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NASA NTRS2024

Short-Term Elevated Temperature Mechanical Performance and Microstructure of A Niobium-Zirconium Alloy Produced via Laser Powder Bed Fusion In-Situ Alloying

Nb-1Zr is a readily fabricable, dispersion-strengthened niobium alloy with improved elevated temperature properties compared to commercially pure niobium. This low to moderate strength niobium alloy is desirable in thermal management systems for fission power and propulsion applications; however, pre-alloyed spherical feedstock for powder-based additive manufacturing processes is generally unavailable. Laser powder bed fusion (L-PBF) in-situ alloying of a Nb-1Zr chemistry was performed using a high-purity niobium feedstock coated with 1 wt% of zirconium-based ceramic compound nano-powders: ZrO 2 , ZrC, and ZrH 2 . The additively manufactured material was mechanically tested at elevated temperatures within a controlled environment in the as-built condition. For comparison, traditionally manufactured wrought feedstock was also tested within an identical environment. Examination of the materials’ microstructure and short-term elevated temperature mechanical response determined: in-situ alloying of spherical Nb powder feedstock with Zr-based ceramic nanoparticles can be successfully implemented; the ZrO 2 addition offered the greatest elevated temperature stability and strength but exhibited brittle behavior; the ZrC addition achieved a balance of room temperature ductility and elevated temperature strength; and the ZrH 2 -modified material had the lowest as-built interstitial content and showed high ductility with mechanical performance most similar to wrought Nb-1Zr.

Niobium Alloy↗

NASA NTRS2017

Advanced Environmental Barrier Coating Development for SiC-SiC Ceramic Matrix Composite Components

This presentation reviews the NASA advanced environmental barrier coating (EBC) system development for SiC-SiC Ceramic Matrix Composite (CMC) combustors particularly under the NASA Environmentally Responsible Aviation, Fundamental Aeronautics and Transformative Aeronautics Concepts Programs. The emphases have been placed on the current design challenges of the 2700-3000F capable environmental barrier coatings for low NOX emission combustors for next generation turbine engines by using advanced plasma spray based processes, and the coating processing and integration with SiC-SiC CMCs and component systems. The developments also have included candidate coating composition system designs, degradation mechanisms, performance evaluation and down-selects; the processing optimizations using TriplexPro Air Plasma Spray Low Pressure Plasma Spray (LPPS), Plasma Spray Physical Vapor Deposition and demonstration of EBC-CMC systems. This presentation also highlights the EBC-CMC system temperature capability and durability improvements under the NASA development programs, as demonstrated in the simulated engine high heat flux, combustion environments, in conjunction with high heat flux, mechanical creep and fatigue loading testing conditions.

CMAS↗

NASA NTRS2009

Recent Developments in Ultra High Temperature Ceramics at NASA Ames

NASA Ames is pursuing a variety of approaches to modify and control the microstructure of UHTCs with the goal of improving fracture toughness, oxidation resistance and controlling thermal conductivity. The overall goal is to produce materials that can perform reliably as sharp leading edges or nose tips in hypersonic reentry vehicles. Processing approaches include the use of preceramic polymers as the SiC source (as opposed to powder techniques), the addition of third phases to control grain growth and oxidation, and the use of processing techniques to produce high purity materials. Both hot pressing and field assisted sintering have been used to make UHTCs. Characterization of the mechanical and thermal properties of these materials is ongoing, as is arcjet testing to evaluate performance under simulated reentry conditions. The preceramic polymer approach has generated a microstructure in which elongated SiC grains grow in the form of an in-situ composite. This microstructure has the advantage of improving fracture toughness while potentially improving oxidation resistance by reducing the amount and interconnectivity of SiC in the material. Addition of third phases, such as Ir, results in a very fine-grained microstructure, even in hot-pressed samples. The results of processing and compositional changes on microstructure and properties are reported, along with selected arcjet results.

Johnson, Sylvia M.↗

NASA NTRS1983

A basic design fault in ceramic flat packs

Drotman, B.↗

NASA NTRS1983

A basic design fault in ceramic flat packs

Recent moisture resistance tests of various multilayer top brazed ceramic flat packs and leaded and unleaded chip carriers has revealed a serious design defect. These packages, which utilize a tungsten interconnect system, in the presence of high humidity, suffer a galvanic corrosion which anodically consumes the tungsten. This process can continue until the package suffers an open circuit. The test results indicate that the lead plating system does not adequately seal off the interface area where the tungsten stripe egresses from the inside of the package. Leaded and leadless chip carrier packages were also subjected to the moisture resistance test. The familiar red and green corrosion products were visible after the test was completed. Careful sectioning of the chip carriers has revealed that the tungsten interconnect stripe instead of exiting under the castellations, exits at the top of the castellation and is thus vulnerable to the attack of moisture. These basic design faults severely impact the reliability of these packages.

Drotman, B.↗

NASA NTRS1988

Preparation for microgravity - The role of the Microgravity Material Science Laboratory

Experiments at the NASA Lewis Research Center's Microgravity Material Science Laboratory using physical and mathematical models to delineate the effects of gravity on processes of scientific and commercial interest are discussed. Where possible, transparent model systems are used to visually track convection, settling, crystal growth, phase separation, agglomeration, vapor transport, diffusive flow, and polymer reactions. Materials studied include metals, alloys, salts, glasses, ceramics, and polymers. Specific technologies discussed include the General Purpose furnace used in the study of metals and crystal growth, the isothermal dendrite growth apparatus, the electromagnetic levitator/instrumented drop tube, the high temperature directional solidification furnace, the ceramics and polymer laboratories and the center's computing facilities.

Johnston, J. Christopher↗

NASA NTRS1999

X-33/RLV Program Aerospike Engines

Substantial progress was made during the past year in support of the X-33/RLV program. X-33 activity was directed towards completing the remaining design work and building hardware to support test activities. RLV work focused on the nozzle ramp and powerpack technology tasks and on supporting vehicle configuration studies. On X-33, the design activity was completed to the detail level and the remainder of the drawings were released. Component fabrication and engine assembly activity was initiated, and the first two powerpacks and the GSE and STE needed to support powerpack testing were completed. Components fabrication is on track to support the first engine assembly schedule. Testing activity included powerpack testing and component development tests consisting of thrust cell single cell testing, CWI system spider testing, and EMA valve flow and vibration testing. Work performed for RLV was divided between engine system and technology development tasks. Engine system activity focused on developing the engine system configuration and supporting vehicle configuration studies. Also, engine requirements were developed, and engine performance analyses were conducted. In addition, processes were developed for implementing reliability, mass properties, and cost controls during design. Technology development efforts were divided between powerpack and nozzle ramp technology tasks. Powerpack technology activities were directed towards the development of a prototype powerpack and a ceramic turbine technology demonstrator (CTTD) test article which will allow testing of ceramic turbines and a close-coupled gas generator design. Nozzle technology efforts were focused on the selection of a composite nozzle supplier and on the fabrication and test of composite nozzle coupons.

Source record↗

NASA NTRS2000

Development and Testing of Cooled CMCs for High Thermal Flux Applications

Ceramic Matrix Composites (CMCS) offer the potential for significant weight savings and improved performance for a range of propulsion components utilizing refractory materials. This paper describes the fabrication and testing of functionally graded CMCs produced via a low cost process that represents an order of magnitude cost savings over conventionally fabricated CMCS. Test cylinders were fabricated, characterized and evaluated during exposure to high thermal fluxes of up to 10MW/meters squared at the Laser Hardened Materials Evaluation Laboratory (LHMEL). The bulk density of the CMC tubes was approximately 2.2 grams per cubic centimeters. The performance of cryogenically cooled CMCs was compared with uncooled CMCs against similar thermal loads, and fundamental property data collected for this relatively new breed of CMC. Finally, test thrust cells were fabricated from the functionally graded composite and tested using liquid H2 and O2 propellants at NASA Glen.

Patterson , Mark↗

NASA NTRS2002

HfB2-SiC Materials for Sharp Leading Edges

Future reentry vehicles will need better maneuverability to improve safety and performance. Vehicles with sharp leading edges, as opposed to the blunt nose and leading edges on the current space shuttle, can provide improved lift-to-drag and thus improved maneuverability. Materials capable of operating at temperatures in excess of 2000 C are required. Ultrahigh temperature ceramics (UHTCs) are one class of material being investigated for this application. These materials are diborides of hafnium or zirconium with a second phase of sic. The benefits of using these materials will be discussed as developments in the processing of HfB2/SiC.

Johnson, Sylvia M.↗

NASA NTRS1987

Zirconia toughened SiC whisker reinforced alumina composites small business innovation research

The objective of this phase 1 project was to develop a ceramic composite with superior fracture toughness and high strength, based on combining two toughness inducing materials: zirconia for transformation toughening and SiC whiskers for reinforcement, in a controlled microstructure alumina matrix. The controlled matrix microstructure is obtained by controlling the nucleation frequency of the alumina gel with seeds (submicron alpha-alumina). The results demonstrate the technical feasibility of producing superior binary composites (Al2O3-ZrO2) and tertiary composites (Al2O3-ZrO2-SiC). Thirty-two composites were prepared, consolidated, and fracture toughness tested. Statistical analysis of the results showed that: (1) the SiC type is the key statistically significant factor for increased toughness; (2) sol-gel processing with a-alumina seed had a statistically significant effect on increasing toughness of the binary and tertiary composites compared to the corresponding mixed powder processing; and (3) ZrO2 content within the range investigated had a minor effect. Binary composites with an average critical fracture toughness of 6.6MPam sup 1/2, were obtained. Tertiary composites with critical fracture toughness in the range of 9.3 to 10.1 MPam sup 1/2 were obtained. Results indicate that these composites are superior to zirconia toughened alumina and SiC whisker reinforced alumina ceramic composites produced by conventional techniques with similar composition from published data.

Loutfy, R. O.↗

NASA NTRS1988

Composites That Exceed Superalloys In Rupture Strength

Ceramic-fiber-reinforced iron alloys show promise as turbine parts for intermediate-temperature service. Intermediate-temperature composites reduce weights of turbine blades by 40 percent and increase life expectancies of blades. In study, relatively-low-temperature fabrication process, hollow-cathode sputtering developed.

Petrasek, Donald W.↗

NASA NTRS1988

Proposal for a lunar tunnel-boring machine

A need exists for obtaining a safe and habitable lunar base that is free from the hazards of radiation, temperature gradient, and micrometeorites. A device for excavating lunar material and simultaneously generating living space in the subselenian environment was studied at the conceptual level. Preliminary examinations indicate that a device using a mechanical head to shear its way through the lunar material while creating a rigid ceramic-like lining meets design constraints using existing technology. The Lunar Tunneler is totally automated and guided by a laser communication system. There exists the potential for the excavated lunar material to be used in conjunction with a surface mining process for the purpose of the extraction of oxygen and other elements. Experiments into lunar material excavation and further research into the concept of a mechanical Lunar Tunneler are suggested.

Allen, Christopher S.↗

NASA NTRS1999

Method for Forming Fiber Reinforced Composite Bodies with Graded Composition and Stress Zones

A near-net, complex shaped ceramic fiber reinforced silicon carbide based composite bodies with graded compositions and stress zones is disclosed. To provide the composite a fiber preform is first fabricated and an interphase is applied by chemical vapor infiltration, sol-gel or polymer processes. This first body is further infiltrated with a polymer mixture containing carbon, and/or silicon carbide, and additional oxide, carbide, or nitride phases forming a second body. One side of the second body is spray coated or infiltrated with slurries containing high thermal expansion and oxidation resistant. crack sealant phases and the other side of this second body is coated with low expansion phase materials to form a third body. This third body consisting of porous carbonaceous matrix surrounding the previously applied interphase materials, is then infiltrated with molten silicon or molten silicon-refractory metal alloys to form a fourth body. The resulting fourth body comprises dense composites consisting of fibers with the desired interphase which are surrounded by silicon carbide and other second phases materials at the outer and inner surfaces comprising material of silicon, germanium, refractory metal suicides, borides, carbides, oxides, and combinations thereof The resulting composite fourth body has different compositional patterns from one side to the other.

Singh, Mrityunjay↗

NASA NTRS1999

Optical Fiber Protection

F&S Inc. developed and commercialized fiber optic and microelectromechanical systems- (MEMS) based instrumentation for harsh environments encountered in the aerospace industry. The NASA SBIR programs have provided F&S the funds and the technology to develop ruggedized coatings and coating techniques that are applied during the optical fiber draw process. The F&S optical fiber fabrication facility and developed coating methods enable F&S to manufacture specialty optical fiber with custom designed refractive index profiles and protective or active coatings. F&S has demonstrated sputtered coatings using metals and ceramics and combinations of each, and has also developed techniques to apply thin coatings of specialized polyimides formulated at NASA Langley Research Center. With these capabilities, F&S has produced cost-effective, reliable instrumentation and sensors capable of withstanding temperatures up to 800? C and continues building commercial sales with corporate partners and private funding. More recently, F&S has adapted the same sensing platforms to provide the rapid detection and identification of chemical and biological agents

Source record↗

NASA NTRS1999

Monte Carlo Simulation of Nanoparticle Encapsulation in Flames

Gas-phase combustion (flame) synthesis has been an essential industrial process for producing large quantities of powder materials such as carbon black, titanium dioxide, and silicon dioxide. Flames typically produce simple oxides, with carbon black being the noted exception because the oxides of carbon are gaseous and are easily separated from the particulate matter that is formed during fuel pyrolysis. Furthermore, the powders produced in flames are usually agglomerated, nanometer-sized particles (nanoparticles). This composition and morphology is acceptable for many applications. However, the present interest in nanoparticles for advanced materials application has led to efforts to employ flames for the synthesis of unagglomerated nanoparticles (2 to 100 nm) of metals and non-oxide ceramics. Sodium-halide chemistry has proven to be viable for producing metals and non-oxide ceramics in flames. Materials that have been produced to date include Si (Calcote and Felder, 1993), TiN, TiB2, TiC, TiSi2, SiC, B4C (Glassman et al, 1993) Al, W, Ti, TiB2, AlN, and W-Ti and Al-AlN composites (DuFaux and Axelbaum, 1995, Axelbaum et al 1996,1997). Many more materials are possible. The main challenge that faces application of flame synthesis for advanced materials is overcoming formation of agglomerates in flames (Brezinsky, 1997). The high temperatures and high number densities in the flame environment favor the formation of agglomerates. Agglomerates must be avoided for many reasons. For example, when nanopowders are consolidated, agglomerates have a deleterious effect on compaction density, leading to voids in the final part. Efforts to avoid agglomeration in flames without substantially reducing particle number density and, consequently, production rate, have had limited success. Another critical challenge that faces all synthesis routes for nanopowders is ensuring that the powders are high purity and that the process is scaleable. Though the containerless, high temperature environment of a flame is excellent for producing high-purity simple compounds, ultrafine metals and non-oxide ceramic powders are inherently reactive in the presence of oxygen and/or moisture. Thus, the handling of these powders after synthesis poses a challenging problem. Impurities acquired during handling of nanoparticles have plagued the advancement of nanostructured materials technology.

Sun, Z.↗

NASA NTRS2015

Ultra High Temperature (UHT) SiC Fiber (Phase 2)

Silicon-carbide fiber-reinforced silicon-carbide ceramic matrix composites (SiCSiC CMC) are emerginglightweight re-usable structural materials not only for hot section components in gas turbine engines, but also for controlsurfaces and leading edges of reusable hypersonic vehicles as well as for nuclear propulsion and reactor components. Ithas been shown that when these CMC are employed in engine hot-section components, the higher the upper usetemperature (UUT) of the SiC fiber, the more performance benefits are accrued, such as higher operating temperatures,reduced component cooling air, reduced fuel consumption, and reduced emissions. The first generation of SiCSiC CMC with a temperature capability of 2200-2400F are on the verge of being introduced into the hot-section components ofcommercial and military gas turbine engines.Today the SiC fiber type currently recognized as the worlds best in terms ofthermo-mechanical performance is the Sylramic-iBN fiber. This fiber was previously developed by the PI at NASA GRC using patented processes to improve the high-cost commercial Sylramic fiber, which in turn was derived from anotherlow-cost low-performance commercial fiber. Although the Sylramic-iBN fiber shows state-of-the art creep and rupture resistance for use temperatures above 2550oF, NASA has shown by fundamental creep studies and model developmentthat its microstructure and creep resistance could theoretically be significantly improved to produce an Ultra HighTemperature (UHT) SiC fiber.This Phase II Seedling Fund effort has been focused on the key objective of effectively repeating the similar processes used for producing the Sylramic-iBN fiber using a design of experiments approach to first understand the cause of the less than optimum Sylramic-iBN microstructure and then attempting to develop processconditions that eliminate or minimize these key microstructural issues. In so doing, it is predicted that that theseadvanced process could result in an UHT SiC fiber with 20 times more creep resistance than the Sylramic-iBN fiber,which in turn would allow SiCSiC CMC to operate up to 2700oF and above, thereby further enhancing the performancebenefits of SiCSiC components in aero-propulsion engines. It was also envisioned that the fiber processes developedduring Phase II efforts would not only reduce production costs for the UHT fiber by using low-cost precursor fibers andcombined processes, but also allow the UHT fibers to be directly produced in preforms of the precursor fibers, possibly atthe facilities of the CMC fabricator.

SiC Ceramic Fiber↗

NASA NTRS2012

Demonstration of Minimally Machined Honeycomb Silicon Carbide Mirrors

Honeycomb silicon carbide composite mirrors are made from a carbon fiber preform that is molded into a honeycomb shape using a rigid mold. The carbon fiber honeycomb is densified by using polymer infiltration pyrolysis, or through a reaction with liquid silicon. A chemical vapor deposit, or chemical vapor composite (CVC), process is used to deposit a polishable silicon or silicon carbide cladding on the honeycomb structure. Alternatively, the cladding may be replaced by a freestanding, replicated CVC SiC facesheet that is bonded to the honeycomb. The resulting carbon fiber-reinforced silicon carbide honeycomb structure is a ceramic matrix composite material with high stiffness and mechanical strength, high thermal conductivity, and low CTE (coefficient of thermal expansion). This innovation enables rapid, inexpensive manufacturing. The web thickness of the new material is less than 1 millimeter, and core geometries tailored. These parameters are based on precursor carbon-carbon honeycomb material made and patented by Ultracor. It is estimated at the time of this reporting that the HoneySiC(Trademark) will have a net production cost on the order of $38,000 per square meter. This includes an Ultracor raw material cost of about $97,000 per square meter, and a Trex silicon carbide deposition cost of $27,000 per square meter. Even at double this price, HoneySiC would beat NASA's goal of $100,000 per square meter. Cost savings are estimated to be 40 to 100 times that of current mirror technologies. The organic, rich prepreg material has a density of 56 kilograms per cubic meter. A charred carbon-carbon panel (volatile organics burnt off) has a density of 270 kilograms per cubic meter. Therefore, it is estimated that a HoneySiC panel would have a density of no more than 900 kilograms per cubic meter, which is about half that of beryllium and about onethird the density of bulk silicon carbide. It is also estimated that larger mirrors could be produced in a matter of weeks. Each cell is completely uniform, maintaining the shape of the inserted mandrel. Furthermore, the layup creates pressure that insures node bond strength. Each node is a composite laminate using only the inherent resin system to form the bond. This contrasts starkly with the other known method of producing composite honeycomb, in which individual corrugations are formed, cured, and then bonded together in a secondary process. By varying the size of the mandrels within the layup, varying degrees of density can be achieved. Typical sizes are 3/8 and 3/16 in. (approximately 10 and 5 millimeters). Cell sizes up to 1 in. (approximately 25 millimeters) have been manufactured. Similarly, the shape of the core can be altered for a flexible honeycomb structure.

Goodman, William↗

NASA NTRS1993

Improved ceramic slip casting technique

A primary concern in modern fluid dynamics research is the experimental verification of computational aerothermodynamic codes. This research requires high precision and detail in the test model employed. Ceramic materials are used for these models because of their low heat conductivity and their survivability at high temperatures. To fabricate such models, slip casting techniques were developed to provide net-form, precision casting capability for high-purity ceramic materials in aqueous solutions. In previous slip casting techniques, block, or flask molds made of plaster-of-paris were used to draw liquid from the slip material. Upon setting, parts were removed from the flask mold and cured in a kiln at high temperatures. Casting detail was usually limited with this technique -- detailed parts were frequently damaged upon separation from the flask mold, as the molded parts are extremely delicate in the uncured state, and the flask mold is inflexible. Ceramic surfaces were also marred by 'parting lines' caused by mold separation. This adversely affected the aerodynamic surface quality of the model as well. (Parting lines are invariably necessary on or near the leading edges of wings, nosetips, and fins for mold separation. These areas are also critical for flow boundary layer control.) Parting agents used in the casting process also affected surface quality. These agents eventually soaked into the mold, the model, or flaked off when releasing the case model. Different materials were tried, such as oils, paraffin, and even an algae. The algae released best, but some of it remained on the model and imparted an uneven texture and discoloration on the model surface when cured. According to the present invention, a wax pattern for a shell mold is provided, and an aqueous mixture of a calcium sulfate-bonded investment material is applied as a coating to the wax pattern. The coated wax pattern is then dried, followed by curing to vaporize the wax pattern and leave a shell mold of the calcium sulfate-bonded investment material. The shell mold is cooled to room temperature, and a ceramic slip is poured therein. After a ceramic shell of desired thickness has set up in the shell mold, excess ceramic slip is poured out. While still wet, the shell mold is peeled from the ceramic shell to expose any delicate or detailed parts, after which the ceramic shell is cured to provide a complete, detailed, precision ceramic article without parting lines.

Buck, Gregory M.↗