WO2022209595A1 - 正極および電気化学デバイス - Google Patents
正極および電気化学デバイス Download PDFInfo
- Publication number
- WO2022209595A1 WO2022209595A1 PCT/JP2022/009535 JP2022009535W WO2022209595A1 WO 2022209595 A1 WO2022209595 A1 WO 2022209595A1 JP 2022009535 W JP2022009535 W JP 2022009535W WO 2022209595 A1 WO2022209595 A1 WO 2022209595A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- ether
- positive electrode
- magnesium
- glycol
- specific surface
- Prior art date
Links
- 239000006229 carbon black Substances 0.000 claims abstract description 59
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 48
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000011593 sulfur Substances 0.000 claims abstract description 46
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 32
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 86
- 239000002904 solvent Substances 0.000 claims description 23
- SMDQFHZIWNYSMR-UHFFFAOYSA-N sulfanylidenemagnesium Chemical compound S=[Mg] SMDQFHZIWNYSMR-UHFFFAOYSA-N 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 description 106
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 76
- 229910052749 magnesium Inorganic materials 0.000 description 75
- 239000010410 layer Substances 0.000 description 53
- -1 for example Substances 0.000 description 50
- 235000019241 carbon black Nutrition 0.000 description 49
- 239000008151 electrolyte solution Substances 0.000 description 43
- 239000003792 electrolyte Substances 0.000 description 36
- 238000003860 storage Methods 0.000 description 32
- 229910052751 metal Inorganic materials 0.000 description 24
- 239000002184 metal Substances 0.000 description 24
- 159000000003 magnesium salts Chemical class 0.000 description 23
- 150000001875 compounds Chemical class 0.000 description 21
- 150000002170 ethers Chemical class 0.000 description 21
- 150000003839 salts Chemical class 0.000 description 21
- 238000000034 method Methods 0.000 description 19
- 239000007773 negative electrode material Substances 0.000 description 19
- 229910052760 oxygen Inorganic materials 0.000 description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 18
- 239000001301 oxygen Substances 0.000 description 18
- 239000000446 fuel Substances 0.000 description 16
- 150000003949 imides Chemical class 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 12
- IUVCFHHAEHNCFT-INIZCTEOSA-N 2-[(1s)-1-[4-amino-3-(3-fluoro-4-propan-2-yloxyphenyl)pyrazolo[3,4-d]pyrimidin-1-yl]ethyl]-6-fluoro-3-(3-fluorophenyl)chromen-4-one Chemical compound C1=C(F)C(OC(C)C)=CC=C1C(C1=C(N)N=CN=C11)=NN1[C@@H](C)C1=C(C=2C=C(F)C=CC=2)C(=O)C2=CC(F)=CC=C2O1 IUVCFHHAEHNCFT-INIZCTEOSA-N 0.000 description 11
- 125000001931 aliphatic group Chemical group 0.000 description 11
- 125000004432 carbon atom Chemical group C* 0.000 description 11
- 238000001514 detection method Methods 0.000 description 11
- 125000000524 functional group Chemical group 0.000 description 11
- 229910052736 halogen Inorganic materials 0.000 description 11
- 150000002367 halogens Chemical class 0.000 description 11
- 150000002430 hydrocarbons Chemical group 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- 230000007246 mechanism Effects 0.000 description 11
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 10
- 238000010586 diagram Methods 0.000 description 10
- 239000007774 positive electrode material Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 9
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 8
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 8
- 239000003990 capacitor Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 7
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- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 6
- 239000011267 electrode slurry Substances 0.000 description 6
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
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- 229920002981 polyvinylidene fluoride Polymers 0.000 description 6
- 230000032258 transport Effects 0.000 description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 5
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 description 5
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- 239000008112 carboxymethyl-cellulose Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
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- 239000003273 ketjen black Substances 0.000 description 5
- 229910001425 magnesium ion Inorganic materials 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 description 4
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- 238000003487 electrochemical reaction Methods 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 229910001507 metal halide Inorganic materials 0.000 description 4
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 4
- 125000002950 monocyclic group Chemical group 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 230000002093 peripheral effect Effects 0.000 description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 4
- GBROPGWFBFCKAG-UHFFFAOYSA-N picene Chemical compound C1=CC2=C3C=CC=CC3=CC=C2C2=C1C1=CC=CC=C1C=C2 GBROPGWFBFCKAG-UHFFFAOYSA-N 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
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- 239000011148 porous material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- BEVWMRQFVUOPJT-UHFFFAOYSA-N 2,4-dimethyl-1,3-thiazole-5-carboxamide Chemical compound CC1=NC(C)=C(C(N)=O)S1 BEVWMRQFVUOPJT-UHFFFAOYSA-N 0.000 description 3
- WGKYSFRFMQHMOF-UHFFFAOYSA-N 3-bromo-5-methylpyridine-2-carbonitrile Chemical compound CC1=CN=C(C#N)C(Br)=C1 WGKYSFRFMQHMOF-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- DTPCFIHYWYONMD-UHFFFAOYSA-N decaethylene glycol Chemical compound OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO DTPCFIHYWYONMD-UHFFFAOYSA-N 0.000 description 3
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
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- GLZWNFNQMJAZGY-UHFFFAOYSA-N octaethylene glycol Chemical compound OCCOCCOCCOCCOCCOCCOCCOCCO GLZWNFNQMJAZGY-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
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- 238000009529 body temperature measurement Methods 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- WDECIBYCCFPHNR-UHFFFAOYSA-N chrysene Chemical compound C1=CC=CC2=CC=C3C4=CC=CC=C4C=CC3=C21 WDECIBYCCFPHNR-UHFFFAOYSA-N 0.000 description 2
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
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- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- SLIUAWYAILUBJU-UHFFFAOYSA-N pentacene Chemical compound C1=CC=CC2=CC3=CC4=CC5=CC=CC=C5C=C4C=C3C=C21 SLIUAWYAILUBJU-UHFFFAOYSA-N 0.000 description 2
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Classifications
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- 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
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/46—Alloys based on magnesium or aluminium
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
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- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
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- 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 positive electrodes and electrochemical devices.
- Electrochemical devices include capacitors, air batteries, fuel cells, and secondary batteries, which are used for various purposes.
- An electrochemical device comprises a positive electrode and a negative electrode, and has an electrolytic solution responsible for ion transport between the positive electrode and the negative electrode.
- an electrode of an electrochemical device typified by a magnesium battery is provided with an electrode made of magnesium or an electrode containing at least magnesium (hereinafter, such an electrode is referred to as “electrode containing magnesium” or simply "magnesium An electrochemical device using an electrode containing magnesium is also referred to as a “magnesium electrode-based electrochemical device”).
- Electrode containing magnesium an electrode made of magnesium or an electrode containing at least magnesium
- An electrochemical device using an electrode containing magnesium is also referred to as a “magnesium electrode-based electrochemical device”).
- Magnesium is abundant in resources and much cheaper than lithium.
- magnesium generally has a large amount of electricity per unit volume that can be taken out by an oxidation-reduction reaction, and is highly safe when used in secondary batteries. Therefore, magnesium batteries are attracting attention as next-generation secondary batteries to replace lithium-ion batteries.
- a magnesium-sulfur secondary battery is a secondary battery comprising a negative electrode containing magnesium as a negative electrode active material and a positive electrode containing sulfur as a positive electrode active material.
- the positive electrode generally contains not only sulfur as a positive electrode active material, but also a conductive aid.
- Carbon materials such as carbon black, carbon fiber, and carbon nanotubes are commonly used as conductive aids.
- An object of the present invention is to provide a positive electrode and an electrochemical device with sufficiently superior discharge capacity.
- a positive electrode comprising sulfur and a carbon material
- the carbon material comprises carbon black having a first specific surface area and carbon black having a second specific surface area, wherein the first specific surface area is lower than the second specific surface area; It relates to chemical devices.
- the positive electrode and electrochemical device of the present invention are sufficiently superior in discharge capacity.
- FIG. 1 is a conceptual diagram of an electrochemical device (particularly a battery) according to one embodiment of the present invention.
- FIG. 2 is a schematic cross-sectional view of a magnesium secondary battery (cylindrical magnesium secondary battery) provided as one embodiment of the present invention.
- FIG. 3 is a schematic perspective view of a magnesium secondary battery (flat-plate laminated film type magnesium secondary battery) provided as one embodiment of the present invention.
- FIG. 4 is a schematic cross-sectional view of an electrochemical device that serves as a capacitor in one embodiment of the present invention.
- FIG. 5 is a schematic cross-sectional view of an electrochemical device that serves as an air battery in one embodiment of the present invention.
- FIG. 6 is a schematic cross-sectional view of an electrochemical device that serves as a fuel cell in one embodiment of the present invention.
- FIG. 7 is a block diagram showing a circuit configuration example when a magnesium secondary battery provided as one embodiment of the present invention is applied to a battery pack.
- 8A, 8B, and 8C are block diagrams respectively showing configurations of an electric vehicle, an electric power storage system, and an electric tool to which a magnesium secondary battery is applied as one embodiment of the present invention.
- FIG. 9 is an exploded view schematically showing the battery produced in [Example] of the present specification.
- FIG. 10 is a graph showing measurement results of the battery produced in Example A1.
- the term “electrochemical device” broadly means a device that can extract energy using an electrochemical reaction.
- the “electrochemical device” in the present invention means a device that has a pair of electrodes and an electrolyte and that is charged and discharged with the movement of ions.
- Electrochemical devices include secondary batteries, capacitors, air batteries, fuel cells, and the like, which are merely examples.
- the positive electrode of the present invention is used in electrochemical devices. That is, the positive electrode described in this specification corresponds to a positive electrode for devices that can extract energy using an electrochemical reaction.
- the positive electrode of the present invention is suitable for use in magnesium-sulfur secondary batteries from the viewpoint of further improving the discharge capacity.
- a magnesium-sulfur secondary battery is a secondary battery comprising a negative electrode containing magnesium as a negative electrode active material and a positive electrode containing sulfur as a positive electrode active material.
- the discharge capacity means the discharge capacity per unit weight of sulfur at the time of initial discharge. The higher the discharge capacity, the better.
- the positive electrode of the present invention is a so-called "sulfur electrode", which is a positive electrode containing sulfur as a positive electrode active material and a carbon material as a conductive aid.
- the positive electrode generally includes a positive electrode layer, and the positive electrode layer may contain sulfur and a carbon material.
- Sulfur is not particularly limited as long as it is sulfur used as a positive electrode active material for electrochemical devices, and may be, for example, sulfur (S) such as S8 and/or polymeric sulfur.
- the carbon material includes carbon black having a first specific surface area (hereinafter sometimes simply referred to as “low specific surface area carbon black”) and carbon black having a second specific surface area (hereinafter simply referred to as “high specific surface area carbon black” ), and the first specific surface area is lower (ie smaller) than the second specific surface area.
- low specific surface area carbon black carbon black having a first specific surface area
- high specific surface area carbon black carbon black having a second specific surface area
- the first specific surface area is lower (ie smaller) than the second specific surface area.
- the function and action of the highly insulating sulfur component as a positive electrode active material can be exhibited more sufficiently, and the discharge capacity is sufficiently increased. If the positive electrode does not contain carbon black with a high specific surface area, the discharge capacity will decrease. If the positive electrode does not contain one of the low specific surface area carbon blacks, and if the positive electrode has a positive electrode current collector, the adhesion to the positive electrode current collector is reduced, causing separation of the positive electrode layer, resulting in a decrease in discharge capacity. do.
- a low specific surface area carbon black is a carbon black having a specific surface area lower than that of a high specific surface area carbon black.
- the specific surface area (i.e., the first specific surface area) of the low specific surface area carbon black may generally be 30 m 2 /g or more and 200 m 2 /g or less, and from the viewpoint of further improving the discharge capacity, preferably 30 m 2 / g or more and 150 m 2 /g or less, more preferably 30 m 2 /g or more and 120 m 2 /g or less, still more preferably 40 m 2 /g or more and 100 m 2 /g or less.
- the specific surface area where the peak is located in the specific surface area distribution eg, specific surface area (horizontal axis) - amount (vertical axis) graph
- the specific surface area of carbon black is the specific surface area of the highest peak.
- the specific surface area distribution of carbon black can be measured, for example, by a specific surface area/maximum distribution measuring device such as the BET method.
- the shape of the low specific surface area carbon black is not particularly limited, but from the viewpoint of further improving the discharge capacity, it preferably has a solid particle shape.
- Low specific surface area carbon black is available as a commercial product.
- Commercially available products of low specific surface area carbon black include, for example, solid particle-shaped Denka Black (Denka Co., Ltd.), Super P (Timcal), and the like.
- a high specific surface area carbon black is a carbon black having a specific surface area higher than that of a low specific surface area carbon black.
- the specific surface area (that is, the second specific surface area) of the carbon black with a high specific surface area may usually be 800 m 2 /g or more and 1600 m 2 /g or less, and from the viewpoint of further improving the discharge capacity, preferably 1000 m 2 / g or more and 1500 m 2 /g or less, more preferably 1100 m 2 /g or more and 1400 m 2 /g or less, still more preferably 1200 m 2 /g or more and 1300 m 2 /g or less.
- the shape of the high specific surface area carbon black is not particularly limited, it preferably has a hollow particle shape from the viewpoint of further improving the discharge capacity.
- High specific surface area carbon black is usually 10 ⁇ SA ( m 2 / g) or more, 50 ⁇ SA (m 2 /g) or less specific surface area (that is, the second specific surface area), and from the viewpoint of further improving the discharge capacity, 10 ⁇ SA (m 2 /g) or more, 30 ⁇ SA (m 2 /g) or less, and more preferably 15 ⁇ SA (m 2 /g) or more and 25 ⁇ SA (m 2 /g) or less.
- High specific surface area carbon black is available as a commercial product.
- Commercially available products of high specific surface area carbon black include, for example, Ketjenblack (hollow particle shape).
- the content of the high specific surface area carbon black is usually 5% by weight or more and 75% by weight or less with respect to the total amount of the low specific surface area carbon black and the high specific surface area carbon black, and from the viewpoint of further improving the discharge capacity, it is preferable. is 5% to 65% by weight, more preferably 10% to 65% by weight, more preferably 10% to 55% by weight, particularly preferably 10% to 50% by weight, more preferably is 15% to 50% by weight, most preferably 20% to 50% by weight (especially 30% to 50% by weight).
- the specific surface areas of low specific surface area carbon black and high specific surface area carbon black and their distribution can be measured using a positive electrode taken out from an electrochemical device (eg, secondary battery). For example, first, the electrochemical device is disassembled and the positive electrode is taken out. Next, the positive electrode (particularly the positive electrode layer) is immersed in a solvent to dissolve the binder and sulfur. After that, by measuring the specific surface area distribution of the residue (that is, carbon black), it is possible to calculate the specific surface area of the low specific surface area carbon black and the high specific surface area carbon black and the content relative to the total amount thereof.
- an electrochemical device eg, secondary battery
- the specific surface areas of the low specific surface area carbon black and high specific surface area carbon black measured and calculated by such a method and the content relative to their total amount are the low specific surface area carbon black and high specific surface area carbon used during production, respectively. It is consistent with the specific surface area of blacks and the amount used relative to their total amount used.
- the pore distribution of each of the low specific surface area carbon black and the high specific surface area carbon black can also be evaluated from the pore distribution measured by the method for measuring the content of the low specific surface area carbon black.
- the content of the carbon material is usually 5% by weight or more and 70% by weight or less with respect to the total amount of sulfur and the carbon material, and from the viewpoint of increasing the output of the electrochemical device (especially increasing the battery capacity), preferably 5%. % by weight or more and 60% by weight or less, more preferably 20% by weight or more and 60% by weight or less, and even more preferably 40% by weight or more and 60% by weight or less.
- the content of each of the carbon material and sulfur relative to the total amount of sulfur and carbon material is measured and calculated by dissolving the binder and then dissolving the sulfur to measure and calculate the content of only sulfur. It can be measured and calculated by a method similar to the method for measuring the content of carbon black or the like.
- the carbon material and sulfur contents measured and calculated by such a method correspond to the amount of carbon material and sulfur used in the production, relative to the total amount of sulfur and carbon material. If both (carbon material and sulfur) are dissolved in the cleaning solvent at the same time, thermal analysis or elemental analysis by ICP should be performed.
- the carbon material may contain other carbon materials such as graphite, carbon fiber, and carbon nanotubes.
- the carbon material contains other carbon materials, the total content of the carbon materials including the other carbon materials may be within the above range.
- the carbon fiber for example, vapor growth carbon fiber (VGCF (registered trademark)) or the like can be used.
- VGCF vapor growth carbon fiber
- carbon nanotubes for example, multi-wall carbon nanotubes (MWCNT) such as single-wall carbon nanotubes (SWCNT) and/or double-wall carbon nanotubes (DWCNT) can be used.
- MWCNT multi-wall carbon nanotubes
- SWCNT single-wall carbon nanotubes
- DWCNT double-wall carbon nanotubes
- the positive electrode may contain a binder.
- binders include fluorine-based resins such as polyvinylidene fluoride (PVdF) and/or polytetrafluoroethylene (PTFE), polyvinyl alcohol (PVA)-based resins, styrene-butadiene copolymer rubber (SBR)-based resins, One or two or more polymer resins selected from carboxymethyl cellulose and the like can be mentioned.
- a conductive polymer may be used as the binder. Examples of conductive polymers that can be used include substituted or unsubstituted polyaniline, polypyrrole, polythiophene, and (co)polymers composed of one or two selected from these.
- the content of the binder in the positive electrode is not particularly limited. good too.
- the positive electrode may further contain a conductive aid other than the carbon material.
- a conductive aid other than the carbon material.
- metal materials such as Ni powder and/or conductive polymer materials can be used.
- a positive electrode (especially a positive electrode layer) can be produced, for example, by the following method. First, sulfur and low specific surface area carbon black are dry mixed at a predetermined weight ratio using an agate mortar. To this mixture, carbon black having a high specific surface area is added at a predetermined weight ratio, and dry-mixed with an agate mortar. Next, the resulting carbon-sulfur composite is added to a solvent together with a binder, and mixed with a pencil mixer to obtain a positive electrode slurry. The positive electrode slurry is applied onto the positive electrode current collector using a bar coater, vacuum dried at 10° C. or higher and 50° C. or lower for 6 hours or longer and 24 hours or shorter, and then dried at 50° C. or higher and 80° C. or lower for 10 minutes or longer for 120 minutes. Dry at normal pressure for 1 minute or less.
- the solvent for the positive electrode slurry is not particularly limited as long as it can dissolve the binder.
- the solid content concentration of the positive electrode slurry is not particularly limited, and is usually 2% by weight or more and 80% by weight or less, and particularly preferably 5% by weight or more and 60% by weight or less.
- the negative electrode may be an electrode containing magnesium.
- the material that constitutes the negative electrode (specifically, the negative electrode active material) is an "electrode containing magnesium", and therefore preferably consists of a magnesium metal simple substance, a magnesium alloy, or a magnesium compound.
- the negative electrode is composed of a magnesium metal simple substance (such as a magnesium plate)
- the Mg purity of the metal simple substance is 90% or more, preferably 95% or more, and more preferably 98% or more.
- the negative electrode can be made of, for example, a plate-like material or a foil-like material, but is not limited to this, and can be formed (shaped) using powder.
- the negative electrode can also have a structure in which a negative electrode active material layer is formed in the vicinity of its surface.
- the negative electrode active material layer may include a magnesium ion conductive layer containing magnesium (Mg) and at least one of carbon (C), oxygen (O), sulfur (S) and halogen. negative electrode.
- Mg magnesium ion conductive layer containing magnesium
- C carbon
- O oxygen
- S sulfur
- halogen include at least one selected from the group consisting of fluorine (F), chlorine (Cl), bromine (Br) and iodine (I).
- the negative electrode active material layer may have a single magnesium-derived peak in the range of 40 eV or more and 60 eV or less over a depth of 2 ⁇ 10 ⁇ 7 m from the surface of the negative electrode active material layer.
- the negative electrode active material layer exhibits good electrochemical activity from the surface to the inside.
- the oxidation state of magnesium may be substantially constant over a depth of 2 ⁇ 10 ⁇ 7 m from the surface of the negative electrode active material layer.
- the surface of the negative electrode active material layer means one of the two surfaces of the negative electrode active material layer that constitutes the surface of the electrode, and the back surface means the surface opposite to this surface, that is, the surface of the collector.
- the negative electrode active material layer contains the above elements can be confirmed based on the XPS (X-ray Photoelectron Spectroscopy) method. Also, it is possible to similarly confirm that the negative electrode active material layer has the above peak and that it has the oxidation state of magnesium based on the XPS method.
- XPS X-ray Photoelectron Spectroscopy
- the positive electrode and the negative electrode may be separated by an inorganic separator or an organic separator that allows magnesium ions to pass through while preventing short circuits due to contact between the two electrodes.
- inorganic separators include glass filters and glass fibers.
- organic separators include synthetic resin porous membranes made of polytetrafluoroethylene, polypropylene and/or polyethylene, etc., and a structure in which two or more of these porous membranes are laminated. can.
- a polyolefin porous film is preferable because it has an excellent short-circuit prevention effect and can improve the safety of the battery due to the shutdown effect.
- the electrolyte layer in the electrochemical device is composed of an electrolytic solution, and may further contain a polymer compound as a carrier for holding the electrolytic solution.
- An electrolyte layer may be placed impregnated within the separator.
- the polymer compound may be swelled by the electrolytic solution. In this case, the polymer compound swollen by the electrolytic solution may be gel.
- polymer compounds include polyacrylonitrile, polyvinylidene fluoride, copolymers of vinylidene fluoride and hexafluoropropylene, polytetrafluoroethylene, polyhexafluoropropylene, polyethylene oxide, polypropylene oxide, polyphosphazene, and polysiloxane. , polyvinyl acetate, polyvinyl alcohol, polymethyl methacrylate, polyacrylic acid, polymethacrylic acid, styrene-butadiene rubber, nitrile-butadiene rubber, polystyrene and/or polycarbonate.
- polyacrylonitrile, polyvinylidene fluoride, polyhexafluoropropylene, or polyethylene oxide may be used if more emphasis is placed on electrochemical stability.
- the electrolyte layer may be a solid electrolyte layer.
- Electrolytes are equivalent to electrolytes for devices that can extract energy using electrochemical reactions.
- the electrolytic solution may be, as a major premise, an electrolytic solution used in an electrochemical device provided with electrodes containing magnesium.
- it may be an electrolytic solution for an electrochemical device comprising an electrode containing magnesium as a negative electrode.
- the negative electrode is an electrode containing magnesium
- the positive electrode is preferably an electrode containing sulfur, that is, a sulfur electrode. That is, in one preferred aspect, the positive electrode of the present invention is a positive electrode for a magnesium (Mg)-sulfur (S) electrode.
- the electrolytic solution contains at least a solvent and a magnesium salt. More specifically, the electrolyte comprises a magnesium salt and a solvent for dissolving the salt.
- the solvent is not particularly limited as long as it can dissolve the magnesium salt, and from the viewpoint of further improving the discharge capacity, it preferably contains an ether solvent, and more preferably contains only an ether solvent.
- the solvent preferably contains a linear ether, and more preferably contains only a linear ether. That is, rather than a cyclic ether such as tetrahydrofuran, it is preferable that the electrolyte solvent is an ether having a linear molecular structure (preferably only the ether). In short, it can be said that the solvent in the electrolyte is preferably a linear ether solvent.
- the straight-chain ether may be, for example, a straight-chain ether having an ethyleneoxy structural unit represented by the following general formula.
- R' and R'' are each independently a hydrocarbon group having 1 or more and 10 or less carbon atoms, and n is an integer of 1 or more and 10 or less.
- Linear ether solvents contain one or more ethyleneoxy structural units per molecule.
- ethyleneoxy structural unit refers to a molecular structural unit (—O—C 2 H 4 —) in which an ethylene group and an oxygen atom are bonded, and such a molecular structural unit is a linear
- One or more is included in the ether.
- linear ethers such as dimethoxyethane/DME (ethylene glycol dimethyl ether) and/or diethoxyethane/DEE (ethylene glycol diethyl ether). you can
- the linear ether contains two or more molecular structural units (--O--C 2 H 4 --). From another perspective, it can be said that the linear ether in the electrolytic solution preferably has a structure in which two or more glycol molecules are dehydrated and condensed.
- R' and R'' in the above general formula of the linear ether each independently represent a hydrocarbon group.
- R' and R'' may each independently be an aliphatic hydrocarbon group, an aromatic hydrocarbon group and/or an araliphatic hydrocarbon group.
- straight-chain ether as used herein means that at least the site of the ethyleneoxy structural unit is unbranched (that is, does not have a branched structure). This means that R' and R'' in the general formula above do not necessarily have a linear structure, and may have a branched structure.
- the linear ether used in the electrolytic solution not only does not have a branched structure at the ethyleneoxy structural unit site, but also has a branched structure in R′ and R′′. It is a glycol-based ether that does not have
- R' and R'' are each independently preferably an aliphatic hydrocarbon group (especially a saturated aliphatic hydrocarbon group) having 1 to 5 carbon atoms, more preferably is an aliphatic hydrocarbon group (particularly a saturated aliphatic hydrocarbon group) having 1 to 3 carbon atoms.
- n is preferably an integer of 1 or more and 5 or less, more preferably an integer of 1 or more and 3 or less, and still more preferably an integer of 2 or more and 3 or less.
- Linear ethers having two or more ethyleneoxy structural units are not particularly limited, but diethylene glycol-based ethers, triethylene glycol-based ethers, tetraethylene glycol-based ethers, pentaethylene glycol-based ethers, hexaethylene Glycol type ether etc. can be mentioned. Similarly, heptaethylene glycol-based ethers, octaethylene glycol-based ethers, nonaethylene glycol-based ethers, decaethylene glycol-based ethers, and the like may be used, and moreover, polyethylene glycols having more ethyleneoxy structural units than these may be used. system ether.
- the hydrocarbon group having 1 to 10 carbon atoms is an aliphatic hydrocarbon group. That is, for the linear ether contained in the electrolytic solution, R' and R'' in the above general formula may each independently represent 1 or more and 10 or less aliphatic hydrocarbon groups. Examples include, but are not limited to, the following ethylene glycol-based ethers, diethylene glycol-based ethers, triethylene glycol-based ethers, tetraethylene glycol-based ethers, pentaethylene glycol-based ethers, and hexaethylene glycol-based ethers. can be done.
- the linear ether is preferably a diethylene glycol-based ether (especially diethylene glycol dimethyl ether) from the viewpoint of further improving the discharge capacity.
- Triethylene glycol-based ether Triethylene glycol dimethyl ether, triethylene glycol ethyl methyl ether, triethylene glycol methyl propyl ether, triethylene glycol butyl methyl ether, triethylene glycol methyl pentyl ether, triethylene glycol methylhexyl ether, triethylene glycol methylheptyl ether, triethylene glycol methyl octyl ether; triethylene glycol diethyl ether, triethylene glycol ethyl propyl ether, triethylene glycol butyl ethyl ether, triethylene glycol ethyl pentyl ether, triethylene glycol ethylhexyl ether, triethylene glycol ethyl heptyl ether, triethylene glycol ethyl octyl ether; triethylene glycol dipropyl ether, triethylene glycol butyl propyl ether, triethylene glycol propyl pentyl ether
- (Tetraethylene glycol-based ether) Tetraethylene glycol dimethyl ether, tetraethylene glycol ethyl methyl ether, tetraethylene glycol methyl propyl ether, tetraethylene glycol butyl methyl ether, tetraethylene glycol methyl pentyl ether, tetraethylene glycol methylhexyl ether, tetraethylene glycol methylheptyl ether, tetraethylene glycol methyl octyl ether; tetraethylene glycol diethyl ether, tetraethylene glycol ethyl propyl ether, tetraethylene glycol butyl ethyl ether, tetraethylene glycol ethyl pentyl ether, tetraethylene glycol ethylhexyl ether, tetraethylene glycol ethyl heptyl ether, tetraethylene glycol ethy
- Pentaethylene glycol-based ether Pentaethylene glycol dimethyl ether, pentaethylene glycol ethyl methyl ether, pentaethylene glycol methyl propyl ether, pentaethylene glycol butyl methyl ether, pentaethylene glycol methyl pentyl ether, pentaethylene glycol methylhexyl ether, pentaethylene glycol methylheptyl ether, pentaethylene glycol methyl octyl ether; pentaethylene glycol diethyl ether, pentaethylene glycol ethyl propyl ether, pentaethylene glycol butyl ethyl ether, pentaethylene glycol ethyl pentyl ether, pentaethylene glycol ethylhexyl ether, pentaethylene glycol ethyl heptyl ether, pentaethylene glycol ethyl octyl ether; pentaethylene glyco
- (Hexaethylene glycol-based ether) Hexaethylene glycol dimethyl ether, hexaethylene glycol ethyl methyl ether, hexaethylene glycol methyl propyl ether, hexaethylene glycol butyl methyl ether, hexaethylene glycol methyl pentyl ether, hexaethylene glycol methylhexyl ether, hexaethylene glycol methyl heptyl ether, hexaethylene glycol methyl octyl ether; hexaethylene glycol diethyl ether, hexaethylene glycol ethyl propyl ether, hexaethylene glycol butyl ethyl ether, hexaethylene glycol ethyl pentyl ether, hexaethylene glycol ethylhexyl ether, hexaethylene glycol ethyl heptyl ether, hexaethylene glycol e
- it may be a heptaethylene glycol-based ether, an octaethylene glycol-based ether, a nonaethylene glycol-based ether, a decaethylene glycol-based ether, or even a polyethylene glycol-based ether.
- Magnesium salts contained in the electrolytic solution include salts having the general formula MgX n (where n is 1 or 2 and X is a monovalent or divalent anion).
- X is a halogen (F, Cl, Br, I)
- such magnesium salts constitute metal halide salts.
- X may be another anion, in which case the magnesium salt may be, for example, magnesium perchlorate (Mg(ClO 4 ) 2 ), magnesium nitrate (Mg(NO 3 ) 2 ), magnesium sulfate (MgSO4), magnesium acetate (Mg( CH3COO ) 2 ), magnesium trifluoroacetate (Mg( CF3COO ) 2 ), magnesium tetrafluoroborate (Mg (BF4)2 ) , magnesium tetraphenylborate (Mg(B( C6H5 ) 4 ) 2 ), magnesium hexafluorophosphate (Mg( PF6 ) 2 ), magnesium hexafluoroarsenate (Mg (AsF6)2 ) , magnesium perfluoroalkylsulfonate salt ((Mg(R f1 SO 3 ) 2 ), where R f1 is a perfluoroalkyl group), magnesium salt of perfluoro
- the magnesium salt may be a metal halide salt, an imide metal salt, or a combination of a metal halide salt and an imide metal salt.
- the ether-based solvent especially linear ether
- the ether-based solvent may be such that an imide metal salt is added in addition to the halogen metal salt, thereby achieving a higher discharge capacity more effectively. can be obtained.
- Halogen metal salts include at least one selected from the group consisting of magnesium fluoride ( MgF2 ), magnesium chloride (MgCl2), magnesium bromide ( MgBr2 ) and magnesium iodide ( MgI2 ). can.
- magnesium chloride is preferably used as the halogen metal salt. That is, magnesium chloride (MgCl 2 ) is preferable as a magnesium salt to be combined with an ether solvent (especially linear ether). This is because such magnesium chloride (MgCl 2 ) facilitates achieving a higher discharge capacity in the electrochemical device.
- An imide metal salt is a magnesium salt that has an imide as its molecular structure.
- the imide metal salt is a magnesium salt having a sulfonylimide as a molecular structure. This is because a magnesium salt having a sulfonylimide as a molecular structure facilitates achieving a higher discharge capacity in an electrochemical device.
- a magnesium salt having a sulfonylimide as a molecular structure can contribute to achieving a higher discharge capacity in an electrochemical device in combination with the halogen metal salt (eg, magnesium chloride).
- the imide metal salt is preferably a magnesium salt of perfluoroalkylsulfonylimide. That is, the imide metal salt is preferably Mg((R f SO 2 ) 2 N) 2 (wherein R f is a perfluoroalkyl group).
- R f is a perfluoroalkyl group having 1 to 10 carbon atoms, a perfluoroalkyl group having 1 to 8 carbon atoms, a perfluoroalkyl group having 1 to 6 carbon atoms, a perfluoroalkyl group having 1 to 4 carbon atoms, It may be a fluoroalkyl group, a perfluoroalkyl group having 1 or more and 3 or less carbon atoms, or a perfluoroalkyl group having 1 or more and 2 or less carbon atoms.
- the imide metal salt may be magnesium bis(trifluoromethanesulfonyl)imide, Mg(TFSI) 2 .
- Mg(TFSI) 2 tends to achieve higher discharge capacity in electrochemical devices.
- Mg(TFSI) 2 can help achieve higher discharge capacity of electrochemical devices in combination with the metal halide salts (particularly magnesium chloride (MgCl 2 )).
- the content of the magnesium salt may be, for example, 10 M or less (especially more than 0 M and 10 M or less) (the overall standard for the electrolyte), and from the viewpoint of further improving the discharge capacity, preferably 0.2 M or more and 5 M or less (electrolyte overall standard), more preferably 1 M or more and 2 M or less (the overall standard of the electrolytic solution).
- the electrolytic solution contains two or more kinds of magnesium salts, the total content thereof should be within the above range.
- the electrolytic solution contains both a halogen metal salt and an imide metal salt as magnesium salts
- the content of each independently is, for example, 5 M or less (especially more than 0 M and 5 M or less) (the overall standard for the electrolytic solution).
- it is preferably 0.1 M or more and 2.5 M or less (the whole electrolyte solution standard), more preferably 0.3 M or more and 1 M or less (the whole electrolyte solution standard). good too.
- the electrolytic solution may further contain a cyclic organic compound with a two-dimensional structure or a three-dimensional structure.
- a cyclic organic compound is added to the electrolyte solvent as an additive.
- a cyclic organic compound having a two-dimensional structure or a three-dimensional structure is contained as an auxiliary component to an ether solvent containing a magnesium salt, particularly a linear ether solvent. A higher discharge capacity can be obtained by including such a cyclic organic compound in the charge liquid.
- the discharge capacity can be further improved due to the fact that the ether-based solvent of the electrolytic solution contains "a cyclic organic compound with a two-dimensional structure or a three-dimensional structure".
- the discharge capacity can be significantly improved.
- cyclic organic compound having a two-dimensional or three-dimensional structure refers to a substance having a molecular structure in which rings are linked two-dimensionally, or a molecular structure in which rings are linked three-dimensionally. refers to matter.
- a cyclic organic compound having a two-dimensional structure means an organic substance having a cyclic molecular structure so as to form a condensed ring
- a cyclic organic compound having a three-dimensional structure means a tertiary structure. It means an organic substance having a network of cyclic molecules in the original three-dimensional form.
- a representative “3-dimensionally structured cyclic organic compound” is fullerene.
- the "two-dimensional or three-dimensional cyclic organic compound” is a condensed ring compound.
- a cyclic organic compound is an organic substance having a molecular structure resulting from two or more single rings supplying their respective ring sides to each other.
- a two-dimensional planar molecular structure may be formed such that two or more single rings share their respective ring sides.
- the two-dimensional planar molecular structure may be a linear condensed ring type, a winged condensed ring type, or the like.
- a three-dimensional three-dimensional molecular structure may be formed such that two or more monocyclic rings share their ring sides with each other.
- each individual ring in the fused ring compound may be a three-, four-, five-, six-, seven-, or eight-membered ring, and the fused ring compound as a whole may be a combination thereof. may be included.
- the monocyclic structure in the condensed ring compound is not limited to a monocyclic ring, and may be a heterocyclic ring (heterocyclic ring) or a combination thereof.
- the number of rings in the condensed ring compound is not particularly limited.
- the number of rings in the condensed ring compound may be 40 or less, 30 or less, or 20 or less, preferably 15 or less, more preferably 10 or less.
- the lower limit of the number of such rings is not particularly limited, and is 2, for example.
- the number of rings in the condensed ring compound is 2-8 or 2-7, for example 2-6, 3-6 or 3-5.
- the form of condensed ring is not particularly limited, and may be a linear condensed ring type and/or a winged condensed ring type, particularly in the case of a cyclic organic compound having a two-dimensional structure.
- the condensed ring compounds in the present invention include pentalene, indene, naphthalene, azulene, heptalene, biphenylene, as-indacene, s-indacene, acenaphthylene, fluorene, phenalene, phenanthrene, anthracene, fluoranthene, and acephenanth.
- At least one selected from the group consisting of rylene, aceanthrylene, triphenylene, pyrene, chrysene, tetracene, pleiadene, picene, perylene, pentaphene, pentacene, tetraphenylene, hexaphene, and derivatives thereof can be used.
- aromatic condensed ring compounds it may be a cyclic organic compound having a plurality of condensed rings, in which the above number of monocyclic rings are formed by supplying at least one ring edge to each other.
- aromatic condensed rings may be joined together in the form of linear condensed rings or may be joined together in the form of winged condensed rings.
- a cyclic organic compound with a three-dimensional structure has a three-dimensional molecular structure in which each single ring shares two or more sides.
- the cyclic organic compound has a sterically closed molecular structure in which all sides of a single ring are shared between the rings.
- Such cyclic organic compounds are preferably fullerenes or derivatives thereof.
- Fullerene C60 (Chem. 28) is, for example, three-dimensionally composed of 12 five-membered rings and 20 six-membered rings connected to each other. That is, the fullerene is such that the rings are connected to form a three-dimensional shape, and preferably has a spherical shape as a whole.
- a cyclic organic compound as exemplified by fullerene has a non-planar molecular structure (preferably a spherical molecular structure) as a whole.
- the fullerene is not limited to C60, but may be C70, or higher order fullerenes (such as C84, C90 or C96) having a higher molecular weight than C60.
- the condensed ring compound is a benzene-based condensed compound. That is, the condensed ring compound may have a ring structure in which two or more benzene rings are condensed with a benzene ring as a base.
- the number of benzene rings may be two. Also, for example, the number of benzene rings is three, so the condensed ring compound may be phenanthrene, anthracene, or derivatives thereof. Alternatively, the number of benzene rings may be five, and therefore the condensed ring compound may be picene, pentaphene, pentacene or derivatives thereof.
- the condensed ring compound contained in the electrolytic solution may have an anthracene skeleton. That is, it may be a condensed ring compound having a ring structure in which three benzene rings are condensed as a main skeleton.
- substituents include one or more groups selected from the group consisting of hydrocarbon groups, halogen atoms, oxygen-containing functional groups, nitrogen-containing functional groups and sulfur-containing functional groups.
- the hydrocarbon groups may each independently be an aliphatic hydrocarbon group, an aromatic hydrocarbon group or an araliphatic hydrocarbon group.
- the aliphatic hydrocarbon group, aromatic hydrocarbon group and araliphatic hydrocarbon group do not necessarily have a linear structure, and may have a branched structure (branched structure).
- the aliphatic hydrocarbon group may be a saturated hydrocarbon or an unsaturated hydrocarbon.
- Each such hydrocarbon group may have about 1 to 50 carbon atoms (eg, 1 to 40, 1 to 30, 1 to 20 or 1 to 10).
- the oxygen-containing functional group is a functional group containing at least an oxygen atom, and examples thereof include a hydroxy group, a carboxyl group, an epoxy group and/or an aldehyde group. Also, the oxygen-containing functional group may correspond to an ether bond site or an ester bond site.
- a nitrogen-containing functional group is a functional group containing at least a nitrogen atom, and examples thereof include an amino group, a nitro group and/or a nitroso group.
- a sulfur-containing group is a functional group containing at least a sulfur atom, and includes, for example, a thiol group, a sulfide group, a disulfide group, a sulfonyl group, a sulfo group, a thiocarbonyl group and/or a thiourea group.
- the oxygen-containing functional group, nitrogen-containing functional group and sulfur-containing group in the present specification may each have the concept of both sides, and furthermore, hydrocarbon groups (aliphatic hydrocarbon groups, aromatic hydrocarbon groups or araliphatic hydrocarbon groups).
- the "two-dimensional or three-dimensional cyclic organic compound” is preferably a two-dimensional cyclic organic compound, more preferably anthracene or a derivative thereof, from the viewpoint of further improving the discharge capacity.
- the content of the "cyclic organic compound having a two-dimensional structure or three-dimensional structure” may be, for example, 1 M or less (especially more than 0 M or less and 1 M or less) (the overall standard for the electrolyte solution), and from the viewpoint of further improving the discharge capacity, It may be preferably 0.001 M or more and 1 M or less (the whole electrolyte solution standard), more preferably 0.005 M or more and 0.1 M or less (the whole electrolyte solution standard).
- the electrolytic solution contains two or more types of "two-dimensional or three-dimensional cyclic organic compounds"
- the total content thereof should be within the above range.
- the electrochemical device of the present invention can be configured as a secondary battery, and the conceptual diagram in that case is shown in FIG.
- magnesium ions migrate from the positive electrode 10 through the electrolyte layer 12 to the negative electrode 11 to convert electrical energy into chemical energy and store it.
- magnesium ions return from the negative electrode 11 to the positive electrode 10 through the electrolyte layer 12 to generate electrical energy.
- the electrochemical device is a battery (primary battery or secondary battery) composed of the positive electrode of the present invention described above
- a battery is, for example, a notebook personal computer, a PDA (personal digital assistant), a mobile phone, a smartphone , cordless telephone base and slave units, video movies, digital still cameras, e-books, electronic dictionaries, portable music players, radios, headphones, game consoles, navigation systems, memory cards, cardiac pacemakers, hearing aids, power tools, electric shavers , refrigerators, air conditioners, television receivers, stereos, water heaters, microwave ovens, dishwashers, washing machines, dryers, lighting equipment, toys, medical equipment, robots, road conditioners, traffic lights, railway cars, golf carts, It can be used as a driving power supply or an auxiliary power supply for electric carts and/or electric vehicles (including hybrid vehicles).
- a conversion device that converts electric power into driving force by supplying electric power is generally a motor.
- the control device (control unit) that performs information processing related to vehicle control includes a control device that displays the remaining battery level based on information regarding the remaining battery level. Batteries can also be used in power storage devices in so-called smart grids. Such a power storage device can store power not only by supplying power but also by receiving power supply from another power source.
- Other power sources that can be used include, for example, thermal power generation, nuclear power generation, hydraulic power generation, solar cells, wind power generation, geothermal power generation, and/or fuel cells (including biofuel cells).
- control means for controlling the secondary battery
- an exterior housing the secondary battery can be done.
- the control means controls, for example, charging/discharging, over-discharging, or over-charging of the secondary battery.
- the electrochemical device (that is, secondary battery) of the present invention can also be applied to electronic equipment that receives power supply from a secondary battery.
- Two electric vehicles having a conversion device that receives electric power supplied from a secondary battery and converts it into driving force for the vehicle, and a control device (or control unit) that performs information processing related to vehicle control based on information about the secondary battery.
- the electrochemical device of the present invention can also be applied to secondary batteries.
- the conversion device typically receives power supply from a secondary battery to drive a motor to generate driving force. Regenerative energy can also be used to drive the motor.
- the control device (or control unit) performs information processing related to vehicle control, for example, based on the remaining battery level of the secondary battery.
- Such electric vehicles include, for example, electric vehicles, electric motorcycles, electric bicycles, railway vehicles, and so-called hybrid vehicles.
- a power system configured to receive power from a secondary battery and/or supply power to the secondary battery from a power source.
- a power system may be any power system as long as it uses electrical power, including simply power devices.
- Such power systems may include, for example, smart grids, home energy management systems (HEMS), and/or vehicles, etc., and may also store electricity.
- HEMS home energy management systems
- the electrochemical device (that is, the secondary battery) of the present invention can be applied to a power storage power supply that has a secondary battery and is configured to be connected to an electronic device to which power is supplied. Regardless of the application of such a power storage power source, it can basically be used in any power system or power device, and can be used in smart grids, for example.
- magnesium secondary battery Such a secondary battery is hereinafter also referred to as a "magnesium secondary battery".
- the magnesium secondary battery as an electrochemical device of the present invention can be used as a power source for driving and operation or as a power storage source for power storage. aggregate) without any particular limitation.
- a magnesium secondary battery (for example, a magnesium-sulfur secondary battery) used as a power source may be a main power source (preferentially used power source) or an auxiliary power source (instead of the main power source, or It may be a power supply that is used by switching from the main power supply).
- the main power supply is not limited to the magnesium secondary battery.
- magnesium secondary batteries especially magnesium-sulfur secondary batteries
- video cameras camcorders, digital still cameras, mobile phones, personal computers, television receivers, various display devices, cordless telephones, Headphone stereos, music players, portable radios, electronic books and/or electronic paper such as electronic newspapers, various electronic devices such as personal digital assistants including PDAs, electric devices (including portable electronic devices); toys; electric shavers, etc.
- lighting fixtures such as room lights; medical electronic devices such as pacemakers and/or hearing aids; storage devices such as memory cards; battery packs used as removable power sources for personal computers, etc.; / or electric tools such as electric saws; power storage systems such as home battery systems that store power in preparation for emergencies and / or home energy servers (household power storage devices), power supply systems; power storage units and / or backup power supply; electric vehicles such as electric automobiles, electric motorcycles, electric bicycles, and/or Segway (registered trademark); electric power driving force conversion devices for aircraft and/or ships (specifically, for example, power motors) can be exemplified, but it is not limited to these applications.
- magnesium secondary batteries are applied to battery packs, electric vehicles, power storage systems, power supply systems, power tools, electronic devices, and / or electrical devices.
- a battery pack is a power supply using a magnesium secondary battery, and is a so-called assembled battery or the like.
- An electric vehicle is a vehicle that operates (for example, runs) using a magnesium secondary battery as a drive power source, and may be an automobile (for example, a hybrid automobile, etc.) that also includes a drive source other than a secondary battery.
- a power storage system (for example, a power supply system) is a system that uses a magnesium secondary battery as a power storage source.
- a power tool is a tool in which a movable part (for example, a drill or the like) is movable using a magnesium secondary battery as a driving power source.
- Electronic devices and electrical devices are devices that exhibit various functions using a magnesium secondary battery as a power source for operation (that is, a power supply source).
- a cylindrical magnesium secondary battery and a flat laminate film type magnesium secondary battery will be described below.
- FIG. 1 A schematic cross-sectional view of a cylindrical magnesium secondary battery 100 is shown in FIG.
- an electrode structure 121 and a pair of insulating plates 112 and 113 are housed inside a substantially hollow cylindrical electrode structure housing member 111.
- the electrode structure 121 can be produced, for example, by stacking a positive electrode 122 and a negative electrode 124 with a separator 126 interposed therebetween to obtain an electrode structure, and then winding the electrode structure.
- An electrode structure housing member (for example, a battery can) 111 has a hollow structure with one end closed and the other end open, and is made of iron (Fe) and/or aluminum (Al) or the like.
- a pair of insulating plates 112 and 113 are arranged so as to sandwich the electrode structure 121 and extend perpendicularly to the winding peripheral surface of the electrode structure 121 .
- a battery cover 114, a safety valve mechanism 115, and a thermal resistance element (for example, a PTC element, a positive temperature coefficient element) 116 are crimped to the open end of the electrode structure housing member 111 via a gasket 117.
- the electrode structure housing member 111 is hermetically sealed.
- the battery lid 114 is made of the same material as the electrode structure housing member 111, for example.
- the safety valve mechanism 115 and the thermal resistance element 116 are provided inside the battery lid 114 , and the safety valve mechanism 115 is electrically connected to the battery lid 114 via the thermal resistance element 116 .
- the disk plate 115A is reversed when the internal pressure exceeds a certain level due to an internal short circuit and/or external heating. This disconnects the electrical connection between the battery lid 114 and the electrode structure 121 .
- the resistance of the thermal resistance element 116 increases as the temperature rises.
- Gasket 117 is made of, for example, an insulating material. The surface of the gasket 117 may be coated with asphalt or the like.
- a center pin 118 is inserted into the winding center of the electrode structure 121 .
- the center pin 118 does not have to be inserted in the winding center.
- a positive electrode lead portion 123 made of a conductive material such as aluminum is connected to the positive electrode 122 .
- the positive electrode lead portion 123 is attached to the positive electrode current collector.
- a negative electrode lead portion 125 made of a conductive material such as copper is connected to the negative electrode 124 .
- the negative electrode lead portion 125 is attached to the negative electrode current collector.
- the negative electrode lead portion 125 is welded to the electrode structure housing member 111 and electrically connected to the electrode structure housing member 111 .
- the positive electrode lead portion 123 is welded to the safety valve mechanism 115 and electrically connected to the battery lid 114 .
- the negative electrode lead portion 125 is provided at one position (the outermost peripheral portion of the wound electrode structure), but at two positions (the outermost peripheral portion and the outermost portion of the wound electrode structure). inner circumference).
- the electrode structure 121 includes a positive electrode 122 in which a positive electrode active material layer is formed on a positive electrode current collector (more specifically, on both sides of the positive electrode current collector) and a negative electrode current collector (more specifically, on both sides of the positive electrode current collector). is formed by stacking a negative electrode 124 having negative electrode active material layers formed on both sides of a negative electrode current collector with a separator 126 interposed therebetween. No positive electrode active material layer is formed in the region of the positive current collector to which the positive lead portion 123 is attached, and no negative electrode active material layer is formed in the region of the negative electrode current collector to which the negative lead portion 125 is attached.
- the magnesium secondary battery 100 can be manufactured, for example, according to the following procedure.
- positive electrode active material layers are formed on both sides of the positive electrode current collector, and negative electrode active material layers are formed on both sides of the negative electrode current collector.
- the positive electrode lead portion 123 is attached to the positive electrode current collector using a welding method or the like.
- the negative electrode lead portion 125 is attached to the negative electrode current collector using a welding method or the like.
- the positive electrode 122 and the negative electrode 124 are laminated with a separator 126 made of a microporous polyethylene film interposed therebetween, and wound (more specifically, an electrode structure of positive electrode 122/separator 126/negative electrode 124/separator 126).
- a protective tape (not shown) is attached to the outermost periphery. After that, the center pin 118 is inserted into the center of the electrode structure 121 .
- the electrode structure 121 is housed inside the electrode structure housing member 111 .
- the tip of the positive electrode lead portion 123 is attached to the safety valve mechanism 115 and the tip of the negative electrode lead portion 125 is attached to the electrode structure housing member 111 by welding or the like.
- the separator 126 is impregnated with the electrolytic solution by injecting the electrolytic solution based on the depressurization method.
- the battery lid 114 , the safety valve mechanism 115 and the thermal resistance element 116 are crimped to the opening end of the electrode structure housing member 111 via the gasket 117 .
- FIG. 3 shows a schematic exploded perspective view of such a secondary battery.
- an electrode structure 221 basically similar to that described above is accommodated inside an exterior member 200 made of a laminate film.
- the electrode structure 221 can be produced by stacking a positive electrode and a negative electrode with a separator and an electrolyte layer interposed therebetween, and then winding the stacked structure.
- a positive electrode lead portion 223 is attached to the positive electrode, and a negative electrode lead portion 225 is attached to the negative electrode.
- the outermost periphery of the electrode structure 221 is protected with a protective tape.
- the positive lead portion 223 and the negative lead portion 225 protrude in the same direction from the interior of the exterior member 200 toward the exterior.
- the positive electrode lead portion 223 is made of a conductive material such as aluminum.
- Anode lead 225 is formed from a conductive material such as copper, nickel, and/or stainless steel.
- the exterior member 200 is a sheet of film that can be folded in the direction of arrow R shown in FIG. ing.
- the exterior member 200 is, for example, a laminate film in which a fusion layer, a metal layer, and a surface protection layer are laminated in this order.
- the exterior member 200 may be formed by bonding two separate laminate films via an adhesive or the like.
- the fusing layer consists of a film such as polyethylene and/or polypropylene, for example.
- the metal layer is made of, for example, aluminum foil.
- the surface protective layer is made of, for example, nylon and/or polyethylene terephthalate.
- the exterior member 200 may be an aluminum laminate film in which a polyethylene film, an aluminum foil, and a nylon film are laminated in this order.
- the exterior member 200 may be a laminate film having another laminated structure, a polymer film such as polypropylene, or a metal film.
- it may consist of a moisture-resistant aluminum laminate film in which a nylon film, an aluminum foil, and an unstretched polypropylene film are laminated in this order from the outside.
- An adhesive film 201 is inserted between the exterior member 200 and the positive electrode lead portion 223 and between the exterior member 200 and the negative electrode lead portion 225 in order to prevent outside air from entering.
- the adhesive film 201 may be made of a material having adhesiveness to the positive electrode lead portion 223 and the negative electrode lead portion 225, such as polyolefin resin, and more specifically, polyethylene, polypropylene, modified polyethylene, modified polypropylene, or the like. of polyolefin resin.
- the electrochemical device of the present invention can be used as a capacitor, as shown in the schematic cross-sectional view of FIG.
- a positive electrode 31 and a negative electrode 32 are arranged to face each other with a separator 33 impregnated with an electrolytic solution interposed therebetween.
- a gel electrolyte membrane impregnated with an electrolytic solution may be arranged on the surface of at least one of the separator 33 , the positive electrode 31 and the negative electrode 32 .
- Reference numerals 35 and 36 indicate current collectors and reference numeral 37 indicates a gasket.
- the electrochemical device of the present invention can be used as an air battery as shown in the conceptual diagram of FIG.
- Such an air battery includes, for example, an oxygen-selective permeable membrane 47 that is impermeable to water vapor and selectively permeable to oxygen, an air-electrode-side current collector 44 made of a conductive porous material, and the air-electrode-side current collector 44. and the porous positive electrode 41, the porous diffusion layer 46 made of a conductive material, the porous positive electrode 41 containing the conductive material and the catalyst material, the separator and the electrolytic solution (or the electrolytic solution 43, a negative electrode 42 that releases magnesium ions, a negative electrode-side current collector 45, and an exterior body 48 that accommodates these layers.
- Oxygen 52 in air (for example, the atmosphere) 51 is selectively permeated by the oxygen selective permeable membrane 47, passes through the air electrode side current collector 44 made of a porous material, is diffused by the diffusion layer 46, and is diffused by the porous positive electrode. 41.
- the progress of oxygen passing through the oxygen-selective permeable membrane 47 is partially blocked by the cathode-side current collector 44, but the oxygen that has passed through the cathode-side current collector 44 is diffused by the diffusion layer 46 and spreads. , the oxygen is efficiently distributed over the entire surface of the porous positive electrode 41 , and the supply of oxygen to the entire surface of the porous positive electrode 41 is not hindered by the air electrode side current collector 44 .
- the electrochemical device of the present invention can be used as a fuel cell as shown in the conceptual diagram of FIG.
- the fuel cell includes, for example, a positive electrode 61, a positive electrode electrolyte 62, a positive electrode electrolyte transport pump 63, a fuel channel 64, a positive electrode electrolyte storage container 65, a negative electrode 71, a negative electrode electrolyte 72, and a negative electrode electrolyte transport. It is composed of a pump 73 , a fuel channel 74 , a negative electrode electrolyte storage container 75 and an ion exchange membrane 66 .
- the positive electrode electrolyte 62 continuously or intermittently flows (circulates) through the fuel flow path 64 via the positive electrode electrolyte storage container 65 and the positive electrode electrolyte transport pump 63, and the fuel flow is A negative electrode electrolyte 72 continuously or intermittently flows or circulates in the passage 74 via a negative electrode electrolyte storage container 75 and a negative electrode electrolyte transport pump 73 . Electricity is generated between As the positive electrode electrolyte solution 62 , an electrolyte solution to which a positive electrode active material is added can be used, and as the negative electrode electrolyte solution 72 , an electrolyte solution to which a negative electrode active material is added can be used.
- a Mg metal plate can be used, and the negative electrode can also be manufactured by the following method.
- an Mg electrolytic solution (Mg-EnPS) containing MgCl 2 and EnPS (ethyl-n-propylsulfone) is prepared, and using this Mg electrolytic solution, Mg metal is deposited on a Cu foil based on an electrolytic plating method. Then, a Mg plated layer may be formed on the Cu foil as a negative electrode active material layer.
- the electrochemical device according to the present invention can be used particularly as a magnesium secondary battery as described with reference to FIGS. I'll explain. Note that the configuration of each application example described below is merely an example, and the configuration can be changed as appropriate.
- a magnesium secondary battery can be used in the form of a battery pack.
- battery packs are simple battery packs (so-called soft packs) using magnesium secondary batteries, and are mounted in electronic devices such as smartphones, for example.
- an assembled battery composed of six magnesium secondary batteries connected in two parallel and three series may be provided.
- the connection form of the magnesium secondary battery may be series, parallel, or a mixture of both.
- FIG. 7 shows a block diagram showing a circuit configuration example when the magnesium secondary battery of the present invention is applied to a battery pack.
- the battery pack includes cells (eg, assembled battery) 1001 , an exterior member, a switch section 1021 , a current detection resistor 1014 , a temperature detection element 1016 and a control section 1010 .
- the switch section 1021 has a charge control switch 1022 and a discharge control switch 1024 .
- the battery pack also has a positive terminal 1031 and a negative terminal 1032, and the positive terminal 1031 and the negative terminal 1032 are connected to the positive terminal and the negative terminal of the charger, respectively, during charging.
- the positive terminal 1031 and the negative terminal 1032 are connected to the positive terminal and the negative terminal of the electronic device, respectively, and discharge is performed.
- a cell 1001 is configured by connecting a plurality of magnesium secondary batteries 1002 according to the present disclosure in series and/or in parallel.
- FIG. 7 shows a case where six magnesium secondary batteries 1002 are connected in 2-parallel and 3-series (2P3S). Any connection method may be used.
- the switch section 1021 includes a charge control switch 1022 and a diode 1023, a discharge control switch 1024 and a diode 1025, and is controlled by the control section 1010.
- Diode 1023 has a reverse polarity for charging current flowing from positive terminal 1031 to cell 1001 and a forward polarity for discharging current flowing from negative terminal 1032 to cell 1001 .
- Diode 1025 has a forward polarity for charging current and a reverse polarity for discharging current.
- the switch section is provided on the plus (+) side, but it may be provided on the minus (-) side.
- the charge control switch 1022 is closed when the battery voltage reaches the overcharge detection voltage, and is controlled by the controller 1010 so that the charging current does not flow through the current path of the cell 1001 . After the charge control switch 1022 is closed, only discharging is possible through the diode 1023 . Further, when a large current flows during charging, the control unit 1010 controls the cell 1001 so as to be closed and cut off the charging current flowing through the current path of the cell 1001 .
- the discharge control switch 1024 is closed when the battery voltage reaches the overdischarge detection voltage, and is controlled by the controller 1010 so that the discharge current does not flow through the current path of the cell 1001 . After the discharge control switch 1024 is closed, only charging is possible through the diode 1025 . Further, when a large current flows during discharge, the cell 1001 is closed and controlled by the control unit 1010 so as to cut off the discharge current flowing through the current path of the cell 1001 .
- the temperature detection element 1016 is, for example, a thermistor, and is provided near the cell 1001 .
- Voltage measurement unit 1012 measures the voltage of cell 1001 and the voltage of each magnesium secondary battery 1002 that constitutes cell 1001 , A/D-converts the measurement results, and sends them to control unit 1010 .
- Current measurement section 1013 measures current using current detection resistor 1014 and sends the measurement result to control section 1010 .
- Switch control section 1020 controls charge control switch 1022 and discharge control switch 1024 of switch section 1021 based on the voltage and current sent from voltage measurement section 1012 and current measurement section 1013 .
- Switch control unit 1020 switches switch unit 1021 to switch unit 1021 when the voltage of any of magnesium secondary batteries 1002 becomes equal to or lower than the overcharge detection voltage or overdischarge detection voltage and/or when a large current suddenly flows. Overcharging, overdischarging, and overcurrent charging/discharging are prevented by sending a control signal.
- the charge control switch 1022 and the discharge control switch 1024 can be composed of semiconductor switches such as MOSFETs. In this case, diodes 1023 and 1025 are formed by the parasitic diodes of the MOSFETs.
- switch control section 1020 supplies control signal DO and control signal CO to the gate sections of charge control switch 1022 and discharge control switch 1024, respectively.
- Charge control switch 1022 and discharge control switch 1024 are turned on by a gate potential lower than the source potential by a predetermined value or more. That is, in normal charging and discharging operations, the control signal CO and the control signal DO are set to low level, and the charge control switch 1022 and the discharge control switch 1024 are set to the conducting state. Then, for example, in the case of overcharge or overdischarge, the control signal CO and the control signal DO are set to high level, and the charge control switch 1022 and the discharge control switch 1024 are closed.
- the memory 1011 is composed of, for example, an EPROM (Erasable Programmable Read Only Memory), which is a non-volatile memory.
- the memory 1011 stores in advance the numerical value calculated by the control unit 1010 and/or the internal resistance value of the magnesium secondary battery in the initial state of each magnesium secondary battery 1002 measured at the stage of the manufacturing process. Moreover, rewriting is possible as appropriate. Further, by storing the full charge capacity of the magnesium secondary battery 1002, it is possible to calculate, for example, the remaining capacity together with the control unit 1010.
- the temperature measurement unit 1015 measures the temperature using the temperature detection element 1016, performs charge/discharge control when abnormal heat is generated, and performs correction in calculating the remaining capacity.
- FIG. 8A is a block diagram showing the configuration of an electric vehicle such as a hybrid vehicle, which is an example of an electric vehicle.
- the electric vehicle includes, for example, a control unit 2001, various sensors 2002, a power supply 2003, an engine 2010, a generator 2011, inverters 2012 and 2013, a drive motor 2014, a differential gear 2015, It has a transmission 2016 and a clutch 2017 .
- the electric vehicle includes, for example, a front wheel drive shaft 2021 , front wheels 2022 , rear wheel drive shaft 2023 , and rear wheels 2024 connected to a differential 2015 and/or transmission 2016 .
- the electric vehicle can run using either the engine 2010 or the motor 2014 as a drive source.
- Engine 2010 is a main power source, such as a gasoline engine.
- the driving force (rotational force, for example) of the engine 2010 is transmitted to the front wheels 2022 or the rear wheels 2024 via, for example, a differential device 2015, a transmission 2016, and a clutch 2017, which are driving units.
- the rotational force of the engine 2010 is also transmitted to the generator 2011, and the generator 2011 uses the rotational force to generate AC power, which is converted into DC power via the inverter 2013 and stored in the power supply 2003. .
- the motor 2014 which is a conversion unit
- the power for example, DC power
- the AC power is used to drive the motor 2014.
- a driving force (rotational force, for example) converted from electric power by the motor 2014 is transmitted to the front wheels 2022 or the rear wheels 2024 via a differential gear 2015, a transmission 2016, and a clutch 2017, which are driving units, for example.
- the control unit 2001 controls the operation of the entire electric vehicle, and includes, for example, a CPU.
- Power source 2003 may comprise one or more magnesium secondary batteries (not shown) in accordance with the present invention.
- the power supply 2003 may be configured to be connected to an external power supply and store power by receiving power supply from the external power supply.
- Various sensors 2002 are used, for example, to control the rotational speed of engine 2010 and to control the opening of a throttle valve (not shown) (throttle opening).
- Various sensors 2002 include, for example, a speed sensor, an acceleration sensor, and/or an engine speed sensor.
- the electric vehicle may be a vehicle that operates using only the power source 2003 and the motor 2014 without using the engine 2010 (for example, an electric vehicle).
- FIG. 8B A block diagram showing the configuration of a power storage system (for example, a power supply system) is shown in FIG. 8B.
- the power storage system includes, for example, a control unit 3001, a power source 3002, a smart meter 3003, and a power hub 3004 inside a house 3000 such as a general house or commercial building.
- the power supply 3002 is connected to, for example, an electric device (for example, an electronic device) 3010 installed inside the house 3000 and can be connected to an electric vehicle 3011 parked outside the house 3000 .
- the power source 3002 is connected, for example, to a private power generator 3021 installed in the house 3000 via a power hub 3004, and is connectable to an external centralized power system 3022 via a smart meter 3003 and the power hub 3004. be.
- Electrical equipment (eg, electronic equipment) 3010 includes, for example, one or more home appliances. Home appliances include, for example, refrigerators, air conditioners, television receivers, and/or water heaters.
- Private power generator 3021 is composed of, for example, a solar power generator and/or a wind power generator.
- Examples of the electric vehicle 3011 include an electric vehicle, a hybrid vehicle, an electric motorcycle, an electric bicycle, and/or a Segway (registered trademark).
- Centralized power system 3022 can include utility power, generators, power grids, and/or smart grids (eg, next-generation power grids), and can include, for example, thermal power plants, nuclear power plants, hydroelectric power plants. , and/or wind farms, etc., and the power generators included in the centralized power system 3022 include various solar cells, fuel cells, wind power generators, micro-hydro power generators, and/or geothermal power generators. Devices and the like can be exemplified, but are not limited to these.
- the control unit 3001 controls the operation of the entire power storage system (including the usage state of the power supply 3002), and includes, for example, a CPU.
- Power source 3002 may comprise one or more magnesium secondary batteries (not shown) in accordance with the present invention.
- the smart meter 3003 is, for example, a network-compatible power meter installed in the house 3000 on the power demand side, and can communicate with the power supply side.
- electric power is stored in the power supply 3002 from the centralized electric power system 3022, which is an external power supply, via the smart meter 3003 and the power hub 3004, and is stored from the private power generator 3021, which is an independent power supply, via the power hub 3004.
- Power is stored in the power supply 3002 as a result. Since the electric power accumulated in the power source 3002 is supplied to the electric device (eg, electronic device) 3010 and the electric vehicle 3011 in accordance with an instruction from the control unit 3001, the electric device (eg, electronic device) 3010 can be operated. , the electric vehicle 3011 can be charged. That is, the power storage system is a system that enables the storage and supply of power within the house 3000 using the power source 3002 .
- the power stored in the power supply 3002 can be used arbitrarily. Therefore, for example, power can be stored in the power supply 3002 from the centralized power system 3022 at midnight when the electricity rate is low, and the power stored in the power supply 3002 can be used during the day when the power rate is high.
- the power storage system described above may be installed for each household (for example, one household), or may be installed for multiple households (for example, multiple households).
- the power tool is, for example, an electric drill, and includes a control unit 4001 and a power supply 4002 inside a tool body 4000 made of plastic material or the like.
- a drill portion 4003, which is a movable portion, is rotatably attached to the tool body 4000, for example.
- the control unit 4001 controls the overall operation of the power tool (including the use state of the power source 4002), and includes, for example, a CPU.
- Power source 4002 may comprise one or more magnesium secondary batteries (not shown) in accordance with the present invention.
- the control unit 4001 supplies electric power from the power supply 4002 to the drill unit 4003 according to the operation of an operation switch (not shown).
- Electrolytes can also be mixed with organic polymers (eg, polyethylene oxide, polyacrylonitrile and/or polyvinylidene fluoride (PVdF)) and used as gel electrolytes.
- organic polymers eg, polyethylene oxide, polyacrylonitrile and/or polyvinylidene fluoride (PVdF)
- Example A1 (material) ⁇ MgCl2 (anhydrous): Sigma-Aldrich ⁇ MgTFSI2 (magnesium bistrifluoromethanesulfonylimide): Toyama Pharmaceutical ⁇ Dimethoxyethane (DME): Toyama Pharmaceutical ⁇ Diethylene glycol dimethyl ether (G2): Toyama Pharmaceutical ⁇ Sulfur crystal (S): Acetylene black (AB) manufactured by Wako Pure Chemical Industries, Ltd.): Denka black (DB): manufactured by Denki Kagaku Kogyo (specific surface area 68 m 2 /g) ⁇ Ketjen Black (KB): Made by Lion (specific surface area 1270m 2 /g) ⁇ Styrene-butadiene rubber (SBR): manufactured by JSR ⁇ Carboxymethylcellulose: manufactured by Daiichi Kogyo Seiyaku ⁇ Mg plate (purity 99.9%, thickness 200 ⁇ m): manufactured by Rikazai ⁇ G
- Sulfur and carbon materials were used in a weight ratio of 50:50.
- Denka black and Ketjen black were used as the carbon material in a weight ratio of 50:50.
- Sulfur and Denka black were weighed out in a predetermined weight ratio and dry-mixed using an agate mortar.
- Ketjen Black was weighed and added so as to have a predetermined weight ratio, and dry-mixed with an agate mortar to obtain a carbon-sulfur composite.
- a carbon-sulfur composite, styrene-butadiene rubber, and carboxymethyl cellulose were added to a mixed solution of water/methanol at a volume ratio of 10:90, and mixed with a pencil mixer to prepare a positive electrode slurry (solid content: 20% by weight).
- the total amount of styrene-butadiene rubber and carboxymethylcellulose was 1% by weight relative to the carbon-sulfur composite, and the weight ratio of styrene-butadiene rubber and carboxymethylcellulose was 1:25.
- the positive electrode slurry was applied onto a SUS304 foil using a bar coater, and subjected to vacuum drying at 40° C. for 12 hours and normal pressure drying at 80° C. for 30 minutes to prepare a positive electrode sheet (formation of positive electrode layer). This was punched out so as to have a diameter of 15 mm to obtain a sulfur positive electrode.
- FIG. 9 shows a schematic exploded view of the produced battery.
- a gasket 22 is placed on a coin battery can 21, and a sulfur positive electrode 23, a glass fiber separator 24, a negative electrode 25, a spacer 26 made of a stainless steel plate with a thickness of 0.5 mm, and a coin battery lid 27 are laminated in this order, and then the coin battery can is placed.
- 21 was crimped and sealed.
- the spacer 26 was previously spot welded to the coin cell lid 27 .
- the electrolytic solution was used in the form of being contained in the separator 24 of the coin battery 20 .
- FIG. 10 shows the measurement results.
- the discharge conditions were as follows. Discharge conditions: CC discharge 0.1mA/-0.6V cutoff Temperature: 25°C
- Example A2 Comparative Example A1, Examples B1 and B2, Comparative Example B1, Example C1, and Comparative Example C1, which will be described later, the discharge capacity was measured in the same manner as in Example A1.
- the discharge capacities of the examples were evaluated by the rate of increase from the discharge capacities of the respective comparative examples. Details are as follows.
- the discharge capacities of Examples A1 and A2 were evaluated by the rate of increase from the discharge capacity of Comparative Example A1.
- the discharge capacities of Examples B1 and B2 were evaluated by the rate of increase from the discharge capacity of Comparative Example B1.
- the discharge capacity of Example C1 was evaluated by the rate of increase from the discharge capacity of Comparative Example C1.
- Example A2 Comparative Example A1, Examples B1 and B2, Comparative Example B1, Example C1 and Comparative Example C1
- a coin battery was manufactured and the discharge capacity was measured in the same manner as in Example A1, except that the weight ratio of sulfur and carbon materials and the weight ratio of Denka Black and Ketjenblack were changed to the ratios shown in the table. .
- the positive electrode layers in the positive electrodes obtained in Example A1 and Comparative Example A1 were subjected to EDS mapping (2500 times) for elemental sulfur.
- the sulfur element was sufficiently uniformly dispersed.
- sulfur elements were aggregated and not uniformly dispersed.
- the positive electrode of the present invention can be used in various fields where energy is extracted using electrochemical reactions.
- the positive electrode of the present invention can be used not only in secondary batteries but also in various electrochemical devices such as capacitors, air batteries and fuel cells.
- electrochemical devices particularly secondary batteries, capacitors, air batteries and fuel cells
- containing the positive electrode according to the present invention can be used in the electronics packaging field.
- the electrochemical device containing the positive electrode according to one embodiment of the present invention is also used in the electric, information, and communication fields where mobile devices are used (e.g., mobile phones, smartphones, laptops, digital cameras, activity meters, arm computers, etc.) , electronic paper, wearable devices, RFID tags, card-type electronic money, small electronic devices such as smart watches, etc.), home and small industrial applications (e.g., electric tools, golf carts, home/nursing/industrial robots), large industrial applications (e.g. forklifts, elevators, harbor cranes), transportation systems (e.g.
- mobile devices e.g., mobile phones, smartphones, laptops, digital cameras, activity meters, arm computers, etc.
- electronic paper e.g., electronic paper, wearable devices, RFID tags, card-type electronic money, small electronic devices such as smart watches, etc.
- home and small industrial applications e.g., electric tools, golf carts, home/nursing/industrial robots
- large industrial applications e.g. forklifts, elevator
- hybrid vehicles electric vehicles, buses, trains, electrically assisted bicycles, electric motorcycles, etc.
- electric power system applications for example, various power generation, road conditioners, smart grids, general household electrical storage systems, etc.
- medical applications medical equipment such as earphone hearing aids
- medical applications dosing management systems, etc.
- space/deep-sea applications for example, space probes, submersible research ships, etc.
- Positive electrode Electrolyte solution for positive electrode 63
- Positive electrode electrolyte transport pump 64
- Fuel channel 65
- Positive electrode electrolyte storage container 71
- Negative electrode 72
- Negative electrode electrolyte 73
- Negative Electrolyte Transport Pump 74
- Fuel Channel 75
- Negative Electrolyte Storage Container 66
- Ion Exchange Membrane 100
- Magnesium Secondary Battery 111
- Insulating plate 114
- Battery cover 115
- Thermal resistance element PTC element
- Adhesive film 221... Electrode structure, 223... Positive electrode lead part, 225... Negative lead part, 1001... Cell (assembled battery) 1002
- Magnesium secondary battery 1010 Control unit 1011 Memory 1012 Voltage measurement unit 1013 Current measurement unit 1014 Current detection Resistor 1015 Temperature measurement unit 1016 Temperature detection element 1020 Switch control unit 1021 Switch unit 1022 Charge control switch 1024 Discharge control switch 1023, 1025 Diode 1031 Positive terminal 1032 Negative terminal CO, DO Control signal 2000 Housing 2001 Control section 2002 Various Sensor, 2003... Power source, 2010... Engine, 2011... Generator, 2012, 2013... Inverter, 2014...
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Abstract
Description
導電助剤としてカーボンブラックを用いた場合、より十分な放電容量(または放電容量効率)が得られなかった。
硫黄および炭素材料を含む正極であって、
炭素材料は、第1の比表面積を有するカーボンブラックおよび第2の比表面積を有するカーボンブラックを含み、第1の比表面積は第2の比表面積よりも低い、正極、ならびに
当該正極を含む、電気化学デバイスに関する。
本発明の正極は、電気化学デバイスに用いられる。つまり、本明細書で説明する正極は、電気化学的な反応を利用してエネルギーを取り出すことができるデバイスのための正極に相当する。本発明の正極は、放電容量のさらなる向上の観点から、マグネシウム-硫黄二次電池での使用に好適である。マグネシウム-硫黄二次電池は、負極活物質としてマグネシウムを含む負極および正極活物質として硫黄を含む正極を備えた二次電池のことである。本明細書中、放電容量とは、初回放電時における硫黄単位重量あたりの放電容量のことである。放電容量は高いほど、好ましい。
まず、硫黄および低比表面積カーボンブラックを所定の重量比にて、メノウ乳鉢を用いて乾式混合する。この混合物に、高比表面積カーボンブラックを所定の重量比にて添加し、メノウ乳鉢により乾式混合を行う。次いで、得られた炭素硫黄複合体を、結着剤とともに、溶媒に添加し、ペンシルミキサーにより混合することで正極スラリーを得る。正極スラリーを、正極集電体上にバーコーターを用いて塗布し、10℃以上50℃以下で6時間以上24時間以下の真空乾燥を行った後、50℃以上80℃以下で10分間以上120分間以下の常圧乾燥を行う。
本発明において負極はマグネシウムを含む電極であってもよい。負極を構成する材料(具体的には、負極活物質)は、“マグネシウムを含む電極”ゆえ、好ましくはマグネシウム金属単体、マグネシウム合金あるいはマグネシウム化合物から成っている。負極がマグネシウムの金属単体物(例えばマグネシウム板など)から成る場合、その金属単体物のMg純度は90%以上、好ましくは95%以上、更に好ましくは98%以上となっている。負極は、例えば、板状材料あるいは箔状材料から作製することができるが、これに限定するものではなく、粉末を用いて形成(賦形)することも可能である。
本発明の電気化学デバイスにおいて、正極と負極とは、両極の接触による短絡を防止しつつ、マグネシウムイオンを通過させる無機セパレータあるいは有機セパレータによって分離されていてもよい。無機セパレータとしては、例えば、ガラスフィルター、グラスファイバーを挙げることができる。有機セパレータとしては、例えば、ポリテトラフルオロエチレン、ポリプロピレンおよび/またはポリエチレン等から成る合成樹脂製の多孔質膜を挙げることができ、これらの2種類以上の多孔質膜を積層した構造とすることもできる。中でも、ポリオレフィン製の多孔質膜は短絡防止効果に優れ、且つ、シャットダウン効果による電池の安全性向上を図ることができるので好ましい。
電気化学デバイスにおける電解質層は電解液から構成され、電解液を保持する保持体として高分子化合物をさらに含んでもよい。電解質層は上記セパレータ内に含浸されて配置されてもよい。高分子化合物は、電解液によって膨潤されるものであってもよい。この場合、電解液により膨潤された高分子化合物はゲル状であってもよい。かかる高分子化合物として、例えば、ポリアクリロニトリル、ポリフッ化ビニリデン、フッ化ビニリデンとヘキサフルオロプロピレンとの共重合体、ポリテトラフルオロエチレン、ポリヘキサフルオロプロピレン、ポリエチレンオキサイド、ポリプロピレンオキサイド、ポリフォスファゼン、ポリシロキサン、ポリ酢酸ビニル、ポリビニルアルコール、ポリメタクリル酸メチル、ポリアクリル酸、ポリメタクリル酸、スチレン-ブタジエンゴム、ニトリル-ブタジエンゴム、ポリスチレンおよび/またはポリカーボネートを挙げることができる。特に、電気化学的な安定性の観点をより重視するならば、ポリアクリロニトリル、ポリフッ化ビニリデン、ポリヘキサフルオロプロピレンあるいはポリエチレンオキサイドであってよい。電解質層は固体電解質層としてもよい。
エチレングリコールジメチルエーテル、エチレングリコールエチルメチルエーテル、エチレングリコールメチルプロピルエーテル、エチレングリコールブチルメチルエーテル、エチレングリコールメチルペンチルエーテル、エチレングリコールメチルヘキシルエーテル、エチレングリコールメチルへプチルエーテル、エチレングリコールメチルオクチルエーテル;
エチレングリコールジエチルエーテル、エチレングリコールエチルプロピルエーテル、エチレングリコールブチルエチルエーテル、エチレングリコールエチルペンチルエーテル、エチレングリコールエチルヘキシルエーテル、エチレングリコールエチルへプチルエーテル、エチレングリコールエチルオクチルエーテル;
エチレングリコールジプロピルエーテル、エチレングリコールブチルプロピルエーテル、エチレングリコールプロピルペンチルエーテル、エチレングリコールプロピルヘキシルエーテル、エチレングリコールプロピルへプチルエーテル、エチレングリコールプロピルオクチルエーテル;
エチレングリコールジブチルエーテル、エチレングリコールブチルペンチルエーテル、エチレングリコールブチルヘキシルエーテル、エチレングリコールブチルへプチルエーテル、エチレングリコールブチルオクチルエーテル;
エチレングリコールジペンチルエーテル、エチレングリコールヘキシルペンチルエーテル、エチレングリコールへプチルペンチルエーテル、エチレングリコールオクチルペンチルエーテル;
エチレングリコールジヘキシルエーテル、エチレングリコールへプチルヘキシルエーテル、エチレングリコールヘキシルオクチルエーテル;
エチレングリコールジへプチルエーテル、エチレングリコールへプチルオクチルエーテル;
エチレングリコールジオクチルエーテル
ジエチレングリコールジメチルエーテル、ジエチレングリコールエチルメチルエーテル、ジエチレングリコールメチルプロピルエーテル、ジエチレングリコールブチルメチルエーテル、ジエチレングリコールメチルペンチルエーテル、ジエチレングリコールメチルヘキシルエーテル、ジエチレングリコールメチルへプチルエーテル、ジエチレングリコールメチルオクチルエーテル;
ジエチレングリコールジエチルエーテル、ジエチレングリコールエチルプロピルエーテル、ジエチレングリコールブチルエチルエーテル、ジエチレングリコールエチルペンチルエーテル、ジエチレングリコールエチルヘキシルエーテル、ジエチレングリコールエチルへプチルエーテル、ジエチレングリコールエチルオクチルエーテル;
ジエチレングリコールジプロピルエーテル、ジエチレングリコールブチルプロピルエーテル、ジエチレングリコールプロピルペンチルエーテル、ジエチレングリコールプロピルヘキシルエーテル、ジエチレングリコールプロピルへプチルエーテル、ジエチレングリコールプロピルオクチルエーテル;
ジエチレングリコールジブチルエーテル、ジエチレングリコールブチルペンチルエーテル、ジエチレングリコールブチルヘキシルエーテル、ジエチレングリコールブチルへプチルエーテル、ジエチレングリコールブチルオクチルエーテル;
ジエチレングリコールジペンチルエーテル、ジエチレングリコールヘキシルペンチルエーテル、ジエチレングリコールへプチルペンチルエーテル、ジエチレングリコールオクチルペンチルエーテル;
ジエチレングリコールジヘキシルエーテル、ジエチレングリコールへプチルヘキシルエーテル、ジエチレングリコールヘキシルオクチルエーテル;
ジエチレングリコールジへプチルエーテル、ジエチレングリコールへプチルオクチルエーテル;
ジエチレングリコールジオクチルエーテル
トリエチレングリコールジメチルエーテル、トリエチレングリコールエチルメチルエーテル、トリエチレングリコールメチルプロピルエーテル、トリエチレングリコールブチルメチルエーテル、トリエチレングリコールメチルペンチルエーテル、トリエチレングリコールメチルヘキシルエーテル、トリエチレングリコールメチルへプチルエーテル、トリエチレングリコールメチルオクチルエーテル;
トリエチレングリコールジエチルエーテル、トリエチレングリコールエチルプロピルエーテル、トリエチレングリコールブチルエチルエーテル、トリエチレングリコールエチルペンチルエーテル、トリエチレングリコールエチルヘキシルエーテル、トリエチレングリコールエチルへプチルエーテル、トリエチレングリコールエチルオクチルエーテル;
トリエチレングリコールジプロピルエーテル、トリエチレングリコールブチルプロピルエーテル、トリエチレングリコールプロピルペンチルエーテル、トリエチレングリコールプロピルヘキシルエーテル、トリエチレングリコールプロピルへプチルエーテル、トリエチレングリコールプロピルオクチルエーテル;
トリエチレングリコールジブチルエーテル、トリエチレングリコールブチルペンチルエーテル、トリエチレングリコールブチルヘキシルエーテル、トリエチレングリコールブチルへプチルエーテル、トリエチレングリコールブチルオクチルエーテル;
トリエチレングリコールジペンチルエーテル、トリエチレングリコールヘキシルペンチルエーテル、トリエチレングリコールへプチルペンチルエーテル、トリエチレングリコールオクチルペンチルエーテル;
トリエチレングリコールジヘキシルエーテル、トリエチレングリコールへプチルヘキシルエーテル、トリエチレングリコールヘキシルオクチルエーテル;
トリエチレングリコールジへプチルエーテル、トリエチレングリコールへプチルオクチルエーテル;
トリエチレングリコールジオクチルエーテル
テトラエチレングリコールジメチルエーテル、テトラエチレングリコールエチルメチルエーテル、テトラエチレングリコールメチルプロピルエーテル、テトラエチレングリコールブチルメチルエーテル、テトラエチレングリコールメチルペンチルエーテル、テトラエチレングリコールメチルヘキシルエーテル、テトラエチレングリコールメチルへプチルエーテル、テトラエチレングリコールメチルオクチルエーテル;
テトラエチレングリコールジエチルエーテル、テトラエチレングリコールエチルプロピルエーテル、テトラエチレングリコールブチルエチルエーテル、テトラエチレングリコールエチルペンチルエーテル、テトラエチレングリコールエチルヘキシルエーテル、テトラエチレングリコールエチルへプチルエーテル、テトラエチレングリコールエチルオクチルエーテル;
テトラエチレングリコールジプロピルエーテル、テトラエチレングリコールブチルプロピルエーテル、テトラエチレングリコールプロピルペンチルエーテル、テトラエチレングリコールプロピルヘキシルエーテル、テトラエチレングリコールプロピルへプチルエーテル、テトラエチレングリコールプロピルオクチルエーテル;
テトラエチレングリコールジブチルエーテル、テトラエチレングリコールブチルペンチルエーテル、テトラエチレングリコールブチルヘキシルエーテル、テトラエチレングリコールブチルへプチルエーテル、テトラエチレングリコールブチルオクチルエーテル;
テトラエチレングリコールジペンチルエーテル、テトラエチレングリコールヘキシルペンチルエーテル、テトラエチレングリコールへプチルペンチルエーテル、テトラエチレングリコールオクチルペンチルエーテル;
テトラエチレングリコールジヘキシルエーテル、テトラエチレングリコールへプチルヘキシルエーテル、テトラエチレングリコールヘキシルオクチルエーテル;
テトラエチレングリコールジへプチルエーテル、テトラエチレングリコールへプチルオクチルエーテル;
テトラエチレングリコールジオクチルエーテル
ペンタエチレングリコールジメチルエーテル、ペンタエチレングリコールエチルメチルエーテル、ペンタエチレングリコールメチルプロピルエーテル、ペンタエチレングリコールブチルメチルエーテル、ペンタエチレングリコールメチルペンチルエーテル、ペンタエチレングリコールメチルヘキシルエーテル、ペンタエチレングリコールメチルへプチルエーテル、ペンタエチレングリコールメチルオクチルエーテル;
ペンタエチレングリコールジエチルエーテル、ペンタエチレングリコールエチルプロピルエーテル、ペンタエチレングリコールブチルエチルエーテル、ペンタエチレングリコールエチルペンチルエーテル、ペンタエチレングリコールエチルヘキシルエーテル、ペンタエチレングリコールエチルへプチルエーテル、ペンタエチレングリコールエチルオクチルエーテル;
ペンタエチレングリコールジプロピルエーテル、ペンタエチレングリコールブチルプロピルエーテル、ペンタエチレングリコールプロピルペンチルエーテル、ペンタエチレングリコールプロピルヘキシルエーテル、ペンタエチレングリコールプロピルへプチルエーテル、ペンタエチレングリコールプロピルオクチルエーテル;
ペンタエチレングリコールジブチルエーテル、ペンタエチレングリコールブチルペンチルエーテル、ペンタエチレングリコールブチルヘキシルエーテル、ペンタエチレングリコールブチルへプチルエーテル、ペンタエチレングリコールブチルオクチルエーテル;
ペンタエチレングリコールジペンチルエーテル、ペンタエチレングリコールヘキシルペンチルエーテル、ペンタエチレングリコールへプチルペンチルエーテル、ペンタエチレングリコールオクチルペンチルエーテル;
ペンタエチレングリコールジヘキシルエーテル、ペンタエチレングリコールへプチルヘキシルエーテル、ペンタエチレングリコールヘキシルオクチルエーテル;
ペンタエチレングリコールジへプチルエーテル、ペンタエチレングリコールへプチルオクチルエーテル;
ペンタエチレングリコールジオクチルエーテル
ヘキサエチレングリコールジメチルエーテル、ヘキサエチレングリコールエチルメチルエーテル、ヘキサエチレングリコールメチルプロピルエーテル、ヘキサエチレングリコールブチルメチルエーテル、ヘキサエチレングリコールメチルペンチルエーテル、ヘキサエチレングリコールメチルヘキシルエーテル、ヘキサエチレングリコールメチルへプチルエーテル、ヘキサエチレングリコールメチルオクチルエーテル;
ヘキサエチレングリコールジエチルエーテル、ヘキサエチレングリコールエチルプロピルエーテル、ヘキサエチレングリコールブチルエチルエーテル、ヘキサエチレングリコールエチルペンチルエーテル、ヘキサエチレングリコールエチルヘキシルエーテル、ヘキサエチレングリコールエチルへプチルエーテル、ヘキサエチレングリコールエチルオクチルエーテル;
ヘキサエチレングリコールジプロピルエーテル、ヘキサエチレングリコールブチルプロピルエーテル、ヘキサエチレングリコールプロピルペンチルエーテル、ヘキサエチレングリコールプロピルヘキシルエーテル、ヘキサエチレングリコールプロピルへプチルエーテル、ヘキサエチレングリコールプロピルオクチルエーテル;
ヘキサエチレングリコールジブチルエーテル、ヘキサエチレングリコールブチルペンチルエーテル、ヘキサエチレングリコールブチルヘキシルエーテル、ヘキサエチレングリコールブチルへプチルエーテル、ヘキサエチレングリコールブチルオクチルエーテル;
ヘキサエチレングリコールジペンチルエーテル、ヘキサエチレングリコールヘキシルペンチルエーテル、ヘキサエチレングリコールへプチルペンチルエーテル、ヘキサエチレングリコールオクチルペンチルエーテル;
ヘキサエチレングリコールジヘキシルエーテル、ヘキサエチレングリコールへプチルヘキシルエーテル、ヘキサエチレングリコールヘキシルオクチルエーテル;
ヘキサエチレングリコールジへプチルエーテル、ヘキサエチレングリコールへプチルオクチルエーテル;
ヘキサエチレングリコールジオクチルエーテル
窒素含有官能基は、少なくとも窒素原子を含有する官能基であって、例えば、アミノ基、ニトロ基および/またはニトロソ基などを挙げることができる。
硫黄含有基は、少なくとも硫黄原子を含有する官能基であって、例えば、チオール基、スルフィド基、ジスルフィド基、スルホニル基、スルホ基、チオカルボニル基および/またはチオ尿素基などを挙げることができる。
本明細書における酸素含有官能基、窒素含有官能基および硫黄含有基は、それぞれ、互いに双方の概念を有するものであってよく、さらには、炭化水素基(脂肪族炭化水素基、芳香族炭化水素基または芳香脂肪族炭化水素基)の範疇に入るものであってもよい。
本発明の電気化学デバイスは、二次電池として構成することができ、その場合の概念図を図1に示す。図示するように、充電時、マグネシウムイオン(Mg2+)が正極10から電解質層12を通って負極11に移動することにより電気エネルギーを化学エネルギーに変換して蓄電する。放電時には、負極11から電解質層12を通って正極10にマグネシウムイオンが戻ることにより電気エネルギーを発生させる。
(材料)
・MgCl2(無水物):シグマアルドリッチ製
・MgTFSI2(マグネシウムビストリフルオロメタンスルホニルイミド):富山薬品工業製
・ジメトキシエタン(DME):富山薬品工業製
・ジエチレングリコールジメチルエーテル(G2):富山薬品工業製
・硫黄結晶(S):和光純薬製
・アセチレンブラック(AB)):デンカブラック(DB):電気化学工業製(比表面積68m2/g)
・ケッチェンブラック(KB):ライオン製(比表面積1270m2/g)
・スチレンブタジエンゴム(SBR):JSR製
・カルボキシメチルセルロース:第一工業製薬製
・Mg板(純度99.9%、厚さ200μm):リカザイ製
・グラスファイバー(GC50):Advantec製
硫黄および炭素材料を重量比が50:50となるように用いた。
炭素材料としては、デンカブラックおよびケッチェンブラックを重量比が50:50となるように用いた。
硫黄およびデンカブラックを所定の重量比となるように秤取し、メノウ乳鉢を用いて乾式混合した。これに、ケッチェンブラックを所定の重量比となるように秤量して添加し、メノウ乳鉢により乾式混合を行い、炭素硫黄複合体を得た。炭素硫黄複合体、スチレンブタジエンゴムおよびカルボキシメチルセルロースを、水/メタノールの体積比10:90の混合溶液に添加し、ペンシルミキサーにより混合することで正極スラリー(固形分20重量%)を作製した。スチレンブタジエンゴムおよびカルボキシメチルセルロースの合計量は炭素硫黄複合体に対して1重量%であり、スチレンブタジエンゴムおよびカルボキシメチルセルロースの重量比は1:25であった。正極スラリーを、SUS304箔上にバーコーターを用いて塗布し、40℃で12時間の真空乾燥および80℃で30分間の常圧乾燥を行うことで正極シートを作製した(正極層の形成)。これを直径が15mmとなるように打ち抜いて硫黄正極を得た。
以下の仕様で、マグネシウム-硫黄二次電池のコイン電池を製造した。
●正極:上記硫黄正極
●負極:直径16mmおよび厚み200μmのMg板/純度99.9%(リカザイ株式会社製のマグネシウム板)
●電解液
・マグネシウム塩:ハロゲン金属塩(MgCl2(無水物):シグマアルドリッチ製、品番449172、0.8M)、およびイミド金属塩(Mg(TFSI)2:富山薬品工業株式会社製、品番MGTFSI、0.8M)
・直鎖エーテル溶媒:ジエチレングリコールジメチルエーテル(超脱水品)、(富山薬品工業、品番G2)
●セパレータ:グラスファイバー(Advantec製グラスファイバー、品番GC50)
●二次電池形態:コイン電池CR2016タイプ
コイン電池缶21にガスケット22を載せ、硫黄正極23、グラスファイバー製のセパレータ24、負極25、厚さ0.5mmのステンレス鋼板から成るスペーサ26、コイン電池蓋27の順に積層した後、コイン電池缶21をかしめて封止した。スペーサ26はコイン電池蓋27に予めスポット溶接しておいた。電解液は、コイン電池20のセパレータ24に含ませる形態で用いた。
作製した電池を放電に付し、放電容量を測定した。測定結果を図10に示す。放電条件は、以下の通りであった。
放電条件:CC放電0.1mA/-0.6Vカットオフ
温度:25℃
実施例の放電容量は、それぞれの比較例の放電容量からの上昇率により評価した。
詳しくは以下の通りである。
実施例A1~A2の放電容量は、比較例A1の放電容量からの上昇率により評価した。
実施例B1~B2の放電容量は、比較例B1の放電容量からの上昇率により評価した。
実施例C1の放電容量は、比較例C1の放電容量からの上昇率により評価した。
○;110%≦上昇率<130%(優良);
×;上昇率<110%(実用上問題あり)。
硫黄および炭素材料の重量比ならびにデンカブラックおよびケッチェンブラックの重量比を表に記載の比率に変更したこと以外、実施例A1と同様の方法により、コイン電池の製造および放電容量の測定を行った。
実施例A1の正極層においては、硫黄元素は十分に均一に分散されていた。
比較例A1の正極層においては、硫黄元素は凝集しており、均一に分散されていなかった。
2・・・電源、3003・・・スマートメータ、3004・・・パワーハブ、3010・・・電気機器(電子機器)、3011・・・電動車両、3021・・・自家発電機、3022・・・集中型電力系統、4000・・・工具本体、4001・・・制御部、4002・・・電源、4003・・・ドリル部
Claims (12)
- 硫黄および炭素材料を含み、
前記炭素材料は、第1の比表面積を有するカーボンブラックおよび第2の比表面積を有するカーボンブラックを含み、前記第1の比表面積は前記第2の比表面積よりも低い、正極。 - 前記第1の比表面積は30m2/g以上200m2/g以下であり、
前記第2の比表面積は800m2/g以上1600m2/g以下である、請求項1に記載の正極。 - 前記第1の比表面積をSA(m2/g)としたとき、
前記第2の比表面積は10×SA(m2/g)以上、30×SA(m2/g)以下である、請求項1または2に記載の正極。 - 前記第2の比表面積を有するカーボンブラックの含有量は、前記第1の比表面積を有するカーボンブラックおよび前記第2の比表面積を有するカーボンブラックの合計量に対して、5重量%以上75重量%以下である、請求項1~3のいずれかに記載の正極。
- 前記第2の比表面積を有するカーボンブラックの含有量は、前記第1の比表面積を有するカーボンブラックおよび前記第2の比表面積を有するカーボンブラックの合計量に対して、20重量%以上50重量%以下である、請求項1~4のいずれかに記載の正極。
- 前記炭素材料の含有量は、前記硫黄および前記炭素材料の合計量に対して、5重量%以上70重量%以下である、請求項1~5のいずれかに記載の正極。
- 前記炭素材料の含有量は、前記硫黄および前記炭素材料の合計量に対して、20重量%以上60重量%以下である、請求項1~6のいずれかに記載の正極。
- 電気化学デバイスで使用される、請求項1~7のいずれかに記載の正極。
- 前記電気化学デバイスはマグネシウム-硫黄二次電池である、請求項8に記載の正極。
- 請求項1~9のいずれかに記載の正極を含む、電気化学デバイス。
- 前記電気化学デバイスは溶媒をさらに含み、
前記溶媒はエーテル系溶媒を含む、請求項10に記載の電気化学デバイス。 - 前記電気化学デバイスはマグネシウム-硫黄二次電池である、請求項10または11に記載の電気化学デバイス。
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EP1653534A1 (en) * | 2004-10-28 | 2006-05-03 | Samsung SDI Co., Ltd. | Conductive agent - positive active material composite for lithium secondary battery, method of preparing the same, and positive electrode and lithium secondary battery comprising the same |
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