Method for producing ceramic particles and agglomerates

• US 6,261,484 B1
• Filed: 08/11/2000
• Issued: 07/17/2001
• Est. Priority Date: 08/11/2000
• Status: Expired due to Term

• Current Assignee: TRIAD National Security, LLC
• Original Assignee: Regents of the University of California (University of California)
• Inventors: Phillips, Jonathan, Chen, Chun-Ku, Gleiman, Seth S.
• Primary Examiner(s): Fiorilla, Christopher A.
• Application Number:
  US09/637,172
• Time in Patent Office: 340 Days
• Field of Search: 264/5, 264/6, 264/11, 264/12, 264/430
• US Class Current: 264/5
• CPC Class Codes: B01J 2/02 by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
• CPC Class Codes: C01B 13/145 After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
• CPC Class Codes: C01F 7/027 Treatment involving fusion or vaporisation
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/32 Spheres
• CPC Class Codes: C01P 2004/50 Agglomerated particles
• CPC Class Codes: C01P 2004/51 Particles with a specific particle size distribution
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C23C 4/123 Spraying molten metal

Abstract

A method for generating spherical and irregularly shaped dense particles of ceramic oxides having a controlled particle size and particle size distribution. An aerosol containing precursor particles of oxide ceramics is directed into a plasma. As the particles flow through the hot zone of the plasma, they melt, collide, and join to form larger particles. If these larger particles remain in the hot zone, they continue melting and acquire a spherical shape that is retained after they exit the hot zone, cool down, and solidify. If they exit the hot zone before melting completely, their irregular shape persists and agglomerates are produced. The size and size distribution of the dense product particles can be controlled by adjusting several parameters, the most important in the case of powder precursors appears to be the density of powder in the aerosol stream that enters the plasma hot zone. This suggests that particle collision rate is responsible for determining ultimate size of the resulting sphere or agglomerate. Other parameters, particularly the gas flow rates and the microwave power, are also adjusted to control the particle size distribution.

Claims

1. A method of generating ceramic particles, comprising the steps of:

(a) generating an aerosol comprising precursor ceramic powder particles suspended in plasma gas;

(b) generating a plasma comprising a plasma hot zone sufficiently hot to melt the precursor ceramic powder particles;

(c) directing the aerosol into the plasma hot zone and allowing the particles in the hot zone to melt, collide, and join to form larger particles;

(d) allowing these larger particles to exit the hot zone, whereby they cool and solidify to form a product comprising dense, ceramic particles that are larger than the precursor ceramic particles.

2. The method of claim 1, wherein the ceramic powder comprises at least one oxide ceramic material.

3. The method of claim 2, wherein the oxide ceramic material is selected from the group consisting of alumina, silica, titanium oxide, magnesium oxide, nickel oxide, iron oxide, chromium oxide, manganese oxide, cobalt oxide, zirconium oxide, hafnium oxide, tantalum oxide, niobium oxide, tungsten oxide, lanthanum oxide, cerium oxide, praseodymium oxide, and mixtures thereof.

4. The method of claim 2, wherein the precursor ceramic particles are selected from the group consisting of spherically shaped particles and irregularly shaped powder particles.

5. The method of claim 1, wherein the aerosol comprises ceramic powder particles suspended in plasma gas.

6. The method of claim 5, wherein the aerosol is generated by mechanically dispersing the ceramic particles in a stream of plasma gas.

7. The method of claim 5, wherein the aerosol comprises ceramic powder particles having a desired powder particle density in the plasma gas.

8. The method of claim 7, wherein the particle density in the aerosol is chosen to produce a desired and controlled particle shape, a desired and controlled particle size, and a desired and controlled particle size distribution.

9. The method of claim 8, wherein said powder density is about 0.01-100 grams of powder per liter of aerosol.

10. The method of claim 9, wherein said powder density is 0.5 grams of powder per liter of aerosol.

11. The method of claim 1, wherein the plasma is generated by supplying energy to plasma gas, the plasma gas being selected from the group consisting of air, argon, neon, xenon, nitrogen, oxygen, chlorine, fluorine, hydrogen, and mixtures thereof.

12. The method of claim 11, wherein the energy is generated from a DC discharge.

13. The method of claim 12, wherein the energy is from electromagnetic radiation.

14. The method of claim 13, wherein the electromagnetic radiation is in the radiofrequency (RF) region of the electromagnetic spectrum.

15. The method of claim 14, wherein the electromagnetic radiation is microwave radiation.

16. The method of claim 15, wherein the plasma is generated using about 100-30,000 watts of power.

17. The method of claim 16, wherein the plasma is generated using about 300-1200 watts of power.

18. The method of claim 17, wherein the plasma gas is at a gas pressure of about 0.01-10 atmospheres.

19. The method of claim 18, wherein the plasma gas is at a gas pressure of about 1 atmosphere.

20. The method of claim 1, wherein the aerosol flow rate is adjusted to produce product ceramic particles having a desired particle shape and a controlled particle size/size distribution.

21. The method of claim 1, wherein the ceramic powder resides within the hot zone of the plasma for about 0.001-10 seconds.

22. The method of claim 1, wherein the solidified product particles have an average size of about 10-200 microns.

23. The method of claim 1, wherein said step of cooling includes cooling particles using a gas stream separate from the plasma gas stream and the aerosol gas stream.

24. The method of claim 23 wherein the ceramic powder resides within the hot zone for about 0.1 second.

25. The method of claim 1, wherein the product ceramic particles are spherical ceramic particles.

26. The method of claim 1, wherein said product ceramic particles are irregularly- shaped agglomerates.

27. The method of claim 1, wherein the product ceramic particles comprises spherical ceramic particles.