits the spring and fluid pressure to seat the plunger, halting the flow of fluid. The valve body is fabricated from 304L corrosion resistant steel (CRES) and while the parts that form the magnetic circuit are fabricated from 430 CRES. This material does not have optimum magnetic properties, but its corrosion resistance permits incorporation into a design without requiring an additional plating process. A viton O-ring compound (Parker V0884-75), selected for its mechanical strength at elevated temperatures, was used for the valve seat seal. The design was based solely on the use of analytical sizing calculations, as opposed to a more rigorous finite element analysis. While this valve is small and relatively lightweight, it does not represent a design that is optimized for mass and/or a given volume envelope. The piezoelectric valve is a "puller" valve design. Applying a voltage to the piezo crystal causes it to elongate and pull a pintle off the seat, opening the valve. The valve seal consists of the pintle with an external, spherically-formed tip fabricated from Inconel 625 and the seat fabricated from Inconel 718 and possessing a spherical surface that permits the pintle to align with the valve body centerline after each cycle, maintaining the circumferential metal-on-metal seal. The contact stress on the valve pintle is expected in the worst case to be 96.5 MPa (14 ksi), which is well below the work hardening value of 413.7 MPa (60 ksi) for Inconel 615. Results presented in this work will compare the performance of each valve, both to each other and to the valve design requirements given in Table 1. In general, both valves meet all the performance envelope requirements, but the piezoelectric valve consumes considerably less power and has a faster response time over the conventional solenoid-driven valves.

Burkhardt, Wendel M.↗

Fracture Mechanics Testing of Titanium 6AL-4V in AF-M315E

The Green Propellant Infusion Mission (GPIM) will demonstrate the performance of AF-M315E monopropellant on orbit. Flight certification requires a safe-life analysis of the titanium alloy fuel tank to ensure inherent processing flaws will not cause failure during the design life of the tank. Material property inputs for this analysis require testing to determine the stress intensity factor for environment-assisted cracking (KEAC) of Ti 6Al-4V in combination with the AF-M315E monopropellant. Testing of single-edge notched, or SE(B), specimens representing the bulk tank membrane and weld material were performed in accordance with ASTM E1681. Specimens with fatigue pre-cracks were loaded into test fixtures so that the crack tips were exposed to AF-M315E at 50 C for a duration of 1,000 hours. Specimens that did not fail during exposure were opened to inspect the crack surfaces for evidence of crack growth. The threshold stress intensity value, KEAC, is the highest applied stress intensity that produced neither a failure of the specimen during the exposure nor showed evidence of crack growth. The threshold stress intensity factor for environment-assisted cracking of the Ti 6Al-4V forged tank material was found to be at least 22 ksi√in and at least 31 ksi√in for the weld material when exposed to AF-M315E monopropellant.

AF-M315E↗

Characterization of SiC/SiC Composites Subjected to Sequential Tensile Creep and Dwell Fatigue in Air under Thermal Gradient Conditions

Uncoated SiC/SiC composites, with 2D and 3D fiber architectures, were investigated under steady state thermal gradient conditions with sequential tensile creep and dwell fatigue. Melt infiltration (MI), chemical vapor infiltration (CVI), polymer impregnation and pyrolysis (PIP), and hybrid (CVI and PIP) techniques were used to fabricate ceramic matrix composites (CMCs) with a 2D balanced fiber architecture. CMCs with 3D fiber weaves were also fabricated using MI and hybrid methods. Steady state through the thickness thermal gradients were generated for the tensile specimens using laser heating on the front (hot side) and forced air cooling on the back (cold side). Hot side and cold side temperatures of 2400 and 2200 °F, respectively, were used for testing CMCs fabricated with the MI process, whereas hot side and cold side temperatures of 2700 and 2400 °F, respectively, were used for CMCs fabricated with CVI, PIP, and hybrid processes. Each CMC specimen was initially tested under tensile creep at 69 MPa (10 ksi) for 80 hours, which was then followed by tensile dwell fatigue testing at a maximum stress of 69 MPa (10 ksi) for another 80 hours for a total of 160 hours. This type of sequential tensile creep followed by tensile dwell fatigue testing was performed to ascertain the integrity of uncoated CMCs under steady state thermal gradient conditions. Tensile creep and dwell fatigue test results, generated under steady state thermal gradient conditions on different types of SiC/SiC composites, are compared with corresponding creep behaviors observed under isothermal conditions to determine the influence of both monotonic creep (static fatigue) and dwell fatigue on accumulated strains and deformation behaviors of the CMCs.

Kalluri, Sreeramesh↗

Fracture Mechanics Testing of Titanium 6AL-4V in LMP-103S Propellant

Propellant tank safe-life analysis is a spacecraft propulsion subsystem Launch Range processing requirement. The material property inputs for the safe-life analysis include the stress intensity factor for environment-assisted cracking (KEAC). The KEAC for titanium alloy Ti 6Al-4V in LMP-103S propellant was determined experimentally using an innovative test method following ASTM E1681, Standard Test Method for Determining Threshold Stress Intensity Factor for Environment-Assisted Cracking of Metallic Materials. This effort was a collaboration between NASA Goddard Space Flight Center and NASA Kennedy Space Center to expose the test specimens in the propellant, while loaded in the test fixtures, for 1000- hour (42 days) at 50°C. Two test rounds have been completed to date; 1) testing mechanically loaded specimens but without propellant and 2) testing mechanically loaded specimens wetted with LMP-103S propellant. The dry test was to evaluate the crack growth without exposure to the LMP-103S propellant, and further assess the un-wetted stress intensity factor for the full 1000-hour duration. The second round of testing included the propellant soak for the requisite 1000- hour at 50°C. Current results show that the threshold intensity factor for environment-assisted cracking (exposed to LMP103S) is 22.5 ksi√in for the bulk material and 36. 2 ksi√in for the weld material. A generic ‘candidate’ tank geometry and material thickness is developed for a damage tolerance of known surface cracks below the nondestructive inspection technique detection limit. Evaluations with and without the use of a threshold intensity factor for environment-assisted cracking is performed for the required 4x propellant tank service life using the software tool NASGRO. SP2024_00239

Green propulsion↗

Effect of heterogeneous microstructure on the tensile and creep performances of cast Haynes 282 alloy

Precipitation-strengthened Ni-based superalloys are leading candidate materials for advanced ultra-supercritical (A-USC) plants with steam conditions up to 760 °C (1400 °F) and 35 MPa (5 ksi). This study evaluates representative specimens from a large casting of Haynes 282 to study the effect of microstructural heterogeneity on the mechanical behavior of this alloy. The tensile test results of cast Haynes 282 over the temperature range 20–816 °C exhibited lower tensile strength and ductility in comparison with the reference wrought Haynes 282. However, the creep rupture tests of the cast alloy below 704–788 °C and 190–431 MPa presented a similar stress-Larson-Miller parameter to that of the wrought material. Microstructural and dislocation characterizations using scanning electron microscopy, conventional transmission electron microscopy, and scanning transmission electron microscopy in conjunction with energy dispersive X-ray spectroscopy were performed to understand the microstructural evolution before and after the mechanical tests. The heterogeneous microstructures of the cast Haynes 282 material, including the coarse grains, potential casting defects, and a bimodal size distribution of γ' precipitates, were detrimental to the tensile behavior, whereas the coarse-scale grains had a positive effect on the creep performance because diffusional creep was the dominant creep mechanism.

tensile testing↗

Consortium for Production of Affordable Carbon Fibers in the United States (Final Report)

Various feedstocks from coal, petroleum and bio-based acrylonitrile were investigated for their ability to produce carbon fiber within DOE strength (250 ksi), modulus (25 Msi), elongation (>1%) and cost (≤$5/lb) goals for wider utilization in light-weight vehicles for the automotive industry. The overarching approach was to chemically identify and map the various feedstocks, understand the molecular transformation to produce carbon fiber precursors (mesophase for pitch materials of polyacrylonitrile polymer) and how these impact carbon fiber quality. Predictive models were built to relate the feedstocks and precursors to carbon fiber properties using atomistic and micro-scale modeling within ±15%. Using tow-level carbon fiber epoxy composites, carbon fibers tow-level predictions of elastic components of the carbon fibers were also successfully modeled within ±15%, using finite element analysis to confirm single filament carbon fiber properties. These models were validated with tow-level epoxy composite experiments from carbon fibers produced in this study.

01 COAL, LIGNITE, AND PEAT↗