Method for manufacturing a lithium transition metal phosphate

Patent metadata

Field	Value
Publication number	US-9537149-B2
Application number	US-201113695342-A
Country	US
Kind code	B2
Filing date	Apr 20, 2011
Priority date	Apr 30, 2010
Publication date	Jan 3, 2017
Grant date	Jan 3, 2017

Abstract

Disclosed is a method for manufacturing a lithium transition metal phosphate. The disclosed method for manufacturing a lithium transition metal phosphate comprises the steps of: injecting reaction materials containing lithium, a transition metal, and a phosphate, into a reactor, and mixing the raw materials at the molecular level in the reactor; and allowing the reaction materials to chemically react in the reactor so as to cause nucleation.

First claim

The invention claimed is:

1. A method of preparing lithium transition metal phosphate, the method comprising:
feeding reactants comprising an acidic source material and a basic source material into a reactor, and mixing the reactants at a molecular level in the reactor;
generating a crystal nucleus by chemically reacting the reactants in the reactor, wherein a time (T M ) taken to mix the reactant at the molecular level is shorter than a time (T N ) taken to generate the crystal nucleus, and T M is in a range of 10 to 100 μs and T N is 1 ms or less;
growing the crystal nucleus into a nano-sized crystal to obtain a slurry comprising a lithium transition metal phosphate; and then
filtering, washing, drying and/or heating the slurry to prepare a nanoparticle lithium transition metal phosphate,
wherein the acidic source material is fed into the reactor through a first source material feeding line and the basic source material is fed into the reactor through a second source material feeding line,
wherein the acidic source material comprises lithium, a transition metal, and phosphoric acid, and the basic source material comprises an inorganic base; the acidic source material comprises a transition metal and phosphoric acid, and the basic source material comprises lithium; the acidic source material comprises lithium and phosphoric acid, and the basic source material comprises a transition metal; or the basic source material comprises lithium and a transition metal, and the acidic source material comprises phosphoric acid,
wherein the reactor is a high gravity rotating packed bed reactor including:
a chamber that defines an inner space;
a permeable packed bed that is rotatable, is disposed inside the chamber, and is filled with a porous filler;
at least one source material feeding line through which the reactants are fed into the inner space; and
a slurry outlet through which a slurry is discharged from the inner space.

2. The method of claim 1 , wherein the transition metal comprises at least one selected from the group consisting of Fe, Mn, Co, and Ni.

3. The method of claim 1 , wherein the chemical reaction is an acid-base reaction.

4. The method of claim 1 , wherein the reactants are fed in at least one of a solution form and a suspension form into the reactor.

5. The method of claim 1 , wherein an inner temperature of the reactor is maintained in a range of 0 to 90° C.

6. The method of claim 1 , wherein a molar ratio of lithium and the transition metal to the phosphoric acid ((Li+M)/phosphoric acid) in the reactants is in a range of about 1.5 to about 2.5.

7. The method of claim 1 , wherein a retention time of the reactants in the reactor is in a range of 1 ms to 10s.

8. The method of claim 1 , wherein a centrifugal acceleration of the permeable packed bed is in a range of 10 to 100,000 m/s 2 .

9. The method of claim 1 , wherein the lithium transition metal phosphate has an olivine type crystal structure.

Assignees

• Kim Chun Joong
• Park Yun Jung
• Chang Dong Gyu
• Park Ji Ho
• Yang Woo Young
• Samsung Sdi Co Ltd

Inventors

• Kim Chun Joong
• Park Yun Jung
• Chang Dong Gyu
• Park Ji Ho
• Yang Woo Young

Classifications

• C01B25/45 Primary

  containing plural metal, or metal and ammonium · CPC title

• B01J8/10

  moved by stirrers or by rotary drums or rotary receptacles {or endless belts} · CPC title

• H01M4/5825 Primary

  Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title