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WO2018029991A1 - Batterie secondaire redox au vanadium et film conducteur d'ions pour batteries - Google Patents

Batterie secondaire redox au vanadium et film conducteur d'ions pour batteries Download PDF

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Publication number
WO2018029991A1
WO2018029991A1 PCT/JP2017/022662 JP2017022662W WO2018029991A1 WO 2018029991 A1 WO2018029991 A1 WO 2018029991A1 JP 2017022662 W JP2017022662 W JP 2017022662W WO 2018029991 A1 WO2018029991 A1 WO 2018029991A1
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Prior art keywords
diaphragm
battery
vanadium
thickness
less
Prior art date
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Ceased
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PCT/JP2017/022662
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English (en)
Japanese (ja)
Inventor
吉田　茂樹
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Brother Industries Ltd
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Brother Industries Ltd
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Filing date
Publication date
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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
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • 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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/489—Separators, membranes, diaphragms or spacing elements inside the cells, characterised by their physical properties, e.g. swelling degree, hydrophilicity or shut down properties
    • 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 defines a vanadium redox secondary battery that contains vanadium ions or vanadium ions as an active material and charges and discharges using an oxidation-reduction reaction by the active material, and a positive electrode and a negative electrode.
  • the present invention relates to an ion conductive membrane for a battery used for a diaphragm or the like.
  • an ion exchange membrane is often used as the diaphragm.
  • the cost per unit area of the ion exchange membrane is high, there is a problem that the cost of the entire vanadium redox secondary battery using the ion exchange membrane is increased.
  • diaphragms for lithium ion secondary batteries and lead storage batteries as diaphragms for vanadium redox secondary batteries, low cost and excellent input / output characteristics (rate characteristics) can be realized, but ion selectivity is insufficient. Therefore, there is a problem that the self-discharge characteristics and the Coulomb efficiency (cycle characteristics) when the battery cycle is repeated are poor.
  • the vanadium redox secondary battery according to the present invention includes a positive electrode containing an active material containing vanadium ions or vanadium-containing ions, a negative electrode containing an active material containing vanadium ions or vanadium-containing ions, A diaphragm for partitioning a positive electrode and a negative electrode, and the diaphragm includes an ethylene vinyl alcohol copolymer having an ethylene ratio of 30 mol% or less, from an X-ray diffraction pattern of the ethylene vinyl alcohol copolymer.
  • the obtained crystallite size (crystallite size t) is 1.3 nm or more and 8.8 nm or less.
  • 5 is a graph showing a relationship between a charge rate characteristic @ 10 mA / cm 2 and a lattice constant in a battery of an example having a diaphragm having a thickness of 10 ⁇ m.
  • 5 is a graph showing a relationship between a discharge rate characteristic @ 10 mA / cm 2 and a lattice constant in a battery of an example having a diaphragm having a thickness of 10 ⁇ m.
  • 6 is a graph showing the relationship between charge rate characteristics @ 10 mA / cm 2 and thickness in a battery of an example in which the ethylene ratio is 24 mol% and the crystallite size is 5 nm or less.
  • 5 is a graph showing the relationship between discharge rate characteristics @ 10 mA / cm 2 and thickness in a battery of an example having an ethylene ratio of 24 mol% and a crystallite size of 5 nm or less. It is a graph which shows the relationship between a voltage maintenance factor and thickness in the battery of the Example whose ethylene ratio is 24 mol% and crystallite size is 5 nm or less.
  • 6 is a graph showing the relationship between the sheet resistance value and the crystallite size in the diaphragm of the example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m.
  • 6 is a graph showing the relationship between pentavalent ion transmission concentration and crystallite size in a diaphragm of an example in which the ethylene ratio is 25 to 29% and the thickness is 10 ⁇ m.
  • 4 is a graph showing the relationship between sheet resistance and lattice constant in a battery of an example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m.
  • 6 is a graph showing the relationship between pentavalent ion transmission density and lattice constant in a battery of an example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m.
  • 6 is a graph showing a relationship between charge rate characteristics @ 10 mA / cm 2 and crystallite size in a battery of an example in which an ethylene ratio is 25 to 29 mol% and a thickness is 10 ⁇ m.
  • 6 is a graph showing the relationship between discharge rate characteristics @ 10 mA / cm 2 and crystallite size in a battery of an example having an ethylene ratio of 25 to 29 mol% and a thickness of 10 ⁇ m.
  • 6 is a graph showing the relationship between the charge rate characteristic @ 10 mA / cm 2 and the lattice constant in the battery of the example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m.
  • 6 is a graph showing the relationship between the discharge rate characteristic @ 10 mA / cm 2 and the lattice constant in a battery of an example having an ethylene ratio of 25 to 29 mol% and a thickness of 10 ⁇ m.
  • 6 is a graph showing the relationship between CE at 20th cycle and crystallite size in a battery of an example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m.
  • 6 is a graph showing the relationship between the CE at the 20th cycle and the lattice constant in the battery of the example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m.
  • 6 is a graph showing the relationship between the voltage maintenance ratio and the crystallite size in a battery of an example in which the ethylene ratio is 25 to 29 mol% and the thickness is 10 ⁇ m. 6 is a graph showing the relationship between the voltage maintenance ratio and the lattice constant in a battery of an example having an ethylene ratio of 25 to 29 mol% and a thickness of 10 ⁇ m.
  • the positive electrode terminal 3 and the negative electrode terminal 4 protrude from a part of the peripheral edge portion of the outer bag 2 in a state where the base end side is covered with the sealing materials 30 and 40.
  • the battery 1 alone or a combination of the battery 1 and another battery 1 may be accommodated in a case (not shown).
  • the electrode material 5 includes an electrode 50, a conductor 51, a protective layer 52, and a sealant 54.
  • the conductor 51 has a rectangular flat plate shape and is disposed on the upper surface of the lower half 22 in FIG. 2 of the outer bag 2, and the upper surface of the conductor 51 is covered with a protective layer 52.
  • a square plate-like electrode 50 is provided on the inner side of the peripheral edge of the upper surface of the protective layer 52.
  • the sealant 54 has a frame shape having an edge portion, and is bonded to the peripheral edge portion and the half body 22. The conductor 51 is sealed by the half body 22 and the protective layer 52.
  • the half 22 is electrolyte impermeable.
  • the half 22 is preferably composed of a laminate sheet containing a synthetic resin layer and a metal layer.
  • the material for the synthetic resin layer include polypropylene, polyethylene, polyamide such as nylon 6, nylon 66, and the like.
  • the material for the metal layer include aluminum, aluminum alloy, copper, copper alloy, iron, stainless steel, titanium, and titanium alloy.
  • the planar area of the conductor 51 is smaller than the planar area of the half body 22.
  • the conductor 51 is preferably made of a metal foil such as copper, aluminum, or nickel.
  • the conductor 51 has a tab (not shown) protruding from a part of the peripheral edge, and the tip of the tab is connected to the positive electrode terminal 3.
  • the protective layer 52 is formed by providing a graphite sheet on one surface of the conductor 51 with, for example, a conductive adhesive sheet.
  • the material of the protective layer 52 is not limited to the graphite sheet.
  • the protective layer 52 may be conductive and non-permeable to electrolyte solution, and a conductive film or a sheet-like conductive rubber may be used.
  • the protective layer 52 is formed by coating one surface of the conductor 51 with a coating liquid in which a carbon material such as graphite powder, carbon black, and carbon nanotubes and a binder are mixed and then drying. Also good. Further, when the aqueous electrolyte is not acidic or alkaline and there is no possibility that the conductor 51 is corroded, the protective layer 52 may not be provided.
  • the electrode 50 is provided inside the peripheral edge of the upper surface of the protective layer 52, that is, at a portion other than the peripheral edge of the upper surface of the protective layer 52.
  • the electrode 50 includes a carbon material and vanadium (V) ions whose oxidation number changes between pentavalent and tetravalent by an oxidation-reduction reaction, or ions containing V whose oxidation number changes between pentavalent and tetravalent.
  • a positive electrode active material made of a vanadium solid salt containing a solid material containing a binder, and an aqueous electrolyte.
  • the pentavalent and ions containing the V oxidation number changes between tetravalent, VO 2+ (IV), VO 2 + (V) are exemplified.
  • the vanadium compound which is an active material for the positive electrode include vanadium oxide (IV) (VOSO 4 ⁇ nH 2 O) and vanadium oxide (V) ((VO 2 ) 2 SO 4 ⁇ nH 2 O). it can.
  • N represents an integer of 0 to 6.
  • binder examples include polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), and a copolymer of vinylidene fluoride and hexafluoropropylene (PVDF / HFP).
  • PTFE polytetrafluoroethylene
  • PVDF polyvinylidene fluoride
  • HFP hexafluoropropylene
  • Examples of the carbon material of the electrode 50 include carbon black such as acetylene black and ketjen black (registered trademark), and graphite.
  • the carbon material can use 1 type (s) or 2 or more types.
  • the aqueous electrolyte contained in the electrode 50 is preferably an aqueous sulfuric acid solution.
  • As the sulfuric acid aqueous solution for example, sulfuric acid having a concentration of less than 90% by mass can be used.
  • the amount of the electrolyte is not excessive or deficient so that the SOC of the battery can be taken from 0 to 100%.
  • the amount of the electrolytic solution is, for example, 70 mL of 2M sulfuric acid with respect to 100 g of the vanadium compound.
  • the inner edge 54 a of the sealant 54 is bonded to the peripheral edge of the upper surface of the protective layer 52, and the inner side surface of the inner edge 54 a is in contact with the side surface of the electrode 50.
  • the outer edge portion 54 b is bonded to the outer surface of the conductor 51 on the surface of the half body 22 on the conductor 51 side.
  • the conductor 51 and the protective layer 52 are sandwiched between the half body 22 and the sealant 54. That is, the conductor 51 is fixed to the half body 22 in a state where the conductor 51 is sealed by the half body 22, the protective layer 52, and the sealant 54.
  • the side surface of the conductor 51 may be bonded to the sealant 54, or may not be bonded.
  • Examples of the material of the sealant 54 include polypropylene or polyethylene. By using polypropylene or polyethylene, the conductor 51 can be easily sealed by heat welding.
  • the electrode material 6 has the same configuration as the electrode material 5, and includes an electrode 60, a conductor 61, a protective layer 62, and a sealant 64.
  • the conductor 61 has a rectangular flat plate shape, and is disposed on the lower surface in FIG. 2 of the half body 21 of the outer bag 1, and the lower surface of the conductor 61 is covered with a protective layer 62.
  • a rectangular flat plate-like electrode 60 having an active material, a carbon material, a binder, and an aqueous electrolyte is provided inside the peripheral edge of the lower surface of the protective layer 62.
  • the lower limit value of the ethylene ratio was determined from the product of the sheet resistance value and the pentavalent ion permeation concentration based on the results of FIGS. In this case, it is preferably 21 mol%.
  • the lower limit value of the ethylene ratio is preferable in the order of 22 mol%, 24 mol%, and 25 mol%, and the upper limit value is preferable in the order of 29 mol%, 28 mol%, and 27 mol%.
  • the crystallite size When the crystallite size is 1.3 nm or more and 8.8 nm or less, the area resistance value of the diaphragm 7 is low and the ion selectivity is good. Since the low sheet resistance value and the high ion selectivity are well balanced, the cycle characteristics, input / output characteristics, and self-discharge characteristics of the battery 1 having the diaphragm 7 are good.
  • the lower limit of the crystallite size is preferably 1.5 nm, 2 nm, 3 nm, 3.2 nm, and 3.3 nm in this order, and the upper limit is 7.8 nm, 7.0 nm, 6.8 nm, 6.5 nm, 6 nm, and 5.5 nm. Are preferred in this order.
  • the diaphragm 7 preferably has a thickness of 90 ⁇ m or less.
  • the area resistance value of the diaphragm 7 is low and the ion selectivity is good. Since the low sheet resistance value and the high ion selectivity are well balanced, the cycle characteristics, input / output characteristics, and self-discharge characteristics of the battery 1 having the diaphragm 7 are good.
  • the lower limit value of the thickness is preferable in the order of 15 ⁇ m and 20 ⁇ m, and the upper limit value is preferable in the order of 80 ⁇ m, 60 ⁇ m and 40 ⁇ m.
  • the battery according to the present embodiment may include an anion exchange membrane 8 that is an anion exchange resin between the diaphragm 7 and the positive electrode 50.
  • FIG. 3 is a schematic cross-sectional view showing a battery 11 having an anion exchange membrane 8 between the diaphragm 7 and the positive electrode 50. Thereby, the oxidation of the diaphragm 7 is suppressed. The cycle characteristics and self-discharge characteristics of the battery 11 are better.
  • the anion exchange membrane 8 is preferably a fluorine-based anion exchange membrane from the viewpoint of good oxidation resistance. And it is preferable that the thickness of the anion exchange membrane 8 is 50 micrometers or less from a viewpoint of suppressing the increase in resistance.
  • the diaphragm 7 and the anion exchange membrane 8 are not separate and may be integrated. That is, the diaphragm 7 may be provided with an anion exchange resin layer.
  • the battery ion conductive membrane according to the embodiment (hereinafter referred to as “ion conductive membrane”) has an ethylene ratio of 30 mol% or less and a crystallite size determined from an XRD pattern of 1.3 nm or more. It has a base layer containing EVOH that is 8.8 nm or less.
  • the ion conductive membrane has good ion selectivity while maintaining a low sheet resistance value, and can pass hydrogen ions (protons) or sulfate ions.
  • the lattice constant determined from the EVOH XRD pattern is preferably 0.435 nm or more and 0.453 nm or less.
  • the sheet resistance value of the ion conductive membrane is low and the ion selectivity is good. Since the low sheet resistance value and the high ion selectivity are well balanced, the cycle characteristics, input / output characteristics, and self-discharge characteristics of the battery having the ion conductive membrane are good.
  • the lower limit values of the lattice constant are preferable in the order of 0.436 nm, 0.437 nm, and 0.438 nm, and the upper limit values are preferable in the order of 0.452 nm, 0.448 nm, 0.446 nm, 0.444 nm, 0.442 nm, and 0.441 nm. .
  • the area resistance value of the base layer of the ion conductive membrane measured at 1 kHz in 0.5 M sulfuric acid is preferably 10 ⁇ ⁇ cm 2 or less. In this case, the input / output characteristics of the battery having the ion conductive film are good.
  • Upper limit of the sheet resistivity is 9 ⁇ ⁇ cm 2, 8 ⁇ ⁇ cm 2, preferably in the order of 7 Ohm ⁇ cm 2.
  • the ion conductive membrane can be used for vanadium redox secondary batteries, redox flow batteries, lead storage batteries, nickel metal hydride batteries, silver oxide batteries, fuel cell diaphragms, and the like.
  • the ethylene ratio, thickness, lattice constant, or crystallite size is set according to the required battery cycle characteristics, input characteristics, output characteristics, and self-discharge characteristics, and the area resistance value and pentavalent ion transmission concentration are set. Select an ion-conducting membrane with controlled pressure.
  • EVOH resin pellets (“M100B”, ethylene ratio 24 mol%, manufactured by Kuraray Co., Ltd.) formed into a film were used.
  • the size of the apparatus, the die and the extruder used for film forming is as follows.
  • the area resistance values of the diaphragm 7 and the films of Comparative Examples 1 to 3 were measured using an ion exchange membrane resistance measuring instrument manufactured by AGC Engineering Co., Ltd.
  • the resistance measurement conditions are as follows. Electrolyte: 0.5M sulfuric acid Frequency: 1kHz
  • the pentavalent ion transmission concentration was measured as follows. Between the flange glass cells of the H-type cell, the diaphragm 7 as a measurement object and the film of the comparative example were sandwiched separately, and the flange glass cell was fixed with a flange fixing clamp. An H-type cell (model name: VB-9) manufactured by EC Frontier Co., Ltd. was used as the H-type cell. The inner diameter of the flange portion in the flange glass cell is 12 mm.
  • V vanadium oxide sulfate
  • ICPE-9000 high frequency inductively coupled plasma
  • the diaphragm 7 of Example 1 has a slightly higher area resistance than the films of Comparative Examples 1 to 3, but the pentavalent ion permeation concentration is significantly lower than that of Comparative Examples 1 to 3, indicating that the area resistance is lower. It can be seen that the ion selectivity is improved without a significant increase.
  • the battery of Example 1 has higher 20th cycle capacity, 40th cycle capacity, 20th cycle CE, and 40th cycle CE than the batteries of Comparative Examples 1 to 3, and the cycle characteristics are good. It can be seen that the rate characteristics and the discharge rate characteristics are high, the input / output characteristics are good, the voltage maintenance ratio after 80 hours is high, and the self-discharge characteristics are good.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Cell Separators (AREA)

Abstract

L'invention concerne : une batterie secondaire redox au vanadium qui possède des caractéristiques de cycle, des caractéristiques d'entrée/sortie et des caractéristiques d'auto-décharge, qui sont bonnes, et qui peut être produite à bas coût ; ainsi qu'un film conducteur d'ions pour batteries. Selon la présente invention, une batterie 1 est pourvue : d'une électrode positive 50 qui contient un matériau actif contenant des ions vanadium ou des ions contenant du vanadium ; d'une électrode négative 60 qui contient un matériau actif contenant des ions vanadium ou des ions contenant du vanadium ; et d'un diaphragme 7 qui sépare l'électrode positive 50 et l'électrode négative 60 l'une de l'autre. Le diaphragme 7 contient un copolymère d'éthylène alcool vinylique ayant un rapport éthylène de 30 % en moles ou moins ; et la taille des cristallites du copolymère d'éthylène-alcool vinylique, telle que déterminée à partir du diagramme de diffraction des rayons X, est comprise entre 1,3 nm et 8,8 nm (inclus).
PCT/JP2017/022662 2016-08-09 2017-06-20 Batterie secondaire redox au vanadium et film conducteur d'ions pour batteries Ceased WO2018029991A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2016156747A JP2018026242A (ja) 2016-08-09 2016-08-09 バナジウムレドックス二次電池、及び電池用イオン伝導性膜
JP2016-156747 2016-08-09

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021215126A1 (fr) * 2020-04-24 2021-10-28 旭化成株式会社 Membrane pour batteries à flux redox, procédé de production de membrane pour batteries à flux redox, ensemble d'électrode à membrane pour batteries à flux redox, élément pour batteries à flux redox et batterie à flux redox

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1044232A (ja) * 1996-08-02 1998-02-17 Unitika Ltd 二軸配向エチレン−ビニルアルコール共重合体フィルム及びその製造方法
JP2009290116A (ja) * 2008-05-30 2009-12-10 Kaneka Corp エネルギー貯蔵デバイス
WO2011049103A1 (fr) * 2009-10-20 2011-04-28 国立大学法人東北大学 Pile au vanadium
JP2011228034A (ja) * 2010-04-16 2011-11-10 Japan Vilene Co Ltd リチウムイオン二次電池
JP2013084521A (ja) * 2011-10-12 2013-05-09 National Institute Of Advanced Industrial & Technology 耐熱性リチウムイオン二次電池
WO2016006075A1 (fr) * 2014-07-10 2016-01-14 日新電機 株式会社 Batterie à flux rédox

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1044232A (ja) * 1996-08-02 1998-02-17 Unitika Ltd 二軸配向エチレン−ビニルアルコール共重合体フィルム及びその製造方法
JP2009290116A (ja) * 2008-05-30 2009-12-10 Kaneka Corp エネルギー貯蔵デバイス
WO2011049103A1 (fr) * 2009-10-20 2011-04-28 国立大学法人東北大学 Pile au vanadium
JP2011228034A (ja) * 2010-04-16 2011-11-10 Japan Vilene Co Ltd リチウムイオン二次電池
JP2013084521A (ja) * 2011-10-12 2013-05-09 National Institute Of Advanced Industrial & Technology 耐熱性リチウムイオン二次電池
WO2016006075A1 (fr) * 2014-07-10 2016-01-14 日新電機 株式会社 Batterie à flux rédox

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