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Li-ni-based composite oxide particles for non-aqueous electrolyte secondary battery, process for producing the same, and non-aqueous electrolyte secondary battery

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Li-ni-based composite oxide particles for non-aqueous electrolyte secondary battery, process for producing the same, and non-aqueous electrolyte secondary battery


The present invention relates to Li—Ni-based composite oxide particles comprising Mn, and Co and/or Al, wherein Co and Al are uniformly dispersed within the particles, and Mn is present with a gradient of its concentration in a radial direction of the respective particles such that a concentration of Mn on a surface of the respective particles is higher than that at a central portion thereof. The Li—Ni-based composite oxide particles can be produced by allowing an oxide and a hydroxide comprising Mn to mechanically adhere to Li—Ni-based oxide comprising Co and/or Al; and then heat-treating the obtained material at a temperature of not lower than 400° C. and not higher than 1,000° C. The Li—Ni-based composite oxide particles of the present invention are improved in thermal stability and alkalinity.
Related Terms: Electrolyte Radial Direction

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USPTO Applicaton #: #20130330626 - Class: 429223 (USPTO) - 12/12/13 - Class 429 
Chemistry: Electrical Current Producing Apparatus, Product, And Process > Current Producing Cell, Elements, Subcombinations And Compositions For Use Therewith And Adjuncts >Electrode >Chemically Specified Inorganic Electrochemically Active Material Containing >Nickel Component Is Active Material



Inventors: Akihisa Kajiyama, Kazuhiko Kikuya, Teruaki Santoki, Osamu Sasaki, Satoshi Nakamura, Taiki Imahashi, Hideaki Sadamura

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The Patent Description & Claims data below is from USPTO Patent Application 20130330626, Li-ni-based composite oxide particles for non-aqueous electrolyte secondary battery, process for producing the same, and non-aqueous electrolyte secondary battery.

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This application is a divisional of application Ser. No. 12/742,125 filed Aug. 20, 2010, now allowed, which in turn is the U.S. national phase of International Application No. PCT/JP2008/003259, filed 11 Nov. 2008, which claims priority to Japanese Application No. 2007-293767, filed 12 Nov. 2007, the entire contents of each of which are hereby incorporated by reference.

TECHNICAL FIELD

The present invention relates to Li—Ni-based composite oxide particles for a non-aqueous electrolyte secondary battery which exhibit a large charge/discharge capacity and are excellent in thermal stability upon charging.

BACKGROUND ART

With the recent rapid development of portable and cordless electronic devices such as audio-visual (AV) devices and personal computers, there is an increasing demand for secondary batteries or batteries having a small size, a light weight and a high energy density as a power source for driving these electronic devices. Also, in consideration of global environments, electric cars and hybrid cars have been recently developed and put into practice, so that there is an increasing demand for lithium ion secondary batteries for large size applications having excellent storage characteristics. Under these circumstances, the lithium ion secondary batteries having advantages such as a large charge/discharge capacity and good storage characteristics have been noticed.

Hitherto, as positive electrode active substances useful for high energy-type lithium ion secondary batteries exhibiting a 4 v-grade voltage, there are generally known LiMn2O4 having a spinel structure, LiMnO2 having a zigzag layer structure, LiCoO2 and LiNiO2 having a layer rock-salt structure, or the like. Among the secondary batteries using these active substances, lithium ion secondary batteries using LiNiO2 have been noticed because of a large charge/discharge capacity thereof. However, this material tends to be deteriorated in thermal stability upon charging and charge/discharge cycle durability, and, therefore, it has been required to further improve properties thereof.

Specifically, when lithium is released from LiNiO2, the crystal structure of LiNiO2 suffers from Jahn-Teller distortion since Ni3+ is converted into Ni4+. When the amount of Li released reaches 0.45, the crystal structure of such a lithium-released region of LiNiO2 is transformed from hexagonal system into monoclinic system, and a further release of lithium therefrom causes transformation of the crystal structure from monoclinic system into hexagonal system. Therefore, when the charge/discharge reaction is repeated, the crystal structure of LiNiO2 tends to become unstable, so that the resulting secondary battery tends to be deteriorated in cycle characteristics or suffer from occurrence of undesired reaction between LiNiO2 and an electrolyte solution owing to release of oxygen therefrom, resulting in deterioration in thermal stability and storage characteristics of the cell. To solve these problems, various studies have been made on materials to which Co and Al to are added by substituting a part of Ni in LiNiO2 therewith. However, these materials have still failed to solve the above-described problems. Therefore, it has still been required to provide an Li—Ni-based composite oxide having a higher crystallinity.

Further, in the process for producing the Li—Ni-based composite oxide, in order to obtain the Li—Ni-based composite oxide having a high packing property and a stable crystal structure, it is required to use Ni composite hydroxide particles which are well controlled in properties, crystallinity and contents of impurities, and calcine the particles under the condition which is free from inclusion of Ni2+ into Li sites thereof.

More specifically, it is required to provide Li—Ni-based composite oxide capable of exhibiting a high packing property, a stable crystal structure and an excellent thermal stability upon charging as a positive electrode active substance for a non-aqueous electrolyte secondary battery.

In order to improve the above thermal stability, it is important to suppress a reaction between oxygen released from the composite oxide and an electrolyte solution. Although the Li—Ni-based composite oxide produces Ni4+ in a charged condition of the cell, the Ni ion in such an oxidized state is very unstable. As a result, oxygen tends to be readily released from the composite oxide, so that Ni4+ tends to be reduced into Ni3+ or Ni2+. For this reason, when using the composite oxide as a positive electrode active substance for the lithium secondary battery, problems concerning a thermal stability of the secondary battery such as generation of heat and firing tend to be caused in a charged condition of the cell.

In addition, it is considered that the problems concerning a thermal stability of the lithium secondary battery, in particular, generation of heat and firing, are caused at a solid-liquid boundary between the electrode active substance and the electrolyte solution as a starting point.

In view of these facts, in order to improve a thermal stability of the Li—Ni-based composite oxide, it is considered to be effective that the contact surface thereof with the electrolyte solution, i.e., the surface of the respective particles, is coated with other stable elements.

Hitherto, in order to improve various properties of LiNiO2 particles such as stabilization of a crystal structure and charge/discharge cycle characteristics, various improving methods have been attempted. For example, it is known that the surface of the respective Li—Ni-based oxide particles is coated with a compound such as lithium manganate (Patent Documents 1 to 5).

The safety of lithium ion cells becomes more and more important. For this reason, the studies on surface modification of active substance particles by noticing an interfacial reaction thereof during charging and discharging of the cells have been made as to various materials. For example, there are known many techniques using an Li—Co-based composite oxide as a core material (Japanese Patent Application Laid-Open (KOKAI) Nos. 2006-331939 and 2007-18743) or using an Li—Mn-based spinel oxide as a core material (Japanese Patent Application Laid-Open (KOKAI) No. 11-71114 (1999)). However, in any of these conventional techniques, from the viewpoint of a thermal stability, the core materials used therein are inherently stable. Therefore, the surface modification of the core particles mainly aims at preventing deterioration in cycle characteristics of the cells.

In the present invention, an Li—Ni-based composite oxide is used as the core material, and an object of the present invention is not to improve the cycle characteristics, but to solve the problems concerning a thermal stability peculiar to the Li—Ni-based composite oxide. Patent Document 1: Japanese Patent Application Laid-open (KOKAI) No. 7-235292 Patent Document 2: Japanese Patent Application Laid-open (KOKAI) No. 9-265985 Patent Document 3: Japanese Patent Application Laid-open (KOKAI) No. 10-236826 Patent Document 4: Japanese Patent Application Laid-open (KOKAI) No. 11-67209 Patent Document 5: Japanese Patent Application Laid-open (KOKAI) No. 2007-213866

DISCLOSURE OF THE INVENTION

Problem to be Solved by the Invention

At present, it has been strongly required to provide the Li—Ni-based composite oxide particles as a positive electrode active substance for a non-aqueous electrolyte secondary battery which is improved in thermal stability upon charging. However, the Li—Ni-based composite oxide capable of fully satisfying the above requirement has not been obtained until now.

In the above Patent Document 1 (Japanese Patent Application Laid-Open (KOKAI) No. 7-235292), it is described that the surface of the respective lithium nickelate particles is coated with lithium cobaltate or lithium manganate. However, the resulting particles tend to fail to exhibit a sufficient thermal stability.

Also, in the above Patent Document 2 (Japanese Patent Application Laid-Open (KOKAI) No. 9-265985, LiNiO2 is used as the core material. However, the present invention is different from the Patent Document 2 in that different kinds of metal elements are incorporated into the core material of the present invention to form a solid solution therewith for the purpose of enhancing properties of the core material itself.

In addition, in the above Patent Document 3 (Japanese Patent Application Laid-Open (KOKAI) No. 10-236826) and Patent Document 4 (Japanese Patent Application Laid-Open (KOKAI) No. 11-67209), the Li—Ni-based composite oxide is coated with the Li—Co-based composite oxide to improve an initial capacity and cycle properties of the resulting cell. However, the material of the coating layer used in these Patent Documents is constituted of the Li—Co-based composite oxide as a main component and, therefore, different from the material used in the present invention which is constituted of the Li—Ni-based composite oxide as a main component.

Further, in the above Patent Document 5 (Japanese Patent Application Laid-Open (KOKAI) No. 2007-213866), the Li—Ni-based composite oxide as a core material is coated with a different kind of material. However, the coating layer has an Li—Mn spinel crystal structure for the purpose of obtaining an active substance having a high output. On the other hand, in the present invention, for the purpose of enhancing mainly a thermal stability, the coating layer formed therein is different in crystal structure from that of the Patent Document 5, i.e., the coating layer of the present invention is not mainly constituted of the spinel layer.

Means for Solving the Problem

That is, according to the present invention, there are provided Li—Ni-based composite oxide particles comprising Mn, and Co and/or Al,

Co and Al being present within the particles,

Mn being present with a gradient of its concentration in a radial direction of the respective particles, and

a concentration of Mn on a surface of the respective particles being higher than that at a central portion thereof (Invention 1).

Also, according to the present invention, there are provided Li—Ni-based composite oxide particles comprising secondary particles of Li—Ni-based oxide particles,

Co and/or Al being present therewithin,

Li—Mn-based composite oxide being present on a surface of the respective secondary particles, and

a concentration of Mn being increased from a center toward a surface of the respective particles (Invention 2).

Also, according to the present invention, there are provided the Li—Ni-based composite oxide particles as described in the above Invention 2, wherein the secondary particles of the Li—Ni-based oxide particles as core particles have a composition represented by the formula:

Lix1(Ni1-y1-z1-w1Coy1Mnz1M1w1)O2

(where x1, y1, z1 and w1 satisfy 0.9≦x1≦1.3, 0.1≦y1≦0.3, 0.0≦z1≦0.3 and 0≦w1≦0.1, respectively; and M1 is at least one metal selected from the group consisting of Al, Fe, Mg, Zr, Ti and B) (Invention 3).

Also, according to the present invention, there are provided the Li—Ni-based composite oxide particles as described in the above Invention 2 or 3, wherein the Li—Mn-based composite oxide has a composition represented by the formula:

Lix2(Mn1-z2M2z2)y2O2

(where M2 is at least one metal selected from the group consisting of Co, Ni, Al, Fe, Mg, Zr, Ti and B; and x2, y2 and z2 satisfy 1/2<x2≦4/3, 2/3≦y2≦1 and 0≦z2<4/5, respectively) (Invention 4).

Also, according to the present invention, there are provided the Li—Ni-based composite oxide particles as described in any one of the above Inventions 1 to 4, wherein a suspension prepared by suspending the Li—Ni-based composite oxide particles in distilled water has a pH value of not more than 11.5 as measured after allowing the suspension to stand at room temperature (Invention 5).

In addition, according to the present invention, there is provided a process for producing the Li—Ni-based composite oxide particles as described in any one of the above Inventions 1 to 5, comprising the steps of allowing an oxide and/or a hydroxide which comprise Mn to mechanically adhere to an Li—Ni-based oxide comprising Co and/or Al; and then heat-treating the obtained material at a temperature of not lower than 400° C. and not higher than 1,000° C. (Invention 6).

Also, according to the present invention, there is provided a process for producing the Li—Ni-based composite oxide particles as described in any one of the above Inventions 1 to 5, comprising the steps of allowing an oxide and/or a hydroxide which comprise Mn to mechanically adhere to an Ni-based hydroxide comprising Co and/or Al; mixing the obtained material with a lithium compound; and then heat-treating the obtained mixture at a temperature of not lower than 700° C. and not higher than 1,000° C. in an oxygen-containing atmosphere (Invention 7).

Also, according to the present invention, there is provided a process for producing the Li—Ni-based composite oxide particles as described in any one of the above Inventions 1 to 5, comprising the steps of dropping a manganese-containing solution and an alkali solution to a suspension of Ni-based hydroxide particles comprising Co and/or Al to produce a manganese-containing hydroxide, a manganese-containing oxide hydroxide or a manganese-containing oxide on a surface of a nickel oxide; subjecting the obtained material to washing with water and drying; mixing the dried material with a lithium compound; and then heat-treating the obtained mixture at a temperature of not lower than 700° C. and not higher than 1,000° C. in an oxygen-containing atmosphere (Invention 8).

Further, according to the present invention, there is provided a non-aqueous electrolyte secondary battery comprising the Li—Ni-based composite oxide particles as described in any one of the above Inventions 1 to 5, as a positive electrode active substance (Invention 9).

Also, according to the present invention, there is provided the non-aqueous electrolyte secondary battery as described in the above Invention 9, wherein when using a negative electrode comprising a material capable of absorbing and desorbing a metallic lithium or a lithium ion, an exothermic peak temperature as measured by differential thermal analysis at a positive electrode under the condition in which the cell is charged to 4.5 V is not lower than 240° C. (Invention 10).

Effect of the Invention

In the Li—Ni-based composite oxide particles according to the present invention, when a negative electrode formed from a material capable of absorbing and desorbing a metallic lithium or a lithium ion is used in a cell using the composite oxide particles, an exothermic maximum peak temperature of the cell as measured in the range of 200 to 290° C. by differential thermal analysis under the condition that the cell is charged to 4.5 V is shifted to a high-temperature side. As a result, it is possible to enhance a safety of the lithium ion cell.

In addition, the Li—Ni-based composite oxide particles according to the present invention can exhibit a high discharge capacity at a charge/discharge rate of 0.2 mA/cm2 irrespective of a high thermal safety thereof.

Further, in the Li—Ni-based composite oxide particles according to the present invention, when an Li—Mn-based composite oxide is coated or allowed to be present on or in the vicinity of the surface of respective secondary particles of the Li—Ni-based oxide forming core particles by subjecting these materials to a wet chemical treatment or a dry mechanical treatment, or to further a thermal treatment in addition to the wet or dry treatment, it is possible to produce Li—Ni-based composite particles which can be enhanced in safety upon charging while keeping a high capacity.

Therefore, the Li—Ni-based composite oxide particles according to the present invention are suitable as a positive electrode active substance for a non-aqueous electrolyte secondary battery.

BRIEF DESCRIPTION OF THE DRAWING

FIG. 1 is a photograph showing a compositional distribution of a section of the respective Li—Ni-based composite oxide particles obtained in Example 1.

PREFERRED EMBODIMENT FOR CARRYING OUT THE INVENTION

The present invention is described in detail below.

First, the Li—Ni-based composite oxide particles for a non-aqueous electrolyte secondary battery according to the present invention are described.

In the Li—Ni-based composite oxide particles for a non-aqueous electrolyte secondary battery according to the present invention, an Li—Mn-based composite oxide is coated or allowed to be present on or in the vicinity of the surface of respective secondary particles of an Li—Ni-based composite oxide having a specific composition which form core particles. More specifically, the Li—Ni-based composite oxide particles according to the present invention are intended to involve not only those obtained by coating a whole surface of the secondary particles as the core particles with the Li—Mn-based composite oxide having a specific composition, but also those obtained by allowing the Li—Mn-based composite oxide having a specific composition to be present or adhere in the vicinity of the surface of the secondary particles as the core particles or onto a part of the surface thereof.

The Li—Ni-based oxide forming the core particles preferably has a composition represented by the formula:

Lix1(Ni1-y1-z1-w1Coy1Mnz1M1w1)O2

(where x1, y1, z1 and w1 satisfy 0.9≦x1≦1.3, 0.1≦y1≦0.3, 0.0≦z1≦0.3 and 0≦w1≦0.1, respectively; and M1 is at least one metal selected from the group consisting of Al, Fe, Mg, Zr, Ti and B). When the composition of the Li—Ni-based oxide forming the core particles is out of the above-specified range, it may be difficult to attain a high discharge capacity as a feature of the Li—Ni-based oxide.

The particles which are coated or allowed to be present on the core particles have a composition represented by the formula:

Lix2(Mn1-z2M2z2)y2O2

(where M2 is at least one metal selected from the group consisting of Co, Ni, Al, Fe, Mg, Zr, Ti and B; x2, y2 and z2 satisfy 1/2<x2≦4/3, 2/3≦y2<1 and 0≦z2≦4/5, respectively. When the composition of the above particles is out of the above-specified range, the thermal stability upon charging may be deteriorated.

In the Li—Ni-based composite oxide particles according to the present invention, the concentration of Mn is increased from a center toward the surface of the respective particles. When the concentration of Mn is uniform over a whole part of the respective secondary particles, it may be difficult to achieve enhancement in a thermal stability thereof while keeping a high cell capacity of the secondary particles as core particles, as aimed by the present invention. In addition, when the concentration of Mn at a central portion of the respective particles is higher than that in a surface portion of the respective secondary particles, it may also be difficult to achieve enhancement in a thermal stability thereof while keeping a high cell capacity of the secondary particles as core particles, as aimed by the present invention.

The content of the Li—Mn composite oxide which is coated on the secondary particles of the Li—Ni-based oxide forming the core particles is preferably not less than 0.3% by weight and not more than 20% by weight based on the weight of the Li—Ni oxide. When the content of the Li—Mn composite oxide particles which are coated or allowed to be present on the core particles is less than 0.3% by weight, the resulting particles tend to be deteriorated in thermal stability under a charged condition of the cell although they maintain a high discharge capacity. When the content of the Li—Mn composite oxide particles which is coated or allowed to be present on the core particles is more than 20% by weight, the resulting particles tend to be deteriorated in discharge capacity although they are improved in thermal stability under a charged condition of the cell. The content of the Li—Mn composite oxide is more preferably 0.4 to 10% by weight and still more preferably 0.5 to 5% by weight.

The average secondary particle diameter of the secondary particles forming the core particles is preferably 3 to 20 μm. When the average secondary particle diameter is less than 3 μm, the resulting particles tend to exhibit a low electrode packing density and a large BET specific surface area, resulting in high reactivity with an electrolyte solution and, therefore, deteriorated thermal stability upon charging. When the average secondary particle diameter is more than 20 μm, the resulting cell tends to suffer from increase in resistance within an electrode owing to increase in thickness of the electrode and, therefore, deterioration in charge/discharge rate characteristics thereof. The average secondary particle diameter of the secondary particles forming the core particles is more preferably 5 to 20 μm.

The average primary particle diameter of the core particles is 0.5 to 1.5 μm. The core particles necessarily have such an average primary particle diameter at a temperature generally used for calcination of the particles.

The average primary particle diameter of the Li—Mn composite oxide which is coated or allowed to be present on the core particles is preferably 0.1 to 3.0 μm. The particles of the Li—Mn composite oxide necessarily have such an average primary particle diameter at a temperature generally used for calcination of the particles.

The average secondary particle diameter of the Li—Ni-based composite oxide particles for a non-aqueous electrolyte secondary battery according to the present invention is preferably 5 to 20 μm and more preferably 10 to 20 μm. When the average secondary particle diameter of the Li—Ni-based composite oxide particles is less than 5 μm, the Li—Ni-based composite oxide particles tend to suffer from not only decrease in electrode packing density, but also increase in reactivity with an electrolyte solution owing to increase in BET specific surface area thereof, resulting in deteriorated thermal stability upon charging. When the average secondary particle diameter of the Li—Ni-based composite oxide particles is more than 20 μm, the resulting cell tends to suffer from increase in resistance within an electrode owing to increase in thickness of the electrode and, therefore, deterioration in charge/discharge rate characteristics thereof.

The Li—Ni-based composite oxide particles according to the present invention preferably have a powder pH value of not more than 11.5. When the powder pH value of the Li—Ni-based composite oxide particles is more than 11.5, the resulting particles tends to be deteriorated in thermal stability, or a paint obtained using the particles tends to be undesirably gelled or undergo increase in a viscosity thereof upon forming it into a sheet. Meanwhile, the powder pH value of the Li—Ni-based composite oxide particles is determined from a pH value of a suspension as measured by suspending the Li—Ni-based composite oxide particles in distilled water and allowing the resulting suspension to stand at room temperature.

In the Li—Ni-based composite oxide particles for a non-aqueous electrolyte secondary battery according to the present invention, when using a negative electrode formed from a material capable of absorbing and desorbing a metallic lithium or a lithium ion, an exothermic maximum peak temperature thereof as measured in a differential thermal analysis at a positive electrode under the condition that the cell is charged to 4.5 V is preferably not lower than 240° C.

Next, the process for producing the Li—Ni-based composite oxide particles for a non-aqueous electrolyte secondary battery according to the present invention is described.

The Li—Ni-based composite oxide particles according to the present invention can be produced by any of (1) a process comprising the steps of allowing an oxide and/or a hydroxide which comprise Mn to mechanically adhere to an Li—Ni-based oxide comprising Co and/or Al; and then heat-treating the obtained material at a temperature of not lower than 400° C. and not higher than 1,000° C. (Invention 6), (2) a process comprising the steps of allowing an oxide and/or a hydroxide which comprise Mn to mechanically adhere to an Ni-based hydroxide comprising Co and/or Al; mixing the obtained material with a lithium compound; and then heat-treating the obtained mixture at a temperature of not lower than 700° C. and not higher than 1,000° C. in an oxygen-containing atmosphere (Invention 7), and (3) a process comprising the steps of dropping a manganese-containing solution and an alkali solution to a suspension of Ni-based hydroxide particles comprising Co and/or Al to produce a manganese-containing hydroxide, a manganese-containing oxide hydroxide or a manganese-containing oxide on a surface of an Ni-based hydroxide; subjecting the obtained material to washing with water and drying; mixing the dried material with a lithium compound; and then heat-treating the obtained mixture at a temperature of not lower than 700° C. and not higher than 1,000° C. in an oxygen-containing atmosphere (Invention 8).



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stats Patent Info
Application #
US 20130330626 A1
Publish Date
12/12/2013
Document #
13967395
File Date
08/15/2013
USPTO Class
429223
Other USPTO Classes
4271263
International Class
01M4/48
Drawings
2


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Chemistry: Electrical Current Producing Apparatus, Product, And Process   Current Producing Cell, Elements, Subcombinations And Compositions For Use Therewith And Adjuncts   Electrode   Chemically Specified Inorganic Electrochemically Active Material Containing   Nickel Component Is Active Material