APPROACH FOR MANUFACTURING EFFICIENT MESOPOROUS NANO-COMPOSITE POSITIVE ELECTRODE LiMn1-XFeXPO4 MATERIALS

Patent metadata

Field	Value
Publication number	US-2016308212-A1
Application number	US-201615198323-A
Country	US
Kind code	A1
Filing date	Jun 30, 2016
Priority date	Jun 27, 2011
Publication date	Oct 20, 2016
Grant date	—

Abstract

A mesoporous nano-composite LiMn 1-x Fe x PO 4 (0≦x≦1) particle that has a uniform carbon coating on the surface of the particle. Also disclosed is a mesoporous nano-composite LiMn 1-x Fe x PO 4 particle prepared by a process including steps: (i) providing a mixture of a soft-template compound, a lithium ion-containing compound, an iron ion-containing compound, a manganese ion-containing compound, and a phosphate ion-containing compound in a solvent; (2) removing the solvent to obtain a LiMn 1-x Fe x PO 4 precursor; and (3) calcining the precursor followed by milling and annealing to obtain the LiMn 1-x Fe x PO 4 particle.

First claim

1 . A mesoporous nano-composite particle, comprising:
phospho-olivine LiMn 1-x Fe x PO 4 crystals forming a grain, in which 0≦x≦1, and a uniform carbon coating on the surface of the grain, the coating having an average thickness of 1 to 10 nm, wherein the particle has a particle size of 10 to 100 nm, a surface area of 30 to 50 m 2 g −1 , and a pore size of 3 to 40 nm.

2 . The particle of claim 1 , wherein the particle has a particle size of 50 to 80 nm, a surface area of 40 to 50 m 2 g 1 , and a pore size of 3 to 30 nm, and the carbon coating has an average thickness of 3 to 7 nm.

3 . The particle of claim 1 , wherein the carbon coating is formed of conductive carbon selected from the group consisting of acetylene black, conductive carbon black, carbon nanotubes, and graphitic nano-sheets.

4 . The particle of claim 3 , wherein the conductive carbon is conductive carbon black selected from the group consisting of Printex XE2, Black Pearls 2000, and Ketjenblack.

5 . The particle of claim 2 , wherein the carbon coating is formed of conductive carbon selected from the group consisting of acetylene black, conductive carbon black, carbon nanotubes, and graphitic nano-sheets.

6 . The particle of claim 5 , wherein the conductive carbon is conductive carbon black selected from the group consisting of Printex XE2, Black Pearls 2000, and Ketjenblack.

7 . The particle of claim 1 , wherein x is 0, 0.2, 0.5, or 0.8.

8 . The particle of claim 7 , wherein the particle has a particle size of 50 to 80 nm, a surface area of 40 to 50 m 2 g −1 , and a pore size of 3 to 30 nm, and the carbon coating has an average thickness of 3 to 7 nm.

9 . The particle of claim 7 , wherein the carbon coating is formed of conductive carbon selected from the group consisting of acetylene black, conductive carbon black, carbon nanotubes, and graphitic nano-sheets.

10 . The particle of claim 1 , wherein 0<x<1.

11 . The particle of claim 10 , wherein the particle has a particle size of 50 to 80 nm, a surface area of 40 to 50 m 2 g −1 , and a pore size of 3 to 30 nm, and the carbon coating has an average thickness of 3 to 7 nm.

12 . The particle of claim 10 , wherein the carbon coating is formed of conductive carbon selected from the group consisting of acetylene black, conductive carbon black, carbon nanotubes, and graphitic nano-sheets.

13 . The particle of claim 12 , wherein the conductive carbon is conductive carbon black selected from the group consisting of Printex XE2, Black Pearls 2000, and Ketjenblack.

14 . The particle of claim 11 , wherein the carbon coating is formed of conductive carbon selected from the group consisting of acetylene black, conductive carbon black, carbon nanotubes, and graphitic nano-sheets.

15 . The particle of claim 14 , wherein the conductive carbon is conductive carbon black selected from the group consisting of Printex XE2, Black Pearls 2000, and Ketjenblack.

16 . The particle of claim 10 , wherein x is 0.2, 0.5, or 0.8.

17 . The particle of claim 16 , wherein the particle has a particle size of 50 to 80 nm, a surface area of 40 to 50 m 2 g −1 , and a pore size of 3 to 30 nm, and the carbon coating has an average thickness of 3 to 7 nm.

18 . The particle of claim 16 , wherein the carbon coating is formed of conductive carbon selected from the group consisting of acetylene black, conductive carbon black, carbon nanotubes, and graphitic nano-sheets.

19 . The particle of claim 18 , wherein the conductive carbon is conductive carbon black selected from the group consisting of Printex XE2, Black Pearls 2000, and Ketjenblack.

20 . A mesoporous nano-composite LiMn 1-x Fe x PO 4 particle, wherein the particle is prepared by a process including the following steps:
providing a solvent containing a soft-template compound, a lithium ion-containing compound, an iron ion-containing compound, a manganese ion-containing compound, and a phosphate ion-containing compound; removing the solvent to obtain a LiMn 1-x Fe x PO 4 precursor; calcining the LiMn 1-x Fe x PO 4 precursor to obtain crystalline LiMn 1-x Fe x PO 4 grains; milling the crystalline LiMn 1-x Fe x PO 4 grains in the presence of conductive carbon to obtain nanostructured LiMn 1-x Fe x PO 4 /C particles; and annealing the nanostructured LiMn 1-x Fe x PO 4 /C particles to obtain nano-composite LiMn 1-x Fe x PO 4 /C particles,
wherein the amounts of the lithium ion-containing compound, the ferrous ion-containing compound, the manganese ion-containing compound, and the phosphate ion-containing compound are in stoichiometric proportion; and the weight ratio of the soft-template compound to the lithium ion-containing compound is 1:1 to 10:1.

Assignees

• Nat Univ Singapore

Inventors

• Balaya Palani
• Ramar Vishwanathan

Classifications

• Y02E60/10

  Energy storage using batteries · CPC title

• H01M4/366

  as layered products · CPC title

• H01M4/0471

  involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis · CPC title

• C01B25/45

  containing plural metal, or metal and ammonium · CPC title

• H01M2004/028

  Positive electrodes · CPC title