PROCESS FOR PREPARING ELECTROACTIVE INSERTION COMPOUNDS AND ELECTRODE MATERIALS OBTAINED THEREFROM
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 - 59 . (canceled)
60 . A lithium-ion reversible electrode material, comprising micron size particles and submicron size particles, said micron size particles and submicron size particles having the nominal formula AB(XO 4 )H, said micron size particles having a first pyrolytic carbon deposit wt. % ratio relative to the total weight of the AB(XO 4 )H micron size particles and said submicron size particles having a second pyrolytic carbon deposit wt. % ratio relative to the total weight of the AB(XO 4 )H submicron size particles, wherein said first pyrolytic carbon deposit wt. % ratio is different from said second pyrolytic carbon deposit wt. % ratio, and wherein:
A is lithium, which may be partially substituted with another alkali metal representing less than 20 atomic % 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 atomic % 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 atomic % of the XO 4 oxyanion, including 0.
61 - 65 . (canceled)
66 . The electrode material according to claim 60 , wherein said micron size particles have the nominal formula LiFePO 4 .
67 . The electrode material according to claim 60 , wherein said submicron size particles have the nominal formula LiFePO 4 .
68 . The electrode material according to claim 60 , wherein said material has a particle size distribution comprising up to 40% of submicron size particles.
69 . A method for preparing a lithium-ion reversible electrode material having a pyrolytic carbon deposit, comprising micron size particles and submicron size particles, said micron size particles and submicron size particles having the nominal formula AB(XO 4 )H, said method comprising:
providing AB(XO 4 )H micron size particles having a first pyrolytic carbon deposit wt. % ratio relative to the total weight of the AB(XO 4 )H micron size particles;
providing AB(XO 4 )H submicron size particles having a second pyrolytic carbon deposit wt. % ratio relative to the total weight of the AB(XO 4 )H submicron size particles; and
mixing a mixture comprising said micron size particles and said submicron size particles,
wherein:
A is lithium, which may be partially substituted with another alkali metal representing less than 20 atomic % 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 atomic % 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 atomic % of the XO 4 oxyanion, including 0.
70 . The method according to claim 69 , wherein said first pyrolytic carbon deposit wt. % ratio is different from said second pyrolytic carbon deposit wt. % ratio.
71 . The method according to claim 69 , wherein the mixing is selected from the group consisting of grinding, sieving and mechanofusion.
72 - 73 . (canceled)
74 . The method according to claim 69 , wherein said micron size particles have a particle size distribution that includes a plurality of micron sizes.
75 . The method according to claim 69 , wherein said submicron size particles have a particle size distribution that includes a plurality of submicron sizes.
76 . (canceled)
77 . The method according to claim 69 , wherein said micron size particles have the nominal formula LiFePO 4 .
78 . The method according to claim 69 , wherein said submicron size particles have the nominal formula LiFePO 4 .
79 . The method according to claim 69 , wherein said mixing is in a liquid medium.
80 . A method for preparing a lithium-ion reversible electrode material, comprising micron size particles and submicron size particles, said micron size particles and submicron size particles having the nominal formula AB(XO 4 )H, said method comprising:
providing at least a starting AB(XO 4 )H material; and
processing said starting AB(XO 4 )H material so as to obtain said AB(XO 4 )H micron size particles and submicron size particles,
wherein:
A is lithium, which may be partially substituted with another alkali metal representing less than 20 atomic % 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 atomic % 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 atomic % of the XO 4 oxyanion, including 0.
81 . The method according to claim 80 , wherein said processing is selected from the group consisting of grinding, sieving and mechanofusion.
82 . The method according to claim 80 , wherein said micron size particles have a particle size distribution that includes a plurality of micron sizes.
83 . The method according to claim 80 , wherein said submicron size particles have a particle size distribution that includes a plurality of submicron sizes.
84 . The method according to claim 80 , wherein said micron size particles have the nominal formula LiFePO 4 .
85 . The method according to claim 80 , wherein said submicron size particles have the nominal formula LiFePO 4 .
86 . The method according to claim 81 , wherein said grinding is in a liquid medium.
87 . The method according to claim 80 , wherein said at least starting AB(XO 4 )H material consists of a single starting AB(XO 4 )H material.