KR100262852B1 - A positive active material lixmymn-2-yo4 and its manufacturing method - Google Patents

A positive active material lixmymn-2-yo4 and its manufacturing method Download PDF

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KR100262852B1
KR100262852B1 KR1019970067614A KR19970067614A KR100262852B1 KR 100262852 B1 KR100262852 B1 KR 100262852B1 KR 1019970067614 A KR1019970067614 A KR 1019970067614A KR 19970067614 A KR19970067614 A KR 19970067614A KR 100262852 B1 KR100262852 B1 KR 100262852B1
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li
nitrate
mn
active material
ni
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KR19990048820A (en
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선양국
오승모
장동훈
홍진규
이종화
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유현식
제일모직주식회사
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • C01G45/006Compounds containing, besides manganese, two or more other elements, with the exception of oxygen or hydrogen
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy

Abstract

The cathode active material for a lithium secondary battery of the present invention uses a chelating agent citric acid, and as a metal precursor, lithium nitrate and / or acetate, manganese nitrate and / or acetate, and other metals (Al, Co, Li). Or Ni) nitrate, which is represented by the following structural formula.
Li x M y Mn 2-y O 4
In the formula, M is Al, Co, Li or Ni, x is 0.9 ~ 1.1 and 0 <y <0.2.
The positive active material for a lithium secondary battery of the present invention mixes citric acid as a chelating agent and lithium nitrate and / or lead acetate as a metal precursor, manganese nitrate and / or acetate, and nitrates of other metals; Dehydrating the mixed solution at a temperature of 50 ° C. in a rotary evaporator; Dehydration at a temperature of 70 ° C. in a vacuum dryer to prepare an amorphous gel precursor; And the gel precursor is prepared by calcination (calcination) for 5 to 24 hours at a temperature of 500 ~ 900 ℃ in an electric bath.

Description

LithMyMn2-yO4 Powder and Preparation Method for Anode Material for Lithium Secondary Battery.

1 is a process chart for preparing Li x M y Mn 2-y O 4 powder according to the present invention.

FIG. 2 is a graph showing a TG curve (raising rate of 5 ° C./min) showing the process of conversion from gel precursor to ceramics.

Figure 3 shows the results of X-ray diffraction analysis of (a) LiCo 0.05 Mn 1.95 O 4. (B) Li 1.05 Co 0.1 Mn 1.9 O 4 and Li 0.95 Co 0.2 Mn 1.8 O 4 having a spinel structure according to the present invention Picture.

4 shows Li x M 0.05 Mn 1.95 0 4 having a spinel structure according to the present invention (x = 0.9 to 1.1) (a) M = A1, (b) M = Li, (c) M = Ni and (d) The figure shows the result of X-ray diffraction analysis of M = Mn.

5 shows (a) LiCo 0.05 Mn 1.95 O 4. (B) Li 1.05 Co 0.1 Mn 1.9 O 4 and Li 0.95 Co 0.2 Mn 1.8 O 4 as a cathode to change the capacity of the rechargeable lithium battery The figure shows.

6 shows Li x M 0.05 Mn 1.95 0 4 (x = 0.9 ~ 1.1) (a) Lithium secondary battery charging using M = A1, (b) M = Li and (c) M = Ni as a cathode The figure shows the change of discharge capacity according to discharge.

Seventh turn (a) Li x Mn 2 0 4 (x = 0.9~1.1) and (b) Li x Ni Mn O.05 l.95 constant current charge and discharge curves of a lithium secondary battery, the positive electrode 04 to the (cathode) The figure shows.

[Field of Invention]

The present invention is used as a positive electrode active material for lithium secondary batteries and has a spinel structure Li x MyMn 2-y O 4 (where M is Al, Co, Li or Ni, x is 0.9 to 1.1, 0 <y <0.2) and It relates to a method for producing the positive electrode active insol. More specifically, the present invention prepares Li x MyMn 2-y O 4 powder, which is a cathode active material for lithium ion batteries and lithium polymer batteries, using citric acid method, and the electrochemical properties of carbon cells or Li / organic electrolyte / Li x MyMn 2. A positive electrode active material investigated using a -y O 4 cell.

Background of the Invention and Prior Art

Lithium secondary batteries are composed of carbon or Li metal / electrolyte (organic electrolyte or polymer electrolyte) / oxide positive electrode. Li x Co0 2 , Li x Ni0 2 , Li x Mn 2 0 4, etc. are being researched and developed. Currently, the commercialized anode material is Li x CoO 2, and since the price of the cathode material is about one third of the manufacturing cost of the battery, the development of cheap anode material is required. Since manganese has a lot of reserves, the price is only 1/20 of that of cobalt, so researches to develop manganese oxide as an anode material have been actively conducted. Among them, Li x Mn 2 O 4 having a spinel structure has the advantages of low manufacturing cost, high operating voltage of the battery, excellent thermal stability than other oxides, harmless to the human body, and low pollution. However, Li x Mn 2 O 4 has a problem of continuous capacity reduction with repeated charging and discharging, and a solution for this has been sought. This problem is attributed to the fact that as the charge and discharge of the earthquake, the crystal structure of the positive electrode material is destroyed or a phase change is caused, and manganese ions are dissolved into the electrolyte. In order to solve the above problems in the present invention, a part of Mn ions forming a spinel lattice (within 20%)

By substituting for other metal ions of Al, Co, Li, or Ni, it was found that the destruction and dissolution of the crystal structure can be suppressed and the life of the anode can be greatly increased.

The most common method for producing Li x M y Mn 2-y O 4 is a solid phase reaction. This method is made by mixing and firing these powders several times using carbonates, oxides and hydroxides of each element. This method is difficult to synthesize the powder with uniform phase, difficult to control the size of powder particles uniformly, it has to be manufactured for a long time at high temperature, and it is necessary to use a large amount of metal ions to obtain the effect of substitution. There is a disadvantage that the discharge capacity is lowered. On the other hand, citric acid method, which is a kind of liquid phase reaction method, is easy to synthesize powder having a uniform phase, can be manufactured at a relatively low firing temperature and a short time, and can easily control the composition ratio. There is an advantage that can be obtained.

[Purpose of invention]

An object of the present invention is to use citric acid as a chelating agent, lithium nitrate and / or acetate, manganese nitrate and / or acetate, and other metals (Al, Co, Li or Ni) as metal precursors. Nitrate to provide a Li x M y Mn 2-y O 4 powder having a uniform phase.

Another object of the present invention is the Li x M y Mn 2-y O 4 (M = Al, Co, Li, Ni, x = 0.9 which can suppress the capacity reduction even with a small amount of metal ion replacement using the citric acid method) It is for providing -1.1, y <0.2) powder.

Another object of the present invention is the Li x M y Mn 2-y O 4 powder which can be manufactured in a relatively low firing temperature and a short time by using citric acid method, which is a kind of liquid phase reaction, and can easily control the composition ratio of metal ions. It is to provide.

It is yet another object of the present invention to provide a Li x M y Mn 2-y O 4 powder which does not lower the initial discharge even with relatively small amounts of metal ion substitution.

[Summary of invention]

The cathode active material for a lithium secondary battery of the present invention uses citric acid as a chelating agent, and lithium nitrate and / or acetate, manganese nitrate and / or acetate as a metal precursor, and other metals (Al, Co). Prepared using nitrates of Li or Ni), represented by the following structural formula:

Li x M y Mn 2-y O 4

In the above formula, M is Al, Co, Li or Ni, x is 0.9 to 1.1, and 0 &lt; y &lt; 0.2.

The positive electrode active material for a lithium secondary battery of the present invention mixes citric acid as a chelating agent and lithium nitrate and / or acetate as a metal precursor, manganese nitrate and / or acetate, and nitrates of other metals; Dehydrating the mixed solution at a temperature of 50 ° C. in a rotary evaporator; Dehydration at a temperature of 70 ° C. in a vacuum dryer to prepare an amorphous gel precursor; And the gel precursor is prepared by calcination (calcination) for 5 to 24 hours at a temperature of 500 ~ 900 ℃ in an electric bath.

Hereinafter, the details of the present invention will be described below.

Detailed Description of the Invention

The cathode active material for a lithium secondary battery of the present invention uses citric acid as a chelating agent, and lithium nitrate and / or acetate, manganese nitrate and / or acetate as a metal precursor, and other metals (Al, Co, Prepared using a nitrate of Li or Ni), represented by the following structural formula:

Li x M y Mn 2-y O 4

In the formula, M is Al, Co, Li or Ni, x is 0.9 to 1.1, 0 <y <0.2.

Starting materials of lithium (Li) used in the present invention are LiN0 3 and Li (CH 3 C0 2 ), the starting materials of manganese (Mn) Mn (NO 3 ) 2 and Mn (CH 3 C0 2 ) There are two . Other metal nitrates include Al 2 (NO 3 ) 3 · xH 2 0.

Each starting material is weighed and then dissolved in distilled water and mixed with citric acid. After confirming that all components are completely dissolved, water is slowly removed from a rotary vacuum dryer to obtain a sol, and then dried in a vacuum oven to gel. When heat-treated for 5 to 24 hours in the temperature range of 500 to 900 ℃ Li x M y Mn 2-y O 4 (M = Al, Co, Li, Ni, x = 0.9 to 1.1, 0 <y <0.2 ) Can be obtained. At this time, the temperature increase and temperature reduction rate of the electric furnace were 1 to 5 ° C / min.

The battery is constituted with an electrolyte using the positive electrode active material of the present invention as the positive electrode and carbon (MCMB or graphite) or lithium (Li) metal as the negative electrode. The electrolyte used here is IM LiC10 4 / polycarbonate + dimethylether (1: 1), 1M LiPF 6 / ethylene carbonate + diethylcarbonate (1: 1 and 2: 1), 1M LiPF 6 / ethylene carbonate + dimethyl carbonate (2: 1 ), And 1M LiBF 4 / ethylene carbonate + diethyl carbonate (1: 1). The positive plate comprises Li x M y N n 2-y O 4 (M = Al, CO, Li, Ni, x = 0.9 to 1.1, 0 <V <0.2): Ketjen black: PTFE (73: 20: 7) After weighing and dispersing, it was produced by bonding to the current collector.

The invention can be better understood by the following examples, which are intended for the purpose of illustration of the invention and are not intended to limit the scope of protection defined by the appended claims.

Manufacture of cathode active material Li x M y MN 2-y O 4

Example 1

1.4 g of LiN0 3 Mn (NO 3 ) 2 · 6H 2 0 11.4 g and 0.3 g of Co (NO 3 ) 2 · 6H 2 O were dissolved in distilled water, and 14 g of citric acid was dissolved in the solution and mixed well. The solution was mixed well and water was evaporated in a rotary vacuum dryer to obtain a solid product, and the obtained solid product was further dried in a vacuum oven. This was reacted at 800 ° C. for 8 hours in an electric furnace to obtain a powder. The obtained powder was washed with acetone and then filtered at 400 mesh to remove impurities. As a result of chemical analysis of the powder produced, it was confirmed that the composition was LiCo 0.05 Mn 1.95 0 4 , and the spinel structure of the X-ray diffraction analysis was shown in FIG.

Example 2

Except for using Mn (CH 3 CO 2 ) 2 · 4H 2 0 9.3g instead of Mn (N0 3 ) 2 · 6H 2 0 11.4g used as a manganese precursor in Example 1 Powder was obtained, and the chemical analysis and X-ray diffraction analysis confirmed that the spinel structure of Li l.05 Co 0.1 Mn l.9 0 4 . X-ray diffraction analysis of Li l.05 Co 0.1 Mn l.9 0 4 is shown in FIG. 3 (b).

Example 3

A powder was obtained through the same process as in Example 1 except that 1.9 g of LiCH 3 C0 2 · 4H 2 0 was used instead of 14 g of LiN0 3 used as the lithium precursor in Example 1, and the chemical analysis and the X-ray diffraction analysis result it was confirmed that the spinel structure Li O.95 Co O.2 Mn l.8 0 4 . Li a Co O.95 O.2 X- ray diffraction analysis of Mn l.8 0 4 shown in FIG. 3 (C).

Example 4

A powder was obtained by the same procedure as in Example 1 except that Al 2 (NO 3 ) 3 · 9H 2 0 0.4 g was used instead of 0.3 g of CO (NO 3 ) 2 · 6H 2 O used in Example 1. , are shown the chemical analysis and X- ray diffraction analysis LiAl 0.05 Mn 1.95 04 was identified as LiAl 0.05 Mn 1.95 X- ray diffraction analysis of the 04 in FIG. 4 (3).

Example 5

A powder was obtained through the same process as in Example 1 except that 1.5g of LiN0 3 was used in Example 1, and the result of chemical analysis and X-ray diffraction analysis showed that Li 1.05 Mn 1.95 0 4 . X-ray diffraction analysis of Li 1.05 Mn 1.95 0 4 is shown in FIG. 4 (b).

Example 6

Powder was obtained through the same process as in Example 1 except that 0.3 g of Ni (NO 3 ) 2 6H 2 0 was used instead of 0.3 g of Co (NO 3 ) 2 · 6H 2 O used in Example 1. analysis and X- ray diffraction patterns showed that LiNi 0.05 Mn 1.95 0 4 was identified as .LiNi 0.05 Mn 1.95 X- ray diffraction analysis of the 04 is shown in FIG. 4 (c)

Comparative Example 1

The powder was obtained by the same procedure as in Example 1 except that 11,7 g of Mn (NO 3 ) 2 · 6H 2 O was used in Example 1, and the chemical analysis and the X-ray diffraction analysis showed that LiMn 2 0 4 It was confirmed. The X-ray diffraction analysis of LiMn 2 O 4 is shown in FIG. 4 (d).

Use of the positive electrode active material Li x M y Mn 2-y O 4 in a lithium secondary battery:

Example 7

Charge / discharge experiment with constant current (C / 2) by constructing a lithium secondary battery using Li x M y Mn 2-y O 4 (x = 0.9 to 1.1, 0 <y <0.2) obtained from Example 1 as a positive electrode material Was performed. Lithium metal was used as a negative electrode, and an electrolyte in which 1M LiBF 4 was dissolved in a solvent of ethylene carbonate and diethyl carbonate in a volume ratio of 1: 1 was used. 5 shows the change in discharge capacity according to the number of cycles as a result of performing charging and discharging when Li x CO y Mn 2-y O 4 (x = 0.9 to 1.1, 0 <y <0.2) is used as the positive electrode material. In FIG. 5, (a) is y, which is a composition ratio of Co, 0.05, (b) is y, 0.1, and (c) is y, 0.2.

Example 8

Lithium secondary batteries using Li x M y Mn 2-y O 4 (M = Al, Li, Ni, x = 0.9 to 1.1, 0 <y <0.2) obtained from Examples 4, 5, and 6 as a positive electrode material The charge and discharge experiment was performed under the same conditions as in Example 7. The result of charge / discharge performance when Li x M y Mn 2-y O 4 (M = ALLl, Ni, x = 0.9 ~ 1.1, 0 <r <0.2) is used as the anode material is used to change the discharge capacity according to the number of cycles. It is shown in 6 degrees. In FIG. 6, (a) is Al, (b) is Ni, and (c) is Li.

Example 9

A lithium secondary battery was constructed using LiMn 2 0 4 obtained from Comparative Example 1 as a positive electrode material, and the charge and discharge experiments were performed under the same conditions as in Example 7, and LiNi 0.05 Mn 1.95 0, which showed the best performance from Example 9, was shown. The change in potential with respect to the capacity according to 4 and the number of charge and discharge cycles is shown in FIG. 7.

Example 10

The initial capacity was 130 mAhg using LiAl 0.05 Mn 1.95 0 4 obtained in Example 4 as a cathode material and carbon (MCMB-28) instead of lithium metal as a cathode material. It was -1 and the capacity at 200 charge / discharge cycles was 115 mAhg -1 .

Example 11

Example 7 using LiAl 0.05 Mn 1.95 0 4 obtained in Example 4 as an anode material and an electrolyte in which 1M LiPF 6 in a solvent of ethylene carbonate: propylene carbonate in a volume ratio of 1: 1 was used instead of the electrolyte used in Example 7. and it was a result of the initial capacity is 135 mAhg a charge and discharge test 1 in the same condition, was 400 times during the charge and discharge capacity of 110 mAhg -1.

Example 12

Example 1 Using LiAl 0.05 Mn 1.95 0 4 obtained in Example 6 as an anode material and an electrolyte in which 1M LiPF 6 was dissolved in a solvent in which ethylene carbonate: dimethyl carbonate was 1: 1 in volume ratio instead of the electrolyte used in Example 7 Charging and discharging experiments under the same conditions as 8 showed an initial capacity of 127 mAhg −1 and a capacity of 120 mAhg −1 at 200 charge / discharge cycles.

The cathode active material of the present invention can be manufactured in a relatively low firing temperature and a short time by using citric acid method, which is a kind of liquid phase reaction method, and it is easy to control the composition ratio of metal ions, and the initial discharge is possible even with relatively small amount of metal ion substitution. It has the effect of the invention that does not lower the capacity.

Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.

Claims (5)

  1. Citric acid is used as a chelating agent, lithium nitrate and / or acetate, manganese nitrate and / or acetate, and nitrates of other metals (Al, Co, Li or Ni) as metal precursors. A cathode active material prepared for and represented by the following structural formula:
    Li x M y Mn 2-y O 4
    Wherein M is Al, Co, Li or Ni, x is 0.9 to 1.1 and 0 &lt; y &lt;
  2. The metal nitrate of claim 1, wherein the nitrate of the other metal is selected from the group consisting of Al (NO 3 ) 3 xH 2 0, LiN0 3 , Co (NO 3 ) XH 2 0 and Ni (NO 3 ) 2 .xH 2 O. A cathode active material for a lithium secondary battery, characterized in that selected.
  3. Mixing citric acid as a chelating agent and lithium nitrate and / or lead acetate as a metal precursor, manganese nitrate and / or acetate, and nitrates of other metals; Dehydrating the mixed solution at a temperature of 50 ° C. in a rotary evaporator; Dehydration at a temperature of 70 ° C. in a vacuum dryer to prepare an amorphous gel precursor; And the method of producing a cathode active material for a lithium secondary battery represented by the following structural formula characterized in that the gel precursor is prepared by calcination (calcination) for 5 to 24 hours at a temperature of 500 ~ 900 ℃ in an electric bath:
    Li x M y Mn 2-y O 4
    Wherein M is Al, Co, Li or Ni, x is 0.9 to 1.1 and 0 &lt; y &lt;
  4. 4. The method of claim 3, wherein the nitrate of the other metal is selected from the group consisting of Al 2 (N0 3 ) 3 .xH 2 0, LiN0 3 Co (NO 3 ) .xH 2 O and Ni (NO 3 ) 2 .xH 2 0. Method for producing a cathode active material for a lithium secondary battery, characterized in that selected.
  5. The method of manufacturing a cathode active material for a lithium secondary battery according to claim 3, wherein the temperature increase and temperature reduction rate of the electric furnace in the calcination step is 1 to 5 ° C / min.
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WO2013157867A1 (en) * 2012-04-20 2013-10-24 주식회사 엘지화학 Lithium secondary battery having improved rate characteristics
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KR101479559B1 (en) * 2012-05-23 2015-01-08 순천대학교 산학협력단 Cathode active materials for lithium secondary battery and lithium secondary battery comprising the same, and preparation method for the cathode active material
WO2018132903A1 (en) * 2017-01-18 2018-07-26 Nano One Materials Corp. One-pot synthesis for lithium ion battery cathode material precursors

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WO2013157867A1 (en) * 2012-04-20 2013-10-24 주식회사 엘지화학 Lithium secondary battery having improved rate characteristics
WO2013157883A1 (en) * 2012-04-20 2013-10-24 주식회사 엘지화학 Electrolyte for lithium secondary battery and lithium secondary battery containing same
US9954254B2 (en) 2012-04-20 2018-04-24 Lg Chem, Ltd. Electrolyte for lithium secondary battery and lithium secondary battery including the same
US10170796B2 (en) 2012-04-20 2019-01-01 Lg Chem, Ltd. Lithium secondary battery of improved rate capability with cathode containing nickel manganese complex oxide for high-voltage applications

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