Process for preparing electroactive insertion compounds and electrode materials obtained therefrom

Abstract

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.