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NASA NTRS1986

SiC fiber reinforced reaction-bonded Si3N4 composites

A technique for fabricating strong and tough SiC fiber reinforced reaction bonded Si3N4 matrix composites (SiC/RBSN) was developed. Using this technique, composites containing approximately 23, 30, and 40 volume fractions of aligned 140 micron diameter, chemically vapor deposited SiC fibers were fabricated. The room temperature physical and mechanical properties were evaluated. The results for composite tensile strength, bend strength, and fracture strain indicate that the composite displays excellent properties when compared with the unreinforced matrix of comparable porosity. The composite stress at which the matrix first cracks and the ultimate composite fracture strength increase with increasing volume fraction of fibers, and the composite fails gracefully. The mechanical property data of this ceramic composite are compared with similar data for unreinforced commercially available Si3N4 materials and for SEP SiC/SiC composites.

Bhatt, Ramakrishna T.↗

DOE OSTI2026

Efficient Silicon Carbide (SiC) Fiber Manufacture: Continuous Processing of Novel Precursors via Modified Material Handling

General Atomics Electromagnetic Systems (GA-EMS) together with The Nonwovens Institute (NWI) and Harper International have executed on a development project to improve the production efficiency and reduce the production cost of silicon carbide (SiC) fiber – a critical material that advances US energy security and aerospace leadership. In the first budget period (BP1), the modified tow throughput (MTT) apparatus was developed, enabling fiber spinning in the form of loose coils rather than tightly packed spools (Figure 1) for batch processing of SiC fiber. This coil-based approach was proven to be capable of uniform fiber crosslinking and ceramic conversion, as well as demonstrating key process efficiencies while meeting the program fiber property targets.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1992

Oxidation effects on the mechanical properties of a SiC-fiber-reinforced reaction-bonded Si3N4 matrix composite

The room-temperature mechanical properties of SiC fiber reinforced reaction bonded silicon nitride composites were measured after 100 hrs exposure at temperatures to 1400 C in nitrogen and oxygen environments. The composites consisted of approx. 30 vol percent uniaxially aligned 142 micron diameter SiC fibers in a reaction bonded Si3N4 matrix. The results indicate that composites heat treated in a nitrogen environment at temperatures to 1400 C showed deformation and fracture behavior equivalent to that of the as-fabricated composites. Also, the composites heat treated in an oxidizing environment beyond 400 C yielded significantly lower tensile strength values. Specifically in the temperature range from 600 to 1000 C, composites retained approx. 40 percent of their as-fabricated strength, and those heat treated in the temperatures from 1200 to 1400 C retained 70 percent. Nonetheless, for all oxygen heat treatment conditions, composite specimens displayed strain capability beyond the matrix fracture stress; a typical behavior of a tough composite.

Bhatt, Ramakrishna T.↗

NASA NTRS1998

Interfacial Thickness Guidelines for SiC(Fiber)/SiC(Matrix) Composites

Researchers at the NASA Lewis Research Center have developed a guideline for the interface thickness necessary for SiC(Fiber)/SiC(Matrix) composites to demonstrate good composite properties. These composite materials have potential commercial applications for high-temperature structural components such as engine hot sections. Several samples of each were composed from three different small-diameter (less than 20 mm), polymer-derived SiC fibers that were woven into two-dimensional cloths and laid up as preforms. The preforms were treated with a chemical-vapor-infiltrated boron nitride layer as an interfacial coating on the fiber surfaces to provide the necessary debonding characteristics for successful composite behavior. Then, the preforms were filled with additional SiC as a matrix phase.

Hurst, Janet B.↗

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 NTRS1990

Influence of interfacial shear strength on the mechanical properties of SiC fiber reinforced reaction-bonded silicon nitride matrix composites

The influence of fiber/matrix interface microstructure and interfacial shear strength on the mechanical properties of a fiber-reinforced ceramic composite was evaluated. The composite consisted of approximately 30 vol percent uniaxially aligned 142 microns diameter SiC fibers (Textron SCS-6) in a reaction-bonded Si3N4 matrix (SiC/RBSN). The interface microstructure was varied by controlling the composite fabrication conditions and by heat treating the composite in an oxidizing environment. Interfacial shear strength was determined by the matrix crack spacing method. The results of microstructural examination indicate that the carbon-rich coating provided with the as-produced SiC fibers was stable in composites fabricated at 1200 C in a nitrogen or in a nitrogen plus 4 percent hydrogen mixture for 40 hr. However this coating degraded in composites fabricated at 1350 C in N2 + 4 percent H2 for 40 and 72 hr and also in composites heat treated in an oxidizing environment at 600 C for 100 hr after fabrication at 1200 C in a nitrogen. It was determined that degradation occurred by carbon removal which in turn had a strong influence on interfacial shear strength and other mechanical properties. Specifically, as the carbon coating was removed, the composite interfacial shear strength, primary elastic modulus, first matrix cracking stress, and ultimate tensile strength decreased, but the first matrix cracking strain remained nearly the same.

Bhatt, Ramakrishna T.↗

NASA NTRS1991

The microstructure of SCS-6 SiC fiber

A thorough investigation of the microstructure of single SCS-6 SiC fibers widely used as reinforcements in metal-matrix and ceramic-matrix composites has been made. Various techniques of EM including SEM, TEM, HREM parallel electron energy loss spectroscopy (PEELS), and SAM have been used to analyze and characterize the microstructure. The fiber is a complicated composite consisting of many different layers of SiC deposited on a carbon core and different carbonaceous coatings covering the SiC layers. The structural and chemical aspects of each layer are characterized and discussed.

Ning, X. J.↗

NASA NTRS2008

Processing and Structural Advantages of the Sylramic-iBN SiC Fiber for SiC/SiC Components

The successful high-temperature application of complex-shaped SiC/SiC components will depend on achieving as high a fraction of the as-produced fiber strength as possible during component fabrication and service. Key issues center on a variety of component architecture, processing, and service-related factors that can reduce fiber strength, such as fiber-fiber abrasion during architecture shaping, surface chemical attack during interphase deposition and service, and intrinsic flaw growth during high-temperature matrix formation and composite creep. The objective of this paper is to show that the NASA-developed Sylramic-iBN SiC fiber minimizes many of these issues for state-of-the-art melt-infiltrated (MI) SiC/BN/SiC composites. To accomplish this, data from various mechanical tests are presented that compare how different high performance SiC fiber types retain strength during formation of complex architectures, during processing of BN interphases and MI matrices, and during simulated composite service at high temperatures.

Yun, H. M.↗

NASA NTRS1984

Creep of chemically vapor deposited SiC fibers

The creep, thermal expansion, and elastic modulus properties for chemically vapor deposited SiC fibers were measured between 1000 and 1500 C. Creep strain was observed to increase logarithmically with time, monotonically with temperature, and linearly with tensile stress up to 600 MPa. The controlling activation energy was 480 + or - 20 kJ/mole. Thermal pretreatments near 1200 and 1450 C were found to significantly reduce fiber creep. These results coupled with creep recovery observations indicate that below 1400 C fiber creep is anelastic with neglible plastic component. This allowed a simple predictive method to be developed for describing fiber total deformation as a function of time, temperature, and stress. Mechanistic analysis of the property data suggests that fiber creep is the result of beta-SiC grain boundary sliding controlled by a small percent of free silicon in the grain boundaries.

Dicarlo, J. A.↗

NASA NTRS1999

Thermomechanical Characterization of SiC Fiber Tows and Implications for CMC

In order to better understand SiC fiber behavior within CMC microstructures, mechanical tests were performed on multifilament tows consisting of different types of as produced and pretreated fibers. Tensile strengths of tows and single fibers were measured at room temperature for nonstoichiometric Hi-Nicalon and ZMI fibers and for stoichiometric Hi-Nicalon-S, Tyranno SA. and Sylramic fibers. Based on simple bundle theory, measured strengths for as-produced and sized tows were in general agreement with the single fiber results. However, after sizing removal under inert conditions, tow strengths for the coarser grained stoichiometric fibers were typically lower than those predicted from individual fiber data. This effect is attributed to enhanced fiber-fiber mechanical interaction caused by sizing removal from the rough surfaces of these fibers. In support of this, tow strengths remained high for those fiber types with fine grains or excess surface carbon; and, when re-coated with a BN interphase coating, tow strengths for the coarser grained fibers returned to their as-produced values. When the tows were pretreated in air at intermediate temperatures, tow strengths decreased in a manner that could be correlated with the oxidation characteristics of each fiber type as measured by thermogravimetric analysis. The creep and rupture properties of Hi-Nicalon and Sylramic tows were also measured in air and argon from 1200 to 1400 C. Although displaying transient and environmental effects similar to single fibers, the tows crept faster at short times and slower at long times. This resulted in the tow rupture strengths at long time being much greater than the rupture strengths of single fibers. The CMC implications of the tow results are discussed, as well as the benefits and limitations of tow testing.

Yun, H. M.↗

NASA NTRS2010

Oxidation of SiC Fiber-Reinforced SiC Matrix Composites with a BN Interphase

SiC-fiber reinforced SiC matrix composites with a BN interphase were oxidized in reduced oxygen partial pressures of oxygen to simulate the environment for hypersonic vehicle leading edge applications. The constituent fibers as well as composite coupons were oxidized in oxygen partial pressures ranging from 1000 ppm O2 to 5% O2 balance argon. Exposure temperatures ranged from 816 C to 1353 C (1500 F to 2450 F). The oxidation kinetics of the coated fibers were monitored by thermogravimetric analysis (TGA). An initial rapid transient weight gain was observed followed by parabolic kinetics. Possible mechanisms for the transient oxidation are discussed. One edge of the composite coupon seal coat was ground off to simulate damage to the composite which allowed oxygen ingress to the interior of the composite. Oxidation kinetics of the coupons were characterized by scanning electron microscopy since the weight changes were minimal. It was found that sealing of the coupon edge by silica formation occurred. Differences in the amount and morphology of the sealing silica as a function of time, temperature and oxygen partial pressure are discussed. Implications for use of these materials for hypersonic vehicle leading edge materials are summarized.

Opila, Elizabeth↗

NASA NTRS2005

Toughened Matrix SiC Fiber Reinforced Composites

First matrix cracking stress is a critical parameter for application of Sic fiber reinforced composites in highly stressed, environmentally demanding applications such as turbine blades. High matrix fracture toughness is a key property that contributes to high composite fracture stress. Silicon nitride offers reduced matrix elastic modulus, lower coefficient of thermal expansion, and potentially high fracture toughness compared to Sic matrices. All of these factors can be used to advantage to increase matrix fracture stress. As a first model system we are pursuing toughened silicon nitride matrix composites reinforced with SCS-9 fibers. Fabrication is by tape casting the matrix plies and tape lay-up with fiber plies followed by hot pressing at 1800 C. Progress toward this end will be reported.

Levine, Stanley R.↗

NASA NTRS1995

Effects of Thermal Treatment on Tensile Creep and Stress-Rupture Behavior of Hi-Nicalon SiC Fibers

Tensile creep and stress-rupture studies were conducted on Hi-Nicalon SiC fibers at 1200 and 1400 C in argon and air. Examined were as-received fibers as well as fibers annealed from 1400 to 1800 C for 1 hour in argon before testing. The creep and rupture results for these annealed fibers were compared to those of the as-received fibers to determine the effects of annealing temperature, test temperature, and test environment. Argon anneals up to 1500 C degrade room temperature strength of Hi-Nicalon fibers, but improve fiber creep resistance in argon or air by as much as 100% with no significant degradation in rupture strength. Argon anneals above 1500 C continue to improve fiber creep resistance when tested in argon, but significantly degrade creep resistance and rupture strength when tested in air. Decrease in creep resistance in air is greater at 1200 C than at 1400 C. Mechanisms are suggested for the observed behavior.

Yun, H. M.↗

NASA NTRS1995

Microstructural and strength stability of a developmental CVD SiC fiber

The effects of thermal exposure on the room temperature tensile strength and microstructure of a developmental 50 micron CVD SiC fiber have been studied. The fibers were heat treated between 600 and 2000 C in 0.1 MPa argon and air environments for up to 100 hr. In the as-fabricated condition, the fibers showed approximately 6 GPa tensile strength. After argon treatment, the fibers showed strength degradation after 1 hr exposure beyond 1000 C, but those exposed between 1600 and 2000 C retained approximately 2 GPa strength. TEM results showed microstructural changes both in the surface coating and SiC sheath. Flaws created by the rearrangement of carbon in the surface coating and growth of equiaxed SiC grain zone in the SiC sheath are the suggested mechanisms of strength degradation. After air treatment, fibers showed strength degradation after only 2 min exposure at 600 C. Strength retention after 2 min at 1500 C was approximately 2 GPa. Oxidation of the surface coating is the primary reason for strength degradation.

Bhatt, Ramakrishna T.↗

NASA NTRS2017

SiC Fibers and SiCf/SiC Ceramic Matrix Minicomposites Damage Behavior

Silicon Carbide based Ceramic Matrix Composites (CMCs) are attractive materials for use in high-temperature applications in the aerospace industry. Performance and durability of CMCs depend on the properties of its constituents such as fibers and matrix. Therefore, CMCs constituents limitations and damage mechanisms are discussed and characterized in representative simulated application conditions and dominant damage mechanisms are identified at elevated temperatures. In this work, the initiation and evolution of damage in Hi-Nicalon type S fiber-reinforced minicomposites with different interphases thicknesses from different manufacturers were investigated employing several nondestructive evaluation techniques such as acoustic emission, electrical resistance and microscopy. Moreover, the tensile creep behavior of single Hi-Nicalon Type S SiC fibers were tested and characterized and creep parameters were extracted. Fibers creep tests were performed in air or vacuum at 1200-1482 C under high stresses. Creep parameters was then used in understanding load sharing and lifing of ceramic matrix minicomposites. Future work plans will be reviewed.

SiC fibers↗

NASA NTRS1989

Measurement of interfacial shear strength in SiC-fiber/Si3N4 composites

An indentation method for measuring shear strength in brittle matrix composites was applied to SiC-fiber/Si3N4-matrix samples. Three methods were used to manufacture the composites: reaction bonding of a Si/SiC preform, hot-pressing, and nitrogen-overpressure sintering. An indentation technique developed by Marshall for thin specimens was used to measure the shear strength of the interface and the interfacial friction stresses. This was done by inverting the sample after the initial push through and retesting the pushed fibers. SEM observations showed that the shear strength was determined by the degree of reaction between the fiber and the matrix unless the fiber was pushed out of its (well-bonded) sheath.

Laughner, James W.↗

NASA NTRS1993

Tensile creep and creep-recovery behavior of a SiC-fiber-Si3N4-matrix composite

The tensile creep and creep-recovery behavior of a hot-pressed unidirectional SiC-fiber/Si3N4-matrix composite was investigated at 1200 C in air, in order to determine how various sustained and cyclic creep loading histories would influence the creep rate, accumulated creep strain, and the amount of strain recovered upon specimen unloading. The data accumulated indicate that the fundamental damage mode for sustained tensile creep at stresses of 200 and 250 MPa was periodic fiber fracture and that the creep life and the failure mode at 250 MPa were strongly influenced by the rate at which the initial creep stress was applied. Cyclic loading significantly lowered the duration of primary creep and the overall creep-strain accumulation. The implications of the results for microstructural and component design are discussed.

Holmes, John W.↗

NASA NTRS1994

Tensile Creep and Stress-rupture Behavior of Polymer Derived Sic Fibers

Tensile creep and stress-rupture studies were conducted on polymer derived Nicalon, Hi-Nicalon, and SiC/BN-coated Nicalon SiC fibers. Test conditions were temperatures from 1200 to 1400 C, stresses from 100 to 1600 MPa, stress application times up to 200 hours, and air, argon, and vacuum test environments. For all fibers, creep occurred predominantly in the primary stage. Hi-Nicalon had much higher 0.2 and 1 percent creep strengths than as-produced as well as-coated Nicalon fibers. The stress-rupture strength of Hi-Nicalon up to 100 hours was also higher than that of the coated and as-produced Nicalon fibers. SiC/BN coating on Nicalon increased only the short-term low-temperature rupture strength. Limited testing in argon and vacuum suggests that for all fiber types, creep and rupture resistances are reduced in comparison to the results in air. Possible mechanisms for the observed behavior are discussed.

Yun, H. M.↗