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At least 163 records · Page 9

Final Report

This cooperative agreement explored the novel polymerization of vinylsilane, alone and in combination with other alkenylsilanes, alkylsilanes, and/or crosslinking agents, using dimethyltitanocene as homogeneous catalyst. The reactions were found to be initiated photochemically under mild conditions, and no hydrogen gas was evolved when alkenylsilanes were polymerized. The polymers were found to have predominately a carbosilane-type backbone containing -SiH2-CH2-CH2-Si and -SiH2-CH(CH3)-Si type linkages. The mechanism of polymerization was found to be step-growth. Despite the relatively low molecular weight of the polymer (M(sub n) - 500 and M(sub W) - 1500), pyrolysis resulted in conversion to C-rich SiC ceramic in high char yields (-60%). Copolymerization with methylsilane resulted in higher chars and more crystalline polymer. Addition of crosslinking agents such as polybutadiene or methyltrivinylsilane increased the viscosity of the polymer produced and enabled application as coatings to fiber toes.

Source record↗

Mechanical Behavior of Notched SiC/SiC Composites

Gas turbine components such as combustor liners or turbine vanes are subject to regions of high stress-concentration, e.g., attachment to the frame or at cooling holes. Ceramic matrix composites (CMCs) are potential materials for high temperature applications in gas turbines. They offer some capability to relieve stress at regions of high stress-concentration via matrix damage accumulation. In this study notch sensitivity was examined for woven SiC fiber reinforced, melt-infiltrated SiC matrix composites with a BN interphase, utilizing either Hi-Nicalo(TM) fibers or the stiffer Sylramic fibers. The double-edge notched tensile test approach was used for a wide range of notch sizes and specimen widths. Both composite systems exhibited mild notch sensitivity similar to other CMC systems. Acoustic emission, detected during the tensile tests, indicated that matrix cracking occurred around notches at net-section stresses below the stress where matrix cracking first occurs in unnotched specimens. However, thermoelastic stress analysis did not show any measurable stress relief around notches after the specimens were preloaded.

Morscher, Gregory N.↗

Thermal response and ablation characteristics of light weight ceramic ablators

An account is given of the thermal performance and ablation characteristics of the NASA-Ames Lightweight Ceramic Ablators (LCAs) in supersonic, high-enthalpy convective environments, which use low density ceramic or carbon fiber matrices as substrates for main structural support, with organic resin fillers. LCA densities are in the 0.224-1.282 g/cu cm range. In-depth temperature data have been obtained to determine thermal penetration depths and conductivity. The addition of SiC and PPMA is noted to significantly improve the ablation performance of LCAs with silica substrates. Carbon-based LCAs are the most mass-efficient at high flux levels.

Tran, Huy K.↗

Ceramic Composite Experimental Testing Status

Over recent years, ceramic matrix materials such as SiC–SiC and C–C have been gaining interest for use in fusion reactors, light water reactors (LWRs), and high-temperature reactors (HTRs). These materials are good candidates to operate in very high temperature and moderate to high radiation environments. The evaluation of composite materials, in general, is challenging because of variations in precursor materials, variations in the fabrication process across fabricators, and the wide range of potential fiber architectures, to name a few. However, the need to evaluate neutron-irradiated properties adds another layer of complexity, which includes cost, timeline, and specimen size limitations (often associated with irradiation testing). A qualification methodology for the use of ceramic composites is provided in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code Section III-5-HHB. The methodology is supported by ASTM International (ASTM) guides, which provide a pathway to accomplish this effort. Part of the qualification strategy is for the designer to collect material property data on environmental conditions representative of its design envelope. These data include irradiation effects. This report presents an experimental study and test campaign developed to partially address this gap by providing initial mechanical and physical property data required for design. A variety of different materials using different manufacturing techniques are considered as part of this campaign. The test plan suggests performing a screening or partial irradiation study to assist the designer during the material selection process. The designer can then perform a more comprehensive qualification study if the material performance is promising. This work focuses on the status of the specimen preparations (machining of samples), the current test methods and failure analysis as well as the preparation of irradiation vehicles for the irradiation campaign. The irradiation will be performed at Oak Ridge National Laboratory (ORNL) in the High Flux Isotope Reactor (HFIR) and at Idaho National Laboratory (INL) in the Advanced Test Reactor (ATR).

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Factors Controlling Elevated Temperature Strength Degradation of Silicon Carbide Composites

For 5 years, the cooperative agreement NCC3-763 has focused on the development and understanding of Sic-based composites. Most of the work was performed in the area of SiC fiber-reinforced composites for UEET and NGLT and in collaboration with Goodrich Corporation under a partially reimbursable Space Act Agreement. A smaller amount of work was performed on C fiber-reinforced SiC matrix composites for NGLT. Major accomplishments during this agreement included: Improvements to the interphase used in melt-infiltrated (MI) SiC/SiC composites which increases the life under stressed-oxidation at intermediate temperatures referred to as "outside-debonding". This concept is currently in the patent process and received a Space Act Award. Mechanistic-based models of intermediate temperature degradation for MI SiC/SiC Quantification and relatively robust relationships for matrix crack evolution under stress in SiC/SiC composites which serve as the basis for stress-strain and elevated temperature life models The furthering of acoustic emission as a useful tool in composite damage evolution and the extension of the technique to other composite systems Development of hybrid C-SiC fiber-reinforced SiC matrix composites Numerous presentations at conferences, industry partners, and government centers and publications in recognized proceedings and journals. Other recognition of the author's accomplishments by NASA with a TGIR award (2004), NASA's Medal for Public Service (2004), and The American Ceramic Society s Richard M. Fulrath Award (2005). The following will briefly describe the work of the past five years in the three areas of interest: SiC/SiC composite development, mechanistic understanding and modeling of SiC/SiC composites, and environmental durability of C/SiC composites. More detail can be found in the publications cited at the end of this report.

Source record↗

Scatter in Carbon/Silicon Carbide (C/SiC) Composites Quantified

Carbon-fiber-reinforced silicon carbide matrix (C/SiC) composites processed by chemical vapor infiltration are candidate materials for aerospace thermal structures. Carbon fibers can retain properties at very high temperatures, but they are known to have poor oxidation resistance in adverse, high-temperature environments. Nevertheless, the combination of CVI-SiC matrix with higher stiffness and oxidation resistance, the interfacial coating, and additional surface-seal coating provides the necessary protection to the carbon fibers, and makes the material viable for high-temperature space applications operating under harsh environments. Furthermore, C/SiC composites, like other ceramic matrix composites (CMCs), exhibit graceful non-catastrophic failure because of various inherent energy dissipating mechanisms. The material exhibits nonlinearity in deformation even at very low stress levels. This is the result of the severe matrix microcracking present in the as processed composite because of large differences between the coefficients of thermal expansion of the fiber and the matrix. Utilization of these advanced composites in next generation space vehicles will require innovative structural configurations, updated materials, and refined analyses. Structural safety issues for these vehicles are in direct competition with performance and cost. One would have to quantify the uncertainties associated with the design using formal probabilistic methods. Specifically four fundamental aspects on which analyses are based-- (1) loading conditions, (2) material behavior, (3) geometrical configurations, and (4) structural connections between the composite components and baseline structure--are stochastic in nature. A direct way to formally account for uncertainties is to develop probabilistic structural analysis methods where all participating variables are described by appropriate probability density functions. The present work, however, focuses on analyzing the stochastic material behavior of these advanced composites using formal probabilistic analysis methods. Often, some of the desirable property characteristics that allow composites to offer advantages over conventional structural materials (like tailoring of composite properties) and the complexity are in fact responsible for their greater statistical variability and the requirements for more characterization tests. Composite properties are anisotropic as well, having different properties in different directions. This means that characterization of a property such as stiffness--which will vary greatly depending on the orientation of the fiber relative to the direction of the testing--must be repeated for several different directions and loading conditions. The fabrication process for composites also introduces statistical variations in properties and geometry. A composite part is produced in a number of steps, each of which introduces statistical variability. The matrix is usually produced from a combination of raw materials; and the fiber, which has its own set of properties, is often coated or surface treated, introducing yet another source of variability.

Murthy, Pappu L. N.↗

Ceramic reinforced zirconium alloy nuclear fuel cladding with intermediate oxidation resistant layer

The invention relates to compositions and methods for coating a zirconium alloy (e.g., ceramic-containing) cladding tube for use with fuel rods in a nuclear water reactor. The coating includes an intermediate oxidation resistant layer and a SiC containing layer at least partially deposited on the intermediate oxidation resistant layer. The SiC containing layer can include a plurality of fibers. The SiC containing layer may also be on the outer surface of end plugs. The invention provides improved capability for the zirconium alloy cladding to withstand normal and accident conditions in the nuclear water reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ceramic Matrix Composite (CMC) Materials Characterization

Under the former NASA EPM Program, much initial progress was made in identifying constituent materials and processes for SiC/SiC ceramic composite hot-section components. This presentation discusses the performance benefits of these approaches and elaborates on further constituent and property improvements made under NASA UEET. These include specific treatments at NASA that significantly improve the creep and environmental resistance of the Sylramic(TM) SiC fiber as well as the thermal conductivity and creep resistance of the CVI Sic matrix. Also discussed are recent findings concerning the beneficial effects of certain 2D-fabric architectures and carbon between the BN interphase coating and Sic matrix.

Calomino, Anthony↗

Ceramic Matrix Composite (CMC) Materials Development

Under the former NASA EPM Program, much initial progress was made in identifying constituent materials and processes for SiC/SiC ceramic composite hot-section components. This presentation discusses the performance benefits of these approaches and elaborates on further constituent and property improvements made under NASA UEET. These include specific treatments at NASA that significantly improve the creep and environmental resistance of the Sylramic(TM) Sic fiber as well as the thermal conductivity and creep resistance of the CVI Sic matrix. Also discussed are recent findings concerning the beneficial effects of certain 2D-fabric architectures and carbon between the BN interphase coating and Sic matrix.

DiCarlo, James↗

Multiscale Modeling of Ceramic Matrix Composites

Results of multiscale modeling simulations of the nonlinear response of SiC/SiC ceramic matrix composites are reported, wherein the microstructure of the ceramic matrix is captured. This micro scale architecture, which contains free Si material as well as the SiC ceramic, is responsible for residual stresses that play an important role in the subsequent thermo-mechanical behavior of the SiC/SiC composite. Using the novel Multiscale Generalized Method of Cells recursive micromechanics theory, the microstructure of the matrix, as well as the microstructure of the composite (fiber and matrix) can be captured.

ceramic matrix composites↗

Spatially Resolved Raman Spectroscopy of Thin Carbon Interphase in SiC Ceramic Matrix Composites

A dedicated analysis method is presented to extract the Raman spectrum of an interphase layer thinner than the laser spot size. We focused on spatial correlations between the contrast of optical micrographs and Raman hyperspectral data to predict the constituents of the mixed spectra measured near the interphase. By employing a mapping step size of 0.1 μm, the Raman spectrum of approximately 0.3-μm-thick carbon interphase in a SiC fiber-reinforced SiC matrix composite was extracted from data acquired with a theoretical spot size of about 0.7 μm. Notably, conventional chemometrics procedures were unable to isolate the interphase signal, instead producing a spectrum representing a mixture of interphase and matrix. This study used another composite with approximately 0.9-μm-thick interphase to validate the analysis method, enabling direct measurement of the interphase spectrum. The proposed Raman analysis method has advantages in specimen volume and turnaround time compared to traditional characterization methods, such as transmission electron microscopy. In conclusion, this study also evaluates the applicability of the analysis method to different composite materials and identifies key requirements of the measurements, including the ratio of interphase thickness to spot size and the homogeneity of the surrounding matrix.

ceramic matrix composite↗

Facility for continuous CVD coating of ceramic fibers

An inductively heated CVD furnace of pilot-plant scale, whose hot zone is 150 mm in diameter x 300 mm in length, has been adapted for continuous coating of ceramic yarns. Coatings at very low pressures are possible in this facility due to the fact that the entire apparatus, including yarn feeding and collecting equipment, is under vacuum. SiC yarn has been coated with 0.1-0.2 microns of BN at yarn speeds of 60 cm/min; a 500-m spool; was coated in about 14 hrs. Coating capacity was tripled by adding pulleys to allow three yarn passes through the furnace.

Moore, Arthur W.↗

Chemical Stability of the Fiber Coating/Matrix Interface in Silicon-Based Ceramic Matrix Composites

Carbon and boron nitride are used as fiber coatings in silicon-based composites. In order to assess the long-term stability of these materials, reactions of carbon/Si3N4 and BN/SiC were studied at high temperatures with Knudsen effusion, coupon tests, and microstructural examination. In the carbon/Si3N4 system, carbon reacted with Si3N4 to form gaseous N2 and SiC. The formation of SiC limited further reaction by physically separating the carbon and Si3N4. Consequently, the development of high p(N2) at the interface, predicted from thermochemical calculations, did not occur, thus limiting the potential deleterious effects of the reaction on the composite. Strong indications of a reaction between BN and SiC were shown by TEM and SIMS analysis of the BN/SiC interface. In long-term exposures, this reaction can lead to a depletion of a BN coating and/or an unfavorable change of the interfacial properties, limiting the beneficial effects of the coating.

Lee, Kang N.↗

Characterization of Ceramic Matrix Composite Vane Subelements Subjected to Rig Testing in a Gas Turbine Environment

Vane subelements were fabricated from a silicon carbide fiber-reinforced silicon carbide matrix (SiC/SiC) composite. A cross-sectional slice of an aircraft engine metal vane was the basis of the vane subelement geometry. To fabricate the small radius of the vane's trailing edge using stiff Sylramic SiC fibers, a unique SiC fiber architecture was developed. A test configuration for the vanes in a high pressure gas turbine environment was designed and fabricated. Testing was conducted using a pressure of 6 atm and combustion flow rate of 0.5 kg/sec, and consisted of fifty hours of steady state operation followed by 102 2-minute thermal cycles. A surface temperature of 1320 C was obtained for the EBC-coated SiC/SiC vane subelement. This paper will briefly discuss the vane fabrication, test configuration, and results of the vane testing. The emphasis of the paper is on characterization of the post-test condition of the vanes.

Verrilli, Michael↗

High Temperature Solid Particle Erosion in a Melt-Infiltrated SiC/SiC Ceramic Matrix Composite

Ceramic matrix composites (CMCs) are an enabling propulsion material system that offer weight benefits over current Ni-based superalloys, and have higher temperature capabilities that can reduce cooling requirements. Incorporating CMCs into the hot section of gas-turbine engines therefore leads to an increase in engine efficiency. While significant advancements have been made, challenges still remain for current and next-generation gas-turbines; particularly when operating in dust-laden or erosive environments. Solid particles entrained in the gas flow can impact engine hardware resulting in localized damage and material removal due to repeated, cumulative impacts. In this study, the erosion behavior of a melt-infiltrated (MI) silicon carbide fiber-reinforced silicon carbide (SiC/SiC) CMC is investigated at high temperature (1,200 °C) in a simulated combustion environment using 150 µm alumina particles as erodent. Particle impact velocities ranged from 100 to 200 m/s and the angle of impingement varied from 30° to 90°. Erosion testing was also performed on α-SiC to elucidate similarities and differences in the erosion response of the composite compared to that of a monolithic ceramic. Scanning electron microscopy (SEM) was used to study the post-erosion damage morphology and the governing mechanisms of material removal.

Ceramic matrix composites (CMCs), solid particle e↗

Thermal and mechanical behavior of metal matrix and ceramic matrix composites

The present conference discusses local stresses in metal-matrix composites (MMCs) subjected to thermal and mechanical loads, the computational simulation of high-temperature MMCs' cyclic behavior, an analysis of a ceramic-matrix composite (CMC) flexure specimen, and a plasticity analysis of fibrous composite laminates under thermomechanical loads. Also discussed are a comparison of methods for determining the fiber-matrix interface frictional stresses of CMCs, the monotonic and cyclic behavior of an SiC/calcium aluminosilicate CMC, the mechanical and thermal properties of an SiC particle-reinforced Al alloy MMC, the temperature-dependent tensile and shear response of a graphite-reinforced 6061 Al-alloy MMC, the fiber/matrix interface bonding strength of MMCs, and fatigue crack growth in an Al2O3 short fiber-reinforced Al-2Mg matrix MMC.

Kennedy, John M.↗

High spatial resolution thermal conductivity mapping of SiC/SiC composites

Herein, silicon carbide (SiC) ceramic matrix composites are being investigated as a new generation of fuel cladding materials due to its higher accident tolerance compared to Zircaloy. Characterization of the thermal conductivity of SiC constituents and their interfaces and interphases in SiC/SiC composites is needed as inputs to models of cladding performance. We used time-domain thermoreflectance (TDTR) to map the thermal conductivity with a spatial resolution of 2 µm. The SiC/SiC composite is comprised of Hi-Nicalon Type S fibers in a matrix made by chemical vapor infiltration (CVI matrix). The interphase material is a pyrolytic carbon/SiC multilayer. We report thermal conductivity maps of the SiC fiber and SiC matrix at temperatures of 25 °C, 90 °C, 164 °C, and 250 °C. The fiber has a uniform and isotropic thermal conductivity of 22 W m -1 K -1 at 25 °C; the thermal conductivity of fiber is approximately independent of temperature. The matrix thermal conductivity is not uniform and varies from 50 to 120 W m -1 K -1 at 25 °C; the thermal conductivity of the matrix scales approximately with the inverse of the square root of temperature, i.e., ∝ 1/T 1/2 . The thermal conductivity of the interphase at room temperature is 6 W m -1 K -1 . The calculated spatially averaged thermal conductivity of this SiC/SiC composite at 1000°C is 29 W m -1 K -1 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Synthesis and Characterization of Silicon Carbide Ceramic Composites with CeO 2 Powder

This study pioneers the fabrication and characterization of silicon carbide (SiC) containing cerium dioxide (CeO 2 ). CeO 2 powder was tested as a surrogate for actinide oxide waste forms such as uranium dioxide (UO 2 ) and plutonium dioxide (PuO 2 ). Several syntheses were evaluated with varying amounts of preceramic polymer (SMP-10 resin) and CeO 2 containing either SiC fiber, carbon fiber, or no fibers. Scanning electron microscopy (SEM) was used to characterize morphology and compositional differences, and energy-dispersive x-ray spectroscopy (EDS) was used to provide semiquantitative elemental analysis. In addition, each sample was characterized by density, powder x-ray diffraction (pXRD), and Raman spectroscopy. Samples containing nearly more than four times CeO 2 powder than SMP-10 resin by mass had the best properties. This research establishes a unique synthesis for SiC containing high concentrations of CeO 2 powder to illustrate how it may be managed as a potential waste form.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗