Process for preparing electroactive insertion compounds and electrode materials obtained therefrom
View Patent ↗A process for preparing an at least partially lithiated transition metal oxyanion-based lithium-ion reversible electrode material, which includes providing a precursor of said lithium-ion reversible electrode material, heating said precursor, melting same at a temperature sufficient to produce a melt including an oxyanion containing liquid phase, cooling said melt under conditions to induce solidification thereof and obtain a solid electrode that is capable of reversible lithium ion deinsertion/insertion cycles for use in a lithium battery. Also, lithiated or partially lithiated oxyanion-based-lithium-ion reversible electrode materials obtained by the aforesaid process.
1. A pure, partially substituted or doped lithium-ion reversible electrode material, said material having a particle size distribution comprising micron size particles and submicron size particles, said micron size particles and submicron size particles having the nominal formula AB(XO 4 )H in which:
A is lithium, which may be partially substituted with another alkali metal representing less than 20% at. of said A;
B is a main redox metal at oxidation level of +2 selected from the group consisting of Fe, Mn, Ni and any mixture thereof, which may be partially substituted by one or more additional metal at oxidation level between +1 and +5 and representing less than 35% at. of said main +2 redox metal, including 0;
XO 4 is any oxyanion wherein X is selected from the group consisting of P, S, V, Si, Nb, Mo and any combination thereof; and
H is a fluoride, hydroxide or chloride anion representing less that 35% at. of the XO 4 oxyanion, including 0.
2. The electrode material according to claim 1 , wherein A is lithium, partially substituted with another alkali metal representing less than 20% at. of said A.
3. The electrode material according to claim 2 , wherein B is a main redox metal at oxidation level of +2 selected from the group consisting of Fe, Mn, Ni and any mixture thereof, partially substituted by one or more additional metal at oxidation level between +1 and +5 and representing less than 35% at. of said main +2 redox metal, including 0.
4. The electrode material according to claim 1 , wherein said micron size particles have a particle size distribution that includes a plurality of micron sizes.
5. The electrode material according to claim 1 , wherein said submicron size particles have a particle size distribution that includes a plurality of submicron sizes.
6. The electrode material according to claim 1 , wherein said micron size particles have a particle size distribution that includes a plurality of micron sizes and said submicron size particles have a particle size distribution that includes a plurality of submicron sizes.
7. The electrode material according to claim 1 , wherein said electrode material has the nominal formula LiFePO 4 .
8. The electrode material according to claim 6 , wherein said electrode material has the nominal formula LiFePO 4 .
9. The electrode material according to claim 1 , wherein said material has a particle size distribution comprising up to 40% of submicron size particles.
10. The electrode material according to claim 6 , wherein said material has a particle size distribution comprising up to 40% of submicron size particles.
11. The electrode material according to claim 8 , wherein said material has a particle size distribution comprising up to about 40% of submicron size particles.
12. The electrode material according to claim 1 , wherein said particles have a mean size of about 1.5 μm.
13. The electrode material according to claim 1 , wherein said particles have a mean size of about 1 μm to about 5 μm.
14. The electrode material according to claim 1 , wherein said particles have a pyrolytic carbon deposit.
15. The electrode material according to claim 7 , wherein said particles have a pyrolytic carbon deposit.
16. The electrode material according to claim 8 , wherein said particles have a pyrolytic carbon deposit.
17. The electrode material according to claim 11 , wherein said particles have a pyrolytic carbon deposit.
18. A cathode electrode comprising the electrode material according to claim 1 .
19. cathode electrode comprising the electrode material according to claim 6 .
20. A cathode electrode comprising the electrode material according to claim 7 .
21. A cathode electrode comprising the electrode material according to claim 8 .
22. A cathode electrode comprising the electrode material according to claim 14 .
23. A cathode electrode comprising the electrode material according to claim 15 .
24. A cathode electrode comprising the electrode material according to claim 16 .
25. A cathode electrode comprising the electrode material according to claim 17 .