Lithium transition metal phosphate, method for producing same, and lithium secondary battery produced using same

Patent metadata

Field	Value
Publication number	US-10020509-B2
Application number	US-201415109417-A
Country	US
Kind code	B2
Filing date	Aug 14, 2014
Priority date	Dec 30, 2013
Publication date	Jul 10, 2018
Grant date	Jul 10, 2018

Abstract

The present invention relates to a lithium transition metal phosphate including nano rod-like Fe 2 P crystals, a method of preparing the same, and a lithium secondary battery manufactured by using the lithium transition metal phosphate. According to the present invention, a lithium transition metal phosphate including nano rod-like Fe 2 P crystals may be provided, thereby enhancing high rate capability and low-temperature properties of a lithium secondary battery prepared by using the same. Further, the whole or a part of an airflow direction in a firing furnace may be controlled to be in a direction opposite to a proceeding direction of a fired raw material by adjusting the exhaust conditions in the firing process, thereby providing a method of preparing a lithium transition metal phosphate, in which the nano rod-like Fe 2 P crystals are reproducibly included.

First claim

What is claimed is:

1. A lithium transition metal phosphate represented by the following Formula 1, which comprises nano rod-like Fe 2 P crystals, a nano rod-like Fe2P crystal of the crystals having a length in a range from 1 μm to 10 μm and a ratio of length to thickness in a range from 1 to 200:
LiFe x M 1−x PO 4   Formula 1

(where 0 <X ≤1, and M is one or more selected from Ni, Mn, Co, V, Cr, Cu, Ti, and Zr).

2. The lithium transition metal phosphate of claim 1 , wherein the nano rod-like Fe 2 P crystal has a thickness in a range from 50 nm to 1 μm.

3. The lithium transition metal phosphate of claim 1 , wherein the lithium transition metal phosphate has diffraction peaks at a diffraction angle (2θ) in ranges from 40° to 40.5° and from 47° to 47.5°, respectively, in the X-ray diffraction (XRD) measurement.

4. The lithium transition metal phosphate of claim 1 , wherein the lithium transition metal phosphate is in the form of secondary particles that are formed by aggregation of primary particles.

5. The lithium transition metal phosphate of claim 4 , wherein the secondary particles have a specific surface area in a range from 20 m 2 /g to 80 m 2 /g.

6. A method of preparing a lithium transition metal phosphate represented by the following Formula 1, the method comprising a firing process performed by heat-treating while transferring a raw material in a firing furnace, in which a temperature-elevation interval, a retention interval, and a cooling interval are sequentially provided, wherein each interval comprises one exhaust port or a plurality of exhaust ports, wherein the whole or a part of an airflow direction in the firing furnace is in a direction opposite to a transferring direction of the fired raw material by adjusting an exhaust amount of the plurality of exhaust ports:
LiFe x M 1−x PO 4   Formula 1

(where 0 <X ≤1, and M is one or more selected from Ni, Mn, Co, V, Cr, Cu, Ti, and Zr).

7. The method of claim 6 , wherein the lithium transition metal phosphate comprises Fe 2 P crystals having diffraction peaks at a diffraction angle (2θ) in ranges from 40° to 40.5° and from 47° to 47.5°, respectively, in the X-ray diffraction (XRD) measurement.

8. The method of claim 6 , wherein when a starting point of the temperature-elevation interval is set to I point, and a final point of the retention interval (a point where the retention interval and the cooling interval meet) is set to II point, each exhaust amount of the plurality of the exhaust ports is adjusted so as to satisfy one of the following Equations (1) to (6):
X >Y  (1)

Y >Z  (2)

X >Z  (3)

X ≥Y >Z  (4)

X >Y ≥Z  (5)

Y >X ≥Z  (6)

(where X is an exhaust amount of an exhaust port disposed relatively close to I point, Z is an exhaust amount of an exhaust port disposed relatively close to II point, and Y is an exhaust amount of an exhaust port positioned between the X and Z measurement exhaust ports).

9. The method of claim 6 , wherein airflow in the firing furnace is allowed to proceed in a direction of the temperature-elevation interval in the retention interval by adjusting the total exhaust amount of the temperature-elevation interval to be larger than the total exhaust amount of the retention interval.

10. The method of claim 6 , wherein a heat-treatment temperature in the retention interval is in a range from 600° C. to 900° C.

11. The method of claim 6 , wherein the heat-treatment is performed under a reduction atmosphere using H 2 , N 2 , and a mixed gas thereof, wherein H 2 and N 2 are introduced at a rate in a range from 5 to 50 L/min and at a rate in a range from 250 to 295 L/min, respectively.

Assignees

• Samsung Sdi Co Ltd

Inventors

• Shin Jae Seung
• Kim Jong Min
• Chang Dong Gyu
• Song Hyun A

Classifications

• C01P2006/12

  Surface area · CPC title

• Y02E60/122

  Cross-Sectional Technologies · mapped topic

• H01M4/623

  fluorinated polymers · CPC title

• H01M4/661

  Metal or alloys, e.g. alloy coatings (H01M4/669 take precedence) · CPC title

• C01B25/45

  containing plural metal, or metal and ammonium · CPC title