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NASA NTRS1996

Development of a material property database on selected ceramic matrix composite materials

Ceramic Matrix Composites, with fiber/whisker/particulate reinforcement, possess the attractive properties of ceramics such as high melting temperature, high strength and stiffness at high temperature, low density, excellent environmental resistance, combined with improved toughness and mechanical reliability. These unique properties have made these composites an enabling technology for thermomechanically demanding applications in high temperature, high stress and aggressive environments. On a broader scale, CMC's are anticipated to be applicable in aircraft propulsion, space propulsion, power and structures, in addition to ground based applications. However, it is also true that for any serious commitment of the material toward any of the intended critical thermo-mechanical applications to materialize, vigorous research has to be conducted for a thorough understanding of the mechanical and thermal behavior of CMC's. The high technology of CMC'S is far from being mature. In view of this growing need for CMC data, researchers all over the world have found themselves drawn into the characterization of CMC's such as C/SiC, SiC/SiC, SiC/Al203, SiC/Glass, SiC/C, SiC/Blackglas. A significant amount of data has been generated by the industries, national laboratories and educational institutions in the United States of America. NASA/Marshall Space Flight Center intends to collect the 'pedigreed' CMC data and store those in a CMC database within MAPTIS (Materials and Processes Technical Information System). The task of compilation of the CMC database is a monumental one and requires efforts in various directions. The project started in the form of a summer faculty fellowship in 1994 and has spilled into the months that followed and into the summer faculty fellowship of 1995 and has the prospect of continuing into the future for a healthy growth, which of course depends to a large extent on how fast CMC data are generated. The 10-week long summer fellowship has concentrated, basically, on establishing the procedure for a smooth transfer of data into a CMC database on MAPTIS which is a vital part of the following broader picture of the project.

Mahanta, Kamala↗

NASA NTRS1995

Microstructural Characterization of Reaction-Formed Silicon Carbide Ceramics

Microstructural characterization of two reaction-formed silicon carbide ceramics has been carried out by interference layering, plasma etching, and microscopy. These specimens contained free silicon and niobium disilicide as minor phases with silicon carbide as the major phase. In conventionally prepared samples, the niobium disilicide cannot be distinguished from silicon in optical micrographs. After interference layering, all phases are clearly distinguishable. Back scattered electron (BSE) imaging and energy dispersive spectrometry (EDS) confirmed the results obtained by interference layering. Plasma etching with CF4 plus 4% O2 selectively attacks silicon in these specimens. It is demonstrated that interference layering and plasma etching are very useful techniques in the phase identification and microstructural characterization of multiphase ceramic materials.

Singh, M.↗

NASA NTRS1996

Durability Testing of Commercial Ceramic Materials

Technical efforts by AlliedSignal Engines in DOE/NASA-funded project from February, 1978 through December, 1995 are reported in the fields ceramic materials for gas turbine engines and cyclic thermal durability testing. A total of 29 materials were evaluated in 40 cyclic oxidation exposure durability tests. Ceramic test bars were cyclically thermally exposed to a hot combustion environment at temperatures up to 1371 C (2500 F) for periods of up to 3500 hours, simulating conditions typically encountered by hot flowpath components in an automotive gas turbine engine. Before and after exposure, quarter-point flexure strength tests were performed on the specimens, and fractography examinations including scanning electron microscopy (SEM) were performed to determine failure origins.

Schienle, J. L.↗

NASA NTRS1997

Estimation of Slow Crack Growth Parameters for Constant Stress-Rate Test Data of Advanced Ceramics and Glass by the Individual Data and Arithmetic Mean Methods

The two estimation methods, individual data and arithmetic mean methods, were used to determine the slow crack growth (SCG) parameters (n and D) of advanced ceramics and glass from a large number of room- and elevated-temperature constant stress-rate ('dynamic fatigue') test data. For ceramic materials with Weibull modulus greater than 10, the difference in the SCG parameters between the two estimation methods was negligible; whereas, for glass specimens exhibiting Weibull modulus of about 3, the difference was amplified, resulting in a maximum difference of 16 and 13 %, respectively, in n and D. Of the two SCG parameters, the parameter n was more sensitive to the estimation method than the other. The coefficient of variation in n was found to be somewhat greater in the individual data method than in the arithmetic mean method.

Choi, Sung R.↗

NASA NTRS1997

Chemical Vapor Deposited SiC (SCS-0) Fiber-Reinforced Strontium Aluminosilicate Glass-Ceramic Composites

Unidirectional SrO Al2O3 2SiO2 glass-ceramic matrix composites reinforced with uncoated Chemical Vapor Deposited (CVD) SiC (SCS-0) fibers have been fabricated by hot-pressing under appropriate conditions using the glass-ceramic approach. Almost fully dense composites having a fiber volume fraction of 0.24 have been obtained. Monoclinic celsian, SrAl2Si2O8, was the only crystalline phase observed in the matrix by x-ray diffraction. No chemical reaction was observed between the fiber and the matrix after high temperature processing. In three-point flexure, the composite exhibited a first matrix cracking stress of approx. 231 +/- 20 MPa and an ultimate strength of 265 +/- 17 MPa. Examination of fracture surfaces revealed limited short length fiber pull-out. From fiber push-out, the fiber/matrix interfacial debonding and frictional strengths were evaluated to be approx. 17.5 +/- 2.7 MPa and 11.3 +/- 1.6 MPa, respectively. Some fibers were strongly bonded to the matrix and could not be pushed out. The micromechanical models were not useful in predicting values of the first matrix cracking stress as well as the ultimate strength of the composites.

Bansal, Narottam P.↗

NASA NTRS1997

Accelerated Testing Methodology for the Determination of Slow Crack Growth of Advanced Ceramics

Constant stress-rate (dynamic fatigue) testing has been used for several decades to characterize slow crack growth behavior of glass and ceramics at both ambient and elevated temperatures. The advantage of constant stress-rate testing over other methods lies in its simplicity: Strengths are measured in a routine manner at four or more stress rates by applying a constant crosshead speed or constant loading rate. The slow crack growth parameters (n and A) required for design can be estimated from a relationship between strength and stress rate. With the proper use of preloading in constant stress-rate testing, an appreciable saving of test time can be achieved. If a preload corresponding to 50 % of the strength is applied to the specimen prior to testing, 50 % of the test time can be saved as long as the strength remains unchanged regardless of the applied preload. In fact, it has been a common, empirical practice in strength testing of ceramics or optical fibers to apply some preloading (less then 40%). The purpose of this work is to study the effect of preloading on the strength to lay a theoretical foundation on such an empirical practice. For this purpose, analytical and numerical solutions of strength as a function of preloading were developed. To verify the solution, constant stress-rate testing using glass and alumina at room temperature and alumina silicon nitride, and silicon carbide at elevated temperatures was conducted in a range of preloadings from O to 90 %.

Choi, Sung R.↗

NASA NTRS1997

Creep Life Prediction of Ceramic Components Using the Finite Element Based Integrated Design Program (CARES/Creep)

The desirable properties of ceramics at high temperatures have generated interest in their use for structural applications such as in advanced turbine systems. Design lives for such systems can exceed 10,000 hours. Such long life requirements necessitate subjecting the components to relatively low stresses. The combination of high temperatures and low stresses typically places failure for monolithic ceramics in the creep regime. The objective of this work is to present a design methodology for predicting the lifetimes of structural components subjected to multiaxial creep loading. This methodology utilizes commercially available finite element packages and takes into account the time varying creep stress distributions (stress relaxation). In this methodology, the creep life of a component is divided into short time steps, during which, the stress and strain distributions are assumed constant. The damage, D, is calculated for each time step based on a modified Monkman-Grant creep rupture criterion. For components subjected to predominantly tensile loading, failure is assumed to occur when the normalized accumulated damage at any point in the component is greater than or equal to unity.

Jadaan, Osama M.↗

NASA NTRS1997

CARES/Life Software for Designing More Reliable Ceramic Parts

Products made from advanced ceramics show great promise for revolutionizing aerospace and terrestrial propulsion, and power generation. However, ceramic components are difficult to design because brittle materials in general have widely varying strength values. The CAPES/Life software eases this task by providing a tool to optimize the design and manufacture of brittle material components using probabilistic reliability analysis techniques. Probabilistic component design involves predicting the probability of failure for a thermomechanically loaded component from specimen rupture data. Typically, these experiments are performed using many simple geometry flexural or tensile test specimens. A static, dynamic, or cyclic load is applied to each specimen until fracture. Statistical strength and SCG (fatigue) parameters are then determined from these data. Using these parameters and the results obtained from a finite element analysis, the time-dependent reliability for a complex component geometry and loading is then predicted. Appropriate design changes are made until an acceptable probability of failure has been reached.

Nemeth, Noel N.↗

NASA NTRS1997

Evaluation of Thermal Control Coatings for Flexible Ceramic Thermal Protection Systems

This report summarizes the evaluation and testing of high emissivity protective coatings applied to flexible insulations for the Reusable Launch Vehicle technology program. Ceramic coatings were evaluated for their thermal properties, durability, and potential for reuse. One of the major goals was to determine the mechanism by which these coated blanket surfaces become brittle and try to modify the coatings to reduce or eliminate embrittlement. Coatings were prepared from colloidal silica with a small percentage of either SiC or SiB6 as the emissivity agent. These coatings are referred to as gray C-9 and protective ceramic coating (PCC), respectively. The colloidal solutions were either brushed or sprayed onto advanced flexible reusable surface insulation blankets. The blankets were instrumented with thermocouples and exposed to reentry heating conditions in the Ames Aeroheating Arc Jet Facility. Post-test samples were then characterized through impact testing, emissivity measurements, chemical analysis, and observation of changes in surface morphology. The results show that both coatings performed well in arc jet tests with backface temperatures slightly lower for the PCC coating than with gray C-9. Impact testing showed that the least extensive surface destruction was experienced on blankets with lower areal density coatings.

Kourtides, Demetrius↗

NASA NTRS1996

High Temperature Mechanical Behavior of Ceramic Matrix Composites

The research accomplishments under this grant were very extensive in the areas of the high temperature behavior of ceramics, ceramic composites and testing standards for these materials. Rather than try to summarize all this research I have enclosed research papers and reports which were completed with the funding provided by the grant.

Hemann, John↗

NASA NTRS1998

Crack Branching and Fracture Mirror Data of Glasses and Advanced Ceramics

The fracture mirror and crack branching constants were determined from three glasses and nine advanced ceramics tested under various loading and specimen configurations in an attempt to use the constants as a data base for fractography. The ratios of fracture mirror or crack branching constant to fracture toughness were found to be approximately two for most ceramic materials tested. A demonstration of how to use the two constants as a tool for verifying stress measurements was presented for silicon nitride disk specimens subjected to high-temperature, constant stress-rate biaxial flexure testing.

Choi, Sung R.↗

NASA NTRS1998

Properties of PZT-Based Piezoelectric Ceramics Between -150 and 250 C

The properties of three PZT-based piezoelectric ceramics and one PLZT electrostrictive ceramic were measured as a function of temperature. In this work, the dielectric, ferroelectric polarization versus electric field, and piezoelectric properties of PZT-4, PZT-5A, PZT-5H, and PLZT-9/65/35 were measured over a temperature range of -150 to 250 C. In addition to these measurements, the relative thermal expansion of each composition was measured from 25 to 600 C and the modulus of rupture of each material was measured at room temperature. This report describes the experimental results and compares and contrasts the properties of these materials with respect to their applicability to intelligent aerospace systems.

Hooker, Matthew W.↗

NASA NTRS1999

Temperature Measurement of a Miniature Ceramic Heater in the Presence of an Extended Interfering Background Radiation Source Using a Multiwavelength Pyrometer

Temperature measurement of small (millimeter size) objects is generally difficult and demanding. Measurement involving ceramic materials using the traditional one- and two-color pyrometer is difficult because of their complex optical properties, such as low emissivity which may vary with both temperature and wavelength. Pyrometry applications in an environment with an interfering radiation source of extended dimension adds extra complexity to the process. We show that the multiwavelength pyrometer successfully measured the temperatures of a millimeter (mm) size ceramic heater under these demanding conditions.

Ng, Daniel↗

NASA NTRS1999

Elevated-Temperature "Ultra" Fast Fracture Strength of Advanced Ceramics: An Approach to Elevated-Temperature "Inert" Strength

The determination of "ultra" fast fracture strengths of five silicon nitride ceramics at elevated temperatures has been made by using constant stress-rate ("dynamic fatigue") testing with a series of "ultra" fast test rates. The test material included four monolithic and one SiC whisker-reinforced composite silicon nitrides. Of the five test materials, four silicon nitrides exhibited the elevated -temperature strengths that approaches their respective room-temperature strengths at an "ultra" fast test rate of 3.3 x 10(exp 4) MPa/s. This implies that slow cracks growth responsible for elevated-temperature failure can be eliminated or minimized by using the "ultra" fast test rate. These ongoing experimental results have shed light on laying a theoretical and practical foundation on the concept and definition of elevated-temperature "inert" strength behavior of advanced ceramics.

Choi, S. R.↗

NASA NTRS1999

Critical Needs for Robust and Reliable Database for Design and Manufacturing of Ceramic Matrix Composites

Ceramic matrix composite (CMC) components are being designed, fabricated, and tested for a number of high temperature, high performance applications in aerospace and ground based systems. The critical need for and the role of reliable and robust databases for the design and manufacturing of ceramic matrix composites are presented. A number of issues related to engineering design, manufacturing technologies, joining, and attachment technologies, are also discussed. Examples of various ongoing activities in the area of composite databases. designing to codes and standards, and design for manufacturing are given.

Singh, M.↗

NASA NTRS1988

High-Temperature Properties of Ceramic Fibers and Insulations for Thermal Protection of Atmospheric Entry and Hypersonic Cruise Vehicles

Multilayer insulations which will operate in the 500C to 1000C temperature range are being considered for possible applications on aerospace vehicles subject to convective and radiative heating during atmospheric entry. The insulations described in this paper consist of ceramic fabrics, insulations, and metal foils quilted together using ceramic thread. As these types of insulations have highly anisotropic properties, the total heat transfer characteristics of these insulations must be determined. Data are presented on the thermal diffusivity and thermal conductivity of four types of multilayer insulations and are compared to the baseline Advanced Flexible Reusable Surface Insulation

Kourtides, Demetrius A.↗

NASA NTRS1999

Key Durability Issues with Mullite-Based Environmental Barrier Coatings for Si-Based Ceramics

Plasma-sprayed mullite (3Al2O3 central dot 2SiO2) and mullite/yttria-stabilized-zirconia (YSZ) dual layer coatings have been developed to protect silicon-based ceramics from environmental attack. Mullite-based coating systems show excellent durability in air. However, in combustion environments, corrosive species such as molten salt or water vapor penetrate through cracks in the coating and attack the Si-based ceramics along the interface, Thus modification of the coating system for enhanced crack-resistance is necessary for long-term durability in combustion environments. Other key durability issues include interfacial contamination and coating/substrate bonding. Interfacial contamination leads to enhanced oxidation and interfacial pore formation, while weak coating/substrate bonding leads to rapid attack of the interface by corrosive species, both of which can cause premature failure of the coating. Interfacial contamination can be minimized by limiting impurities in coating and substrate materials. The interface may be modified to improve the coating/substrate bond.

Lee, Kang N.↗

NASA NTRS1998

Factors Affecting Fiber Design and Selection for Advanced Ceramic Composites

Structural Ceramic Matrix Composites (CMC) have the potential for application in the hot sections of a variety of advanced propulsion and power systems. It is therefore necessary to have a general understanding of the key properties of CMC and Reinforcing Fibers. This need is complicated by the wide variety of application conditions and structural requirements for which CMC's will be used, and the proprietary concerns of the design engineers. CMC's, to be successful, must display properties which are competitive with the currently used high temperature structural materials: (i.e., Iron and Nickel based superalloys, tough monolithic ceramics, and carbon/carbon composites.) Structural CMC offers several areas of competition: (1) performance, (i.e., strength and strength retention, creep resistance, and thermal conductivity), (2) reliability (i.e., environmental durability, and damage tolerance) and (3) processing (i.e., capability for varying sizes and shapes, and cost effective fabrication). The presentation further discusses, and illustrates with fiber and CMC data the key fiber properties and processes which strongly affect each CMC area of competition. The presentation further discusses the current knowledge of the important factors which control the key fiber properties. A design guidelines for the optimum fiber characteristics is developed, and the currently available fibers are compared against those guidelines.

DiCarlo, James A.↗