The Carborundum Company

Kennecott Corporation

The Standard Oil Company

Stemcor Corporation

Carl H McMurtry

John A Coppola

Sai-Kwing Lau

Wolfgang D Boecker

Stephen Chwastiak

Laurence N Hailey

Robert G Naum

Gajawalli V Srinivasan

Martin R Kasprzyk

Francis J Frechette

Yorihiro Murata

Dean P Owens

Michael T Hortman

Paul F Forsyth

Jonathan J Kim

Joel D Katz

Tadeusz M Korzekwa

Viswanathan Venkateswaran

Sa-Kwing Lau

Harry A Lawler

Lawrence N Hailey

The invention includes a process for producing a reaction bonded silicon carbide composite reinforced with coated silicon carbide fibers which is suitable for high temperature applications. The process includes the steps of coating SiC fibers with AlN, BN or TiB.sub.2 ; treating the coated fibers with a mixture of SiC powder, water and a surfactant; preparing a slurry comprising SiC powder and water; infiltrating the coated fibers with the slurry to form a cast; drying the cast to form a green body; and reaction bonding the green body to form a dense SiC fiber reinforced reaction bonded matrix composite. The invention further includes a SiC fiber reinforced SiC composite comprising a reaction bonded SiC matrix, a SiC fiber reinforcement possessing thermal stability at high temperatures and an interface coating on the fibers having chemical and mechanical compatibility with the SiC matrix and with the SiC fibers.

Silicon carbide reinforced reaction bonded silicon carbide composite

Process for manufacturing a silicon carbide composition

The invention provides a silicon carbide fiber carrying an aluminum nitride coating between about 1 and about 15 micrometers thick. The AlN coating serves as a debond layer which improves the fracture toughness of composite materials in which the coated fiber is a reinforcement phase.

Aluminum nitride-coated silicon carbide fiber

The invention provides silicon carbide fiber-reinforced, reaction-bonded silicon carbide composites suitable for high temperature applications in which the silicon carbide fiber is coated with AlN, BN or TiB.sub.2. The composites offer superior fracture toughness which is ascribed to fiber pullout. The invention also includes a process for making the composites.

A process for the manufacture of high purity, ultra-fine aluminum nitride powder by the carbo-nitridization of alumina. Agglomerates uniform in both size, chemical composition and porosity are formed containing a stoichiometric mixture of alumina and carbon with the addition of a small amount of catalyst. The agglomerates are furnaced in a controlled manner in a well-mixed reaction vessel to achieve a uniform and consistent level of conversion. Milling of the as-reacted agglomerates under a controlled atmosphere will produce high purity, micron sized aluminum nitride powder.

Process for the continuous production of high purity, ultra-fine,

A high temperature, preferably polycrystalline, ceramic fiber having a selectable diameter of between 1 and 200 microns. The fiber is stable in an inert atmosphere at a temperature above about 1700.degree. C. and is often stable even in air at a temperature above 1500.degree. C. The fiber comprises a sintered ceramic powder having a maximum particle size less than the diameter of the fiber and an average particle size less than 0.2 times the diameter of the fiber. The ceramic powder is also stable in an inert atmosphere at a temperature above about 1700.degree. C. At least 90% of the ceramic is selected from borides, nitrides, carbides, and silicides. The fiber is characterized by a smooth surface and is preferably out of round. The invention further comprises a textilable sinterable filament, comprising a flexible polymer matrix containing high temperature sinterable ceramic powder particles. The ceramic powder particles are selected from ceramic borides, nitrides, carbides, and silicides. The diameter of the filament is from 2 to 300 microns. The invention also comprises the method for making textilable filament by fiberizing a mixture of a polymer and a sinterable non-oxide fiber and the method wherein the high temperature ceramic fiber is prepared by sintering the textilable sinterable filament as previously described. The invention also includes composites containing such filaments.

Non-oxide sintered ceramic fibers

Sintered silicon carbide body having a D.C. electrical resistivity of at least 10.sup.8 Ohm cm at 25.degree. C., a density of at least 2.95 g/cm.sup.3 is formed upon sintering in a nitrogenous atmosphere at a temperature of about 2250.degree. C. or greater, a shaped body composed essentially of carbon or carbon source material in amount sufficient to provide up to 2.5 percent uncombined carbon; from about 0.4 to about 2.0 percent boron carbide; up to 25 percent of temporary binder and a balance of silicon carbide which is predominantly alpha-phase. The shaped body may additionally include other sintering aids such as BN or Al without destruction of desired high electrical resistivity.

Sintered silicon carbide ceramic body of high electrical resistivity

A method for reducing the particle size of an initial silicon carbide powder to a milled powder having an average particle size of below 1 micron but greater than an average of about 0.2 micron, without grinding media contamination. The method comprises milling the larger particles in a vibratory mill in the presence of sintered silicon carbide media comprising silicon carbide pellets having both curved and flat surfaces and a maximum dimension of from about 0.5 to 5 centimeters. The grinding occurs in the presence of a fluid, preferably a liquid, for a sufficient time and at a sufficient vibrational energy to obtain said milled powder having such smaller average particle size. At least 90% of the pellets in the silicon carbide media have a specific gravity (density) greater than 3.05 g/cm.sup.3. The invention includes the unique media, which may be used for various grinding operations, and includes unique milled powders. One of the unique powders has particles which have an average length to width ratio of greater than 2.5. Another of the unique powders is black silicon carbide containing from 200 to 2,000 parts per million of aluminum in solid solution.

Vibratory grinding of silicon carbide

Pressureless sintered silicon carbide ceramic bodies, having an equiaxed microstructure and an alpha crystalline habit can be produced by firing shaped bodies, containing finely divided silicon carbide, boron source such as boron carbide, carbon source such as phenolic resin and a temporary binder, at a sintering temperature of from about 1900.degree. C. to about 2250.degree. C., depending on the sintering atmosphere, under conditions such that a coating of carbon source is maintained on the finely divided silicon carbide, and sufficient boron is maintained within the shaped body during firing. Boron can be maintained within the shaped body by various techniques, such as the use of a 'seasoned boat' or graphite container for the body being sintered, which has been saturated with boron by exposure to boron at or about the temperature of sintering. There is also disclosed a process for producing a sintered silicon carbide ceramic body, with or without the equiaxed crystal microstructure, from silicon carbide powders of alpha or beta crystal structure, or amorphous noncrystalline silicon carbide, or mixtures thereof.

Sintered alpha silicon carbide ceramic body having equiaxed

A composite, neutron absorbing, coated article, normally flat and thin and of comparatively light weight, suitable for installation in storage racks for spent nuclear fuel and for other neutron absorbing applications, includes a backing member, preferably of flexible material such as woven fiberglass cloth, a synthetic organic polymeric coating or a plurality of such coatings on the backing member, preferably of cured phenolic resin, such as phenol formaldehyde or trimethylolphenol formaldehyde and boron carbide particles held to the backing member by the cured coating or a plurality of such coatings. Also described is a method for the manufacture of the neutron absorbing coated article and the use of such an article. In a preferred method the backing member is first coated on both sides thereof with a filling coating of thermosettable liquid phenolic resin, which is then partially cured to solid state, one side of the backing member is then coated with a mixture of thermosettable liquid resin and finely divided boron carbide particles and the resin is partially cured to solid state, the other side is coated with a similar mixture, larger boron carbide particles are applied to it and the resin is partially cured to solid state, such side of the article is coated with thermosettable liquid phenolic resin, the resin is partially cured to solid state and such resin, including previously applied partially cured resins, is cured to final cross-linked and permanently set form.

Method for manufacture of neutron absorbing article

Pressureless sintering of silicon carbide to produce ceramic bodies having 75% and greater theoretical densities, can be accomplished by firing shaped bodies, containing finely divided silicon carbide, boron source such as boron carbide, carbon source such as phenolic resin and a temporary binder, at a sintering temperature of from about 1900.degree. C. to about 2500.degree. C.

Sintered silicon carbide ceramic body

A neutron absorbing article, preferably in long, thin, flat form, suitable for but not necessarily limited to use in storage racks for spent nuclear fuel at locations between volumes of such stored fuel to absorb neutrons from said spent fuel and prevent uncontrolled nuclear reaction of the spent fuel material, is composed of finely divided boron carbide particles and a solid, irreversibly cured phenolic polymer forming a continuous matrix about the boron carbide particles, in such proportions that at least 6% of B.sup.10 from the boron carbide content is present therein. The described structures possess a multiplicity of desirable properties for the use mentioned, including withstanding thermal cycling from repeated spent fuel insertions and removals, withstanding radiation from said spent nuclear fuel over long periods of time without losing desirable neutron absorbing and physical properties, being sufficiently chemically inert to water so as to retain neutron absorbing properties if brought into contact with it, not being galvanically corroding and being sufficiently flexible so as to withstand operational basis earthquake and safe shutdown earthquake seismic events without loss of neutron absorbing capability and other desirable properties when installed in storage racks for spent nuclear fuel. In preferred embodiments of the invention the phenolic polymer is a phenol formaldehyde type polymer, such as a trimethylol phenol formaldehyde type polymer, the boron carbide contains at least 12% of B.sup.10, the plate contains from 8.0 to 11.5% thereof, the plate density is 1.6 to 2.1 g./cc. and the proportions of boron carbide (which may be accompanied by limited amounts of certain impurities) and phenol formaldehyde type polymer (preferably free of halogens, mercury, lead and sulfur) are from 20 to 35% of the former and 65 to 80% of the latter. The invention also relates to a plurality of such neutron absorbing articles in a storage rack for spent nuclear fuel and to a method for the manufacture of the articles. In the manufacturing method a portion of the phenol formaldehyde type resin, in liquid state, is mixed with the boron carbide particles, compacted and cured, after which the cured article is impregnated with additional phenol formaldehyde type resin, which is then cured to make the final product.

Method for manufacturing neutron absorbing article

A neutron absorbing article, preferably in long, thin, flat form, suitable for but not necessarily limited to use in storage racks for spent nuclear fuel at locations between volumes of such stored fuel, to absorb neutrons from said spent fuel and prevent uncontrolled nuclear reaction of the spent fuel material, is composed of finely divided boron carbide particles and a solid, irreversibly cured phenolic polymer, forming a continuous matrix about the boron carbide particles, in such proportions that at least 6% of B.sup.10 from the boron carbide content is present therein. The described articles withstand thermal cycling from repeated spent fuel insertions and removals, withstand radiation from said spent nuclear fuel over long periods of time without losing desirable neutron absorbing and physical properties, are sufficiently chemically inert to water so as to retain neutron absorbing properties if brought into contact with it, are not galvanically corrodible and are sufficiently flexible so as to withstand operational basis earthquake and safe shutdown earthquake seismic events, without loss of neutron absorbing capability and other desirable properties, when installed in storage racks for spent nuclear fuel. The disclosure also relates to a plurality of such neutron absorbing articles in a storage rack for spent nuclear fuel and to a method for the manufacture of the articles.

Growing community of inventors

Youngstown, NY, United States of America

Carl H McMurtry