Ford Motor Company Limited

John A Mangels

Ray A Dickie

John Richard Baer

Gerald J Tennenhouse

The method disclosed in this specification is one of reducing the green density of an article cast in a slip casting operation. The article is cast from a casting slip containing silicon metal particles, yttrium containing particles, and a small amount of a fluoride salt which is effective to suppress flocculation of the silicon metal particles by y.sup.+3 ions derived from the yttrium containing particles. The method is characterized by the following step. A small amount of compound which produces a cation which will partly flocculate the particles of silicon metal is added to the casting slip. The small amount of this compound is added so that when the casting slip is slip cast into a casting mold, the partly flocculated particles of silicon will interrupt an otherwise orderly packing of the particles of silicon and particles of yttrium. In this manner, the green density of the slip cast article is reduced and the article may be more easily nitrided.

Method of reducing the green density of a slip cast article

The method concerns forming a relatively stable slip of silicon metal particles and yttrium containing particles. In one embodiment, a casting slip of silicon metal particles is formed in water. Particles of a yttrium containing sintering aid are added to the casting slip. The yttrium containing sintering aid is a compound which has at least some solubility in water to form Y.sup.+3 ions which have a high potential for totally flocculating the silicon metal particles into a semiporous solid. A small amount of a fluoride salt is added to the casting slip which contains the yttrium containing sintering aid. The fluoride salt is one which will produce fluoride anions when dissolved in water. The small amount of the fluoride anions produced are effective to suppress the flocculation of the silicon metal particles by the Y.sup.+3 ions so that all particles remain in suspension in the casting slip and the casting slip has both an increased shelf life and can be used to cast articles having a relatively thick cross-section. The pH of the casting slip is maintained in a range from 7.5 to 9. Preferably, the fluoride salt used is one which is based on a monovalent cation such as sodium or ammonia. The steps of adding the yttrium containing sintering aid and the fluoride salt may be interchanged if desired, and the salt may be added to a solution containing the sintering aid prior to addition of the silicon metal particles.

Method of forming a relatively stable slip of silicon metal particles

A thermally stable, oxidation resistant ceramic Si.sub.3 N.sub.4 material is disclosed. The material has a substantially pure primary phase formed of substantially pure silicon nitride. A substantially pure secondary phase of the material is formed of a material selected from the group consisting essentially of Si.sub.3 N.sub.4 /SiO.sub.2 /4Y.sub.2 O.sub.3, Si.sub.3 N.sub.4 /SiO.sub.2 /2Y.sub.2 O.sub.3 and Si.sub.3 N.sub.4 /4SiO.sub.2 /5Y.sub.2 O.sub.3. The primary phase may be in the form of individual grains and the secondary phase may be in the form of grain boundaries between the individual grains.

Thermally stable silicon nitride material

A method is disclosed in this specification for forming a densified silicon nitride article. The method is initiated by forming a reaction bonded article of moderate density. This moderate density reaction bonded article has a primary phase of substantially pure grains of silicon nitride surrounded by a secondary grain boundary phase. The secondary grain boundary phase contains silicon nitride, silicon dioxide and a densification aid incorporated in the reaction bonded article of moderate density. The compounds forming the secondary grain boundary phase are present either in their pure forms or interacted with one another. The reaction bonded article is packed in a packing powder which contains portions of the pure compounds found in or interacted with one another to define the secondary grain boundary phase. The reaction bonded article of moderate density is heated in the packing powder to a temperature and for a time whereby interaction of the secondary grain boundary phase and the packing powder may take place. The interaction takes place so that a new grain boundary phase can be developed about the substantially pure grains of silicon nitride. The new grain boundary phase developed is a unitary phase of a selected composition.

Method of forming a densified silicon nitride article

A method of densifying an article formed of reaction bonded silicon nitride is disclosed. The reaction bonded silicon nitride article is packed in a packing mixture consisting of silicon nitride powder and a densification aid. The reaction bonded silicon nitride article and packing powder are sujected to a positive, low pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause any open porosity originally found in the reaction bonded silicon nitride article to be substantially closed. Thereafter, the reaction bonded silicon nitride article and packing powder are subjected to a positive high pressure nitrogen gas treatment while being heated to a treatment temperature and for a treatment time to cause a sintering of the reaction bonded silicon nitride article whereby the strength of the reaction bonded silicon nitride article is increased.

Method of densifying an article formed of reaction bonded silicon nitride

A method of densifying a reaction bonded silicon nitride article is disclosed. In accordance with the broadest principles disclosed, a densification aid is incorporated into a reaction bonded silicon nitride article. The so-made reaction bonded silicon nitride article is enclosed in a chamber which also contains a mixture of silicon nitride powder and powder the same as the densification aid incorporated into the reaction bonded silicon nitride article. The reaction bonded silicon nitride article, and the powder mixture associated therewith, is subjected to a nitrogen gas pressure sufficient to prohibit a significant volatilization of silicon nitride at a sintering temperature. The reaction bonded silicon nitride article, the powder mixture and nitrogen gas associated therewith are heated to a temperature above 1700.degree. C. for a time sufficient to permit sintering of that article whereby the strength of the reaction bonded silicon nitride article is increased. In accordance with preferred teachings, the densification aid can be selected from the group of materials consisting of magnesium oxide, yttrium oxide, cerium oxide and zirconium oxide.

Method of densifying a reaction bonded silicon nitride article

A method of manufacturing silicon nitride particles, either in an aglomerated or unaglomerated form, is disclosed. Basically, the particles to be nitrided are placed in an enclosed furnace and heated to a suitable temperature at which the enclosed furnace is filled with an initial gaseous mixture of nitrogen and hydrogen, the mixture containing not more than about 6% by volume hydrogen. Thereafter, the material is heated in the enclosed furnace to a temperature of about 900.degree. C. to about 1000.degree. C. at which time the nitrogen starts to react with the silicon in the furnace. Thereafter, the enclosed furnace is demand filled with a nitriding gas mixture consisting essentially of 1 to 10% by volume helium and about 99 to 90% by volume nitrogen. The furnace is heated to a suitable nitriding temperature and the demand filling of the chamber with the nitriding gas helium/nitrogen combination is continued until the nitriding operation is terminated. The enclosed furnace is then cooled to room temperature and the nitrided silicon material recovered. The use of helium in the nitriding gas obtained all of the benefits one obtains when nitriding gas is a combination of hydrogen and nitrogen, but does not produce an explosive mixture.

Method of nitriding silicon

A method of increasing the oxidation resistance of silicon nitride is disclosed. A furnace is preheated to a temperature in the range of 2500.degree.F to 2750.degree.F. The silicon nitride body to be treated is inserted into the preheated furnace. The silicon nitride article is maintained in the furance for a period of time sufficient to develop an oxidation resistant surface on the article. The period of time is generally in the range from one-half hour to five hours.

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Flat Rock, MI, United States of America

John A Mangels