Pressureless Sintering Beryllium Containing Silicon Carbide Powder Composition

The invention will now be illustrated by more specific examples which further illustrate various aspects of the invention but are not intended to limit it. Where not otherwise specified in this specification and claims, temperatures are given in degrees Celsius, and all parts and percentages are by weight.

A silicon carbide powder having the following specifications was utilized as a starting material. The silicon carbide powder had a surface area greater than 8.0 m.sup.2 /gm and the following analysis in percent by weight:

A composition comprised of 95% of the silicon carbide powder characterized above was mixed in acetone with 5% of a phenolic resin known as Resin No. 8121, a product of Varcum Chemical Company. The slurry was comprised of about one part by weight mixture to about one part by weight acetone. The slurry was mixed for about 30 minutes and the acetone then allowed to evaporate. The resulting powder mixture was pressed into 1/2 inch diameter pellets weighing about 11/2 grams each. The pellets or powder compacts typically had a density of about 1.76 gm/cm.sup.3.

Pellets prepared by the above procedure were placed in a graphite crucible, the crucible covered and pushed through a graphite resistance heating element tube furnace having a hot zone temperature of 2080.degree. C. using an argon atmosphere. The bulk density of the pellets after passing through the tube furnace was 1.83 gm/cm.sup.3, about 57% of theoretical.

Six mixes having the powder composition of Example 1 were prepared, except that varying amounts of beryllium in the form of beryllium carbide, having a particle size of less than 10 microns, were added to each mix. The composition of the mixes is shown in Table I. Four pellets 1/2 inch in diameter and weighing about 11/2 grams each were pressed from each mix, using the technique of Example 1. These pellets were divided into two sets, A and B, with two pellets per mix in each set.

The pellets from Set A were fired in a graphite resistance heating element tube furnace in accord with the procedure utilized in Example 1. Pellets from Set B were fired in a manner similar to Set A, with the exception that a cover mix was used to surround the pellets in the crucible. The cover mix was in the form of a powder having the composition 97.5% silicon carbide, 2.0% carbon and 0.5% beryllium in the form of beryllium carbide. The purpose of the cover mix was to increase the amount of beryllium in the atmosphere around the pellets.

The bulk density of the pellets was determined both before and after sintering and is shown in Table I. Thus, the pellets in Set A, fired in crucibles having no beryllium-containing atmosphere, ranged in fired density from 68.5 to 75.4% of theoretical. The pellets in Set B, fired in crucibles having a beryllium-containing atmosphere, ranged in fired density from 68.8 to 93.5% of theoretical.

A silicon carbide powder having a composition similar to that in Example 1 was prepared and divided into batches. Various amounts of finelydivided boron carbide and beryllium carbide were separately added to each batch to obtain the powder compositions recited in Table II. The various batches were then mixed with a carbon source and pressed into pellets as in Example 1.

Two pellets from each batch were placed into a crucible of the same composition, covered with a crucible lid and placed within a graphite boat 4 inches in diameter and 19 inches in length. The pellets were sintered by pushing the boat containing the pellets through a graphite resistance element tube furnace operated under an argon atmosphere. The pellets had a residence time at 2150.degree. C. of 30 minutes. The results are shown in Table II. Thus, following this procedure, in Mix #8, a silicon carbide starting material containing 0.10% boron, 0.10% beryllium, 2.0% carbon and 97,80% silicon carbide was pelleted to a cured density of 1.72 gm/cm.sup.3, or 53.6% of theoretical. After firing, the density was found to be 2.98 gm/cm.sup.3, or 92.8% of the theoretical density of silicon carbide.

A control sample containing only 0.5% boron and no beryllium was prepared as above described. The control sample was sintered in a manner similar to that described above, except that beryllium and boron were absent from the sintering atmosphere. After firing, the control sample was found to have a bulk density of 79.0% of theoretical.

The foregoing description and embodiments are intended to illustrate the invention without limiting it thereby. Various modifications can be made in the invention without departing from the spirit or scope thereof.