Complexometric precursors formulation methodology for industrial production of high performance fine and ultrafine powders and nanopowders for specialized applications
A method of forming a powder M j X p wherein M j is a positive ion or several positive ions selected from alkali metal, alkaline earth metal or transition metal; and X p is a monoatomic or a polyatomic anion selected from Groups IIIA, IVA, VA, VIA or VIIA; called complexometric precursor formulation or CPF. The method includes the steps of: providing a first reactor vessel with a first gas diffuser and an first agitator; providing a second reactor vessel with a second gas diffuser and a second agitator; charging the first reactor vessel with a first solution comprising a first salt of M j ; introducing gas into the first solution through the first gas diffuser, charging the second reactor vessel with a second solution comprising a salt of M p ; adding the second solution to the first solution to form a complexcelle; drying the complexcelle, to obtain a dry powder; and calcining the dried powder of said M j X p .
1. A method of forming a powder M j X p wherein M j is a positive ion or several positive ions selected from alkali metal, alkaline earth metal or transition metal; and X p is a monoatomic or a polyatomic anion selected from Groups IIIA, IVA, VA, VIA or VIIA; comprising:
providing a first reactor vessel with a first gas diffuser and a first agitator;
providing a second reactor vessel with a second gas diffuser and a second agitator;
charging said first reactor vessel with a first solution comprising first salt of M j ;
introducing gas into said first solution through said first gas diffuser,
charging said second reactor vessel with a second solution comprising a salt of X p ;
adding said second solution to said first solution while agitating same to form a complexcelle;
drying said complexcelle, to obtain a dried powder of said M j X p ; and
calcining said dried powder of said M j X p to form a calcined powder.
2. The method of forming a powder of claim 1 wherein at least one of said first diffuser or said second diffuser is selected from the group consisting of a porous ceramic, a tube, a membrane and a dome diffuser.
3. The method of forming a powder of claim 1 further comprising adjusting a final pH of at least one of said first solution, said second solution or said complexcelle.
4. The method of forming a powder of claim 1 wherein said gas is introduced into said first solution at a rate sufficient to increase a volume of said first solution by at least 5%.
5. The method of forming a powder of claim 1 wherein said gas is introduced into said first solution at a rate of at least one liter of said gas per liter of said first solution per minute.
6. The method of forming a powder of claim 1 wherein at least one of said first agitator or said second agitator comprises concentric wires.
7. The method of forming a powder of claim 1 wherein at least one of said first agitator or said second agitator comprises at least one blade.
8. The method of forming a powder of claim 7 wherein at least one said blade rotates on a shaft and on a blade axis.
9. The method of forming a powder of claim 1 wherein at least one of said first agitator or said second agitator has a mixing speed of at least 100 rpm.
10. The method of forming a powder of claim 1 wherein said gas comprises a gas selected from the group consisting of air, carbon dioxide, methane, SF 6 , HF, HCl, NH 3 , propane, O 2 and inert gas.
11. The method of forming a powder of claim 1 comprising a salt of said M j wherein said salt is selected from the group consisting of chloride hydroxide, nitrate, phosphate, oxalate, carbonate, acetate, sulfate, hydroxycarbonate, hydroxyl phosphate, hydroxysilicate, and silicate.
12. The method of forming a powder of claim 1 wherein said first solution comprises up to 30 wt. % of said first salt of M j .
13. The method of forming a powder of claim 1 wherein said second solution comprises up to 30 wt. % of said salt of X p .
14. The method of forming a powder of claim 1 wherein said powder of said M j X p is selected from the group consisting of lithium metal oxides, calcium phosphates, lithium aluminosilicates, lithium aluminates and lithium metal phosphates.
15. The method of forming a powder of claim 1 wherein said powder further comprises a dopant.
16. The method of forming a powder of claim 15 wherein said dopant is selected from the group consisting of alkali metals, alkaline earth metals, Group III A elements, Group IV A elements and transition metals.
17. The method of forming a powder of claim 15 wherein said dopant is selected from the group consisting of cobalt, aluminum and gadolinium.
18. The method of forming a powder of claim 15 wherein said dopant is present in an amount of up to 10 weight % of said dried powder.
19. The method of forming a powder of claim 1 further comprising applying a coating to said calcined powder.
20. The method of forming a powder of claim 19 wherein said coating is selected from the group consisting of an organic compound and an inorganic compound.
21. The method of forming a powder of claim 19 wherein said coating comprises carbon.
22. The method of forming a powder of claim 1 wherein said powder of said M j X p is selected from the group consisting of lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide, and lithium mixed oxides of cobalt, nickel and manganese.
23. The method of forming a powder of claim 1 wherein said forming said complexcelle is at a temperature of no more than 100° C.
24. The method of forming a powder of claim 1 wherein said drying is at a temperature of no more than 350° C.
25. The method of forming a powder of claim 1 wherein said drying is done by a method selected from the group consisting of spray drying, freeze drying, tray drying and evaporation drying.
26. The method of forming a powder of claim 1 wherein said calcining is in an apparatus selected from the group consisting of a box furnace, a rotary calciner, a fluidized bed calciner and a spray pyrolyzer.
27. The method of forming a powder of claim 1 wherein said calcining is at a temperature of from 350-3000° C.
28. The method of forming a powder of claim 1 wherein said calcined powder has a particle size of less than 1 micron.
29. The method of forming a powder of claim 1 wherein said calcined powder has a surface area of more than 1 m 2 /gm.
30. The method of forming a powder of claim 1 wherein said adding said second solution to said first solution is through a tube.
31. The method of forming a powder of claim 30 wherein said tube has an inner diameter of at least 2 cm.
32. The method of forming a powder of claim 30 wherein said tube further comprises at least one of an atomizer, sprinkler or nozzle.
33. The method of forming a powder in claim 1 , wherein said calcined powder has a structure selected from a microstructure and a nanostructure.
34. A method of forming a powder M j X p wherein M j is a positive ion or several positive ions selected from alkali metal, alkaline earth metal or transition metal; and X p is a monoatomic or a polyatomic anion selected from Groups IIIA, IVA, VA, VIA or VIIA; comprising:
providing a first reactor vessel with a first gas diffuser and a first agitator;
providing a second reactor vessel with a second gas diffuser and a second agitator;
charging said first reactor vessel with a first solution comprising first salt of X p ;
introducing gas into said first solution through said first gas diffuser,
charging said second reactor vessel with a second solution comprising a salt of Mj;
adding said second solution to said first solution while agitating same to form a complexcelle;
drying said complexcelle, to obtain a dried powder of said M j X p ; and calcining said dried powder of said M j X p .