JP3978881B2 - Non-aqueous electrolyte and lithium secondary battery using the same - Google Patents

Non-aqueous electrolyte and lithium secondary battery using the same Download PDF

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Publication number
JP3978881B2
JP3978881B2 JP23106498A JP23106498A JP3978881B2 JP 3978881 B2 JP3978881 B2 JP 3978881B2 JP 23106498 A JP23106498 A JP 23106498A JP 23106498 A JP23106498 A JP 23106498A JP 3978881 B2 JP3978881 B2 JP 3978881B2
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non
carbonate
lithium secondary
secondary battery
weight
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JP2000003724A (en
Inventor
幸夫 仲田
浩司 安部
敦男 日高
俊一 浜本
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宇部興産株式会社
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies or technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage
    • Y02E60/12Battery technologies with an indirect contribution to GHG emissions mitigation
    • Y02E60/122Lithium-ion batteries

Description

[0001]
The present invention relates to a lithium secondary battery excellent in battery characteristics such as battery cycle characteristics and storage characteristics, and a non-aqueous electrolyte used therein.
[0002]
[Prior art]
In recent years, electronic devices are becoming smaller and more portable, and as a driving power source for them, development of a high energy density battery, particularly a secondary battery, is required. As a promising candidate, the positive electrode has attracted attention as a positive electrode material because lithium-containing composite oxides such as LiCoO 2 , LiMn 2 O 4 , and LiNiO 2 can extract high electromotive force, and the negative electrode has carbon such as coke and graphite. Since the material does not short-circuit with the positive electrode due to the growth of dendritic electrodeposited lithium and does not drop off lithium from the negative electrode, it is a negative electrode material with high performance and high safety that replaces lithium secondary batteries using metallic lithium negative electrodes. It is getting more and more attention.
[0003]
[Problems to be solved by the invention]
However, when the carbon material is used for the negative electrode, there is a problem in that the battery capacity gradually decreases due to decomposition of the nonaqueous solvent used as the electrolytic solution on the carbon negative electrode along with the number of charge / discharge cycles. For this reason, at present, battery characteristics such as battery cycle characteristics and storage characteristics are not always satisfactory.
[0004]
In particular, in a lithium secondary battery using the lithium-containing composite oxide as a positive electrode and a highly crystallized carbon material such as natural graphite or artificial graphite as a negative electrode, peeling of the carbon material is observed, depending on the degree of the phenomenon. However, there is a problem that the electric capacity and cycle characteristics are lowered. This exfoliation of the carbon material may be caused by the decomposition of the non-aqueous solvent in the electrolyte during charging, and the decomposition of the non-aqueous solvent that causes the exfoliation is not caused at the interface between the carbon material and the electrolyte. It is thought to result from the electrochemical reduction of the aqueous solvent.
[0005]
For example, cyclic carbonate is preferably used as the non-aqueous solvent, but when cyclic carbonate such as ethylene carbonate (EC) is used, decomposition of the non-aqueous solvent occurs during repeated charge and discharge, Battery performance is degraded. Among them, propylene carbonate (PC) having a low melting point and a high dielectric constant is preferable as a non-aqueous solvent because it has a high electric conductivity even at a low temperature, but highly crystallized graphite is used as a negative electrode material. In such a case, the decomposition of PC becomes remarkable, and it cannot be used as an electrolyte for a lithium secondary battery.
[0006]
The present invention solves the above-described problems related to the electrolyte for a lithium secondary battery, has excellent battery cycle characteristics, and has excellent battery characteristics such as storage characteristics in a charged state, and to this It aims at providing the nonaqueous electrolyte to be used.
[0007]
[Means for Solving the Problems]
The present invention relates to a lithium secondary battery comprising a positive electrode, a negative electrode, and a non-aqueous electrolyte in which an electrolyte is dissolved in a non-aqueous solvent, wherein the positive electrode is a material containing a lithium composite oxide, and the negative electrode is a material containing graphite. The non-aqueous solvent is composed mainly of cyclic carbonate (selected from the group consisting of ethylene carbonate and propylene carbonate) and chain carbonate, and 0.1 to 4% by weight of 1,3 in the non-aqueous solvent. -It relates to a lithium secondary battery characterized by containing propane sultone and / or 1,4-butane sultone.
The present invention also relates to a non-aqueous electrolyte for a lithium secondary battery provided with a positive electrode made of a material containing a lithium composite oxide and a negative electrode made of a material containing graphite. The non-aqueous electrolyte has an electrolyte dissolved in a non-aqueous solvent. The non-aqueous electrolyte is a non-aqueous solvent comprising a cyclic carbonate (selected from the group consisting of ethylene carbonate and propylene carbonate) and a chain carbonate as main components, and 0.1 to 0.1 in the non-aqueous solvent. The present invention relates to a non-aqueous electrolyte for a lithium secondary battery, wherein 4% by weight of 1,3-propane sultone and / or 1,4-butane sultone is contained.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
The non-aqueous solvent in the present invention contains a cyclic carbonate and a chain carbonate as main components.
The cyclic carbonate is preferably at least one selected from the group consisting of ethylene carbonate (EC) and propylene carbonate (PC).
[0009]
The chain carbonate is preferably at least one selected from dimethyl carbonate (DMC), methyl ethyl carbonate (MEC), and diethyl carbonate (DEC).
[0010]
In the electrolyte solution for a lithium secondary battery in the present invention, the content of the cyclic carbonate in the non-aqueous solvent is 10% by weight or more and 70% by weight or less, and the content of the chain carbonate is 30% by weight or more and 90% by weight. The content of 1,3-propane sultone and / or 1,4-butane sultone is preferably 0.1 wt% or more and 4 wt% or less.
[0011]
The electrolyte used in the present invention, for example, LiPF 6, LiBF 4, LiClO 4, LiN (SO 2 CF 3) 2, LiN (SO 2 C 2 F 5) 2, LiC (SO 2 CF 3) 3 , etc. Is mentioned. These electrolytes may be used alone or in combination of two or more. These electrolytes are used by being dissolved in the non-aqueous solvent usually at a concentration of 0.1 to 3M, preferably 0.5 to 1.5M.
[0012]
The electrolytic solution of the present invention is obtained, for example, by mixing the cyclic carbonate and the chain carbonate, dissolving the electrolyte, and dissolving 1,3-propane sultone and / or 1,4-butane sultone. It is done.
[0013]
The constituent members other than the electrolytic solution constituting the secondary battery are not particularly limited, and various conventionally used constituent members can be used.
[0014]
For example, a composite metal oxide of at least one metal selected from the group consisting of cobalt, manganese, nickel, chromium, iron, and vanadium and lithium is used as the positive electrode active material. Examples of such a composite metal oxide include LiCoO 2 , LiMn 2 O 4 , and LiNiO 2 .
[0015]
The positive electrode is obtained by kneading the positive electrode active material with a conductive agent such as acetylene black or carbon black, a binder such as polytetrafluoroethylene (PTFE) or polyvinylidene fluoride (PVDF), and a solvent to form a positive electrode mixture. By applying this positive electrode material to an aluminum foil or stainless steel lath plate as a current collector, and after drying and pressure molding, heat treatment is performed under vacuum at a temperature of about 50 ° C. to 250 ° C. for about 2 hours. Produced.
[0016]
As the negative electrode active material, a material containing graphite having a graphite-type crystal structure capable of inserting and extracting lithium, such as natural graphite and artificial graphite, is used. In particular, it is preferable to use a carbon material having a graphite-type crystal structure in which the lattice spacing ( 002 ) (d 002 ) is 3.35 to 3.40 Å (angstrom). A powder material such as a carbon material is kneaded with a binder such as ethylene propylene diene terpolymer (EPDM), polytetrafluoroethylene (PTFE), or polyvinylidene fluoride (PVDF) and used as a negative electrode mixture.
[0017]
In the present invention, 1,3-propane sultone and / or 1,4-butane sultone contained in the electrolytic solution contributes to the formation of a passive film on the surface of the carbon material, and has high activity such as natural graphite and artificial graphite. It is considered that the crystallized carbon material is coated with a passive film and has an effect of suppressing the decomposition of the electrolyte without impairing the normal reaction of the battery.
[0018]
The structure of the lithium secondary battery is not particularly limited, and a coin-type battery having a positive electrode, a negative electrode, and a single-layer or multi-layer separator, and a cylindrical battery or a square type having a positive electrode, a negative electrode, and a roll separator. An example is a battery. A known polyolefin microporous film, woven fabric, non-woven fabric or the like is used as the separator.
[0019]
【Example】
Next, although an Example and a comparative example are given and this invention is demonstrated concretely, these do not limit this invention at all.
[0020]
Example 1
(Preparation of electrolyte)
Propylene carbonate (PC) and dimethyl carbonate (DMC) were prepared so as to have a weight ratio of 1: 1, and 1,3-propane sultone (PS) was further added so as to be 0.1% by weight. An electrolytic solution was prepared by dissolving LiPF 6 to a concentration of 1M.
[0021]
[Production of lithium secondary battery and measurement of battery characteristics]
80% by weight of LiCoO 2 (positive electrode active material), 10% by weight of acetylene black (conductive agent), and 10% by weight of polytetrafluoroethylene (binder) were mixed, and this was mixed with 1-methyl-2- A pyrrolidone solvent was added and the mixture was applied onto an aluminum foil, dried, pressure-molded, and heat treated to prepare a positive electrode. 90% by weight of natural graphite (negative electrode active material) and 10% by weight of polyvinylidene fluoride (binder) are mixed, and a 1-methyl-2-pyrrolidone solvent is added thereto, and the resulting mixture is added to a copper foil. The negative electrode was prepared by drying, pressure molding, and heat treatment. In this case, the positive electrode and the negative electrode were adjusted so that their electric capacities were almost the same. And using the separator of a polypropylene microporous film, said electrolyte solution was inject | poured and the coin battery (diameter 20mm, thickness 3.2mm) was produced.
Using this coin battery, at room temperature (25 ° C.), it was charged at a constant current and constant voltage of 0.8 mA for 5 hours to a final voltage of 4.2 V, and then at a constant current of 0.8 mA and a final voltage of 2. The battery was discharged to 7 V, and this charge / discharge was repeated. The initial charge capacity is 415 mAh / g carbon, the discharge capacity is 319 mAh / g carbon, which is almost the same as when EC / DMC (1/1) is used as the electrolyte (Comparative Example 1), and charge / discharge 50 When the battery characteristics after cycling were measured, the discharge capacity retention rate was 82.3% when the initial discharge capacity was 100%. The results are shown in Table 1. Separately, at room temperature (25 ° C.), after charging for 5 hours to a final voltage of 4.2 V at a constant current and a constant voltage of 0.8 mA, it is set to −20 ° C. to a final voltage of 2.7 V at a constant current of 0.8 mA. Discharged. The initial discharge capacity at this time was 88% in terms of the initial discharge capacity ratio to room temperature.
[0022]
Example 2 to Example 5
A coin battery was produced by the same method as in Example 1 except that the positive electrode active material, the negative electrode active material, and the electrolyte composition were as shown in Table 1, and the battery characteristics were measured. Table 1 shows the discharge capacity retention ratio after 50 cycles at room temperature.
[0023]
Example 6
A charge / discharge test was conducted in the same manner as in Example 1 except that the positive electrode active material was changed from LiCoO 2 to LiMn 2 O 4 and the electrolyte composition was as shown in Table 1. Table 1 shows the discharge capacity retention ratio after 50 cycles at room temperature.
[0024]
Example 7
A lithium secondary battery was prepared in the same manner as in Example 1 except that the negative electrode active material was changed from natural graphite to artificial graphite (MCMB manufactured by Osaka Gas Chemical Co., Ltd.) and the electrolyte composition was as shown in Table 1. A charge / discharge test was conducted. Table 1 shows the discharge capacity retention ratio after 50 cycles at room temperature.
[0025]
Comparative Example 1
A lithium secondary battery was prepared and a charge / discharge test was performed in the same manner as in Example 1 except that the electrolyte composition was EC / DMC (weight ratio 1/1). The initial charge capacity was 411 mAh / g carbon, and the discharge capacity was 326 mAh / g carbon. Table 2 shows the discharge capacity retention ratio after 50 cycles at room temperature. Further, the initial discharge capacity at −20 ° C. was 62% in terms of the initial discharge capacity ratio to room temperature.
[0026]
Comparative Example 2
A lithium secondary battery was produced in the same manner as in Example 1 except that the electrolyte solution composition was PC / DMC (weight ratio 1/1), and a charge / discharge test was performed. However, in this case, the electrolytic solution was decomposed at the time of the first charge and could not be charged. The results are shown in Table 2.
[0027]
Example 8
A coin battery was produced in the same manner as in Example 1 except that the amount of 1,3-propane sultone added was 1% by weight and the non-aqueous solvent was EC-DMC (weight ratio 1/2). It was measured. Table 3 shows the discharge capacity retention rate after 50 cycles at room temperature.
[0028]
Example 9
A coin battery was produced by the same method as in Example 8 except that the amount of 1,3-propane sultone added was 3% by weight, and the battery characteristics were measured. Table 3 shows the discharge capacity retention rate after 50 cycles at room temperature.
[0029]
Example 10
A coin battery was produced in the same manner as in Example 8 except that 3% by weight of 1,4-butane sultone was added instead of 1,3-propane sultone, and the battery characteristics were measured. Table 3 shows the discharge capacity retention rate after 50 cycles at room temperature.
[0030]
Example 11
A coin battery was produced by the same method as in Example 9 except that LiMn 2 O 4 was used as the positive electrode active material, and the battery characteristics were measured. Table 3 shows the discharge capacity retention rate after 50 cycles at room temperature.
[0031]
Example 12
A coin battery was produced in the same manner as in Example 11 except that 3% by weight of 1,4-butane sultone was added instead of 1,3-propane sultone, and the battery characteristics were measured. Table 3 shows the discharge capacity retention rate after 50 cycles at room temperature.
In addition, this invention is not limited to the Example described, The various combination which can be substituted easily from the meaning of invention is possible. In particular, the combination of solvents in the above examples is not limited. Furthermore, although the said Example is related with a coin battery, this invention is applied also to a cylindrical type | mold and a square-shaped battery.
[0032]
【The invention's effect】
According to the present invention, a lithium secondary battery excellent in battery characteristics such as battery cycle characteristics and storage characteristics can be provided.
[0033]
[Table 1]
[0034]
[Table 2]
[0035]
[Table 3]

Claims (12)

  1. In a lithium secondary battery including a positive electrode, a negative electrode, and a non-aqueous electrolyte in which an electrolyte is dissolved in a non-aqueous solvent, the positive electrode is a material containing a lithium composite oxide, the negative electrode is a material containing graphite, and a non-aqueous solvent Is composed mainly of a cyclic carbonate and a chain carbonate selected from the group consisting of ethylene carbonate and propylene carbonate , and 0.1 to 4% by weight of 1,3-propane sultone and / or in a non-aqueous solvent. Alternatively, a lithium secondary battery containing 1,4-butane sultone.
  2. The cyclic carbonate content in the non-aqueous solvent is 10% by weight or more and 70% by weight or less, the chain carbonate content is 30% by weight or more and 90% by weight or less, and the 1,3-propane sultone and 2. The lithium secondary battery according to claim 1, wherein the content of 1,4-butane sultone is 0.1 wt% or more and 4 wt% or less.
  3. The lithium secondary battery according to claim 1, wherein the cyclic carbonate is propylene carbonate.
  4. The lithium secondary battery according to claim 1, wherein the chain carbonate is at least one selected from dimethyl carbonate, diethyl carbonate, and methyl ethyl carbonate.
  5. The lithium secondary battery according to claim 1, wherein the graphite is natural graphite or artificial graphite.
  6. 2. The lithium secondary battery according to claim 1, wherein a plane interval (d 002 ) of a lattice plane (002) of the graphite is 3.35 to 3.40 angstroms (Å).
  7. A non-aqueous electrolyte for a lithium secondary battery having a positive electrode made of a material containing a lithium composite oxide and a negative electrode made of a material containing graphite, wherein the non-aqueous electrolyte is a non-aqueous electrolyte in which an electrolyte is dissolved in a non-aqueous solvent. The non-aqueous solvent is mainly composed of a cyclic carbonate and a chain carbonate selected from the group consisting of ethylene carbonate and propylene carbonate , and 0.1 to 4% by weight of 1,3 in the non-aqueous solvent. -Propane sultone and / or 1,4-butane sultone is contained, The nonaqueous electrolyte for lithium secondary batteries characterized by the above-mentioned.
  8. The cyclic carbonate content in the non-aqueous solvent is 10% by weight or more and 70% by weight or less, the chain carbonate content is 30% by weight or more and 90% by weight or less, and the 1,3-propane sultone and 8. The nonaqueous electrolytic solution for a lithium secondary battery according to claim 7, wherein the content of 1,4-butane sultone is 0.1 wt% or more and 4 wt% or less.
  9. The non-aqueous electrolyte for a lithium secondary battery according to claim 7, wherein the cyclic carbonate is propylene carbonate.
  10. The non-aqueous electrolyte for a lithium secondary battery according to claim 7, wherein the chain carbonate is at least one selected from dimethyl carbonate, diethyl carbonate, and methyl ethyl carbonate.
  11. The non-aqueous electrolyte for a lithium secondary battery according to claim 7, wherein the graphite is natural graphite or artificial graphite.
  12. The nonaqueous electrolytic solution for a lithium secondary battery according to claim 7, wherein a plane interval (d 002 ) of a lattice plane (002) of the graphite is 3.35 to 3.40 angstroms (Å).
JP23106498A 1997-08-22 1998-08-18 Non-aqueous electrolyte and lithium secondary battery using the same Expired - Lifetime JP3978881B2 (en)

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JP22615797 1997-08-22
JP9-226157 1998-04-14
JP10241598 1998-04-14
JP10-102415 1998-04-14
JP23106498A JP3978881B2 (en) 1997-08-22 1998-08-18 Non-aqueous electrolyte and lithium secondary battery using the same

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