Polycrystalline diamond material with extremely fine microstructures
View Patent ↗A sintered polycrystalline diamond material (PCD) of extremely fine grain size is manufactured by sintering under high pressure/high temperature (HP/HT) processing, a diamond powder which is blended with a pre-milled source catalyst metal compound. The PCD material has an average sintered diamond grain structure of less than about 1.0 μm.
1. A method for producing a polycrystalline diamond (PCD) body with an arithmetic mean as-sintered grain size less than 1 μm, comprising:
providing diamond particles having a volumetric mean particle size of less than about 1.0 μm and greater than about 0.1 μm;
blending, with the diamond particles, a source catalyst metal compound selected from the group of cobalt oxalate dihydrate, cobalt acetate, cobalt boride, cobalt citrate dihydrate, cobalt hydroxide, cobalt isopropoxide, cobalt pentanedionate, and dodecacarbonyltretracobalt to form a diamond powder blend; and
processing the diamond powder blend using a pressure and a temperature for a time sufficient to cause intercrystalline bonding between adjacent diamond grains.
2. The method of claim 1 , wherein the source catalyst metal compound comprises up to about 50% by weight of the diamond powder blend.
3. The method of claim 1 , wherein the source catalyst metal compound comprises nanocrystalline particles.
4. The method of claim 1 , wherein the pressure is between about 20 Kbar and 80 Kbar, and wherein the temperature is at least about 1000° C., for up to about 120 minutes.
5. The method of claim 1 , further comprising processing the diamond powder blend together with a cemented metal carbide support.
6. The method of claim 1 , wherein the metal carbide support comprises a support annulus and the diamond power blend is disposed within the support annulus.
7. A method for producing a polycrystalline diamond (PCD) body with an arithmetic mean as-sintered grain size less than 1 μm, comprising:
milling a source catalyst metal compound selected from the group of cobalt oxalate dihydrate, cobalt acetate, cobalt boride, cobalt citrate dihydrate, cobalt hydroxide, cobalt isopropoxide, cobalt pentanedionate, and dodecacarbonyltretracobalt;
providing diamond particles having a volumetric mean particle size of less than about 1.0 μm and greater than about 0.1 μm;
blending, with the diamond particles, said source catalyst metal compound wherein said catalyst has an average particle size that is less than that of the diamond grain size, to form a diamond powder blend;
heating said diamond powder blend; and
processing the diamond powder blend using a pressure and a temperature for a time sufficient to cause intercrystalline bonding between adjacent diamond grains.
8. The method of claim 7 , wherein said milling step comprises a carrier liquid.
9. The method of claim 7 , wherein the temperature of said heating step is between about 500° C. to about 1200° C.
10. The method of claim 7 , wherein said step of heating said diamond powder blend further comprises reducing said source catalyst metal compound to a reduced catalyst metal.
11. The method of claim 7 , wherein said method for producing a polycrystalline diamond (PCD) body with an arithmetic mean as-sintered grain size less than 1 μm further comprising a second heating step after said heating step.
12. The method of claim 10 , wherein the reduced catalyst metal comprises about 0.5% to about 5% by weight of the diamond powder blend.
13. The method of claim 12 , wherein the reduced catalyst metal comprises about 1.0% to about 3% by weight of the diamond powder blend.