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NASA NTRS2008

Monitoring Damage Accumulation in Ceramic Matrix Composites Using Electrical Resistivity

The electric resistance of woven SiC fiber reinforced SiC matrix composites were measured under tensile loading conditions. The results show that the electrical resistance is closely related to damage and that real-time information about the damage state can be obtained through monitoring of the resistance. Such self-sensing capability provides the possibility of on-board/in-situ damage detection and accurate life prediction for high-temperature ceramic matrix composites. Woven silicon carbide fiber-reinforced silicon carbide (SiC/SiC) ceramic matrix composites (CMC) possess unique properties such as high thermal conductivity, excellent creep resistance, improved toughness, and good environmental stability (oxidation resistance), making them particularly suitable for hot structure applications. In specific, CMCs could be applied to hot section components of gas turbines [1], aerojet engines [2], thermal protection systems [3], and hot control surfaces [4]. The benefits of implementing these materials include reduced cooling air requirements, lower weight, simpler component design, longer service life, and higher thrust [5]. It has been identified in NASA High Speed Research (HSR) program that the SiC/SiC CMC has the most promise for high temperature, high oxidation applications [6]. One of the critical issues in the successful application of CMCs is on-board or insitu assessment of the damage state and an accurate prediction of the remaining service life of a particular component. This is of great concern, since most CMC components envisioned for aerospace applications will be exposed to harsh environments and play a key role in the vehicle s safety. On-line health monitoring can enable prediction of remaining life; thus resulting in improved safety and reliability of structural components. Monitoring can also allow for appropriate corrections to be made in real time, therefore leading to the prevention of catastrophic failures. Most conventional nondestructive evaluation (NDE) techniques such as ultrasonic C-scan, x-ray, thermography, and eddy current are limited since they require structural components of complex geometry to be taken out of service for a substantial length of time for post-damage inspection and assessment. Furthermore, the typical NDE techniques are useful for identifying large interlaminar flaws, but insensitive to CMC materials flaws developed perpendicular to the surface under tensile creep conditions. There are techniques such as piezoelectric sensor [7,8], and optical fiber [9,10] that could be used for on-line health monitoring of CMC structures. However, these systems involve attaching an external sensor or putting special fibers in CMC composites, which would be problematic at high temperature applications.

Smith, Craig E.↗

NASA NTRS2004

High-Performance SiC/SiC Ceramic Composite Systems Developed for 1315 C (2400 F) Engine Components

As structural materials for hot-section components in advanced aerospace and land-based gas turbine engines, silicon carbide (SiC) ceramic matrix composites reinforced by high performance SiC fibers offer a variety of performance advantages over current bill-of-materials, such as nickel-based superalloys. These advantages are based on the SiC/SiC composites displaying higher temperature capability for a given structural load, lower density (approximately 30- to 50-percent metal density), and lower thermal expansion. These properties should, in turn, result in many important engine benefits, such as reduced component cooling air requirements, simpler component design, reduced support structure weight, improved fuel efficiency, reduced emissions, higher blade frequencies, reduced blade clearances, and higher thrust. Under the NASA Ultra-Efficient Engine Technology (UEET) Project, much progress has been made at the NASA Glenn Research Center in identifying and optimizing two highperformance SiC/SiC composite systems. The table compares typical properties of oxide/oxide panels and SiC/SiC panels formed by the random stacking of balanced 0 degrees/90 degrees fabric pieces reinforced by the indicated fiber types. The Glenn SiC/SiC systems A and B (shaded area of the table) were reinforced by the Sylramic-iBN SiC fiber, which was produced at Glenn by thermal treatment of the commercial Sylramic SiC fiber (Dow Corning, Midland, MI; ref. 2). The treatment process (1) removes boron from the Sylramic fiber, thereby improving fiber creep, rupture, and oxidation resistance and (2) allows the boron to react with nitrogen to form a thin in situ grown BN coating on the fiber surface, thereby providing an oxidation-resistant buffer layer between contacting fibers in the fabric and the final composite. The fabric stacks for all SiC/SiC panels were provided to GE Power Systems Composites for chemical vapor infiltration of Glenn designed BN fiber coatings and conventional SiC matrices. Composite panels with system B were heat treated at Glenn, and the pores that remained open were filled by silicon melt infiltration (MI). Panels with system A and the other SiC/SiC systems were not heat treated, and remaining open pores in these systems were filled with SiC slurry and silicon MI.

DiCarlo, James A.↗

NASA NTRS1994

The Influence of SiC on the Ablation Response of Advanced Refractory Composite Materials

In continuing our studies of advanced refractory composite materials we have recently completed an arc-jet test series of a diverse group of ceramics and ceramic matrix composites. The compositions range from continuous fiber reinforced ceramics to monoliths. Many of these materials contain SiC and one objective of this test series was to identify the influence of SiC oxidation mechanisms on material performance. Hence the arc heater was operated at two conditions; one in which the passive oxidation of SiC would be dominant and the other where the active oxidation of SiC would be dominant. It is shown here that the active oxidation mechanism of SiC does not dominate material performance when it is present at levels equal to or below 20 volume percent.

Bull, Jeffrey D.↗

NASA NTRS1986

Polymer precursors for ceramic matrix composites

The synthesis and characterization of a polycyclohexasilane is reported. Because of its cyclic structure, it is anticipated that this polymer might serve as a precursor to SIC having a high char yield with little rearrangement to form small, volatile cyclic silanes, and, as such, would be of interest as a precursor to SiC composite matrices and fibers, or as a binder in ceramic processing. Several approaches to the synthesis of a bifunctional cyclic monomer were attempted; the most successful of these was metal coupling of PhMeSiCl2 and Me2SiCl2. The procedure gives six-membered ring compounds with all degrees of phenyl substitution, from none to hexaphenyl. The compounds with from 0-2 groups were isolated and characterized. The fraction with degree of phenyl substitution equal to 2, a mixture of cis and trans 1,2-; 1,3-; and 1,4 isomers, was isolated in 32 percent yield. Pure 1,4 diphenyldecamethylcyclohexasilane was isolated from the mixed diphenyl compounds and characterized. Diphenyldecamethylcyclohexasilanes were dephenylated to dichlorodecamethylcyclohexasilanes by treating with H2SO4.NH4Cl in benzene. The latter were purified and polymerized by reacting with sodium in toluene. The polymers were characterized by HPGPC, elemental analysis, proton NMR, and IR. Thermogravimetric analyses were carried out on the polymers. As the yield of residual SiC was low, polymers were heat treated to increase the residual char yield. As high as 51.52 percent residual char yield was obtained in one case.

Litt, M. H.↗

NASA NTRS1993

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.↗

NASA NTRS2017

Effect of Mechanical and Thermal Loading Histories on Residual Properties of SiCf/SiC Ceramic Matrix Composites

Silicon Carbide based Ceramic Matrix Composites (CMCs) are attractive materials for use in high-temperature structural applications in the aerospace and nuclear industries. Under high stresses and temperatures, creep degradation is the dominant damage mechanism in CMCs. Consequently, chemical vapor infiltration (CVI) SiCf/SiC ceramic matrix composites (CMC) incorporating SylramicTM-iBN SiC fibers coated with boron nitride (BN) interphase and CVI-SiC matrix were tested to examine creep behavior in air at a range of elevated temperatures of (2200 - 2700 F). Samples that survived creep tests were evaluated via RT fast fracture tensile tests to determine residual properties, with the use of acoustic emission (AE) to assess stress dependent damage initiation and progression. Microscopy of regions within the gage section of the tested specimens was performed. Observed material degradation mechanisms are discussed.

creep↗

DOE OSTI2021

Integrated TBC/EBC for SiC Fiber Reinforced SiC Matrix Composites for Next Generation Gas Turbines (Final Report)

In this ambitious project, a significant challenge preventing widespread use of ceramic matrix composites in hot section components of gas power generating turbines was addressed. Hot section components made from SiC fiber reinforced SiC matrix composites (SiC/SiC composites), have the potential to achieve a combined cycle energy efficiency of above 65%. To achieve this efficiency, the temperature of the combustion gases on the turbine component surface is expected to reach as high as ~1700ºC (3100ºF). However, SiC/SiC composites suffer from volatilization at high temperature under high velocity steam environment – typical in a turbine hot chamber. This integrated collaborative project, between two research groups at Clemson University and a team of engineers and scientists at GE Gas Power, focused on design, fabrication and evaluation of a new graded environmental barrier coating. Using the excellent compositional tailorability of polymer derived ceramics (PDCs), we developed an integrated EBC/BC that smoothly transitions from bottom SiC/SiC bond interface to hermetic sesquioxide (Y 2 O 3 ) top surface. This smooth compositional transition avoided the sharp CTE mismatch at interfaces to greatly reduce the thermal stress. The developed EBC is compatible with and bonds well with the bond coat that GE uses. The top hermetic oxide surface ensures low oxygen transportation and volatilization rates under the high velocity steam environment. The graded microstructure with increasing sesquioxide concentration also decreases the amount of Si and C elements near the top hermetic sesquioxide layer. Coatings made using a process suitable for manufacturing – atmospheric plasma spraying was demonstrated. The microstructure of coatings made using this process were fully characterized. Finally, the performance of these coatings was investigated under the most demanding conditions for this application. Specifically, high temperature, high velocity steam exposure; thermal shock test; and thermal cycling tests. The graded coatings performed exceptionally well in all these tests. Specific suggestions for future development in this area have also been identified. In addition to the excellent technical progress, this project helped initiate a robust collaboration between the research groups at Clemson and GE Gas Power. It also provided a high-quality learning and mentoring opportunity for the three post-doctoral research associates and two UG students at Clemson University who worked on this project. All proposed tasks, sub-tasks were completed, and all milestones achieved.

03 NATURAL GAS↗

NASA NTRS1993

Ceramic fiber reinforced glass-ceramic matrix composite

A slurry of BSAS glass powders is cast into tapes which are cut to predetermined sizes. Mats of continuous chemical vapor deposition (CVD)-SiC fibers are alternately stacked with these matrix tapes. This tape-mat stack is warm-pressed to produce a 'green' composite which is heated to burn out organic constituents. The remaining interim material is then hot-pressed to form a BSAS glass-ceramic fiber-reinforced composite.

Bansal, Narottam P.↗

NASA NTRS1998

Probabilistic Modeling of Ceramic Matrix Composite Strength

Uncertainties associated with the primitive random variables such as manufacturing process (processing temperature, fiber volume ratio, void volume ratio), constituent properties (fiber, matrix and interface), and geometric parameters (ply thickness, interphase thickness) have been simulated to quantify the scatter in the first matrix cracking strength (FMCS) and the ultimate tensile strength of SCS-6/RBSN (SiC fiber (SCS-6) reinforced reaction-bonded silicon nitride composite) ceramic matrix composite laminate at room temperature. Cumulative probability distribution function for the FMCS and ultimate tensile strength at room temperature (RT) of (0)(sub 8), (0(sub 2)/90(sub 2), and (+/-45(sub 2))(sub S) laminates have been simulated and the sensitivity of primitive variables to the respective strengths have been quantified. Computationally predicted scatter of the strengths for a uniaxial laminate have been compared with those from limited experimental data. Also the experimental procedure used in the tests has been described briefly. Results show a very good agreement between the computational simulation and the experimental data. Dominating failure modes in (0)(sub 8), (0/90)(sub s) and (+/-45)(sub S) laminates have been identified. Results indicate that the first matrix cracking strength for the (0)(sub S), and (0/90)(sub S) laminates is sensitive to the thermal properties, modulus and strengths of both the fiber and matrix whereas the ultimate tensile strength is sensitive to the fiber strength and the fiber volume ratio. In the case of a (+/-45)(sub S), laminate, both the FMCS and the ultimate tensile strengths have a small scatter range and are sensitive to the fiber tensile strength as well as the fiber volume ratio.

Shan, Ashwin R.↗

NASA NTRS1999

Novel Approach for Positioning Sensor Lead Wires on SiC-Based Monolithic Ceramic and FRCMC Components/Subcomponents Having Flat and Curved Surfaces

A novel attachment approach for positioning sensor lead wires on silicon carbide-based monolithic ceramic and fiber reinforced ceramic matrix composite (FRCMC) components has been developed. This approach is based on an affordable, robust ceramic joining technology, named ARCJoinT, which was developed for the joining of silicon carbide-based ceramic and fiber reinforced composites. The ARCJoinT technique has previously been shown to produce joints with tailorable thickness and good high temperature strength. In this study, silicon carbide-based ceramic and FRCMC attachments of different shapes and sizes were joined onto silicon carbide fiber reinforced silicon carbide matrix (SiC/ SiC) composites having flat and curved surfaces. Based on results obtained in previous joining studies. the joined attachments should maintain their mechanical strength and integrity at temperatures up to 1350 C in air. Therefore they can be used to position and secure sensor lead wires on SiC/SiC components that are being tested in programs that are focused on developing FRCMCs for a number of demanding high temperature applications in aerospace and ground-based systems. This approach, which is suitable for installing attachments on large and complex shaped monolithic ceramic and composite components, should enhance the durability of minimally intrusive high temperature sensor systems. The technology could also be used to reinstall attachments on ceramic components that were damaged in service.

Kiser, J. Douglas↗

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 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 NTRS2005

SiC/SiC Ceramic Matrix Composites Developed for High-Temperature Space Transportation Applications

Researchers at the NASA Glenn Research Center have been developing durable, high-temperature ceramic matrix composites (CMCs) with silicon carbide (SiC) matrices and SiC or carbon fibers for use in advanced reusable launch vehicle propulsion and airframe applications in the Next Generation Launch Technology (NGLT) Program. These CMCs weigh less and are more durable than competing metallic alloys, and they are tougher than silicon-based monolithic ceramics. Because of their high specific strength and durability at high temperatures, CMCs such as C/SiC (carbon- fiber-reinforced silicon carbide) and SiC/SiC (silicon-carbide-fiber-reinforced silicon carbide) may increase vehicle performance and safety significantly and reduce the cost of transporting payloads to orbit.

Kiser, J. Douglas↗

DOE OSTI2023

Silicon carbide fiber manufacturing: Cost and technology

Significant advances have been made in the past decade concerning silicon carbide fiber manufacturing methods resulting in near-stoichiometric small-diameter fibers that meet the property requirements for most of the ceramic matrix composites (CMC) and nuclear applications. The manufacturing cost, however, remained prohibitively high, preventing the use of it in different applications requiring much lower cost. Silicon carbide (SiC) fiber reinforced CMC is dominated by the cost of SiC fiber which comprises more than 50 % of the finished part cost. Here, this article provides insight into the SiC fiber manufacturing costs and highlights the need for an alternative SiC fiber precursor and manufacturing method. Analysis of the existing polycarbosilane (PCS)-based SiC fiber manufacturing shows that the crosslinking (curing) and raw material preparation steps are high-cost steps that need lower cost options. Alternative SiC fiber precursor should be sought for lowering the cost of SiC fibers.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Fracture Mechanisms For SiC Fibers And SiC/SiC Composites Under Stress-Rupture Conditions at High Temperatures

The successful application of SiC/SiC ceramic matrix composites as high-temperature structural materials depends strongly on maximizing the fracture or rupture life of the load-bearing fiber and matrix constituents. Using high-temperature data measured under stress-rupture test conditions, this study examines in a mechanistic manner the effects of various intrinsic and extrinsic factors on the creep and fracture behavior of a variety of SiC fiber types. It is shown that although some fiber types fracture during a large primary creep stage, the fiber creep rate just prior to fracture plays a key role in determining fiber rupture time (Monkman-Grant theory). If it is assumed that SiC matrices rupture in a similar manner as fibers with the same microstructures, one can develop simple mechanistic models to analyze and optimize the stress-rupture behavior of SiC/SiC composites for applied stresses that are initially below matrix cracking.

DiCarlo, James A.↗

NASA NTRS1985

Preparation of silicon carbide-silicon nitride fibers by the pyrolysis of polycarbosilazane precursors

The development of silicon carbide-silicon nitride fibers (SiC-Si3N4) by the pyrolysis of polycarbosilazane precursors is reviewed. Precursor resin, which was prepared by heating tris(N-methylamino)methylsilane or tris(N-methylamino)phenylsilane to about 520 C, was drawn into fibers from the melt and then made unmeltable by humidity conditioning at 100 C and 95 percent relative humidity. The humidity treated precursor fibers were pyrolyzed to ceramic fibers with good mechanical properties and electrical resistivity. For example, SiC-Si3N4 fibers derived from tris(N-methylamino)methylsilane had a tensile rupture modulus of 29 million psi and electrical resistivity of 6.9 x ten to the 8th power omega-cm, which is ten to the twelfth power times greater than that obtained for graphite fibers.

Penn, B. G.↗

NASA NTRS1986

Preparation of silicon carbide-silicon nitride fibers by the pyrolysis of polycarbosilazane precursors - A review

Penn, B. G.↗

NASA NTRS2002

Tensile Behavior of As-Fabricated and Burner-Rig Exposed SiC/SiC Composites with Hi-Nicalon Type-S Fibers

Tensile stress-strain curves were measured at room temperature and 1315 C for 2D-woven SiC/BN/SiC ceramic matrix composites (CMC) reinforced by two variations of Hi-Nicalon Type-S SiC fibers. These fibers, which contained a thin continuous carbon-rich layer on their as-produced surface, provided the as-fabricated CMC with good composite behavior and an ultimate strength and strain of -350 MPa and -0.5%, respectively. However, after un-stressed burner-rig exposure at 815 C for -100 hrs, CMC tensile specimens with cut edges and exposed interphases showed a significant decrease in ultimate properties with effectively no composite behavior. Microstructural observations show that the degradation was caused by internal fiber-fiber oxide bonding after removal of the carbon-rich fiber surface layer by the high-velocity combustion gases. On the other hand, SiC/BN/SiC CMC with Sylramic-iBN fibers without carbon-rich surfaces showed higher as-fabricated strength and no loss in strength after the same burner rig exposure. Based on the strong role of the carbon layer in these observations, a process method was developed and demonstrated for achieving better strength retention of Hi-Nicalon Type-S CMC during burner rig exposure. Other general approaches for minimizing this current deficiency with as-produced Type-S fibers are discussed.

Yun, H. M.↗