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WO2012073642A1 - Batterie secondaire à électrolyte non aqueux - Google Patents

Batterie secondaire à électrolyte non aqueux Download PDF

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Publication number
WO2012073642A1
WO2012073642A1 PCT/JP2011/075373 JP2011075373W WO2012073642A1 WO 2012073642 A1 WO2012073642 A1 WO 2012073642A1 JP 2011075373 W JP2011075373 W JP 2011075373W WO 2012073642 A1 WO2012073642 A1 WO 2012073642A1
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WIPO (PCT)
Prior art keywords
aqueous electrolyte
secondary battery
electrolyte secondary
negative electrode
discharge
Prior art date
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Ceased
Application number
PCT/JP2011/075373
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English (en)
Japanese (ja)
Inventor
真治 山本
亮仁 大和
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Murata Manufacturing Co Ltd
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Murata Manufacturing Co Ltd
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Publication date
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Publication of WO2012073642A1 publication Critical patent/WO2012073642A1/fr
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0569—Liquid materials characterised by the solvents
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • H01M2300/0037—Mixture of solvents
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention generally relates to a non-aqueous electrolyte secondary battery, and more particularly to a non-aqueous electrolyte secondary battery having improved cycle characteristics as well as discharge rate characteristics.
  • a non-aqueous electrolyte secondary battery generally, for example, a non-aqueous electrolyte obtained by dissolving a lithium salt such as lithium hexafluorophosphate as an electrolyte in a non-aqueous solvent such as ethylene carbonate or dimethyl carbonate.
  • a lithium transition metal composite oxide as a positive electrode active material, and a carbon material as a negative electrode active material.
  • ⁇ -butyrolactone as a thermally stable non-aqueous solvent having a high boiling point.
  • Patent Document 1 Japanese Patent Application Laid-Open No. 2004-296181 (hereinafter referred to as Patent Document 1), in a lithium secondary battery using ⁇ -butyrolactone as a solvent for a nonaqueous electrolytic solution, a natural negative electrode active material is used.
  • a spinel type lithium titanium composite oxide such as lithium titanate
  • Patent Document 2 JP-A-2006-318797 (hereinafter referred to as Patent Document 2), spinel type lithium titanate is used as the negative electrode active material, and propylene carbonate, ethylene carbonate is used as the non-aqueous solvent.
  • non-aqueous electrolyte secondary batteries using a mixed solvent in which two or more of the group consisting of ⁇ -butyrolactone are mixed have been proposed.
  • Patent Document 2 describes an example in which a non-aqueous electrolyte secondary battery was produced using a mixed solvent of ethylene carbonate and ⁇ -butyrolactone (volume ratio 1: 2).
  • Patent Document 1 it is preferable that ⁇ -butyrolactone is used as a main solvent in the nonaqueous electrolytic solution, and specifically, it is preferable that 90% or more of ⁇ -butyrolactone is contained in the entire mixed solvent. Are listed.
  • an object of the present invention is to provide a non-aqueous electrolyte secondary battery capable of improving cycle characteristics as well as large current discharge characteristics.
  • the non-aqueous electrolyte secondary battery according to the present invention includes a positive electrode, a negative electrode, and a non-aqueous electrolyte.
  • the negative electrode includes a spinel type lithium titanium composite oxide.
  • the non-aqueous electrolyte contains a non-aqueous solvent in which propylene carbonate and ⁇ -butyrolactone are mixed at a volume ratio of 6: 4 to 4: 6.
  • the non-aqueous electrolyte secondary battery of the present invention it is preferable that the non-aqueous electrolyte contains trioctyl phosphate.
  • the negative electrode includes a spinel-type lithium titanium composite oxide
  • the non-aqueous electrolyte includes propylene carbonate and ⁇ -butyrolactone in a volume ratio of 6: 4 to 4: 6. Since the non-aqueous solvent mixed in (1) is included, it is possible to improve cycle characteristics as well as large current discharge characteristics.
  • FIG. 1 It is a perspective view which fractures
  • FIG. 1 It is sectional drawing which shows schematically the structure of the battery element accommodated in the outer packaging member of the non-aqueous-electrolyte secondary battery shown by FIG.
  • FIG. 1 It is a figure which shows the relationship between the discharge rate and discharge capacity in the nonaqueous electrolyte secondary battery produced in Example A of this invention.
  • the present inventors have proposed a non-aqueous electrolyte for improving both large current discharge characteristics and cycle characteristics, that is, a non-aqueous electrolyte.
  • a non-aqueous electrolyte for improving both large current discharge characteristics and cycle characteristics.
  • Various studies were made on the composition of the aqueous solvent. As a result, it has been found that if the non-aqueous solvent is a mixture of propylene carbonate and ⁇ -butyrolactone in a volume ratio of 6: 4 to 4: 6, both the large current discharge characteristics and the cycle characteristics are improved. It was.
  • the present invention has been made based on such knowledge of the present inventors.
  • the non-aqueous electrolyte secondary battery of the present invention includes a positive electrode, a negative electrode, a non-aqueous electrolyte, and a separator.
  • the negative electrode includes a spinel type lithium titanium composite oxide.
  • the non-aqueous electrolyte contains a non-aqueous solvent in which propylene carbonate and ⁇ -butyrolactone are mixed at a volume ratio of 6: 4 to 4: 6.
  • the non-aqueous electrolyte is configured as described above, it is possible to improve the discharge rate characteristics, particularly the high rate characteristics, that is, the large current discharge characteristics, and the cycle characteristics. Specifically, for example, the cycle characteristics at 60 ° C. can be improved together with the discharge rate characteristics at 25 ° C., particularly the high rate characteristics.
  • volume ratio of ⁇ -butyrolactone is less than 40% by volume, the large current discharge characteristics deteriorate.
  • volume ratio of ⁇ -butyrolactone exceeds 60% by volume, cycle characteristics deteriorate.
  • the non-aqueous electrolyte secondary battery of the present invention it is preferable that the non-aqueous electrolyte contains trioctyl phosphate.
  • the liquid content per unit time with respect to the electrolyte solution of a separator can be improved.
  • the discharge rate characteristic particularly the high rate characteristic, that is, the large current discharge characteristic.
  • the discharge rate characteristic at 25 ° C., particularly the high rate characteristic can be further improved.
  • the negative electrode includes a spinel type lithium titanium composite oxide as a negative electrode active material.
  • the negative electrode active material is a carbon-based material
  • ⁇ -butyrolactone may decompose, but when the negative electrode active material contains a spinel-type lithium titanium composite oxide, ⁇ -butyrolactone does not decompose. . For this reason, the lifetime of a battery can be improved.
  • the positive electrode and the negative electrode of the non-aqueous electrolyte secondary battery are alternately stacked via a separator.
  • the structure of the battery element may be composed of a stack of a plurality of strip-shaped positive electrodes, a plurality of strip-shaped separators and a plurality of strip-shaped negative electrodes, a stack of so-called single-wafer structures. It may be configured by folding and interposing a strip-shaped positive electrode and a strip-shaped negative electrode alternately.
  • a winding type structure in which a long positive electrode, a long separator, and a long negative electrode are wound may be employed as a wound structure is adopted as the structure of the battery element.
  • a positive electrode mixture layer including a positive electrode active material, a conductive agent, and a binder is formed on both surfaces of the positive electrode current collector.
  • the positive electrode current collector is made of aluminum.
  • the positive electrode active materials are lithium cobalt oxide composite oxide (LCO), lithium manganate composite oxide (LMO), lithium nickelate composite oxide (LNO), lithium-nickel-manganese-cobalt composite oxide (LNMCO), lithium -Manganese-nickel composite oxide (LMNO), lithium-manganese-cobalt composite oxide (LMCO), lithium-nickel-cobalt composite oxide (LNCO), or the like can be used.
  • the positive electrode active material may be appropriately selected from the above materials and mixed.
  • the positive electrode active material may be an olivine-based material such as LiFePO 4 . Carbon or the like is used as a conductive agent for the positive electrode. Polyvinylidene fluoride (PVDF) or polyamideimide (PAI) is used as the binder for binding the positive electrode active material and the conductive agent.
  • PVDF polyvinylidene fluoride
  • PAI polyamideimide
  • a negative electrode mixture layer including a negative electrode active material and a binder is formed on both surfaces of a negative electrode current collector.
  • the negative electrode current collector is made of aluminum
  • the negative electrode active material is a spinel-type lithium titanium composite oxide that is a noble material with a lithium storage / release potential of 1.0 V (vs Li / Li + ) or more, for example, It consists of lithium titanate represented by Li 4 Ti 5 O 12 .
  • the negative electrode may contain carbon that acts as a conductive agent.
  • PVDF Polyvinylidene fluoride
  • PAI polyamideimide
  • the nonaqueous electrolytic solution is prepared by dissolving an electrolyte in a nonaqueous solvent.
  • the electrolyte for example, a solution obtained by dissolving LiPF 6 in a nonaqueous solvent at a concentration of 1.0 mol / L is used.
  • an electrolyte other than LiPF 6 lithium salts such as LiBF 4 , LiAsF 6 , LiClO 4 , LiCF 3 SO 3 , LiN (SO 2 CF 3 ) 2 , LiC (SO 2 CF 3 ) 3 , LiAlCl 4 , LiSiF 6 are used. Can be mentioned.
  • LiPF 6 or LiBF 4 is used as the electrolyte.
  • Such an electrolyte is preferably used by being dissolved in a non-aqueous solvent at a concentration of 0.1 mol / L to 3.0 mol / L, and is preferably dissolved at a concentration of 0.5 mol / L to 2.0 mol / L. More preferably, it is used.
  • a non-aqueous solvent a mixed solvent in which propylene carbonate and ⁇ -butyrolactone are mixed at a volume ratio of 6: 4 to 4: 6 is used. It is preferable to prepare the nonaqueous electrolytic solution so that the nonaqueous electrolytic solution contains about 0.1 to 1.0% by mass of trioctyl phosphate, for example.
  • the separator uses a porous film containing polypropylene or polyethylene.
  • a porous film made of polypropylene having a porosity of about 40% to 80% is preferably used as the separator.
  • the liquid content per unit time of the separator with respect to the electrolyte can be further increased.
  • the discharge rate characteristic particularly the high rate characteristic, that is, the large current discharge characteristic.
  • the discharge rate characteristic at 25 ° C., particularly the high rate characteristic can be further improved.
  • Example shown below is an example and this invention is not limited to the following Example.
  • the non-aqueous electrolyte secondary batteries of Examples and Comparative Examples were manufactured by changing the composition of the non-aqueous electrolyte.
  • Lithium-nickel-manganese-cobalt composite oxide represented by the composition formula LiNi 0.33 Mn 0.33 Co 0.33 O 2 as a positive electrode active material, carbon as a conductive agent, and polyvinylidene fluoride (PVDF) as a binder )
  • PVDF polyvinylidene fluoride
  • NMP N-methyl-2-pyrrolidone
  • the basis weight of the positive electrode mixture per unit area at this time was 13.3 mg / cm 2 and the packing density was 3.0 g / cc.
  • the unit capacity of this positive electrode is 1 mol / L LiPF 6 as the electrolyte of the electrolytic solution, and a mixed solvent in which ethylene carbonate (EC) and diethyl carbonate (DEC) are mixed at a volume ratio of 3: 7 as the solvent. Measurement was performed in a voltage range of 2.5 to 4.3 V using lithium metal. As a result, a unit capacity of 150 mAh per 1 g was obtained.
  • a lithium titanate represented by the composition formula Li 4 Ti 5 O 12 as a negative electrode active material, carbon as a conductive agent, and PVDF as a binder were blended in a mass ratio of 93: 3: 4.
  • a negative electrode mixture slurry was prepared by kneading with NMP. This negative electrode mixture slurry was applied to both sides of an aluminum foil as a negative electrode current collector and dried, and then a negative electrode terminal was attached to the one rolled by a rolling roller to produce a negative electrode.
  • the basis weight of the negative electrode mixture per unit area was 14.6 mg / cm 2 , and the packing density was 2.4 g / cc.
  • the unit capacity of this positive electrode is 1 mol / L LiPF 6 as the electrolyte of the electrolytic solution, and a mixed solvent in which ethylene carbonate (EC) and diethyl carbonate (DEC) are mixed at a volume ratio of 3: 7 as the solvent. Measurement was performed in a voltage range of 1.0 to 2.0 V using lithium metal. As a result, a unit capacity of 165 mAh per 1 g was obtained.
  • non-aqueous solvent a mixed solvent in which propylene carbonate (PC) and ⁇ -butyrolactone (GBL) are mixed at a volume ratio of 8: 2, 6: 4, 4: 6, 2: 8 is used.
  • PC propylene carbonate
  • GBL ⁇ -butyrolactone
  • LiPF 6 was dissolved to a concentration of 1 mol / L.
  • the non-aqueous electrolyte of Example 2 were used.
  • a separator 13 having a porosity of 80% made of a lithium ion permeable polypropylene (PP) microporous membrane is interposed between the positive electrode 11 and the negative electrode 12 produced as described above.
  • the battery element (power generation element) 10 was produced by winding in a flat shape.
  • the battery element 10 was accommodated in an outer packaging material 20 made of a laminate film containing aluminum as an intermediate layer.
  • a positive electrode terminal 30 is attached to the positive electrode and a negative electrode terminal 40 is attached to the negative electrode so as to extend from the inside of the outer packaging material 20 to the outside.
  • the batteries were fully charged under the same charging conditions as those for the 1C discharge capacity measurement, and the discharge capacity was measured when each battery was discharged until the voltage became 1.25 V with a discharge current of 750 mA. This discharge capacity was defined as 3C discharge capacity.
  • the battery was fully charged under the same charging conditions as those for the 1C discharge capacity measurement, and the discharge capacity when the discharge current was sequentially increased was measured.
  • the discharge capacity is 1250 mA
  • the discharge capacity is 5 C discharge capacity
  • the discharge capacity is 10 C discharge capacity
  • the discharge current is 3750 mA
  • the discharge capacity is 15 C discharge capacity
  • the discharge current is 50000 A
  • the discharge capacity was set to 20C discharge capacity.
  • FIG. 3 shows the relationship between the discharge rate and the discharge capacity of the nonaqueous electrolyte secondary batteries of Examples 1 and 2 and Comparative Examples 1 and 2 thus obtained.
  • FIG. 4 shows the relationship between the discharge rates and discharge capacity retention rates of the non-aqueous electrolyte secondary batteries of Examples 1 and 2 and Comparative Examples 1 and 2 calculated in this way.
  • FIG. 5 shows the change in the charge capacity with respect to the number of cycles
  • FIG. 6 shows the change in the charge capacity maintenance rate.
  • the discharge rate characteristics of the battery at 25 ° C., particularly the high rate characteristics, specifically the 20C discharge capacity retention rate, of Comparative Example 1 using a non-aqueous electrolyte containing a mixed solvent with a volume ratio of PC: GBL 8: 2
  • Compared with a non-aqueous electrolyte secondary battery it can be suppressed, that is, cycle characteristics can be improved.
  • Example 3 with a battery capacity of 250 mAh (with a porosity of 40), except that the non-aqueous electrolyte was prepared so as to contain 0.5% by mass of trioctyl phosphate. % Separator) and Example 5 (using a separator with a porosity of 80%) non-aqueous electrolyte secondary batteries were fabricated.
  • a separator having a three-layer structure of polypropylene (PP) / polyethylene (PE) / polypropylene (PP) is used as a separator having a porosity of 40%, and a separator made of polypropylene (PP) is used as a separator having a porosity of 80%.
  • the single layer structure was used.
  • Example 4 using a separator with a porosity of 40% and Example 6 using a separator with a porosity of 80%.
  • the measurement result of AC resistance value is also shown about a nonaqueous electrolyte secondary battery.
  • FIG. 7 shows the relationship between the discharge rate and the discharge capacity retention rate measured in the same manner as in FIG. 7 and Example A above.
  • the AC resistance value can be obtained by injecting the nonaqueous electrolyte.
  • the non-aqueous electrolyte decreased to about 1/6 compared with the non-aqueous electrolyte secondary battery of Example 6 that did not contain trioctyl phosphate. It can be seen that the liquidity can be improved.
  • 1 non-aqueous electrolyte secondary battery
  • 10 battery element
  • 11 positive electrode
  • 12 negative electrode
  • 13 separator

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Secondary Cells (AREA)

Abstract

La présente invention concerne une batterie secondaire à électrolyte non aqueux présentant des caractéristiques de décharge d'un courant de forte intensité ainsi que des caractéristiques de cycle améliorées. Un élément (10) d'une batterie secondaire à électrolyte non aqueux est pourvu d'une électrode positive (11), d'une électrode négative (12) et d'une solution d'électrolyte non aqueux. L'électrode négative (12) contient un oxyde complexe lithium-titane du type spinelle. La solution d'électrolyte non aqueux contient un solvant non aqueux dans lequel du carbonate de propylène et du γ-butyrolactone sont mélangés suivant un rapport volumétrique allant de 6:4 à 4:6.
PCT/JP2011/075373 2010-12-01 2011-11-04 Batterie secondaire à électrolyte non aqueux Ceased WO2012073642A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010268387 2010-12-01
JP2010-268387 2010-12-01

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WO2012073642A1 true WO2012073642A1 (fr) 2012-06-07

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001102091A (ja) * 1999-07-29 2001-04-13 Toshiba Corp 非水電解質二次電池
JP2003197190A (ja) * 2001-12-25 2003-07-11 Yuasa Corp 非水電解質二次電池
JP2005093414A (ja) * 2003-03-10 2005-04-07 Sanyo Electric Co Ltd リチウム電池
JP2009021134A (ja) * 2007-07-12 2009-01-29 Toshiba Corp 非水電解質電池及び電池パック
JP2009231245A (ja) * 2008-03-25 2009-10-08 Toshiba Corp 非水電解質電池
JP2010027377A (ja) * 2008-07-18 2010-02-04 Toshiba Corp 電池用活物質、非水電解質電池および電池パック
JP2012006816A (ja) * 2010-06-28 2012-01-12 Hitachi Ltd チタン酸リチウム粒子およびその製造方法、リチウムイオン電池用負極、ならびにリチウム電池

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001102091A (ja) * 1999-07-29 2001-04-13 Toshiba Corp 非水電解質二次電池
JP2003197190A (ja) * 2001-12-25 2003-07-11 Yuasa Corp 非水電解質二次電池
JP2005093414A (ja) * 2003-03-10 2005-04-07 Sanyo Electric Co Ltd リチウム電池
JP2009021134A (ja) * 2007-07-12 2009-01-29 Toshiba Corp 非水電解質電池及び電池パック
JP2009231245A (ja) * 2008-03-25 2009-10-08 Toshiba Corp 非水電解質電池
JP2010027377A (ja) * 2008-07-18 2010-02-04 Toshiba Corp 電池用活物質、非水電解質電池および電池パック
JP2012006816A (ja) * 2010-06-28 2012-01-12 Hitachi Ltd チタン酸リチウム粒子およびその製造方法、リチウムイオン電池用負極、ならびにリチウム電池

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