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WO2002099919A1 - Electrolyte de pile electrochimique - Google Patents

Electrolyte de pile electrochimique Download PDF

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Publication number
WO2002099919A1
WO2002099919A1 PCT/GB2002/002366 GB0202366W WO02099919A1 WO 2002099919 A1 WO2002099919 A1 WO 2002099919A1 GB 0202366 W GB0202366 W GB 0202366W WO 02099919 A1 WO02099919 A1 WO 02099919A1
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WO
WIPO (PCT)
Prior art keywords
electrolyte
volume
cell
range
carbonate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/GB2002/002366
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English (en)
Inventor
Fazlil Coowar
William James Macklin
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AEA TECHNOLOGY BATTERY SYSTEMS Ltd
Accentus Medical PLC
Original Assignee
AEA TECHNOLOGY BATTERY SYSTEMS Ltd
Accentus Medical PLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by AEA TECHNOLOGY BATTERY SYSTEMS Ltd, Accentus Medical PLC filed Critical AEA TECHNOLOGY BATTERY SYSTEMS Ltd
Publication of WO2002099919A1 publication Critical patent/WO2002099919A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • H01M6/00—Primary cells; Manufacture thereof
    • H01M6/14—Cells with non-aqueous electrolyte
    • H01M6/16—Cells with non-aqueous electrolyte with organic electrolyte
    • H01M6/162—Cells with non-aqueous electrolyte with organic electrolyte characterised by the electrolyte
    • H01M6/164—Cells with non-aqueous electrolyte with organic electrolyte characterised by the electrolyte by the solvent
    • 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
    • H01M2300/0031—Chlorinated 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
    • H01M2300/0034—Fluorinated 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
    • 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
    • H01M2300/004—Three 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
    • H01M2300/0042—Four or more 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 relates to an electrolyte for use in a lithium ion cell, and to electrochemical cells incorporating this electrolyte.
  • lithium metal anodes and cathodes of a material into which lithium ions can be intercalated or inserted.
  • Such cells may use, as electrolyte, a solution of a lithium salt in an organic solvent such as propylene carbonate, and a separator such as filter paper or polypropylene.
  • an intercalation material such as graphite has enabled satisfactory cells to be made.
  • Such cells may be referred to as "lithium ion" cells, or “swing” cells, as lithium ions are exchanged between the two intercalation materials during charge and discharge.
  • the electrical properties of the cell are to a significant extent determined by the selection of the electrolyte solvent.
  • Gel or solid electrolytes may be made, as described by Gozdz et al (US 5 296 318) , with a copolymer of 75 to 92% vinylidene fluoride and 8 to 25% hexafluoropropylene as the polymer, this being dissolved in a low boiling- point solvent such as tetrahydrofuran along with a lithium salt and a plasticising electrolyte solvent such as ethylene carbonate/propylene carbonate mixture, and cast from solution.
  • a low boiling- point solvent such as tetrahydrofuran along with a lithium salt
  • a plasticising electrolyte solvent such as ethylene carbonate/propylene carbonate mixture
  • the solvent must not react chemically with the dissolved lithium salt, nor must it react chemically or electrochemically with the electrodes. It desirably has a high dielectric constant, and a low viscosity. It should remain liquid over the expected operating range of the cell, but should have a high boiling point and a high flash point to enhance safety if the cell becomes hot as a result of overcharge. And it should not be too expensive. No one organic liquid has been found to be ideal in all respects .
  • an electrolyte for use in a lithium ion cell comprising an anode layer and a cathode layer each comprising respective lithium ion insertion materials, separated by a separator, the electrolyte comprising gamma- butyrolactone in the range 10-80% by volume, ethylene carbonate in the range 1-30% by volume, and at least one of either vinyl ethylene carbonate in the range 1-8% by volume or methoxyethyl methyl carbonate in the range 8- 80% by volume.
  • gamma-butyrolactone provides good electrical properties it tends to react electrochemically with graphite.
  • the ethylene carbonate (EC) can improve the charge-discharge efficiency, and helps in the formation of a passivating layer on the surface of the graphite (which may be referred to as a "solid/ electrolyte interface" or SEI) .. This passivating layer prevents subsequent side reactions such as reduction of the electrolyte .
  • SEI solid/ electrolyte interface
  • SEI solid/ electrolyte interface
  • This passivating layer prevents subsequent side reactions such as reduction of the electrolyte .
  • the use of a mixture of gBL and EC as solvent for a cell electrolyte is known for example from JP 10-312825 (Toshiba) , but cell properties can be enhanced by adding the other components specified in the present invention.
  • the vinyl ethylene carbonate (VEC) is preferably present at no more than 5% by volume; it is particularly effective at forming a passivating layer which is of low ionic impedance.
  • the methoxyethyl methyl carbonate (MEMC) lowers the melting point of thev electrolyte, so enabling use of the cell at lower temperatures. It is also believed that the -OCH3 group has a role in attaching the solvent molecules during electrochemical reduction, enabling the efficient formation of the SEI as a compact film on the graphite surface.
  • the electrolyte may also comprise chlorodiethyl carbonate (CDEC) (i.e. 1-chloroethyl ethyl carbonate), preferably no more than 5% by volume; this also helps with formation of the passivating layer.
  • CDEC chlorodiethyl carbonate
  • One of the main reason for using this material is it allows graphitic materials to be cycled with gBL (and PC) . It also has the advantages of having a high boiling point (159-1S1°C) and a relatively high flash point (65°C) .
  • the electrolyte may also contain tri-fluoro propylene carbonate (TFPC) , possibly in the range up to 80% by volume, which is more compatible with graphite and also less reactive with the charged cathode material. Carbon dioxide may also be dissolved in the electrolyte with advantage, as this also helps in the formation of the passivating layer.
  • TFPC tri-fluoro propylene carbonate
  • the electrolyte may also contain a dicarbonate such as dimethyl dicarbonate, diethyl dicarbonate or di-tert- butyl dicarbonate, or 1,2 di-phenyl vinylene carbonate, in each case at no more than 10% by volume, preferably about 2%.
  • a dicarbonate such as dimethyl dicarbonate, diethyl dicarbonate or di-tert- butyl dicarbonate, or 1,2 di-phenyl vinylene carbonate, in each case at no more than 10% by volume, preferably about 2%.
  • these additives can also help protect the cell against damage due to overcharge, and also improve rate performance and storage. For example if the cell electrolyte contains 1,2 di-phenyl vinylene carbonate then even when overcharged (at the C rate) to cell voltages above 4.3 V there is no smoke or fire.
  • Such an electrolyte may be used in conjunction with a separator such as microporous polyethylene, or microp ⁇ rous vinylidene fluoride-based polymer, in the latter case forming a gel or solid electrolyte separator.
  • a microporous membrane may be cast from a solvent/non-solvent mixture, or from a latent solvent, s ⁇ that the entire process can be carried out in the absence of water or humidity, reducing the risk of water being present in the final film or membrane (which would be detrimental to the properties of a lithium ion cell) .
  • the non-solvent should not only dissolve in the solvent, but it should be miscible with the solvent in substantially all proportions.
  • the boiling point of the non-solvent is preferably higher than that of the solvent, preferably about 20°C higher.
  • the solvent might be dimethyl formamide or dimethyl acetamide, in which case a suitable non-solvent is 1-octanol which is soluble in those solvents and whose boiling point is about 194°C.
  • the evaporation rate during drying must not be rapid, as rapid drying tends to produce macropores, and also may lead to formation of an impervious skin which prevents evaporation of underlying liquid.
  • the drying process should be carried out at a temperature below the dissolution temperature for the latent solvent. Consequently the polymer precipitates, and it is believed that two phases occur: a polymer-rich phase, and a polymer-poor phase. As the latent solvent evaporates the proportion of the polymer- rich phase gradually increases, but the remaining droplets of polymer-poor phase cause the formation of pores .
  • the electrolyte of the invention is suitable for use with a range of different forms of graphite and carbon in the anode, and for a range of different materials in the cathode . It may for example be used with a cathode comprising the oxides LiCo ⁇ 2 or LiNi ⁇ 2 , or the spinel oxide LiMn 2 ⁇ 4 ; the cathode may also contain conductive material such as carbon black.
  • the electrolyte must have a salt dissolved in it to provide ionic conductivity, this salt for example being LiPF ⁇ , LiBF 4 , lithium imide
  • LiN(CF 3 S0 )2 lithium methide (LiC (S0 CF 3 ) 3 )
  • Figure 1 shows graphically the variation of voltage with charge for a cell of the invention, at different rates of discharge
  • Figure 2 shows graphically the variation of voltage with charge for another cell of the invention, at different rates of discharge
  • Homopolymer PVdF (Solvay grade 6020) , which has a low value of melt flow index (less than 0.7 g/10 min at 10 kg and 230°C), is dissolved in N-methyl pyrrolidone (NMP) at a temperature of 45°C while stirring; 15 g of PVdF were dissolved in 85 g of NMP.
  • NMP N-methyl pyrrolidone
  • a small quantity, 9 g, of 1-octanol is then added dropwise to the polymer solution, and carefully mixed during this addition to ensure the mixture is homogeneous.
  • the quantity of 1- octanol must not be too large, or the solution will gel.
  • the mixture is then mixed for a further period of 2 hours to ensure uniformity.
  • the resulting ternary mixture is then cast, using a doctor blade over a roller, onto an aluminium foil substrate to form a layer initially 0.25 mm thick, and then passed through a 7 m long drying tunnel with two successive drying zones at temperatures of 65°C and 100°C respectively. It moves through the drying tunnel at 0.5 m/min. Within the drying zones the film is exposed to a dry air flow with a velocity of 14 m/s, to remove any solvent and non-solvent that evaporates. The dry air is obtained by passing air through a dehumidifier, so its dewpoint is -40°C.
  • a white polymer membrane is thereby obtained, of thickness about 20 ⁇ m, and analysis with a scanning electron microscope shows it to be microporous.
  • the pores are of size in the range 0.5-2.0 ⁇ m, typically about 1 ⁇ m in diameter, at least at the surface.
  • the membrane has been found to have a porosity of about 53%.
  • a cathode is made by making a mixture of LiCo ⁇ 2
  • NMP N-methyl pyrrolidone
  • An anode is made from a mixture of mesocarbon microbeads of particle size 10 ⁇ m, heat treated at 2800°C (MCMB 1028) , with a small amount of graphite, and homopolymer PVdF 6020 as binder in solution in NMP. This mixture is cast, onto a copper foil, in a similar fashion to that described in relation to the cathode.
  • a cell assembly is then wound with the porous membrane of thickness 20 ⁇ m separating the anode from the cathode.
  • Each such cell assembly is enclosed in a sealed envelope of aluminium laminate, and then vacuum filled with a plasticising liquid electrolyte, for example 1 molar LiBF 4 in an solvent mixture comprising 60.83% gBL,
  • the cell is then charged, aged for two weeks, and then subjected to five discharge and recharge cycles, with the charging and discharging current (in amps) at an estimate of the C/5 value (where C represents the cell capacity in amp hours) , in order to determine the cell capacity, C, this value being referred to as the rated cell capacity.
  • These cells were found to have a rated capacity of 0.61 Ah.
  • the cell is then discharged at a range of different discharge currents.
  • this shows graphically the variation of voltage during discharge of the cell at different discharge currents: C/5, C/2, C and 2C; the larger the discharge current, the lower the cell voltage.
  • the cell does give a smaller capacity at higher discharge currents, nevertheless the capacity remains high (above 95%.) even at the highest discharge current 2C.
  • Two thin microporous copolymer layers ' are made by a similar process, a 12% by weight solution of a copolymer PVdF/6HFP (vinylidene fluoride and 6% by weight hexafluoropropylene) being made by dissolving 12 grams of the copolymer in 88 grams DMF. A small quantity of 1- octanol is then added dropwise to the copolymer solution, and carefully mixed during this addition to ensure the mixture is homogeneous, and is then kept stirred for 2 hours. The resulting ternary mixture is then cast, using a doctor blade over a roller, onto an aluminium foil substrate to form a layer initially 0.06 mm thick, and then dried exactly as described above.
  • PVdF/6HFP vinylene fluoride and 6% by weight hexafluoropropylene
  • the anode and cathode are made by the same process as described above, although in this case the LiCo ⁇ 2 in the cathode was provided by FMC Corp. In both cases the electrodes are double-sided.
  • the cathode is sandwiched between two of the thin copolymer layers so that each surface is completely covered, and these components are laminated together by subjecting them, when placed between release papers, to compressive pressure in a press between rollers giving a compressive force of 20 N, at an elevated temperature of 120°C.
  • the anode is also sandwiched between two thin copolymer layers, and laminated together in the same way.
  • a cell assembly is then wound with a microporous polyethylene membrane of thickness 16 ⁇ m separating the anode from the cathode, this membrane being supplied by Tonen Chemical Corp.
  • Each such cell assembly is enclosed in a sealed envelope of aluminium/plastic laminate, and a small quantity such as 0.5 g of acetone is injected into the envelope.
  • the envelope containing the cell assembly is then held at a temperature of 30°C for a period of at least 5 minutes. This elevated temperature enhances the solvation of the surface of the copolymer layer by the acetone.
  • the cell assembly After cooling to ambient temperature, the cell assembly is removed from the envelope and is then vacuum dried at 60°C for 3 hours to ensure removal of any traces" of acetone.
  • the cell assembly is thenxun vacuum filled with the the four-component plasticising li .iquid electrolyte described above, that is to say 1 molar " LiBF 4 in an solvent mixture comprising 60.83% gBL, 24.33% ⁇ EC, 12.16% MEMC and 2.68% VEC. After storing for 16 houxmurs to ensure the electrolyte has been absorbed 1 by all the cell components, it is then vacuum packed in a - flexible packaging material .
  • a laminated cell of this type may incorporate a different microporous separator in place of the polyethylene membrane, for example a microporous homopolymer PVdF membrane of 6020 PVdF or 1015 PVdF, made as described in relation to the non- laminated cell described above.
  • a microporous homopolymer PVdF membrane of 6020 PVdF or 1015 PVdF made as described in relation to the non- laminated cell described above.
  • the molecular weights of the homopolymers are 240 000 and 300 000 respectively.
  • the ' microporous separator must be of a material that is not significantly solvated by the acetone, as it is important that its porosity is
  • the benefits of the present invention are (i) high boiling and high flash point electrolyte necessary for safety issues, and (ii) low swelling of cells when this electrolyte is used. It is clear from the discharge graphs in the figures that both the non-laminated and laminated cells have good electrical properties.

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

Abstract

La présente invention concerne une pile à ion lithium comprenant une couche d'anode et une couche de cathode, qui présentent respectivement des matériaux d'insertion d'ion lithium, séparés par un séparateur. L'électrolyte comprend de 10 à 80 % en volume de gamma-butyrolactone, de 1 à 30 % en volume de carbonate d'éthylène, de 1 à 8 % en volume de carbonate d'éthylène vinylique et/ou de 8 à 80 % en volume de carbonate de méthyle méthoxyéthylique. Cette pile présente des propriétés électriques satisfaisantes et est comparativement sûre en cas de surcharge du fait que les composants de l'électrolyte présentent un haut point d'ébullition et de hauts points d'éclair.
PCT/GB2002/002366 2001-06-05 2002-05-21 Electrolyte de pile electrochimique Ceased WO2002099919A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GBGB0113544.1A GB0113544D0 (en) 2001-06-05 2001-06-05 Electrochemical cell electrolyte
GB0113544.1 2001-06-05

Publications (1)

Publication Number Publication Date
WO2002099919A1 true WO2002099919A1 (fr) 2002-12-12

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PCT/GB2002/002366 Ceased WO2002099919A1 (fr) 2001-06-05 2002-05-21 Electrolyte de pile electrochimique

Country Status (3)

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GB (1) GB0113544D0 (fr)
TW (1) TW544969B (fr)
WO (1) WO2002099919A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130095379A1 (en) * 2004-04-20 2013-04-18 Minoru Kotato Nonaqueous electrolyte solution and lithium secondary battery using same

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000079632A1 (fr) * 1999-06-18 2000-12-28 Mitsubishi Chemical Corporation Batterie secondaire du type a solution electrolytique non aqueuse
EP1146586A2 (fr) * 2000-04-11 2001-10-17 Matsushita Electric Industrial Co., Ltd. Batterie secondaire à électrolyte nonaqueux
JP2002015771A (ja) * 2000-04-28 2002-01-18 Toshiba Corp 非水電解質及び非水電解質二次電池
EP1193788A2 (fr) * 2000-09-28 2002-04-03 Kabushiki Kaisha Toshiba Electrolyte nonaqueux et batterie secondaire à électrolyte nonaqueux

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000079632A1 (fr) * 1999-06-18 2000-12-28 Mitsubishi Chemical Corporation Batterie secondaire du type a solution electrolytique non aqueuse
EP1205996A1 (fr) * 1999-06-18 2002-05-15 Mitsubishi Chemical Corporation Batterie secondaire du type a solution electrolytique non aqueuse
EP1146586A2 (fr) * 2000-04-11 2001-10-17 Matsushita Electric Industrial Co., Ltd. Batterie secondaire à électrolyte nonaqueux
JP2002015771A (ja) * 2000-04-28 2002-01-18 Toshiba Corp 非水電解質及び非水電解質二次電池
EP1193788A2 (fr) * 2000-09-28 2002-04-03 Kabushiki Kaisha Toshiba Electrolyte nonaqueux et batterie secondaire à électrolyte nonaqueux

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; SEKINO, MASAHIRO ET AL: "Nonaqueous electrolyte solution and secondary nonaqueous electrolyte battery", XP002211588, retrieved from STN Database accession no. 136:105137 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130095379A1 (en) * 2004-04-20 2013-04-18 Minoru Kotato Nonaqueous electrolyte solution and lithium secondary battery using same

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GB0113544D0 (en) 2001-07-25
TW544969B (en) 2003-08-01

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