US 7,348,100 B2
Product and method for the processing of precursors for lithium phosphate active materials
George Adamson, Henderson, Nev. (US); Jeremy Barker, Oxfordshire (United Kingdom); Allan Dirilo, Henderson, Nev. (US); Titus Faulkner, Henderson, Nev. (US); M. Yazid Saidi, Henderson, Nev. (US); and Jeffrey Swoyer, Henderson, Nev. (US)
Assigned to Valence Technology, Inc., Las Vegas, Nev. (US)
Filed on Oct. 08, 2004, as Appl. No. 10/961,673.
Claims priority of provisional application 60/513242, filed on Oct. 21, 2003.
Prior Publication US 2005/0194567 A1, Sep. 08, 2005
This patent is subject to a terminal disclaimer.
Int. Cl. H01M 4/58 (2006.01)
U.S. Cl. 429—218.1  [429/221; 429/224; 429/231.5; 252/182.1; 252/518.1; 252/519.1; 423/179.5; 423/323; 423/593.1; 423/594.1; 423/595.5] 20 Claims
OG exemplary drawing
 
1. A method for producing an electrode active material having the general formula
AaMb(XY4)cZd,
wherein
(i) A is Li or a mixture of Li with an alkali metal selected from the group consisting of Na, K, and mixtures thereof, and 0<a≤9;
(ii) M is one or more metals, comprising at least one metal which is capable of undergoing oxidation to a higher valence state, and 1≤b≤3;
(iii) XY4 is selected from the group consisting of X′O4-xY′x, X′O4-yY′2y, mixtures thereof, and mixtures thereof with X″S4, where X′ is P or a mixture of P with an element selected from the group consisting of As, Sb, Si, Ge, V, S, and mixtures thereof; X″ is P or a mixture of P with an element selected from the group consisting of As, Sb, Si, Ge, V and mixtures thereof; Y′ is selected from the group consisting of halogen, S, N, and mixtures thereof; 0≤x<3; and 0<y≤2; and 0<c≤3;
(iv) Z is OH, halogen, or mixtures thereof, and 0≤d≤6; and
(v) M, XY4, Z, a, b, c, d, x and y are selected so as to maintain electroneutrality of said compound;
said method comprising:
a) forming a first mixture comprising (i) a lithium hydrogen phosphate having a first average particle size, and (ii) a first metal hydroxide having a second average particle size, wherein said first average particle size is between about 70 times and 110 times greater than said second average particle size;
b) grinding said first mixture in a jet mill to form a milled lithium hydrogen phosphate;
c) reacting starting materials comprising said milled lithium hydrogen phosphate to produce said active material, wherein said starting materials comprise at least one source of alkali metal A, at least one source of metal M, at least one source of XY4, and, if d>0, at least one source of halide or hydroxide Z.