Forming a polycrystalline ceramic in multiple sintering phases
View Patent ↗In one aspect of the invention, a method of forming polycrystalline diamond comprises providing a can assembly comprising a preform of diamond powder with a first catalyst, the preform being adjacent a solid substrate with a second catalyst. The pressure and/or temperature on the can assembly increases until the first catalyst and carbon from the diamond powder begin to form a melting composition within the preform. The pressure and temperature may be held substantially constant on the can assembly until the melting composition has catalyzed crystalline growth in at least a portion of the preform. The pressure and/or temperature are then increased on the assembly until the second catalyst within the substrate is released into the preform.
1. A method of forming polycrystalline diamond, comprising the steps of:
providing a can assembly comprising a mixture of diamond powder and a first catalyst, the mixture having a catalyst region and a substantially catalyst-free region, adjacent a solid substrate comprising a second catalyst;
increasing the pressure, temperature or both on the can assembly until a portion of the first catalyst and a portion of carbon from the diamond powder liquefy;
holding the pressure and temperature within ranges that allow the first catalyst to catalyze crystalline growth in portion of the diamond powder; and
increasing the pressure, temperature or both on the assembly until a portion of the second catalyst releases from the solid substrate into the mixture.
2. The method of claim 1 , wherein the first catalyst and the carbon from the diamond powder form a eutectic composition.
3. The method of claim 2 , wherein a eutectic temperature that forms the eutectic composition is lower than a release temperature that releases the second catalyst from the substrate.
4. The method of claim 3 , wherein the eutectic temperature is between 1300 degrees C. and 1400 degrees C.
5. The method of claim 3 , wherein the release temperature is between 1400 degrees C. to 1500 degrees C.
6. The method of claim 1 , wherein the first catalyst comprises a cemented metal carbide.
7. The method of claim 6 , wherein the first catalyst comprises 1% to 7% of the mixture by weight.
8. The method of claim 6 , wherein the cemented metal carbide is tungsten carbide.
9. The method of claim 1 , wherein the first catalyst comprises cobalt.
10. The method of claim 1 , further comprising forming the mixture of diamond powder and first catalyst by milling the diamond powder with pellets comprising the first catalyst in a non-oxidizing fluid.
11. The method of claim 10 , wherein the non-oxidizing fluid comprises acetone.
12. The method of claim 1 , further comprising cleaning the diamond powder by heating the diamond powder in a hydrogen environment and removing oxygen by forming water vapor.
13. The method of claim 1 , further comprising cleaning the diamond powder by heating the diamond powder in a vacuum environment and removing oxygen by forming carbon monoxide.
14. The method of claim 1 , further comprising sealing a lid to the can assembly by melting a sealant located between the can assembly and the lid.
15. The method of claim 1 , wherein the method causes the polycrystalline diamond to have a catalyst concentration by weight of 0.05% to 14%.
16. The method of claim 1 , wherein the method causes the polycrystalline diamond to have tungsten located within its interstitial regions.
17. The method of claim 1 , wherein holding the temperature and pressure includes holding the pressure between 70 and 90 kilobars.
18. The method of claim 1 , wherein holding the temperature and pressure continues for 2 to 5 minutes.
19. The method of claim 1 , wherein the second step of increasing the pressure, temperature or both continues for 1 to 3 minutes.
20. The method of claim 1 , wherein the step of holding the pressure and temperature comprises holding the temperature substantially constant.