Development of a High Strength, High Modulus Ceramic Fiber Final Summary Report, 29 Jun. 1967 - 29 Sep. 1968
Salt decomposition process for production of high strength ceramic continuous fiber
Fetterolf, R. N.↗
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High Strength Ceramic Fibers and Methods of Fabrication
A method and apparatus for forming a plurality of fibers from (e.g., CVD) precursors, including a reactor adapted to grow a plurality of individual fibers; and a plurality of independently controllable lasers, each laser of the plurality of lasers growing a respective fiber. A high performance fiber (HPF) structure, including a plurality of fibers arranged in the structure; a matrix disposed between the fibers; wherein a multilayer coating is provided along the surfaces of at least some of the fibers with an inner layer region having a sheet-like strength; and an outer layer region, having a particle-like strength, such that any cracks propagating toward the outer layer from the matrix propagate along the outer layer and back into the matrix, thereby preventing the cracks from approaching the fibers. A method of forming an interphase in a ceramic matrix composite material having a plurality of SiC fibers, which maximizes toughness by minimizing fiber to fiber bridging, including arranging a plurality of SiC fibers into a preform; selectively removing (e.g., etching) silicon out of the surface of the fibers resulting in a porous carbon layer on the fibers; and replacing the porous carbon layer with an interphase layer (e.g., Boron Nitride), which coats the fibers to thereby minimize fiber to fiber bridging in the preform.
Pegna, Joseph↗
Hybrid aerogel rigid ceramic fiber insulation and method of producing same
A hybrid insulation material comprises of porous ceramic substrate material impregnated with nanoporous material and method of making the same is the topic of this invention. The porous substrate material has bulk density ranging from 6 to 20 lb/ft.sup.3 and is composed of about 60 to 80 wt % silica (SiO.sub.2) 20 to 40 wt % alumina (Al.sub.2 O.sub.3) fibers, and with about 0.1 to 1.0 wt % boron-containing constituent as the sintering agent. The nanoporous material has density ranging from 1.0 to 10 lb/ft.sup.3 and is either fully or partially impregnated into the substrate to block the pores, resulting in substantial reduction in conduction via radiation and convention. The nanoporous material used to impregnate the fiber substrate is preferably formed from a precursor of alkoxysilane, alcohol, water, and an acid or base catalyst for silica aerogels, and from a precursor of aluminum alkoxide, alcohol, water, and an acid or base catalyst for alumina aerogels.
Barney, Andrea O.↗
Sensor Lead Wires Positioned on SiC-based Monolithic Ceramic and Fiber- reinforced Ceramic Matrix Composite Subcomponents with Flat and Curved Surfaces
There is strong interest in the development of silicon carbide-based monolithic ceramic and composite materials and components for demanding, high-temperature applications. Thorough characterization of material properties, including high-temperature testing under simulated or actual operating conditions, is a high priority for programs involved in developing these silicon carbide- (SiC) based materials and components. Members of the Sensors and Electronics Technology Branch at the NASA Lewis Research Center are developing minimally intrusive methods of measuring the properties (such as the surface temperature, strain, and heat flux characteristics) of components and subelements that are being tested or operated in hostile, high-temperature environments. Their primary goal is to instrument the test article or operating component with durable sensors that have a minimal effect on test conditions such as the gas flow across the surface of the item and the material response (including the through-thickness conduction of heat). Therefore, the main thrust of their work has been the development of thin-film sensors (e.g., thermocouples or strain gauges) for use on various advanced material test articles, including SiC/SiC composite components. There was a need for a better method of securing sensor lead wires on SiC-based components and subelements that would be tested at temperatures to 1000 C (or higher), to enhance the durability of the overall minimally intrusive sensor system. To address this need, Lewis researchers devised an alternative approach for positioning the sensor lead wires (which are connected to the thin-film sensors) on SiC or SiC/SiC components. A reaction-forming method of joining was used to strongly bond hoop-shaped monolithic SiC and SiC/SiC composite attachments of various sizes to both flat and curved surfaces of SiC/SiC composite subelements (see the photos). This approach is based on an affordable, robust ceramic joining technology, named ARCJoinT, which was developed at Lewis for the joining of SiC-based ceramics and fiber-reinforced composites.
Kiser, James D.↗
Continuous fiber ceramic matrix composites for heat engine components
High strength at elevated temperatures, low density, resistance to wear, and abundance of nonstrategic raw materials make structural ceramics attractive for advanced heat engine applications. Unfortunately, ceramics have a low fracture toughness and fail catastrophically because of overload, impact, and contact stresses. Ceramic matrix composites provide the means to achieve improved fracture toughness while retaining desirable characteristics, such as high strength and low density. Materials scientists and engineers are trying to develop the ideal fibers and matrices to achieve the optimum ceramic matrix composite properties. A need exists for the development of failure models for the design of ceramic matrix composite heat engine components. Phenomenological failure models are currently the most frequently used in industry, but they are deterministic and do not adequately describe ceramic matrix composite behavior. Semi-empirical models were proposed, which relate the failure of notched composite laminates to the stress a characteristic distance away from the notch. Shear lag models describe composite failure modes at the micromechanics level. The enhanced matrix cracking stress occurs at the same applied stress level predicted by the two models of steady state cracking. Finally, statistical models take into consideration the distribution in composite failure strength. The intent is to develop these models into computer algorithms for the failure analysis of ceramic matrix composites under monotonically increasing loads. The algorithms will be included in a postprocessor to general purpose finite element programs.
Tripp, David E.↗
Rapid Prototyping of Continuous Fiber Reinforced Ceramic Matrix Composites
For ceramics to be used as structural components in high temperature applications, their fracture toughness is improved by embedding continuous ceramic fibers. Ceramic matrix composite (CMC) materials allow increasing the overall operating temperature, raising the temperature safety margins, avoiding the need for cooling, and improving the damping capacity, while reducing the weight at the same time. They also need to be reliable and available in large quantities as well. In this paper, an innovative rapid prototyping technique to fabricate continuous fiber reinforced ceramic matrix composites is described. The process is simple, robust and will be widely applicable to a number of high temperature material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The results of mechanical properties and microstructural characterization are presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts at an order of magnitude lower cost than current CVI and PIP processes.
Vaidyanathan, R.↗
Rapid Prototyping of Continuous Fiber Reinforced Ceramic Matrix Composites
For ceramics to be used as structural components in high temperature applications, their fracture toughness is improved by embedding continuous ceramic fibers. Ceramic matrix composite (CMC) materials allow increasing the overall operating temperature, raising the temperature safety margins, avoiding the need for cooling, and improving the damping capacity, while reducing the weight at the same time. They also need to be reliable and available in large quantities as well. In this paper, an innovative rapid prototyping technique to fabricate continuous fiber reinforced ceramic matrix composites is described. The process is simple, robust and will be widely applicable to a number of high temperature material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The results of mechanical properties and microstructural characterization are presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts at an order of magnitude lower cost than current chemical vapor infiltration (CVI) and polymer impregnation and pyrolysis (PIP) processes.
Vaidyanathan, R.↗
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.↗
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.↗
Oxygen Diffusion and Reaction Kinetics in Continuous Fiber Ceramic Matrix Composites
Previous stressed oxidation tests of C/SiC composites at elevated temperatures (350 C to 1500 C) and sustained stresses (69 MPa and 172 MPa) have led to the development of a finite difference cracked matrix model. The times to failure in the samples suggest oxidation occurred in two kinetic regimes defined by the rate controlling mechanisms (i.e. diffusion controlled and reaction controlled kinetics). Microstructural analysis revealed preferential oxidation along as-fabricated, matrix microcracks and also suggested two regimes of oxidation kinetics dependent on the oxidation temperature. Based on experimental results, observation, and theory, a finite difference model was developed. The model simulates the diffusion of oxygen into a matrix crack bridged by carbon fibers. The model facilitates the study of the relative importance of temperature, the reaction rate constant, and the diffusion coefficient on the overall oxidation kinetics.
Halbig, Michael C.↗
Anisotropic thermal conductivity under compression in two-dimensional woven ceramic fibers for flexible thermal protection systems
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Rodrigo Penide-Fernandez↗
Fundamental studies on the nature and properties of ceramic fiber insulation
Silica and mullite fibers used to fabricate reusable surface insulation (RSI) for the space shuttle orbiter may devitrify/recrystallize within the temperature range anticipated upon reentry. This is shown to be dependent upon impurity level, temperature, and time at temperature. It is determined that the effects of the material improvement and optimization program are positive. The degree of crystallinity is shown to have a predominant effect upon the strength of fabricated RSI tile, and limits are determined. Models are developed to predict tensile strengths and shrinkage rates of silica tile based upon readily measurable parameters. Thermal cycling which simulates reentry results in an increase in the crystallinity and in the porosity of tile coatings.
Mueller, J. I.↗
Early development of ceramic fiber insulation for the Space Shuttle
The evolution of reusable surface insulation is described, with attention to the mullite and other aluminosilicates, zirconia, and silicon carbide-coated carbon compositions experimented with in the late 1960s and early 1970s. Evaluation and development concentrated in this period on such aspects of design and material properties as cold soak performance, attachment, shock impingement, surface coating cracks, and tile gap design and heating. In addressing the central problem of heat-shield thermal conductivity, it was found that for a given density, silica fibers had a lower conductivity than those of mullite. This was due to the one-micron, as opposed to 4.7-micron, diameter of the silica fibers, which resulted in smaller pores and therefore less convective and radiative heat transfer. Attention is also given to tile coating materials and the high-temperature processes by which they were applied.
Buckley, J. D.↗
Optimization of interface layers in the design of ceramic fiber reinforced metal matrix composites
The potential of using an interface layer to reduce thermal stresses in the matrix of composites with a mismatch in coefficients of thermal expansion (CTE) of fiber and matrix was investigated. It was found that the performance of the layer can be defined by the product of the CTE and the thickness, and that a compensating layer with a sufficiently high CTE can reduce the thermal stresses in the matrix significantly. A practical procedure offering a window of candidate layer materials is proposed.
Doghri, I.↗
Tensile strain measurements of ceramic fibers using scanning laser acoustic microscopy
A noncontacting technique using scanning laser acoustic microscopy for making in situ tensile strain measurements of small diameter fibers was implemented for the tensile strain analysis of individual Nicalon SiC fibers (nominal diameter 15 microns). Stress versus strain curves for the fibers were plotted from the experimental data. The mean elastic modulus of the fibers was determined to be 185.3 GPa. Similar measurements were made for Carborundum SiC fibers (nominal diameter 28 microns) and Saphikon sapphire fibers (nominal diameter 140 microns), yielding and elastic modulus of 401 and 466.8 GPa, respectively.
Kent, Renee M.↗
Tensile strain measurements of ceramic fibers using scanning laser acoustic microscopy
A noncontacting technique using scanning laser acoustic microscopy for making in situ tensile strain measurements of small diameter fibers was implemented for the tensile strain analysis of individual Nicalon SiC fibers (nominal diameter 15 microns). Stress vs strain curves for the fibers were plotted from the experimental data. The mean elastic modulus of the fibers was determined to be 185.3 GPa. Similar measurements were made for Carborundum SiC fibers (nominal diameter 28 microns) and Saphikon sapphire fibers (nominal diameter 140 microns).
Kent, Renee M.↗
High-Hot-Strength Ceramic Fibers
Continuous fibers consisting of laminae of alumina and yttrium aluminum garnet offer exceptionally high strength, resistance to creep, and chemical stability at high temperatures. These fibers exceed tensile strength of sapphire fibers. Leading candidates for reinforcement of intermetallic-matrix composites in exhaust nozzles of developmental high-speed civil transport aircraft engines. Other applications are in aerospace, automotive, chemical-process, and power-generation industries.
Sayir, Ali↗
Tensile Strength and Microstructural Characterization of Uncoated and Coated HPZ Ceramic Fibers
Tensile strengths of as-received HPZ fiber and those surface coated with BN, BN/SiC, and BN/Si3N4 have been determined at room temperature using a two-parameter Weibull distribution. Nominally approx. 0.4 micron BN and 0.2 micron SiC or Si3N4 coatings were deposited on the fibers by chemical vapor deposition using a continuous reactor. The average tensile strength of uncoated HPZ fiber was 2.0 +/- 0.56 GPa (290 +/- 81 ksi) with a Weibull modulus of 4.1. For the BN coated fibers, the average strength and the Weibull modulus increased to 2.39 +/- 0.44 GPa (346 +/- 64 ksi) and 6.5, respectively. The HPZ/BN/SiC fibers showed an average strength of 2.0 +/- 0.32 GPa (290 +/- 47 ksi) and Weibull modulus of 7.3. Average strength of the fibers having a dual BN/Si3N4 surface coating degraded to 1.15 +/- 0.26 GPa (166 +/- 38 ksi) with a Weibull modulus of 5.3. The chemical composition and thickness of the fiber coatings were determined using scanning Auger analysis. Microstructural analysis of the fibers and the coatings was carried out by scanning electron microscopy and transmission electron microscopy. A microporous silica-rich layer approx. 200 nm thick is present on the as-received HPZ fiber surface. The BN coatings on the fibers are amorphous to partly turbostratic and contaminated with carbon and oxygen. Silicon carbide coating was crystalline whereas the silicon nitride coating was amorphous. The silicon carbide and silicon nitride coatings are non-stoichiometric, non-uniform, and granular. Within a fiber tow, the fibers on the outside had thicker and more granular coatings than those on the inside.
Bansal, Narottam P.↗