Processes for producing synthetic pyrite
View Patent ↗Process of making high purity, synthetic FeS 2 , and an electrochemical battery employing such synthetic FeS 2 in the positive electrode. Synthetic FeS 2 may be prepared by a sulfidation process comprising reacting ferric oxide, hydrogen sulfide, and elemental sulfur at a temperature above the melting point of element sulfur. Synthetic FeS 2 may also be produced by a milling process that comprises (i) milling iron powder and sulfur powder in the presence of a milling media and a processing agent to provide a homogenous powder mixture, and (ii) treating the powder mixture to form FeS 2 . In the milling process, the powder mixture may be treated to form FeS 2 by heating the powder mixture or subjecting the powder mixture to a subsequent milling operation.
1. A method of producing synthetic FeS 2 comprising:
reacting Fe 2 O 3 , elemental sulfur, and hydrogen sulfide in an inert atmosphere, the reaction being conducted at a temperature of from about 125° C. to about 200° C. for a sufficient period of time to form synthetic FeS 2 particles.
2. The method according to claim 1 , comprising (i) reacting the Fe 2 O 3 , elemental sulfur, and hydrogen sulfide at a temperature of about 125° C. for a selected period of time, and (ii) subsequently raising the temperature of the reaction to no greater than about 200° C.
3. The method according to claim 2 , wherein the selected period of time is less than 5 hours.
4. The method according to claim 1 , wherein the Fe 2 O 3 has an average particle size of about 1 nm to about 100 nm.
5. The method according to claim 1 , wherein the Fe 2 O 3 has an average particle size of about 3 nm to about 10 nm.
6. The method according to claim 1 , comprising applying a protective coating to the synthetic FeS 2 .
7. The method according to claim 6 , wherein the protective coating comprises a conductive material.
8. The method according to claim 7 , wherein the conductive material comprises a carbon material, a metal material, a metal oxide, or an organic conductive material.
9. The method according to claim 6 , wherein the protective coating is applied by spray pyrolysis.
10. The method according to claim 1 , wherein the FeS 2 particles have a particle size of from about 5 to about 600 nm.
11. The method according to claim 1 , wherein the FeS 2 has an average particle size of about 250 nm or less.
12. The method according to claim 1 , wherein the FeS 2 has an average particle size of about 200 nm or less.
13. The method according to claim 1 , wherein the FeS 2 has a crystallite size of from about 5 to about 100 nm.
14. The method according to claim 1 , wherein the Fe 2 O 3 , elemental sulfur and hydrogen sulfide are provided in about a 1:3:0.125 molar ratio of Fe 2 O 3 :hydrogen sulfide:elemental sulfur when the elemental sulfur is provided as S 8 .
15. The method according to claim 1 , comprising sintering the FeS 2 particles at a temperature of about 400° C. to about 700° C. so that the FeS 2 consists essentially of pyrite.
16. The method according to claim 15 , wherein, after sintering, the FeS 2 has a crystallite size of from about 35 nm to about 3 μm.
17. The method according to claim 1 , wherein the hydrogen sulfide is a gas comprising from about 6% by volume to about 99% by volume of hydrogen sulfide in a carrier gas.
18. The method according to claim 1 , wherein the synthetic FeS 2 particles comprise less than 1% by weight of metal impurities.
19. The method according to claim 1 , wherein the synthetic FeS 2 particles comprise less than 3% by weight of oxide impurities.
20. The method according to claim 1 , wherein the synthetic FeS 2 particles contain less than 3% by weight of iron sulfide impurities.
21. The method according to claim 1 , wherein the synthetic FeS 2 particles contain less than 1% by weight of iron sulfide impurities.
22. The method according to claim 1 , wherein the synthetic FeS 2 particles contain less than 0.1% by weight of iron sulfide impurities.
23. The method according to claim 1 , wherein the synthetic FeS 2 particles contain less than 0.01% by weight of iron sulfide impurities.