Preparation of fibered ceramics by mechanical deformation
Preparation of ceramic fibers by extrusion in metal matrix
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Preparation of ceramic fibers by extrusion in metal matrix
Ceramic fibers formation by particles mechanical deformation by extrusion in W matrix, describing grain structure of various extruded metal oxides
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.
The availability of textile grade ceramic fibers has sparked great interest for applications in composite reinforcement and high temperature insulation. This paper summarizes the properties of various small diameter textile grade ceramic fibers currently available. Room temperature mechanical and electrical properties of the fibers are discussed for three cases: ambient conditions, after heat aging in argon, and after heat aging in wet air. Dow Corning (R) HPZ Ceramic Fiber, a silicon nitride type fiber, is shown to have improved retention of mechanical and electrical properties above 1200 C.
A variety of high performance polycrystalline ceramic fibers are currently being considered as reinforcement for high temperature ceramic matrix composites. However, under mechanical loading above 800 C, these fibers display creep-related instabilities which can result in detrimental changes in composite dimensions, strength, and internal stress distributions. As a first step toward understanding these effects, this study examines the validity of mechanistic-based empirical model which describes primary stage tensile creep and stress relaxation of polycrystalline ceramic fibers as independent functions of time, temperature, and applied stress or strain. To verify these functional dependencies, a simple bend test is used to measure stress relaxation for four types of commercial ceramic fibers for which direct tensile creep data are available. These fibers include both nonoxide (SCS-6, Nicalon) and oxide (PRD-166, FP) compositions. The results of the bend stress relaxation (BSR) test not only confirm the stress, time, and temperature dependencies predicted by the model but also allow measurement of model empirical parameters for the four fiber types. In addition, comparison of model predictions and BSR test results with the literature tensile creep data show good agreement, supporting both the predictive capability of the model and the use of the BSR test as a simple method for parameter determination for other fibers.
A variety of high performance polycrystalline ceramic fibers are currently being considered as reinforcement for high temperature ceramic matrix composites. However, under mechanical loading about 800 C, these fibers display creep related instabilities which can result in detrimental changes in composite dimensions, strength, and internal stress distributions. As a first step toward understanding these effects, this study examines the validity of a mechanism-based empirical model which describes primary stage tensile creep and stress relaxation of polycrystalline ceramic fibers as independent functions of time, temperature, and applied stress or strain. To verify these functional dependencies, a simple bend test is used to measure stress relaxation for four types of commercial ceramic fibers for which direct tensile creep data are available. These fibers include both nonoxide (SCS-6, Nicalon) and oxide (PRD-166, FP) compositions. The results of the Bend Stress Relaxation (BSR) test not only confirm the stress, time, and temperature dependencies predicted by the model, but also allow measurement of model empirical parameters for the four fiber types. In addition, comparison of model tensile creep predictions based on the BSR test results with the literature data show good agreement, supporting both the predictive capability of the model and the use of the BSR text as a simple method for parameter determination for other fibers.
Process for fiberizing ceramic materials with high fusion temperatures and tensile strength
A test program to determine the relative sliding durability of an alumina-silica candidate ceramic fiber for high temperature sliding seal applications as described. This work represents the first reporting of the sliding durability of this material system. Pin-on-disk tests were used to evaluate the potential seal material by sliding a tow or bundle of the candidate ceramic fiber against a superalloy test disk. Friction was measured during the tests and fiber wear, indicated by the extent of fibers broken in the tow or bundle, was measured at the end of each test. Test variables studied included ambient temperatures from 25 C to 900 C, loads from 1.3 to 21.2 Newtons, and sliding velocities from 0.025 to 0.25 m/sec. In addition, the effects of fiber diameter, elastic modulus, and a pretest fiber heat treatment on friction and wear were measured. In most cases, wear increased with temperature. Friction ranged from about 0.36 at 500 C and low velocity (0.025 m/s) to over 1.1 at 900 C and high velocity (0.25 m/s). The pretest fiber heat treatment, which caused significant durability reductions for alumina-boria-silica ceramic fibers tested previously, had little effect on the alumina-silica fibers tested here. These results indicate that the alumina-silica (Al2O3-SiO2) fiber is a good candidate material system for high temperature sliding seal applications.
The mechanical behavior of commercially available and developmental ceramic fibers, both oxide and nonoxide, has been experimentally studied at expected use temperatures. In addition, these properties have been compared to results from the literature. Tensile strengths were measured for three SiC-based and three oxide ceramic fibers for temperatures from 25 C to 1400 C. The SiC-based fibers were stronger but less stiff than the oxide fibers at room temperature and retained more of both strength and stiffness to high temperatures. Extensive creep and creep-rupture experiments have been performed on those fibers from this group which had the best strengths above 1200 C in both single filament tests and tests of fiber bundles. The creep rates for the oxides are on the order of two orders of magnitude faster than the polymer derived nonoxide fibers. The most creep resistant filaments available are single crystal c-axis sapphire filaments. Large diameter CVD fabricated SiC fibers are the most creep and rupture resistant nonoxide polycrystalline fibers tested to date.
Simple bend-stress-relaxation test yields information on creep-related properties of polycrystalline ceramic fibers. Determination of these properties important part of efforts to develop ceramic composite materials that retain mechanical strength and resistance to creep at high temperatures. Present test measures effects of time, temperature, and applied strain on creep-related relaxation of bend stress in ceramic fiber of almost any diameter in almost any environment, without need for contact sensors. Degree of relaxation of bend stress determined from radii of curvature.
A test program to determine the relative sliding durability of an alumina-silica candidate ceramic fiber for high temperature sliding seal applications is described. Pin-on-disk tests were used to evaluate the potential seal material by sliding a tow or bundle of the candidate ceramic fiber against a superalloy test disk. Friction was measured during the tests and fiber wear, indicated by the extent of fibers broken in the tow or bundle, was measured at the end of each test. Test variables studied included ambient temperatures from 25 to 900 C, loads from 1.3 to 21.2 N, and sliding velocities from 0.025 to 0.25 m/sec. In addition, the effects of fiber diameter and elastic modulus on friction and wear were measured. Thin gold films deposited on the superalloy disk surface were evaluated in an effort to reduce friction and wear of the fibers. In most cases, wear increased with test temperature. Friction ranged from 0.36 at 500 C and low velocity (0.025 m/sec) to over 1.1 at 900 C and high velocity (0.25 m/sec). The gold films resulted in satisfactory lubrication of the fibers at 25 C. At elevated temperatures diffusion of substrate elements degraded the films. These results indicate that the alumina-silica (Al2O3-SiO2) fiber is a good candidate material system for high temperature sliding seal applications. More work is needed to reduce friction.
Six types of uncoated ceramic fibers were static tensile and tensile creep tested at various elevated temperatures. Three types of boron nitride coated fibers were also tested. Room temperature static tensile tests were initially performed on all fibers, at gage lengths of 1, 2, and 4 inches, to determine the magnitude of end effects from the gripping system used. Tests at one elevated temperature, at gage lengths of 8 and 10 inches, were also conducted, to determine end effects at elevated temperatures. Fiber cross sectional shapes and areas were determined using scanning electron microscopy. Creep testing was typically performed for 4 hours, in an air atmosphere.
Alumina-silica ceramic-fiber paper for traps and baffles in ultrahigh vacuum systems
Static tensile and tensile creep testing of five ceramic fibers at elevated temperature was performed. J.P. Stevens, Co., Astroquartz 9288 glass fiber, Nippon Carbon, Ltd., (Dow Corning) Nicalon NLM-102 silicon carbide fiber, and 3M Company Nextel 312, 380, and 480 alumina/silica/boria fibers were supplied in unsized tows. Single fibers were separated from the tows and tested in static tension and tensile creep. Elevated test temperatures ranged from 400 to 1300 C and varied for each fiber. Room temperature static tension was also performed. Computer software was written to reduce all single fiber test data into engineering constants using ASTM Standard Test Method D3379-75 as a reference. A high temperature furnace was designed and built to perform the single fiber elevated temperature testing up to 1300 C. A computerized single fiber creep apparatus was designed and constructed to perform four fiber creep tests simultaneously at temperatures up to 1300 C. Computer software was written to acquire and reduce all creep data.
Static tensile and tensile creep testing of five ceramic fibers at elevated temperature was performed. J.P. Stevens, Co., Astroquartz 9288 glass fiber; Nippon Carbon, Ltd., (Dow Corning) nicalon NLM-102 silicon carbide fiber; and 3M Company Nextel 312, 380, and 480 alumina/silica/boria fibers were supplied in unsized tows. Single fibers were separated from the tows and tested in static tension and tensile creep. Elevated test temperatures ranged from 400 C to 1300 C and varied for each fiber. Room temperature static tension was also performed. Computer software was written to reduce all single fiber test data into engineering constants using ASTM Standard Test Method D3379-75 as a reference. A high temperature furnace was designed and built to perform the single fiber elevated temperature testing up to 1300 C. A computerized single fiber creep apparatus was designed and constructed to perform four fiber creep tests simultaneously at temperatures up to 1300 C. Computer software was written to acquire and reduce all creep data.
Refinements of the vertical arc fiberizing apparatus resulted in its ability to fiberize very different refractory glasses having wide ranges of properties. Although the apparatus, was originally designed as a laboratory research tool for the evaluation of many compositions daily, up to one quarter pound of fibers of a single composition could be produced in an 8-hour day. Fibers up to six and a half feet long were produced with the apparatus. Studies were conducted of two methods of fiberizing refractory glasses requiring rapid freezing from the melt. The first method consisted of fiberizing droplets of molten glass passing through an annular nozzle. The second method consisted of reconstructing the annular nozzle in. the shape of a horseshoe to achieve a shorter delay in blasting a molten droplet from the tip of a rod. Both methods were judged feasible for producing fibers of glasses requiring rapid freezing. The first method would be more amenable to volume fiber production. Studies of induction heating for fiber formation did not lead to its designation as a very efficient heating method. Problems. remain to be solved, in the design of a suitable susceptor for a higher heating rate, in protecting the susceptor from oxidation with an inert gas, in contamination of the melt from a refractory crucible, and in the protective radiation shielding of the induction concentrator coil. It is not considered practical to continue studies of this heating method. In the course of this program 151 refractory glass compositions were evaluated for fiber, forming characteristics. Of the various types of materials studied, the following showed promise in producing acceptable refractory fibers: sIlica- spinel (magnesium aluminate), silica- spinel-zirconia, silica-zirconia, silica-zinc spinel, aluminum phosphate glasses, and fluoride glasses. Compositions which did not produce acceptable fibers were high zirconia materials, barium spinels, and calcium aluminates. Improvements in the. testing apparatus for single fiber tensile strength increased the precision. of tests conducted on nine fibers. The highest mean tensile strength, a value of 295,000 pounds per square inch, was obtained with R-141 fibers. Treatment of R-74 fibers with anhydrous Linde A-1100 silane finish improved its mean fiber tensile strength by 25 percent. The lapse of time after fiber formation had no measurable effect on tensile strength. A static heating test conducted with various high melting fibers indicated that Fiberfrax and R-108 underwent no significant changes in bulk volume or resiliency on exposure to 2750 degrees Fahrenheit (1510 degrees Centigrade) in an oxidizing atmosphere. For fiber-resin composition fabrication, ten fiber materials were selected on the bases of high fiber yield, fusion temperature, and type of composition. Fiberfrax, a commercial ceramic fiber, was included for comparison. A new, more effective method of removing pellets from blown fibers was developed. The de-pelletized fibers were treated with a silane finish and felted into ten-inch diameter felts prior to resin impregnation. Composites containing 30 percent by weight of CTL 91-LD phenolic resin were molded under high pressure from the impregnated felts and post-cured to achieve optimum properties. Flexural strength, flexural modules of elasticity, and punch shear strength tests were conducted on the composite specimens. The highest average flexural strength obtained was 19,958 pounds per square inch with the R-74-fiber-resin composite. This compares very favorably with the military specification of 13,000 pounds per square inch flexural strength for randomly oriented fiber reinforced composites. The highest punch shear strength (11,509 pounds per square inch) was obtained with the R-89 fiber-resin composite. The effects of anhydrous fiber finishes on composite strength were not clearly indicated. Plasma arc tests at a heat flux of 550 British Thermal Units per square foot per second on eight composite materials indicated ablation rates generally equivalent to Fiberglas-Micarta No. 259-2. The composite reinforced with R-99 fibers had an average ablation rate of 0.008 inch per second and appears quite promising on the basis of these tests. Preliminary studies for processing fibers into yarn and fabric were conducted with R-99 fibers. The use of certain organic gums aided in 2 fabricating by hand several relatively strong yarns and a crude fabric swatch. This indicated the practicality of developing techniques for processing these fibers into yarn and fabric without significant damage to the fibers.
Research and development of fabrication techniques for chemical vapor deposition (CVD) of ceramic fibers presented in two reports. Fibers of SiC, TiB2, TiC, B4C, and CrB2 intended for use as reinforcements in metal-matrix composite materials. CVD offers important advantages over other processes: fibers purer and stronger and processed at temperatures below melting points of constituent materials.
Soaps made from strong organic base guanidine and organic fatty acids serve as vehicles and binders for coating ceramic fibers, various smooth substrates, and other problematic surfaces with thin precious-metal or metal-oxide films. Films needed to serve as barriers to diffusion in fiber/matrix ceramic composite materials. Guanidine soaps entirely organic and burn off, leaving no residues.