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WO2020053920A1 - Matériau conducteur d'ions, couche fonctionnelle pour batterie et son procédé de production - Google Patents

Matériau conducteur d'ions, couche fonctionnelle pour batterie et son procédé de production Download PDF

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Publication number
WO2020053920A1
WO2020053920A1 PCT/JP2018/033375 JP2018033375W WO2020053920A1 WO 2020053920 A1 WO2020053920 A1 WO 2020053920A1 JP 2018033375 W JP2018033375 W JP 2018033375W WO 2020053920 A1 WO2020053920 A1 WO 2020053920A1
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WO
WIPO (PCT)
Prior art keywords
ion
conductive material
battery
anion
material according
Prior art date
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Ceased
Application number
PCT/JP2018/033375
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English (en)
Japanese (ja)
Inventor
和樹 前田
山田　裕久
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.)
Kyoeisha Chemical Co Ltd
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Kyoeisha Chemical Co Ltd
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 Kyoeisha Chemical Co Ltd filed Critical Kyoeisha Chemical Co Ltd
Priority to PCT/JP2018/033375 priority Critical patent/WO2020053920A1/fr
Priority to JP2019160806A priority patent/JP7401889B2/ja
Publication of WO2020053920A1 publication Critical patent/WO2020053920A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • 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
    • H01M10/24—Alkaline accumulators
    • H01M10/30—Nickel accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M12/00—Hybrid cells; Manufacture thereof
    • H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • 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
    • 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to an ion conductive material exhibiting excellent ion conductivity, a functional layer for a battery, and a method for producing the same.
  • Layered double hydroxide (hereinafter, also referred to as LDH) is a substance having an exchangeable anion and H 2 O as an intermediate layer between layered hydroxide layers. It is used as a dispersant and a dispersant in a polymer for improving heat resistance.
  • LDH has recently attracted attention as an ion conductive material, and its addition to an electrolyte of an alkaline fuel cell and a catalyst layer of a zinc-air battery has been studied. Furthermore, the use as an electrolyte for fuel cells and secondary batteries using alkaline electrolytes (alkaline fuel cells, alcohol fuel cells, metal-air secondary batteries, nickel hydrogen secondary batteries and Zn-Ni secondary batteries) Expected.
  • LDHs which have been mainly studied for use as ion conductive materials are Mg / Al-based layered double hydroxides in which carbonate ions are intercalated between layers, and layered composites using Zn as a divalent metal.
  • hydroxides as ionic conductors This is presumed to be due to the fact that LDH containing Zn is more difficult to manufacture than Mg / Al-based ionic conductors, and is likely to generate zinc oxide as an impurity.
  • no sufficient study has been made on a layered double hydroxide in which ions other than carbonate ions are intercalated between layers. This is also presumed to be due to the ease of production of the layered double hydroxide in which carbonate ions were intercalated.
  • a method of heating a metal compound as a raw material in an aqueous medium containing urea is known. According to such a method, urea is gradually decomposed by heating, thereby changing the pH and forming a layered hydroxide, and carbonate ions generated by the decomposition of urea are intercalated between the layers.
  • Such a production method was considered suitable for a method for producing an LDH in which carbonate ions were intercalated, but was not suitable for a method for producing an LDH having a small content of carbonate ions. Therefore, an LDH in which carbonate ions are intercalated by such a production method is produced, and this carbonate ion is replaced with another anion. However, such a method cannot sufficiently reduce the amount of carbonate ions.
  • Patent Literature 1 discloses a layered double hydroxide that can be used as an ion conductor. However, disclosed herein is an Mg / Al-based layered double hydroxide, which is specifically described with respect to a double hydroxide-based layered double hydroxide using zinc as a divalent metal. Not.
  • Patent Document 2 describes a double hydroxide containing Ni, Al, Ti, and Zn. However, used herein are double hydroxides containing many types of metals. Further, although a method for producing a double hydroxide using urea is disclosed, it has been clarified that carbonate ions are trapped between layers.
  • Patent Literature 3 discloses a solid alkaline fuel cell using LDH as a separator. However, even here, only the Mg / Al-based LDH is specifically described, and the one using zinc as the divalent metal is not specifically described.
  • Patent Documents 1 to 3 described above disclose a method for producing LDH using urea.
  • JP 2018-100191 A JP 2018-58766 A JP, 2018-46017, A
  • An object of the present invention is to provide a novel ion conductive material having excellent ion conductivity and a method for producing the same.
  • the present invention is a layered double hydroxide wherein the divalent metal is Zn,
  • the intensity ratio (In / Ic) of the sum of the diffraction intensities (In) of the crystal phase incorporating anions other than carbonate ions and the diffraction intensity (Ic) of the crystal phase incorporating carbonate ions measured by X-ray diffraction is 1
  • An ion conductive material characterized by the above.
  • the ion conductive material preferably has a structural formula represented by the following composition formula. [Zn 1-x M III x (OH) 2] [A n- x / n] ⁇ mH 2 O M III is a trivalent metal and is at least one selected from Al, Fe and Co, and An- represents an n-valent anion. 0.25 ⁇ x ⁇ 0.50 0 ⁇ m ⁇ 2
  • the ion-conductive material the anion represented by A n- is nitrate ion, a hydroxide ion, a chloride ion, a bromine ion, an iodine ion, dodecylsulfate ion, selected from the group consisting of dodecylbenzene sulfonic acid ion It is preferably at least one anion.
  • the anion represented by A n- contains a nitrate ion.
  • the present invention also provides a functional layer for a battery, wherein the above-mentioned ion conductive material is partially or wholly used.
  • the present invention is also a battery having at least a part of the battery functional layer described above.
  • the present invention is also the method for producing an ionic conductive material, comprising a step of mixing the raw materials in an aqueous medium containing urea under heating and reflux conditions.
  • the ion conductive material of the present invention can obtain an ion conductivity superior to the conventional one. Further, it is a method for easily and inexpensively producing an ion conductive material having such performance.
  • the present invention is an ion-conductive material that is a layered double hydroxide in which the divalent metal is zinc. Further, it is characterized in that there are few phases derived from carbonate ions in ions taken in between layers.
  • the present invention has completed the present invention by finding that LDH in which the divalent metal is zinc and the amount of carbonate ions is reduced has a significantly improved ionic conductivity over known ionic conductive materials.
  • Zn in the general formula may be partially substituted with another divalent metal.
  • the divalent metal that may be substituted is not particularly limited, and examples thereof include Mg, Ca, Cu, Zr, Co, Ni, Fe, and Mn.
  • it is preferable that 50 mol% or more of the divalent metal is zinc. More preferably, at least 60 mol% is zinc, and at least 80 mol% is zinc.
  • M III represents a trivalent metal, and is preferably at least one selected from the group consisting of Al, Fe and Co.
  • Al is preferably at least 50 mol% of the trivalent metal. More preferably, at least 60 mol% is zinc, and at least 80 mol% is zinc.
  • the layered double oxide using Al is particularly preferable from the viewpoints of being inexpensive, having no change in valence, and having excellent stability.
  • a n- in the general formula is not particularly limited, and may be, for example, a group consisting of nitrate ion, hydroxide ion, chloride ion, bromide ion, iodine ion, dodecyl sulfate ion, and dodecylbenzene sulfonate ion.
  • nitrate ions are particularly preferred.
  • Nitrate ions are preferable in that they have excellent ionic conductivity and can be easily synthesized by the present method.
  • the LDH of the present invention has a low content of carbonate ions.
  • the sum of the diffraction intensities (It) of the (003) peak (Ic) of carbonate-type LDH and the (003) peak of other anion-type LDH obtained from powder X-ray diffraction measurement (It) ), And (It / Ic) is 1 or more.
  • Such a material is particularly excellent in ionic conduction performance.
  • the strength ratio is more preferably 3 or more, and further preferably 17 or more.
  • the anion contained between layers in the LDH of the present invention is preferably a nitrate ion.
  • the intensity ratio (In / Ic) between the diffraction intensity (In) of the crystal phase incorporating the nitrate ions and the diffraction intensity (Ic) of the crystal phase incorporating the carbonate ions, measured by X-ray diffraction, is as described above (It). / Ic).
  • the ion conductive material of the present invention is not particularly limited in its particle shape, particle size, and the like.
  • the particle diameter is preferably set to 10 ⁇ m or less.
  • the particle diameter is a value measured by measuring the major axis of 50 particles in an electron micrograph and averaging the major axes.
  • the method for producing a layered double hydroxide of the present invention is not particularly limited, but it is preferable to select production conditions such that carbonate ions are not taken in between layers.
  • urea is used in a reaction in an aqueous medium, and the pH is increased (for example, pH 7.0 or more) by ammonia generated by thermally decomposing the urea to form a layered double hydroxide. Is preferred.
  • the production method using urea is a known method for producing a layered double hydroxide. This is to control the pH by ammonia generated by the thermal decomposition of urea under heating. However, in the thermal decomposition of urea, carbonate ions are generated in addition to ammonia. If a layered double hydroxide in which carbonate ions are intercalated between layers is obtained, the presence of such carbonate ions is preferable, but the layered double hydroxide having a reduced amount of carbonate ions as in the present invention. In order to obtain an oxide, such generation of carbonate ions is not preferable.
  • a layered double hydroxide having a reduced amount of carbonate ions can be obtained by adopting a production method in which an open system reaction is performed in consideration of such points. That is, in the present invention, in order to exclude carbonate ions, it is preferable that carbon dioxide is distilled out of the system so that the carbonate ions do not remain in the system. Specifically, a method of heating and refluxing in an open system can be mentioned.
  • Heating / refluxing '' refers to conducting a reaction while heating a reaction solution at a temperature equal to or higher than the boiling point of water under open conditions, providing a cooling pipe in the outlet path of the open system, cooling the vaporized water vapor again to water Means that the reaction is carried out while returning to the reaction vessel. By reacting in this manner, carbon dioxide gas is removed, and a layered double hydroxide having a small amount of carbonate ions can be obtained.
  • the reaction is performed by dissolving and dispersing the metal compound as a raw material in water at a mixing ratio corresponding to the amount of metal in the target double hydroxide, further adding urea, and refluxing under heating conditions.
  • a mixing ratio corresponding to the amount of metal in the target double hydroxide
  • urea urea
  • the molar concentration of the divalent and trivalent metals in the reaction solution was 0.15 M. However, in principle, any concentration can be used to synthesize a layered double hydroxide without any problem.
  • urea / M III 3.0 to 9.0 (molar ratio).
  • zinc oxide may be generated.
  • carbonate ions it is preferable to use urea within the above range to make the change in pH moderate.
  • a salt compound of a metal and an anion intercalated between layers of the layered double hydroxide is preferable.
  • a nitrate compound as a raw material.
  • the use of a carbonate compound is not preferable because a carbonate compound easily becomes an intercalated compound between layers.
  • the reaction conditions it is important to select conditions under which carbonate ions are easily discharged out of the system as carbon dioxide gas. That is, it is preferable that the system at the time of the reaction be an open system and the reaction temperature be as high as 80 ° C. or higher. The processing time is preferably from 6 to 72 hours. It is preferable to use an open system container as the reaction container.
  • the reaction can be performed while bubbling an inert gas such as argon or nitrogen. With such a method, the amount of carbonate ions can be further reduced.
  • a compound corresponding to the structure may be mixed in the mixture. In this case, it can be carried out by adding the corresponding acid to the system.
  • the obtained layered double hydroxide can be made into a powdery state by filtering, washing and drying as necessary.
  • the present invention is also a functional layer formed by the above-mentioned layered double hydroxide. That is, the above-mentioned layered double hydroxide is formed into a layer shape by any known method.
  • the formation into such a layer structure is not particularly limited, and examples thereof include a method by compression molding, and a method of forming a layer structure by molding a resin by adding a binder resin.
  • a binder resin When a binder resin is used, it may be a thermoplastic resin or a curable resin such as a thermosetting resin or an energy ray-curable resin.
  • the functional layer is not particularly limited, and can be used for a solid electrolyte layer of a primary or secondary battery, a separator layer of a battery, an electrode active material layer, and the like. Further, a functional layer may be formed by mixing other components as necessary according to the purpose of use.
  • the present invention is also a battery including at least a part of the functional layer. Since the functional layer of the present invention is made of an ion conductive material, it can be particularly suitably used as a functional layer in a battery. In particular, it can be particularly suitably used as a solid electrolyte layer of an all-solid battery.
  • the types of batteries that can be used are not particularly limited, and fuel cells using an alkaline electrolyte (alkaline fuel cells, alcohol fuel cells), and secondary batteries (metal-air secondary batteries, nickel-metal hydride secondary batteries, Electrolytes for Zn-Ni secondary batteries). It can also be used as the above-mentioned primary battery having the same principle.
  • components constituting layers other than the functional layer of the present invention may have a layer configuration generally used in each battery.
  • Example 1 and Comparative Examples 1 and 2 were identified using an X-ray diffractometer (Smart Lab 3K / PD / INP manufactured by RIGAKU).
  • X-ray diffractometer Smart Lab 3K / PD / INP manufactured by RIGAKU.
  • measurement was performed by a 2 ⁇ / ⁇ method under the conditions of a scan range of 5 ° to 75 °, a tube voltage of 40 kV, a tube current of 30 mA, a scan speed of 10 ° min ⁇ 1 , and a sampling width of 0.01396 °.
  • Example 1 and Comparative Examples 1 and 2 The ionic conductivity of Example 1 and Comparative Examples 1 and 2 was measured using the electrochemical impedance method.
  • the powders of Example 1 and Comparative Examples 1 and 2 were filled in a mold, pressurized at 30 MPa, and formed into pellets having a thickness of about 1.0 mm and a radius of 7 mm.
  • a sample sputtered with Au at 30 mA for 120 seconds on both sides of the pellet is sandwiched between gold electrodes, and connected to an impedance analyzer (Bio-Logic-Science Instruments.
  • the ionic conductivity was measured under the following conditions. All ionic conductivity measurements were performed in a high temperature and humidity chamber at 80 ° C. and 80% RH.
  • the table below summarizes the results of the ionic conductivity of Example 1 and Comparative Examples 1 and 2.
  • Example 1 It is recognized that the ionic conductivity of Example 1 is higher than that of Comparative Example 1 of the carbonate ion type. Further, since it is also recognized that the ionic conductivity is higher than that of Comparative Example 2 which is a MgAl-based layered double hydroxide, Example 1 obtained by the present invention has high hydroxide conductivity. .
  • the LDH of Example 1 was formed into a compact as a compact.
  • a Pt sputtered film was formed on both surfaces of the electrolyte pellet and the contact surface of the gas diffusion electrode with the pellet, and a power generation test was performed while humidifying the fuel electrode under the same conditions at a temperature of 80 ° C. and a relative humidity of 80%. Was.
  • power generation of about 20 mW / cm 2 was achieved. From this result, it became clear that the LDH of the present invention has a function as a battery electrolyte.
  • the ion conductive material of the present invention is a fuel cell and a secondary battery using an alkaline electrolyte (alkaline fuel cell, alcohol fuel cell, metal-air secondary battery, nickel hydrogen secondary battery and Zn-Ni secondary battery). It can be used as an ion conductive material used as an electrolyte for use.
  • alkaline electrolyte alkaline fuel cell, alcohol fuel cell, metal-air secondary battery, nickel hydrogen secondary battery and Zn-Ni secondary battery.

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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)
  • Organic Chemistry (AREA)
  • Sustainable Energy (AREA)
  • Sustainable Development (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Hybrid Cells (AREA)
  • Fuel Cell (AREA)
  • Conductive Materials (AREA)
  • Secondary Cells (AREA)

Abstract

La présente invention aborde le problème de la fourniture d'un matériau conducteur d'ions ayant une excellente conductivité ionique. Ce matériau conducteur d'ions est un hydroxyde double en couches ayant du Zn comme métal divalent. Le rapport d'intensité (It/Ic) entre le total des intensités de diffraction des phases cristallines comprenant des anions autres que des ions carbonate (It/Ic)) et l'intensité de diffraction de la phase cristalline comprenant des ions carbonate (Ic) est supérieure ou égale à 1, tel que déterminé par diffraction des rayons X.
PCT/JP2018/033375 2018-09-10 2018-09-10 Matériau conducteur d'ions, couche fonctionnelle pour batterie et son procédé de production Ceased WO2020053920A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2018/033375 WO2020053920A1 (fr) 2018-09-10 2018-09-10 Matériau conducteur d'ions, couche fonctionnelle pour batterie et son procédé de production
JP2019160806A JP7401889B2 (ja) 2018-09-10 2019-09-04 イオン伝導性材料、電池用機能層及びその製造方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2018/033375 WO2020053920A1 (fr) 2018-09-10 2018-09-10 Matériau conducteur d'ions, couche fonctionnelle pour batterie et son procédé de production

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WO2020053920A1 true WO2020053920A1 (fr) 2020-03-19

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE112020002680T5 (de) * 2019-06-05 2022-03-10 Ngk Insulators, Ltd. Luftelektroden/Separator-Anordnung und einen Metall-Luft-Akkumulator

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH069358A (ja) * 1992-02-21 1994-01-18 Unilever Nv 日焼け止め剤
WO2009072488A2 (fr) * 2007-12-05 2009-06-11 National Institute For Materials Science Procédé pour la production d'hydroxyde double lamellaire échangeur d'anions
WO2010109670A1 (fr) * 2009-03-27 2010-09-30 住友商事株式会社 Membrane électrolytique alcaline, ensemble électrode et pile à combustible à alcool direct
WO2016067884A1 (fr) * 2014-10-28 2016-05-06 日本碍子株式会社 Procédé de formation de membrane dense d'hydroxyde double lamellaire
JP2017114747A (ja) * 2015-12-25 2017-06-29 共栄社化学株式会社 層状複水酸化物

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH069358A (ja) * 1992-02-21 1994-01-18 Unilever Nv 日焼け止め剤
WO2009072488A2 (fr) * 2007-12-05 2009-06-11 National Institute For Materials Science Procédé pour la production d'hydroxyde double lamellaire échangeur d'anions
WO2010109670A1 (fr) * 2009-03-27 2010-09-30 住友商事株式会社 Membrane électrolytique alcaline, ensemble électrode et pile à combustible à alcool direct
WO2016067884A1 (fr) * 2014-10-28 2016-05-06 日本碍子株式会社 Procédé de formation de membrane dense d'hydroxyde double lamellaire
JP2017114747A (ja) * 2015-12-25 2017-06-29 共栄社化学株式会社 層状複水酸化物

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JP2020040872A (ja) 2020-03-19

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