Alcan International Limited

Mukesh K Jain

Sadashiv K Nadkarni

Jean-Paul R Huni

Luc Parent

Lise Castonguay

A process for producing small particles of aluminum nitride suitable for sintering and the particles thus-produced. The process comprises reacting particles of gamma alumina, or a precursor thereof, of less than 1 micron in size with a stoichiometrical excess of finely divided carbon in the presence of nitrogen, or a precursor which provides nitrogen in the reaction conditions, first at a temperature in the range of 1550.degree. to 1700.degree. C. for a period of between 1 and 6 (preferably 1 to 4) hours and then at a temperature in the range of 1750.degree. to 1850.degree. C. for a period of 1 to 4 (preferably 1 to 2) hours, followed by cooling said reaction mixture and reheating to a temperature in the range of 500.degree. to 700.degree. C. in an oxygen-containing atmosphere, and maintaining the temperature until excess unreacted carbon is removed. The alumina or precursor preferably has a particle size of less than 400 nm and the carbon source preferably contains iron as an impurity, and is preferably petroleum coke. The AlN product is particularly suited for use in forming a substrate for electronic components by a process involving sintering of the AlN particles because of the small size (less than 2 microns) and narrow size distribution of the particles.

Process for producing small particles of aluminum nitride and particles

A process for producing fibres composed of or coated with carbides or nitrides. The process involves forming a first reaction zone containing microfine particles of an oxide (or oxide precursor) of silicon or a suitable metal (e.g. boron) uniformly mixed with carbon (or a carbon precursor); forming a second reaction zone comprising a layer having a thickness of 1 cm or less of a porous mass having a density of 1 g/cc or less formed of short or continuous fibres made of or coated with carbon (or carbon precursor); heating the first reaction zone in a non-oxidizing atmosphere to generate a gaseous sub-oxide of the silicon or metal; simultaneously heating the second reaction zone so that the gaseous sub-oxide diffuses into it and reacts with the carbon to form carbide or nitride on the fibres; and separating the resulting fibres from any carbide or nitride whiskers that may have formed in the second rection zone. Short or continuous fibres (e.g. in the form of a fabric or paper-like sheets) consisting of or coated with carbides or nitrides can be formed in this way.

Process for producing fibres composed of or coated with carbides or

A process for producing silicon carbide platelets and the platelets so produced. The process comprises reacting particles of a non-graphitizable form of hard carbon containing 0.5-1.5% by weight of aluminum and at least 0.2% by weight of iron (preferably anthracite coal, most preferably Pennsylvania anthracite), with silica or a silica precursor at a temperature in the range of 1900.degree.-2100.degree. C. under an inert atmosphere. If the carbon contains 0.2-1.0% by weight of iron, 0.1-10% by weight of boron, relative to the weight of SiO.sub.2, is added (if not already present). The carbon is in the form of particles of less than 50.mu. and the silica or precursor is preferably in the form of particles of less than about 1 .mu.. The weight ratio of silica to carbon is greater than 1.67:1. The resulting platelets are substantially unagglomerated and preferably of a size of less than 50.mu. with an aspect ratio greater than 5. The platelets can be used as reinforcements for ceramic and metal matrix materials.

Process for producing silicon carbide platelets and the platelets so

Shaped refractory products, particularly in the form of hollow spheres, and a process for their formation. The process involves dispersing particles of silica or a metal oxide, e.g. Al.sub.2 O.sub.3, in an organic polymer, shaping the dispersion into a desired shape, heating the shaped dispersion in a non-oxidizing atmosphere to carbonize the polymer, and heating the carbonized product at high temperature in a non-oxidizing atmosphere containing nitrogen so that some of the oxide is converted to the corresponding nitride and the particles of unreacted oxide sinter together. The ratio of oxide to carbon should be high so that some but not all of the oxide is converted to the nitride and, preferably, only a relatively small amount should be converted. The resulting refractory material is strong and can be used for a variety of uses, e.g. catalyst supports, packing materials and insulating materials.

Process for producing shaped refractory products

A process for forming silicon nitride containing little or no silicon carbide. The process involves producing a uniform dispersion of finely divided silica particles in a polymer, heating the polymer/silica dispersion in a non-oxidizing atmosphere to carbonize the polymer, and heating the resulting carbonized product to a temperature in the range of 1300.degree.-1800.degree. C. in a non-oxidizing nitrogen-containing atmosphere. This latter heating step is carried out in the presence of a metal oxide (preferably alumina which is capable, in the reaction conditions, of reducing the amount of silicon carbide formed as an undesired by-product.

Process for producing silicon nitride

Porous membranes made of sintered refractory metal oxides, e.g., silica aluimina, titania, zirconia, tungsten oxide, etc., and to a process for their formation. The membranes are formed by dispersing a powder of the metal oxide in an organic polymer. The relative amount of metal oxide to polymer is such that, after the polymer has been carbonized in a subsquent step, there is a stoichiometrical excess of the oxide to carbon. The solution is then shaped to form a desired thin membrane, and the polymer is then carbonized by heating it in a non-oxidizing atmosphere. The resulting oxide/carbon product is heated to a temperature at which (a) the carbon reacts with the oxide to form a volatile sub-oxide and carbon monoxide and (b) the remaining (unreacted) oxide particles sinter together. The heating is carried out in a non-oxidizing atmosphere containing either no nitrogen whatsoever, or an amount of nitrogen less than that which results in the formation of a non-porous product. The sintered membranes can be used, for example, as filters and catalyst supports and have good strength and controlled porosity.

Method of producing porous membranes of sinterable refractory metal

A process for forming carbides of silicon or metals in fine powder or whisker form. The process comprises forming a substantially uniform and non-agglomerated dispersion of a microfine powder of an oxide of silicon or a carbide-forming metal within a matrix of a polymer, carbonizing the oxide-containing polymer in an inert atmosphere and heating the carbonized product at high temperature to cause the oxide to react with carbon to form a carbide. The polymer must have a molecular weight of at least 10,000, a high carbon yield of at least 30% by weight, and a chemical structure which is infusible or capable of being rendered infusible. The preferred polymers are polyacrylonitrile, cellulose and polyvinyl alcohol, but other polymers with similar characteristics can be employed. The process is relatively inexpensive and gives an extremely finely divided product of high purity.

Process for producing silicon carbide and metal carbides

A method of producing whiskers of silicon carbide and other materials. For the formation of silicon carbide, the method involves forming a first reaction zone containing microfine particles of silicon dioxide uniformly mixed with carbon or a carbon precursor, with the ratio of the silicon dioxide to the carbon present as a starting material or derivable from the precursor being greater than about 5 to 1 by weight. A closely adjacent second reaction zone is formed containing a porous fibrous mass of active carbon or an infusible carbon precursor. The reaction zones are heated under a non-oxidizing atmosphere to temperatures at which silicon monoxide is formed in the first reaction zone, diffuses to the second reaction zone and reacts with carbon derived from the carbon precursor in the second reaction zone to form silicon carbide whiskers. A continuous supply of a whisker-forming catalyst is provided in the second reaction zone, at least in the vicinity where the silicon monoxide and carbon react with each other. This can be assured, for example, by providing the whisker-forming catalyst in the first reaction zone together with a catalyst volatilizing aid which enables the catalyst to diffuse to the second reaction zone along with the SiO. The first reaction zone may also contain a catalyst for the SiO producting reaction. By changing the starting materials, reaction temperatures etc. but using the same method steps, whiskers of other materials such as AlN, sialons, Si.sub.3l N.sub.4 l etc. can also be prepared.

Method of preparing whiskers of silicon carbide and other materials

A process of forming hollow microspheres containing carbon or a polymer which is a carbon precursor. The process comprises forming a solution in a liquid solvent of a polymer having the following properties (a) a molecular weight of at least 10,000 and a long chain structure; (b) an ability to be coagulated by or precipitated from the solution by a non-solvent for the polymer; (c) an ability to form a continuous stretchable film when coagulated or precipitated from solution; (d) a chemical structure which is infusible or capable of being rendered infusible, and (e) a high carbon yield of at least 30% by weight upon being carbonized in a non-reactive atmosphere. An insoluble particulate blowing agent is incorporated into the solution and the solution is then divided into droplets and the droplets are introduced into a liquid bath containing a suitable non-solvent for the polymer. The non-solvent causes the polymer to precipitate or coagulate rapidly and simultaneously the blowing agent is decomposed to generate a gas within the droplets so that hollow microspheres are formed. The microspheres are then optionally subjected to carbonization in a non-reactive atmosphere at high temperature to convert the polymer to carbon. Uniformly-sized relatively large hollow microspheres can be produced by this process.

Hollow microspheres

A cement for bonding carbon blocks, particularly the cathode blocks of electrolytic cells, e.g. Hall-Heroult cells used for the production of aluminum. The cement comprises a carbonaceous aggregate of particle size smaller than 48 Tyler mesh, a curable water-soluble liquid polymeric resin (preferably a phenol-formaldehyde resin), water and normally a curing agent for the resin. The water is used in such an amount that the proportion of the resin can be reduced without adversely affecting the viscosity of the cement at ambient temperature. The cement carbonizes when the carbon blocks are subjected to high temperatures and has a linear shrinkage of less than 5%, which reduces the tendency of the carbonized cement to crack.

Cement for cathode blocks

A process for forming hollow microspheres containing carbon or a polymer which is a carbon precursor. The process comprises forming a solution in a liquid solvent of a polymer having the following properties (a) a molecular weight of at least 10,000 and a long chain structure; (b) an ability to be coagulated by or precipitated from the solution by a non-solvent for the polymer; (c) an ability to form a continuous stretchable film when coagulated or precipitated from solution; (d) a chemical structure which is infusible or capable of being rendered infusible, and (e) a high carbon yield of at least 30% by weight upon being carbonized in a non-reactive atmosphere. An insoluble particulate blowing agent is incorporated into the solution and the solution is then divided into droplets and the droplets are introduced into a liquid bath containing a suitable non-solvent for the polymer. The non-solvent causes the polymer to precipitate or coagulate rapidly and simultaneously the blowing agent is decomposed to generate a gas within the droplets so that hollow microspheres are formed. The microspheres are then optionally subjected to carbonization in a non-reactive atmosphere at high temperature to convert the polymer to carbon. Uniformly-sized relatively large hollow microspheres can be produced by this process.

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Jonquiere, Canada

Mukesh K Jain