Dense, shaped articles constructed of a refractory material and methods of preparing such articles
View Patent ↗The invention provides a method of forming a dense, shaped article, such as a crucible, formed of a refractory material, the method comprising the steps of placing a refractory material having a melting point of at least about 2900° C. in a mold configured to form the powder into an approximation of the desired shape. The mold containing the powder is treated at a temperature and pressure sufficient to form a shape-sustaining molded powder that conforms to the shape of the mold, wherein the treating step involves sintering or isostatic pressing. The shape-sustaining molded powder can be machined into the final desired shape and then sintered at a temperature and for a time sufficient to produce a dense, shaped article having a density of greater than about 90% and very low open porosity. Preferred refractory materials include tantalum carbide and niobium carbide.
1. A dense, shaped article comprising at least about 95% by weight of a refractory material selected from the group consisting of carbides of tantalum, niobium or hafnium, nitrides of tantalum, niobium or hafnium, and alloys or powder mixtures thereof, wherein the article has a melting point of at least about 2900° C., a density of at least about 90%, a total porosity of no more than about 10%, and a total open porosity of no more than about 1.0%, wherein the article is a crucible adapted for use in crystal growth by physical vapor transport; and the crucible comprises a wall having a homogeneous structure across its thickness.
2. The article of claim 1 , wherein the article has a melting point of at least about 3200° C.
3. The article of claim 1 , wherein the article has a melting point of at least about 3600° C.
4. The article of claim 1 , wherein the refractory material is tantalum carbide.
5. The article of claim 1 , wherein the article comprises at least about 97% by weight of the refractory material.
6. The article of claim 1 , wherein the article comprises at least about 99% by weight of the refractory material.
7. The article of claim 1 , wherein the article has a density greater than about 95%, a total porosity of no more than about 5%, and a total open porosity of no more than about 0.5%.
8. The article of claim 1 , wherein the article has a density greater than about 97%, a total porosity of no more than 3%, and a total open porosity of no more than about 25%.
9. The article of claim 1 , wherein the article comprises at least about 95% by weight of tantalum carbide, and the article has a density of at least about 95%, a total porosity of no more than about 5%, and a total open porosity of no more than about 0.5%.
10. The article of claim 9 , wherein the article has a density greater than about 97%, a total porosity of no more than 3%, and a total open porosity of no more than about 0.25%.
11. The article of claim 1 , wherein the crucible has a useful life of at least 200 hours at crystal growth temperatures of at least about 2200° C.
12. The article of claim 1 , wherein the crucible comprises at least about 95% by weight of tantalum carbide, the crucible having a density of at least about 95%, a total porosity of no more than about 5%, and a total open porosity of no more than about 0.5%.
13. The article of claim 12 , wherein the crucible has a density of greater than about 97%, a total porosity of no more than 3%, and a total open porosity of no more than about 0.25%.
14. The article of claim 1 , wherein the crucible has a cylindrical shape.
15. The article of claim 14 , wherein the crucible has a height of about 1 to about 10 inches, a wall thickness of about 1/16 to about ⅝ inch, and an outer diameter of about 0.5 to about 5 inches.
16. A crucible adapted for use in crystal growth by physical vapor transport, the crucible comprising at least about 99% by weight of tantalum carbide wherein the crucible has a density of at least about 95%, a total porosity of no more than about 5%, a total open porosity of no more than about 0.5%, a width of about 1 to about 5 inches, and a homogeneous wall structure across its thickness.
17. The crucible of claim 13 , wherein the crucible has a height of about 1 to about 10 inches, a wall thickness of about 1/16 to about ⅝ inches, and a width of about 1 to about 5 inches.