Production method of battery active material, battery active material, nonaqueous electrolyte battery and battery pack

Patent metadata

Field	Value
Publication number	US-10629901-B2
Application number	US-201715645675-A
Country	US
Kind code	B2
Filing date	Jul 10, 2017
Priority date	Nov 8, 2013
Publication date	Apr 21, 2020
Grant date	Apr 21, 2020

Abstract

A production method of a battery active material of the present embodiment includes a step of obtaining a coprecipitated product containing Ti and Nb by mixing a solution with a pH of 5 or lower, in which a Ti compound is dissolved, and a solution with a pH of 5 or lower, in which a Nb compound is dissolved, such that molar ratio of Ti and Nb (Nb/Ti) is adjusted within a range of 1≤Nb/Ti≤28, and then further mixing with an alkali solution with a pH of 8 or higher; and a step of burning the coprecipitated product under condition of 635° C. or higher and 1200° C. or lower.

First claim

The invention claimed is:

1. A production method of a battery active material, the method comprising:
mixing a first solution with a pH of 5 or lower, in which a Ti compound is dissolved, and a second solution with a pH of 5 or lower, in which a Nb compound is dissolved to form a mixture, such that a molar ratio of Ti and Nb (Nb/Ti) in the mixture is adjusted within a range of 1≤Nb/Ti≤28, and then further adding to the mixture an alkali solution with a pH of 8 or higher; thereby obtaining a coprecipitated product comprising Ti and Nb and
burning the coprecipitated product at a burning temperature of 635° C. or higher and 1200° C. or lower,
wherein the battery active material obtained by the burning is represented by formula (1):
Ti x-a M1 a Nb y-b M2 b O z   (1)

wherein, z=2(x+a)+2.5(y+b) is satisfied; x, y, a, b and z respectively satisfy 1≤(y−b)/(x−a)≤28, 0<x≤1, 0<y≤1, 0≤a≤0.1 and 0≤b≤0.1; and
M1 and M2 each independently represents one, or two or more elements selected from the group consisting of Ti, Nb, Zr, B, Na, Mg, Al, Si, S, P, K, Ca, Mo, W, Cr, Mn, Co, Ni and Fe.

2. The production method according to claim 1 , wherein a burning time of the burning is 30 seconds or more and 12 hours or less.

3. The production method according to claim 1 , wherein the Ti compound is any of titanyl sulfate, titanium oxide, titanium ammonium oxalate, metatitanic acid, isopropyl titanate and titanium chloride.

4. The production method according to claim 3 , wherein the Nb compound is any of niobium chloride, niobium hydroxide, ammonium niobium oxalate, niobium oxide and niobium ethoxide.

5. The production method according to claim 4 , further comprising adding a carbon source to the battery active material obtained after the burning, and then additionally burning the battery active material and the carbon source in a reducing atmosphere.

6. The production method according to claim 1 , wherein the Nb compound is any of niobium chloride, niobium hydroxide, ammonium niobium oxalate, niobium oxide and niobium ethoxide.

7. The production method according to claim 1 , further comprising adding a carbon source to the battery active material obtained after the burning, and then additionally burning the battery active material and the carbon source in a reducing atmosphere.

8. The production method according to claim 1 , wherein M1 and M2 each independently represents one or two elements selected from the group consisting of Ti and Nb.

9. A production method of a battery active material comprising:
obtaining a coprecipitated product comprising Ti and Nb by mixing a solution, in which a Ti compound and a Nb compound are dissolved, a molar ratio of Ti and Nb (Nb/Ti) is adjusted within a range of 1≤Nb/Ti≤28, and a pH of the solution is adjusted to 5 or lower, with an alkali solution with a pH of 8 or higher; and
burning the coprecipitated product at a burning temperature of 635° C. or higher and 1200° C. or lower,
wherein a composition of the battery active material obtained by the burning is represented by formula (1):
Ti x-a M1 a Nb y-b M2 b O z   (1)

wherein, z=2(x+a)+2.5(y+b) is satisfied; x, y, a, b and z respectively satisfy 1≤(y−b)/ (x−a)≤28, 0<x≤1, 0<y≤1, 0≤a≤0.1 and 0≤b≤0.1; M1 and M2 each independently represents one, or two or more elements selected from the group consisting of Ti, Nb, Zr, B, Na, Mg, Al, Si, S, P, K, Ca, Mo, W, Cr, Mn, Co, Ni and Fe.

10. The production method according to claim 9 , wherein a burning time of the burning is 1 hour or more and 12 hours or less.

11. The production method according to claim 9 , wherein the Ti compound is any of titanyl sulfate, titanium oxide, titanium ammonium oxalate, metatitanic acid, isopropyl titanate and titanium chloride.

12. The production method according to claim 9 , wherein the Nb compound is any of niobium chloride, niobium hydroxide, ammonium niobium oxalate, niobium oxide and niobium ethoxide.

13. The production method according to claim 9 , wherein a carbon source is added to the battery active material obtained after the burning, and then burning is further carried out in a reducing atmosphere.

Assignees

• Toshiba Kk

Inventors

• Ise Kazuki
• Harada Yasuhiro
• Takami Norio

Classifications

• C01P2002/52

  containing elements as dopants · CPC title

• H01M10/052

  Li-accumulators · CPC title

• C01P2002/72

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

• C01P2002/77

  by unit-cell parameters, atom positions or structure diagrams · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title