WO2019139397A1 - Composition de suspension de cathode, cathode fabriquée à l'aide de cette composition et batterie la comprenant - Google Patents

Composition de suspension de cathode, cathode fabriquée à l'aide de cette composition et batterie la comprenant Download PDF

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Publication number
WO2019139397A1
WO2019139397A1 PCT/KR2019/000442 KR2019000442W WO2019139397A1 WO 2019139397 A1 WO2019139397 A1 WO 2019139397A1 KR 2019000442 W KR2019000442 W KR 2019000442W WO 2019139397 A1 WO2019139397 A1 WO 2019139397A1
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Prior art keywords
positive electrode
alcohol
weight
electrode
slurry composition
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PCT/KR2019/000442
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English (en)
Korean (ko)
Inventor
이재길
양두경
김유미
김윤경
조은경
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주식회사 엘지화학
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Priority to JP2020537476A priority Critical patent/JP7062771B2/ja
Priority to CN201980006826.XA priority patent/CN111542947A/zh
Priority to US16/958,599 priority patent/US11777091B2/en
Priority to EP19739062.8A priority patent/EP3723165A4/fr
Priority claimed from KR1020190003703A external-priority patent/KR102160714B1/ko
Publication of WO2019139397A1 publication Critical patent/WO2019139397A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/40—Alloys based on alkali metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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 a positive electrode composition, a positive electrode prepared using the same, and a battery comprising the same.
  • Li-S batteries have a high energy density and are becoming popular as next-generation secondary batteries that can replace lithium-ion batteries.
  • a lithium-sulfur battery includes a positive electrode containing a sulfur-carbon composite as an electrode active material, a negative electrode including a lithium metal or a lithium alloy, and a separator interposed between the positive electrode and the separator.
  • the positive electrode of such a lithium-sulfur battery is generally prepared by coating a positive electrode slurry on a metal foil.
  • the positive electrode slurry includes a positive electrode active material for storing energy, a conductive material for imparting electrical conductivity, (PVdF) is mixed with a solvent such as water and NMP (N-methyl pyrrolidone).
  • the dispersibility of the positive electrode active material and / or the conductive material significantly affects the processability of the electrode and the characteristics of the electrode formed thereby. Therefore, various methods for improving the dispersibility of the cathode active material and / or the conductive material in the cathode slurry have been studied.
  • Korean Patent Publication No. 10-2015-0025665 discloses a positive electrode active material, a conductive material, a binder, a dispersant and an aqueous solvent, wherein the dispersant includes a main chain of ionic characteristics and a side chain of nonionic surfactant characteristic Quot; positive electrode slurry for a secondary battery "
  • the present invention has been conceived to overcome the above-described problems of the prior art, and an object of the present invention is to provide a positive electrode manufacturing slurry which significantly improves the dispersibility of the positive electrode active material and the conductive material, reduces roughness of the electrode surface, And to provide a composition.
  • Another object of the present invention is to provide a slurry composition for cathode preparation, which has excellent dispersibility without using a separate dispersant and suppresses curling of the electrode, thereby having an advantage in a battery manufacturing process.
  • a positive electrode slurry composition comprising a positive electrode active material, a binder, an alcohol and water, wherein the content of the alcohol is 0.1 to 10% by weight based on the total weight of the composition.
  • a positive electrode prepared by applying the positive electrode slurry composition of the present invention onto a current collector is provided.
  • the positive electrode of the present invention is the positive electrode of the present invention.
  • a negative electrode comprising lithium metal or a lithium alloy as a negative electrode active material
  • a separator provided between the anode and the cathode
  • the slurry composition for preparing an anode of the present invention greatly improves the dispersibility of the cathode active material and the conductive material, reduces the roughness of the electrode surface, and significantly reduces the curling of the electrode. It also provides economic advantages in that no dispersant is used or usage is greatly reduced.
  • the battery including the positive electrode prepared from the slurry composition for positive electrode production provides the effect of greatly improving the capacity, lifetime characteristics, and economical efficiency.
  • Fig. 1 is a photograph showing the electrode curling state of the electrodes of Examples 5 to 8 and Comparative Examples 4 and 5 confirmed by Test Example 1.
  • the present invention relates to a positive electrode slurry composition
  • a positive electrode slurry composition comprising a positive electrode active material, a binder, an alcohol and water, wherein the content of the alcohol is 0.1 to 10% by weight based on the total weight of the composition.
  • the present inventors have paid attention to the reason why the positive electrode active material and the conductive material of the battery do not mix well with a binder or water having a high polarity in an aqueous slurry. That is, materials having extremely low polarity are used as the cathode active material and the conductive material, so that they do not mix well with the polar binder or water in the aqueous slurry. Accordingly, the present invention provides a solution to the above problem. That is, in the present invention, the technical feature is to improve the dispersibility of carbon and sulfur particles having low polarity by adding an alcohol solvent having an amphipathic nature. Since the alcohol solvent evaporates during the drying process and does not remain in the electrode, it does not increase the weight of the electrode and does not increase the resistance, so that the energy density of the electrode does not decrease.
  • a C1-C5 lower alcohol aqueous solution may be used as the alcohol aqueous solution.
  • the solid content in the slurry may be reduced during the slurry production due to the rapid evaporation rate.
  • the drying speed is slow, have.
  • an aqueous propanol solution is more preferably used. This is because the aqueous solution has a vapor pressure similar to that of water at a temperature range of 20 to 80 ° C.
  • aqueous propanol solution examples include 1-propanol aqueous solution.
  • the alcohol may be contained in an amount of 0.1 to 10% by weight, more preferably 1 to 7% by weight based on the total weight of the composition.
  • the content of the aqueous alcohol solution contained in the positive electrode slurry composition is within the range described above, the dispersibility of the positive electrode active material and / or the conductive material is greatly improved, the roughness of the electrode surface is reduced, do.
  • the electrode is dried during manufacturing of the electrode, cracks may be generated in the electrode during the process of manufacturing the battery, or the electrode may be removed from the current collector, so that the process age and cost are increased.
  • the improvement provides significant advantages in the electrode manufacturing process.
  • the content of the alcohol is less than 0.1% by weight, it is difficult to expect the above-mentioned objective effect. If the content of the alcohol is more than 10% by weight, the solubility of the binder in alcohol is lowered, .
  • the positive electrode slurry composition may include, but is not limited to, 10-78 wt% of a positive electrode active material, 1-50 wt% of a binder, 0.1-10 wt% of an alcohol, and residual water, based on the total weight of the composition.
  • composition may further comprise 0.1 to 10% by weight of a conductive material.
  • the positive electrode slurry composition of the present invention may contain alcohol in an amount of 2 to 45 parts by weight, more preferably 5 to 30 parts by weight, based on 100 parts by weight of the positive electrode active material and the conductive material.
  • the positive electrode slurry composition of the present invention may contain 0.1-15 wt% of alcohol and 85-99.9 wt% of water based on the total weight of alcohol and water, more preferably 0.5-10 wt% of alcohol % Of water and 90 to 99.5% by weight of water, more preferably 1 to 7% by weight of alcohol, and 93 to 99% by weight of water.
  • the content ratio of the alcohol contained in the positive electrode slurry composition satisfies the respective ranges described above, the dispersibility of the positive electrode active material and / or the conductive material is greatly improved, the roughness of the electrode surface is reduced, .
  • the electrode is dried during manufacturing of the electrode, cracks may be generated in the electrode during the process of manufacturing the battery, or the electrode may be removed from the current collector, so that the process age and cost are increased.
  • the improvement provides significant advantages in the electrode manufacturing process.
  • the positive electrode slurry composition of the present invention has a very excellent dispersibility of the positive electrode active material and / or the conductive material without using a dispersant.
  • the positive electrode slurry composition of the present invention can be preferably used for producing a positive electrode of a lithium-sulfur battery.
  • a sulfur-carbon composite may be preferably used as the cathode active material.
  • a positive electrode prepared by applying the positive electrode slurry composition of the present invention onto a current collector.
  • the current collector those known in the art may be used, and the method of manufacturing the positive electrode may be performed according to a known method.
  • the positive electrode of the present invention provides a very good effect on the energy density of the electrode.
  • the positive electrode of the present invention is the positive electrode of the present invention.
  • a negative electrode comprising lithium metal or a lithium alloy as a negative electrode active material
  • a separator provided between the anode and the cathode
  • the battery may be a lithium-sulfur battery.
  • the above-described contents can be directly applied.
  • a negative electrode known in the art as a negative electrode containing lithium metal or a lithium alloy as the negative electrode active material can be used without limitation.
  • lithium and an alloy of a metal selected from the group consisting of Na, K, Rb, Cs, Fr, Be, Mg, Ca, Sr, Ba, Ra, Al and Sn may be used as the negative electrode active material.
  • the separator positioned between the positive and negative electrodes separates or insulates the positive and negative electrodes from each other and enables lithium ion transport between the positive and negative electrodes.
  • the separator may be made of a porous nonconductive or insulating material, but is not limited thereto, Separators known in the art can be used.
  • the separator may be an independent member such as a film, or may be a coating layer added to the anode and / or the cathode.
  • the material of the separator includes, for example, a polyolefin such as polyethylene and polypropylene, a glass fiber filter paper, and a ceramic material, but is not limited thereto.
  • the thickness of the separator is about 5 ⁇ to about 50 ⁇ , Lt; / RTI >
  • electrolyte those known in the art may be used, and for example, an electrolyte including a lithium salt and an organic solvent may be used.
  • the electrolyte may be impregnated into a negative electrode, a positive electrode and a separator.
  • the organic solvent contained in the electrolyte for example, a single solvent or a mixed organic solvent of two or more may be used.
  • at least one solvent may be selected from two or more of the weak polar solvent group, the strong polar solvent group, and the lithium metal protective solvent group.
  • said weak polar solvent is defined as a solvent having a dielectric constant of less than 15 that is capable of dissolving a sulfur element in an aryl compound, bicyclic ether, or acyclic carbonate, said strong polar solvent being selected from the group consisting of bicyclic carbonates, sulfoxide compounds,
  • a lithium metal protective solvent is defined as a solvent having a dielectric constant higher than 15 that is capable of dissolving lithium polysulfide in a compound, a ketone compound, an ester compound, a sulfate compound, or a sulfite compound, and the lithium metal protective solvent is a saturated ether compound, an unsaturated ether compound, , A cyclic compound having a cyclic efficiency of not less than 50% to form a stable SEI (Solid Electrolyte Interface) on a lithium metal such as a heterocyclic compound containing O, S, or a combination thereof.
  • SEI Solid Electrolyte Interface
  • the weak polar solvent examples include xylene, dimethoxyethane, 2-methyltetrahydrofuran, diethyl carbonate, dimethyl carbonate, toluene, dimethyl ether, diethyl ether, diglyme and tetraglyme.
  • the present invention is not limited thereto.
  • the strong polar solvent include hexamethyl phosphoric triamide,? -Butyrolactone, acetonitrile, ethylene carbonate, propylene carbonate, N-methylpyrrolidone, 3-methyl- But are not limited to, zolyidone, dimethylformamide, sulfolane, dimethylacetamide, dimethylsulfoxide, dimethylsulfate, ethylene glycol diacetate, dimethylsulfite, ethylene glycol sulfite and the like.
  • lithium protecting solvent examples include tetrahydrofuran, ethylene oxide, dioxolane, 3,5-dimethylisoxazole, furan, 2-methylfuran, 1,4-oxane and 4-methyldioxolane. But is not limited thereto.
  • the battery may be constructed by applying techniques known in the art, except for the characteristic features of the present invention described above.
  • Example 1 Preparation of slurry composition for cathode preparation
  • Sulfur (product of sigma-aldrich) and CNT (carbon nanotube) were mixed and heat-treated at 155 ° C to prepare a sulfur-carbon composite.
  • VGCF vapor-grown carbon fiber
  • the binder a solution of 3% aqueous solution of two kinds of polyacrylic acids (sigma Aldrich product having a molecular weight of 450,000 and 1,250,000 5: 2 weight ratio) completely neutralized with lithium hydroxide (Sigma-aldrich product) was used.
  • the above-described sulfur-carbon composite, conductive material, and binder solution were mixed in an aqueous 1-propanol solution to prepare a slurry composition for producing a positive electrode.
  • the ratio of the solid content: solvent (1-propanol and water) in the weight ratio was 23:77, the content of 1-propanol in the slurry was 1: 0.77% by weight
  • Example 2 Preparation of slurry composition for cathode preparation
  • a slurry composition for preparing a cathode was prepared in the same manner as in Example 1, except that the content of 1-propanol in the slurry in Example 1 was 3.85 wt%.
  • Example 3 Preparation of slurry composition for cathode preparation
  • a slurry composition for preparing a positive electrode was prepared in the same manner as in Example 1, except that the content of 1-propanol in the slurry was changed to 7.7% by weight in Example 1.
  • Example 4 Preparation of slurry composition for cathode preparation
  • Example 1 ethanol was used instead of 1-propanol in the slurry, and a slurry composition for preparing a cathode was prepared in the same manner as in Example 1, except that the content of ethanol was 3.85 wt%.
  • Comparative Example 1 Preparation of a slurry composition for preparing an anode
  • a slurry composition for preparing a positive electrode was prepared in the same manner as in Example 1, except that water was used in place of the 1-propanol aqueous solution as the solvent in Example 1.
  • the sulfur-carbon composite material, the conductive material and the binder used in Comparative Example 1 were further mixed with a dispersant (PVA poly vinyl alcohol) so that the ratio was 87: 5: 7: 1 by weight, and the ratio of solid content: water was 25 : ≪ / RTI > 75 by weight.
  • a dispersant PVA poly vinyl alcohol
  • a slurry composition for preparing a cathode was prepared in the same manner as in Example 1, except that the content of 1-propanol in the slurry was changed to 11.55 wt% in Example 1. However, since the solubility of the binder deteriorated, the viscosity of the slurry was increased to such an extent that mixing could not be performed, and the slurry could not be normally produced.
  • the slurry composition for preparing an anode prepared in Example 1 was coated on an aluminum current collector at 11.4 mg / cm 2 to prepare a positive electrode.
  • the slurry composition for preparing an anode prepared in Example 2 was coated on an aluminum current collector at 11.4 mg / cm 2 to prepare a positive electrode.
  • the slurry composition for preparing an anode prepared in Example 3 was coated on an aluminum current collector at 11.4 mg / cm 2 to prepare a positive electrode.
  • the slurry composition for preparing an anode prepared in Example 4 was coated on an aluminum current collector at 11.4 mg / cm 2 to prepare a positive electrode.
  • the slurry composition for preparing an anode prepared in Comparative Example 1 was coated on the aluminum current collector at 11.4 mg / cm 2 to prepare a positive electrode.
  • the slurry composition for preparing an anode prepared in Comparative Example 2 was coated on an aluminum current collector at 11.4 mg / cm 2 to prepare a positive electrode.
  • Example 5 Preparation Anode (prepared as the slurry of Example 1 (using 0.77 wt% of 1-propanol)
  • Example 10 Example 6 Production anode (prepared from slurry of Example 2 (using 3.85 wt% of 1-propanol))
  • Example 11 Example 7 Preparation Anode (prepared from slurry of Example 3 (using 7.7 wt% of 1-propanol))
  • Example 12 Example 8 Production anode (prepared as the slurry of Example 4 (using 3.85 wt% ethanol)) Comparative Example 6
  • COMPARATIVE EXAMPLE 4 Production anode (prepared as a slurry of Comparative Example 1 (only water as a solvent))
  • Comparative Example 7 COMPARATIVE EXAMPLE 5 Production anode (prepared as a slurry of Comparative Example 2 (using water as a solvent + dispersant))
  • Test Example 1 Physical properties and morphological evaluation of an electrode made of a slurry composition for preparing an anode
  • the surface roughness (roughness) of the positive electrode prepared in Examples 5 to 8 and Comparative Examples 4 and 5 was measured and the shape of the electrode after drying was visually confirmed. The results are shown in Table 2 below.
  • the electrode curl after drying of the electrodes of Examples 5 to 8 of the present invention was remarkably improved as compared with the electrode of Comparative Example 4 using only water as a solvent, and showed an improvement equal to or better than Comparative Example 5 using a dispersant.
  • Test Example 2 Evaluation of energy density of a battery
  • the energy density of the batteries prepared in Examples 9 to 12 and Comparative Example 7 was measured by the following method.
  • the energy of the measured cell was divided by the weight of the anode except the current collector, and the energy density was obtained.
  • Example 9 1-propanol 0.77% (Examples 1 and 5) 1416
  • Example 10 1-propanol 3.85% (Examples 2 and 6) 1381
  • Example 11 1-propanol 7.7% (Examples 3 and 7)
  • Example 12 Ethanol 3.85% (Examples 4 and 8)
  • the batteries of Examples 9 to 12 of the present invention exhibited higher energy densities than the batteries of Comparative Example 7 using the dispersing agent, although no separate dispersing agent was used.

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

Abstract

La présente invention concerne : une composition de suspension de cathode comprenant un matériau actif de cathode, un liant, de l'alcool et de l'eau, la teneur en alcool étant de 0,1 à 10 % en poids sur la base du poids total de la composition; une électrode fabriquée à l'aide de cette composition; et une batterie comprenant l'électrode. La composition de suspension pour la fabrication d'une cathode selon la présente invention présente les avantages suivants : la dispersibilité d'un matériau actif de cathode et d'un matériau conducteur est considérablement améliorée; la rugosité de surface d'une électrode est réduite; et la tendance au roulage de l'électrode est considérablement réduite. De plus, la composition de suspension a un avantage économique du fait qu'il n'est pas nécessaire d'utiliser un dispersant ou son utilisation peut être considérablement réduite.
PCT/KR2019/000442 2018-01-11 2019-01-11 Composition de suspension de cathode, cathode fabriquée à l'aide de cette composition et batterie la comprenant WO2019139397A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2020537476A JP7062771B2 (ja) 2018-01-11 2019-01-11 正極スラリー組成物、これを使用して製造された正極及びこれを含む電池
CN201980006826.XA CN111542947A (zh) 2018-01-11 2019-01-11 正极浆料组合物、使用所述正极浆料组合物制造的正极和包含所述正极的电池
US16/958,599 US11777091B2 (en) 2018-01-11 2019-01-11 Cathode slurry composition, cathode manufactured using same, and battery including same
EP19739062.8A EP3723165A4 (fr) 2018-01-11 2019-01-11 Composition de suspension de cathode, cathode fabriquée à l'aide de cette composition et batterie la comprenant

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KR10-2018-0003656 2018-01-11
KR20180003656 2018-01-11
KR10-2019-0003703 2019-01-11
KR1020190003703A KR102160714B1 (ko) 2018-01-11 2019-01-11 양극 슬러리 조성물, 이를 사용하여 제조된 양극 및 이를 포함하는 전지

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Cited By (1)

* Cited by examiner, † Cited by third party
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EP4040526A4 (fr) * 2020-07-01 2023-01-25 LG Energy Solution, Ltd. Électrode positive pour pile au lithium-soufre et son procédé de fabrication

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KR20190003703A (ko) 2016-05-02 2019-01-09 노벨리스 인크. 증강된 성형성을 갖는 알루미늄 합금들 및 관련된 방법들

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KR20180003656A (ko) 2016-06-30 2018-01-10 엘지디스플레이 주식회사 유기발광 다이오드 표시장치

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See also references of EP3723165A4 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4040526A4 (fr) * 2020-07-01 2023-01-25 LG Energy Solution, Ltd. Électrode positive pour pile au lithium-soufre et son procédé de fabrication
JP2023505468A (ja) * 2020-07-01 2023-02-09 エルジー エナジー ソリューション リミテッド リチウム‐硫黄電池用正極及びこの製造方法

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