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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

Effect of Cooling Rate on Nano-Eutectic Formation in Laser Surface Remelted and Rare Earth Modified Hypereutectic Al-20Si Alloys

Laser Surface Remelting (LSR) was applied to arc-melted Al-20Si-0.2Sr, Al-20Si-0.2Ce, and Al-20Si hypereutectic alloys to refine microstructures. Experiments revealed that microstructures in the melt pool varied from fully eutectic to a mixture of Al dendrites and inter-dendritic eutectic. We calculated cooling rates using the Eagar-Tsai model and correlated cooling rates with characteristic microstructures, revealing that a cooling rate on the order of 104 K/s could lead to maximized fully eutectic microstructure morphology. Due to rapid solidification, the Si composition in the LSR eutectic was measured at 18.2 wt.%, higher than the equilibrium eutectic composition of 12.6 wt.%Si. Compared to Al-20Si, Ce addition had no significant effect on the volume fraction of the fully eutectic structure but refined Si fibers to approximately 30 nm in diameter. Sr addition did not further refine the diameter of eutectic Si fibers compared to Al-20Si but increased the volume fraction of the fully eutectic microstructure morphology. The refinement ratio (φ) of the Si fiber diameter from the bottom of the melt pool to the surface for the three alloys was similar, at around 28%. The established correlation between the cooling rate and the size and morphology of the microstructure within the melt pool will enable tailoring of the microstructure in laser-processed as well as deposited alloys for high strength and plasticity.

36 MATERIALS SCIENCE↗

Ultrahigh strength and plasticity in laser rapid solidified Al–Si nanoscale eutectics

As-cast Al–20wt.% Si alloys were processed via laser rapid solidification (LRS) techniques to create eutectic microstructures with nanoscale interconnected, nanotwinned Si fibers. LRS morphologies exhibit higher flow stress, exceeding 800 MPa and uniform plastic deformation above 20% compared to as-cast alloy that fractures at strains below 8% at flow strength of approximately 200 MPa. The strengthening mechanisms of LRS morphologies are interpreted in terms of the interfacial constraints: increase in yield strength as well as strain hardening rate due to nanoscale confined slip in fibrous Al–Si eutectic, and load transfer and eventual plasticity in the nanoscale Si fibers.

36 MATERIALS SCIENCE↗

Hoop Tensile Characterization Of SiC/SiC Cylinders Fabricated From 2D Fabric

Tensile stress-strain properties in the hoop direction were obtained for 100-mm diameter SiC/SiC cylinders using ring specimens machined from the cylinder ends. The cylinders were fabricated from 2D balanced fabric with several material variants, including wall thickness (6, 8, and 12 plies), Sic fiber type (Sylramic, Sylramic-iBN, Hi-Nicalon, and Hi-Nicalon S), fiber sizing type, and matrix type (full CVI Sic, and partial CVI plus melt-infiltrated SiC-Si). Fiber ply splices existed in the all the hoops. Tensile hoop measurements were made at room temperature and 1200 C using hydrostatic ring test facilities. The hoop results are compared with in-plane data measured on flat panels using same material variants, but containing no splices.

Verrilli, Michael J.↗

Hoop Tensile Properties of Ceramic Matrix Composite Cylinders

Tensile stress-strain properties in the hoop direction were obtained for 100-mm diameter SiC/SiC ceramic matrix composite cylinders using ring specimens machined form the cylinder ends. The cylinders were fabricated from 2D balanced SiC fabric with several material variants, including wall thickness (6,8, and 12 plies), SiC fiber type (Sylramic, Sylramic-iBN, Hi-Nicalon, and Hi-Nicalon S), fiber sizing type, and matrix type (full CVI SiC, and partial CVI SiC plus slurry cast + melt-infiltrated SiC-Si). Fiber ply splices existed in all the hoops. Tensile hoop measurements are made at room temperature and 1200 C using hydrostatic ring test facilities. The failure mode of the hoops, determined through microstructural examination, is presented. The hoop properties are compared with in-plane data measured on flat panels using same material variants, but containing no splices.

Verrilli, Michael J.↗

Electrospun Si and Si/C Fiber Anodes for Li-Ion Batteries

Due to structural changes in silicon during lithiation/delithiation, most Li-ion battery anodes containing silicon show rapid gravimetric capacity fade upon charge/discharge cycling. Herein, we report on a new Si powder anode in the form of electrospun fibers with only poly(acrylic acid) (PAA) binder and no electrically conductive carbon. The performance of this anode was contrasted to a fiber mat composed of Si powder, PAA binder, and a small amount of carbon powder. Fiber mat electrodes were evaluated in half-cells with a Li metal counter/reference electrode. Without the addition of conductive carbon, a stable capacity of about 1500 mAh/g (normalized to the total weight of the anode) was obtained at 1C for 50 charge/discharge cycles when the areal loading of silicon was 0.30 mgSi/cm2, whereas a capacity of 800 mAh/g was obtained when the Si loading was increased to ~1.0 mgSi/cm2. On a Si weight basis, these capacities correspond to >3500 mAh/gSi. The capacities were significantly higher than those found with a slurry-cast powdered Si anode with PAA binder. There was no change in fiber anode performance (gravimetric capacity and constant capacity with cycling) when a small amount of electrically conductive carbon was added to the electrospun fiber anodes when the Si loading was ≤1.0 mgSi/cm2.

Mondal, Abhishek N.↗

Ceramic fibers from Si-B-C polymer precursors

Non-oxide ceramics such as silicon carbide (SiC), silicon nitride (Si3N4), and silicon borides (SiB4, SiB6) have thermal stability, oxidation resistance, hardness, and varied electrical properties. All these materials can be prepared in a fiber form from a suitable polymer precursor. The above mentioned fibers, when tested over a temperature range from 25 to 1400 C, experience degradation at elevated temperatures. Past work in ceramic materials has shown that the strength of ceramics containing both carbides and borides is sustained at elevated temperatures, with minimum oxidation. The work presented here describes the formation of ceramic fibers containing both elements, boron and silicon, prepared via the polymer precursor route previously reported by the authors, and discusses the fiber mechanical properties that are retained over the temperature range studied.

Riccitiello, S. R.↗

Stress-Rupture of New Tyranno Si-C-O-Zr Fiber Reinforced Minicomposites

Minicomposites consisting of two varieties of Zr containing SiC-based fibers from Ube (Tyranno) with BN interphases and CVI SiC matrices were studied. The two fiber-types were the ZMI and ZE fiber-types that contain approximately 8 and 2% oxygen, respectively. The minicomposites were precracked and tested under constant load testing at temperatures ranging from 700 to 1200 C. The data were then compared to the rupture behavior of Hi- Nicalon (TM) fiber reinforced minicomposites tested under identical conditions. It was found that the Ube fiber-types had stress rupture life equivalent to Hi- Nicalon (TM) over the entire temperature range. A potential benefit of the ZMI fiber-type is that it offers rupture properties almost as good as Hi-Nicalon (TM) at the cost of ceramic grade Nicalon (TM).

Morscher, Gregory N.↗

A simple test for thermomechanical evaluation of ceramic fibers

A simple bend stress relaxation (BSR) test was developed to measure the creep related properties of ceramic fibers and whiskers. The test was applied to a variety of commercial and developmental Si based fibers to demonstrate capabilities and to evaluate the relative creep resistance of the fibers at 1200 to 1400 C. The implications of these results and the advantages of the BSR test over typical tensile creep tests are discussed.

Morscher, Gregory N.↗

A simple test for thermomechanical evaluation of ceramic fibers

A simple bend stress relaxation (BSR) test was developed to measure the creep related properties of ceramic fibers and whiskers. The test was applied to a variety of commercial and developmental Si based fibers to demonstrate capabilities and to evaluate the relative creep resistance of the fibers at 1200 to 1400 C. The implications of these results and the advantages of the BSR test over typical tensile creep tests are discussed.

Morscher, Gregory N.↗

Tensile Creep and Fatigue of Sylramic-iBN Melt-Infiltrated SiC Matrix Composites: Retained Properties, Damage Development, and Failure Mechanisms

An understanding of the elevated temperature tensile creep, fatigue, rupture, and retained properties of ceramic matrix composites (CMC) envisioned for use in gas turbine engine applications are essential for component design and life-prediction. In order to quantify the effect of stress, time, temperature, and oxidation for a state-of-the-art composite system, a wide variety of tensile creep, dwell fatigue, and cyclic fatigue experiments were performed in air at 1204 C for the SiC/SiC CMC system consisting of Sylramic-iBN SiC fibers, BN fiber interphase coating, and slurry-cast melt-infiltrated (MI) SiC-based matrix. Tests were either taken to failure or interrupted. Interrupted tests were then mechanically tested at room temperature to determine the residual properties. The retained properties of most of the composites subjected to tensile creep or fatigue were usually within 20% of the as-produced strength and 10% of the as-produced elastic modulus. It was observed that during creep, residual stresses in the composite are altered to some extent which results in an increased compressive stress in the matrix upon cooling and a subsequent increased stress required to form matrix cracks. Microscopy of polished sections and the fracture surfaces of specimens which failed during stressed-oxidation or after the room-temperature retained property test was performed on some of the specimens in order to quantify the nature and extent of damage accumulation that occurred during the test. It was discovered that the distribution of stress-dependent matrix cracking at 1204 C was similar to the as-produced composites at room temperature; however, matrix crack growth occurred over time and typically did not appear to propagate through thickness except at final failure crack. Failure of the composites was due to either oxidation-induced unbridged crack growth, which dominated the higher stress regime (> 179 MPa) or controlled by degradation of the fibers, probably caused by intrinsic creep-induced flaw growth of the fibers or internal attack of the fibers via Si diffusion through the CVI SiC and/or microcracks at the lower stress regime (< 165 MPa).

Morscher, Greg↗

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.↗

Friction and Wear of Monolithic and Fiber Reinforced Silicon-Ceramics Sliding Against IN-718 Alloy at 25 to 800 C in Atmospheric Air at Ambient Pressure

The friction and wear of monolithic and fiber reinforced Si-ceramics sliding against the nickel base alloy IN-718 at 25 to 800 C was measured. The monolithic materials tested were silicon carbide (SiC), fused silica (SiO2), syalon, silicon nitride (Si3N4) with W and Mg additives, and Si3N4 with Y2O3 additive. At 25 C fused silica had the lowest friction while Si3N4 (W,Mg type) had the lowest wear. At 800 C syalon had the lowest friction while Si3N4 (W,Mg type) and syalon had the lowest wear. The SiC/IN-718 couple had the lowest total wear at 25 C. At 800 C the fused silica/IN-718 couple exhibited the least total wear. SiC fiber reinforced reaction bonded silicon nitride (RBSN) composite material with a porosity of 32 percent and a fiber content of 23 vol percent had a lower coefficient of friction and wear when sliding parallel to the fiber direction than in the perpendicular at 25 C. The coefficient of friction for the carbon fiber reinforced borosilicate composite was 0.18 at 25 C. This is the lowest of all the couples tested. Wear of this material was about two decades smaller than that of the monolithic fused silica. This illustrates the large improvement in tribological properties which can be achieved in ceramic materials by fiber reinforcement. At higher temperatures the oxidation products formed on the IN-718 alloy are transferred to the ceramic by sliding action and forms a thin, solid lubricant layer which decreases friction and wear for both the monolithic and fiber reinforced composites.

Deadmore, Daniel L.↗

Intermediate Temperature Strength Degradation in SiC/SiC Composites

Woven silicon carbide fiber-reinforced, silicon carbide matrix composites are leading candidate materials for an advanced jet engine combustor liner application. Although the use temperature in the hot region for this application is expected to exceed 1200 C, a potential life-limiting concern for this composite system exists at intermediate temperatures (800 +/- 200 C), where significant time-dependent strength degradation has been observed under stress-rupture loading. A number of factors control the degree of stress-rupture strength degradation, the major factor being the nature of the interphase separating the fiber and the matrix. BN interphases are superior to carbon interphases due to the slower oxidation kinetics of BN. A model for the intermediate temperature stress-rupture of SiC/BN/SiC composites is presented based on the observed mechanistic process that leads to strength degradation for the simple case of through-thickness matrix cracks. The approach taken has much in common with that used by Curtin and coworkers, for two different composite systems. The predictions of the model are in good agreement with the rupture data for stress-rupture of both precracked and as-produced composites. Also, three approaches that dramatically improve the intermediate temperature stress-rupture properties are described: Si-doped BN, fiber spreading, and 'outside debonding'.

Morscher, Gregory N.↗

Raman Study of Uncoated and P-bn/sic-coated Hi-nicalon Reinforced Celsian Matrix Composites: Residual Stress in the Fibers - Part 2

Band shifts on Raman spectra were used to assess, at a microscopic scale, the residual strain existing in Hi-Nicalon fibers reinforcing celsian matrix composites. Uncoated as well as p-BN/SiC- and p-B(Si)N/SiC-coated Hi-Nicalon fibers were used as the reinforcements. We unambiguously conclude that the fibers are in a state of compressive residual stress. Quantitative determination of the residual stress was made possible by taking into account the heating induced by laser probing and by using a reference line, of fixed wavenumber. We found fiber compressive residual stress values between 110 and 960 MPa depending on the fiber/matrix coating in the composite. A stress relaxation-like phenomenon was observed at the surface of p-BN/SiC-coated Hi-Nicalon fibers whereas the uncoated or p-B(Si)N/SiC-coated Hi-Nicalon fibers did not show any stress relaxation in the Celsian matrix composites.

Gouadec, Gwenael↗

Genesis Concentrator Target Particle Contamination Mapping and Material Identification

The majority of surface particles were found to be < 5 microns in diameter with increasing numbers close to the optical resolution limit of 0.3 microns. Acceleration grid EDS results show that the majority of materials appear to be from the SRC shell and SLA materials which include carbon-carbon fibers and Si-rich microspheres in a possible silicone binder. Other major debris material from the SRC included white paint, kapton, collector array fragments, and Al. Image analysis also revealed that SRC materials were also found mixed with the Utah mud and salt deposits. The EDS analysis of the acceleration grid showed that particles < 1 m where generally carbon based particles. Chemical cleaning techniques with Xylene and HF in an ultrasonic bath are currently being investigated for removal of small particles by the Genesis science team as well as ultra-pure water megasonic cleaning by the JSC team [4]. Removal of organic contamination from target materials is also being investigated by the science team with the use of UV-ozone cleaning devices at JSC and Open University [5]. In preparation for solar wind oxygen analyses at UCLA and Open University [1, 2], surface particle contamination on three Genesis concentrator targets was closely examined to evaluate cleaning strategies. Two silicon carbide (Genesis sample # 60001 and 60003) and one chemical vapor deposited (CVD) 13C concentrator target (60002) were imaged and mosaic mapped with optical microscopes. The resulting full target mosaic images and particle feature maps were subsequently compared with non-flight, but flight-like, concentrator targets and sample return capsule (SRC) materials. Contamination found on the flown concentrator acceleration grid was further examined using a scanning electron microscope (SEM). Energy dispersive X-ray spectroscopy (EDS) for particle identification was subsequently compared with the optical images from the flown targets. Figure 1 show that all three targets imaged in this report are fully intact and do not show any signs of material fractures. However, previous ellipsometry results and overview imaging of both flown SiC targets show a solar wind irradiation gradient from the center focal point to the outer edge [3]. In addition, due to the hard landing, each target has experienced varying degrees of impacts, scratches, and particle debris from the spacecraft and Utah impact site.

Calaway, Michael J.↗

Characterization of Biological Fallout Particles of Cleanrooms to Measure Spacecraft Cleanliness

NASA cleanrooms are humidity, temperature-regulated, and particle contaminant-controlled environments used for spacecraft assembly. Microorganisms, which are crucial contaminants shed from humans and transported through the environment, can adapt to the oligotrophic cleanroom conditions. These biogenic particles need to be identified to extend our knowledge of biological contamination for future NASA mission use. Here, we devised an aluminum coupon with polycarbonate filter setup to collect fallout particles from an ISO 5 and an ISO 7 cleanroom. We demonstrated the presence of microbial particles, as standalone entities and associated with inert particles in cleanroom environments. The contamination was confirmed as biogenic in virtue of estimating the elemental composition of individual and aggregated particles using an epifluorescence and Field Emission Scanning Electron Microscopy (FESEM) coupled with an energy dispersive X-ray analysis (EDX). Epifluorescence microscopy showed that the particles were stained less (25%) with SYTO 9 and more (75%) with propidium iodide, suggesting that the suspected biogenic particles are membrane-compromised. Remarkably, biological particles such as bacteria and fungal spores/hyphae were observed at sizes ranging from 2 to 70 µm, with abundant C and O elemental signatures and essential tracers (Na, Mg, K, Ca and Cl). Inert particles (2 to 500 µm) that were characterized included compositions such as silica (SiO2), aluminosilicates (Al, Si), and carbonaceous fibers. Furthermore, we designed and illustrated a unique correlative epifluorescence and FE-SEM method to strengthen this approach by acquiring the same biogenic particles in the same filter coupon for a one-to-one comparison. Interestingly, the SYTO 9 stained particles showed abundant C and O elemental signature implying that they are viable microbial particles. Constant evaluation of cleanroom biological and inert particles will help to characterize biological contamination for future NASA missions (e.g. Mars 2020).

Malli Mohan, Ganesh Babu↗