WO2015046693A1 - Procédé de formation d'une électrode pour une batterie secondaire au lithium - Google Patents

Procédé de formation d'une électrode pour une batterie secondaire au lithium Download PDF

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Publication number
WO2015046693A1
WO2015046693A1 PCT/KR2014/002963 KR2014002963W WO2015046693A1 WO 2015046693 A1 WO2015046693 A1 WO 2015046693A1 KR 2014002963 W KR2014002963 W KR 2014002963W WO 2015046693 A1 WO2015046693 A1 WO 2015046693A1
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Prior art keywords
lithium
silicon oxide
secondary battery
mixture
electrode
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PCT/KR2014/002963
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English (en)
Korean (ko)
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윤우영
염지호
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고려대학교 산학협력단
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Publication of WO2015046693A1 publication Critical patent/WO2015046693A1/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
    • 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
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/139—Processes of manufacture
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/139—Processes of manufacture
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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 method for forming an electrode for a lithium secondary battery, and more particularly, to a method for forming an electrode for a lithium secondary battery constituting a secondary battery capable of charging and discharging.
  • Lithium secondary battery is a type of secondary battery that is charged and discharged by insertion and desorption of lithium ions in the battery. During charging, lithium ions move from cathode to cathode toward anode. It is inserted into the active material of, on the contrary, during discharge, lithium ions inserted into the negative electrode move toward the positive electrode and are inserted into the active material of the positive electrode.
  • Such lithium secondary batteries have high energy density, large electromotive force, and high capacity, and thus are widely used as power sources for mobile phones and laptops.
  • the lithium secondary battery is usually composed of a negative electrode, a positive electrode, a separator and an electrolyte.
  • the negative electrode and the positive electrode include a negative electrode active material and a positive electrode active material capable of inserting and detaching lithium ions as described above.
  • a separator prevents physical cell contact between the positive and negative electrodes. Instead, the movement of ions through the separator is free.
  • the electrolyte serves as a path through which ions can move freely between the anode and the cathode.
  • carbon for constituting the negative electrode may be used.
  • the carbon material is widely used as a negative electrode material of a lithium ion battery due to its small volume change, excellent reversibility, and relatively low price when intercalating / deintercalating lithium.
  • Carbon materials used as such anode materials include graphite, coke, fiber, pitch, and meso carbon.
  • the graphite has a theoretical limit (372 mAh g-1) in charge capacity per unit mass. Therefore, there has been a demand for the development of a new negative electrode material capable of greatly improving operating characteristics such as energy density, reversible capacity, and initial charging efficiency of a lithium ion battery.
  • Silicon has a lot of interest in the field of lithium ion batteries because it has a theoretical capacity per unit mass (approximately 4,200 mAh g-1) that is more than 10 times higher than the charge capacity of graphite electrodes or other various oxide and nitride material electrodes. It is a material.
  • silicon when silicon is applied to an electrode of a lithium ion battery, due to the insertion / desorption of lithium into the silicon electrode, a large volume change of 400% or more occurs in the silicon electrode, and thus the application to the actual anode material has many limitations.
  • silicon oxide SiOx
  • the silicon oxide is in the form of an oxygen group attached to the silicon and when the reaction with lithium, in addition to the main reaction between lithium and silicon, other oxides are generated.
  • These ancillary products show improved performance by acting to mitigate the volume expansion of silicon.
  • lithium ions used in the reaction of ancillary products are not reversible and thus are not used again during charge and discharge, resulting in loss of lithium ions.
  • the capacity may be reduced due to the loss of lithium ions, which may deteriorate the characteristics of the lithium secondary battery.
  • One object of the present invention is to provide a method for forming an electrode for a lithium secondary battery having an improved capacity and lifetime.
  • silicon oxide powder and lithium metal powder are mixed to form a mixture, and then the mixture is heated to a temperature above the melting point of the lithium metal powder. As a result, the liquid lithium metal and silicon oxide powder are reacted to form lithium silicon oxide from the mixture. Thereafter, an active material body is formed using the lithium silicon oxide and the aqueous binder.
  • a process of placing the mixture in the crucible and directly heating the crucible may be performed.
  • a process of placing the mixture in the crucible and heating the crucible in a bath in order to heat the mixture, a process of placing the mixture in the crucible and heating the crucible in a bath.
  • a process of performing a milling process for the mixture may be additionally performed.
  • the milling process may be carried out for 12-24 hours at a speed between 140 and 200 rpm.
  • a mixture of lithium metal powder and silicon oxide powder is heated to react with a liquid lithium powder and silicon oxide powder to form lithium silicon oxide and lithium silicon oxide
  • irreversible reaction does not occur during charge and discharge, only the reversible reaction may occur during movement between the electrodes of lithium ions.
  • the lithium secondary battery may have a stable cycle characteristics.
  • 1 is a voltage-capacity graph showing cycle characteristics during axial discharge of a lithium secondary battery including an electrode made of silicon oxide and an electrode including lithium silicon oxide, respectively.
  • first and second may be used to describe various components, but the components should not be limited by the terms. The terms are used only for the purpose of distinguishing one component from another.
  • the first component may be referred to as the second component, and similarly, the second component may also be referred to as the first component.
  • silicon oxide powder and lithium metal powder are mixed to form a mixture, and then the mixture is heated to a temperature above the melting point of the lithium metal powder. As a result, the liquid lithium metal and silicon oxide powder are reacted to form lithium silicon oxide from the mixture. Thereafter, an active material body is formed using the lithium silicon oxide and the aqueous binder.
  • a silicon oxide powder and a lithium metal powder are mixed to form a mixture.
  • the lithium metal powder may be formed through a droplet emulsion technique (DET) process. That is, the silicone oil is heated to a temperature above the break point of lithium. Thereafter, lithium foil is charged into the silicone oil to melt the lithium. At this time, the impeller pulverizes the molten lithium by the turbulent energy generated by the high speed rotation by using the rotational force of the motor, and at the same time, the lithium metal and the silicone oil are mixed to form an emulsified solvent. Thereafter, the emulsified solvent may be layered using hexane to obtain lithium powder.
  • DET droplet emulsion technique
  • a homogenizer or a stirrer may be used.
  • lithium metal powder generation of by-products due to side reactions may be suppressed as compared with the case where lithium compounds such as lithium chloride and lithium hydroxide are used.
  • the reaction surface area may be increased during the reaction with the silicon oxide, thereby improving reactivity as compared with the bulk lithium metal. That is, the lithium powder and the silicon oxide powder may easily react at a temperature of 190 to 210 ° C. close to the melting point of the lithium.
  • the lithium powder and the silicon oxide powder may be uniformly mixed at a predetermined ratio in the mixing process as compared with the lithium in the bulk state.
  • the liquid lithium metal and silicon oxide react with each other by heating the mixture to a temperature higher than the melting point of the lithium metal powder.
  • the lithium silicon oxide include lithium silicate (Li 4 SiO 4 ).
  • an irreversible reaction may occur during axial discharge of the lithium secondary battery, and thus may be formed on an irreversible material including lithium.
  • the irreversible material is already formed in the lithium secondary battery electrode made of the lithium silicon oxide corresponding to the irreversible material before the axial discharge of the lithium secondary battery. Therefore, when the electrode including the lithium silicon oxide is used in the lithium secondary battery, the irreversible reaction is suppressed during the axial discharge of the lithium secondary battery so that lithium ions are not consumed.
  • the lithium secondary battery to which the electrode including the lithium silicon oxide is applied may have improved cycle characteristics, that is, improved lifespan.
  • the lithium metal powder and silicon oxide powder is charged to the crucible, the crucible is mounted in a vacuum oven or a furnace to directly melt the crucible at the melting point of the lithium metal (180.54 ° C.).
  • the lithium metal powder can be melted and the liquid lithium metal and the silicon oxide powder can be reacted to form lithium silicon oxide.
  • the heating process may, for example, proceed for 24 hours or more.
  • the lithium metal powder and the silicon oxide powder is charged to the crucible, the crucible is mounted in a silicon oil to heat the crucible in a hot water bath to melt the lithium metal powder, and the liquid lithium metal And reacting the silicon oxide powder to form lithium silicon oxide.
  • the silicone oil may be maintained at a temperature sufficient to melt the lithium metal powder at 200 ° C. or higher. The heating process may, for example, proceed for 24 hours or more.
  • a milling process may be additionally performed on the mixture.
  • the mixture is synthesized so that the liquid lithium metal and silicon oxide can react more easily in a subsequent heating process.
  • the milling process can for example proceed at a speed between 140 and 200 rpm.
  • the milling process may be performed for about 12 hours to 24 hours.
  • the milling process can be performed using, for example, a ball mill apparatus or a planetary mill apparatus.
  • an active material body formed of the lithium silicon oxide and the aqueous binder is formed.
  • the lithium silicon oxide, the conductive material and the binder may be adjusted to a weight ratio of 70: 25: 5, for example.
  • An example of the aqueous binder may be sodium carboxymethyl cellulose (CMC).
  • an aqueous binder When forming an active material body using the lithium silicon oxide, it is not necessary to use a non-aqueous binder to solve the stability problem caused by the reaction of the lithium particles with water. Therefore, when the active material body is formed of lithium silicon oxide, an aqueous binder may be applied. In addition, when the aqueous binder is used, the effect of binding the lithium silicon oxide particles in a smaller amount compared to the non-aqueous binder may be excellent. As a result, the ratio of the aqueous binder in the active material body can be reduced, so that the properties of the active material body can be improved.
  • the carbon-based conductive agent is additionally mixed to improve the electrical conductivity of the active material body.
  • Lithium secondary battery includes a positive electrode, a negative electrode and an electrolyte layer.
  • the positive electrode includes a positive electrode active material capable of inserting and detaching lithium ions.
  • the cathode active material may be a lithium-containing transition metal oxide (lithiated cathode) used in a battery reaction such as LiCoO 2 , LiMnO 2 , LiNiO 2 , LiCrO 2 , LiMn 2 O 4 , and the like.
  • the positive electrode active material included in the positive electrode portion is environmentally friendly, does not use rare metals such as cobalt (Co), and instead contains iron having abundant reserves, thus the raw material is very inexpensive and greatly contributes to battery capacity.
  • Lithium iron phosphate Lithium Iron Phosphate, LiFePO 4
  • the cathode is disposed to face the anode.
  • the negative electrode includes a negative electrode active material composed of lithium silicon oxide and an aqueous binder.
  • aqueous binder may be sodium carboxymethyl cellulose (CMC).
  • the lithium secondary battery When applied to a secondary battery including an electrode including the lithium silicon oxide, irreversible reaction of generating lithium silicate during axial discharge may be suppressed. Therefore, when the electrode including the lithium silicon oxide is applied to the lithium secondary battery, the lithium secondary battery may have a stable cycle characteristics.
  • the electrolyte layer is interposed between the positive electrode and the negative electrode.
  • the electrolyte layer includes an electrolyte solution.
  • the electrolyte may be a non-aqueous organic solvent, which may include a lithium salt.
  • a non-aqueous organic solvent cyclic or acyclic carbonate, an aliphatic carboxylic acid ester, etc. can use what is single or 2 or more types are mixed.
  • Silicon oxide powder and lithium metal powder were mixed to form a mixture.
  • the lithium metal powder was formed by a DiT process.
  • a homogenizer was used to form a mixture in which silicon oxide powder and lithium metal powder were uniformly mixed.
  • the crucible was heat-treated at 200 ° C. for 24 hours in a vacuum oven to form lithium silicon oxide.
  • the lithium silicon oxide, the conductive material, and the aqueous binder were formed with an active material body at a mass ratio of 70: 25: 5 to prepare an electrode for a lithium secondary battery.
  • the electrolyte for the lithium secondary battery as a negative electrode a lithium cobalt oxide (LiCoO 2 ) material as a positive electrode, a polypropylene material as a separator, an electrolyte solution containing 1 mol of LiPF 6 and EC and DEC in a ratio of 1: 1 A coin cell was produced.
  • the coin cell was charged and discharged once between 0 and 1.5 V at a constant current of 0.1 C.
  • 1 is a voltage-capacity graph showing cycle characteristics during axial discharge of a lithium secondary battery including an electrode made of silicon oxide and an electrode including lithium silicon oxide, respectively.
  • the capacity reduction rate of the initial charge amount and the discharge amount is 40.3%, but the lithium secondary battery employing an electrode including lithium silicon oxide in reaction with lithium powder has a capacity of about 12%. A decrease can be seen. That is, it can be seen that the initial efficiency of the lithium secondary battery having the electrode including the lithium silicon oxide has 88%.
  • lithium reversible and irreversible reaction of lithium inserted during charging of the battery occur together, and lithium ions involved in the 40.3% capacity corresponding to the irreversible reaction no longer affect the charge and discharge of the battery.
  • lithium secondary battery including an electrode made of lithium silicon oxide in which an irreversible material is formed prior to charging and discharging, lithium ions inserted during charging do not participate in the irreversible reaction, thereby suppressing generation of the irreversible material. You can see that.
  • the method of manufacturing an electrode for a lithium secondary battery according to embodiments of the present invention may be applied to form an electrode of a lithium secondary battery.

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

Abstract

Dans un procédé de formation d'une électrode pour une batterie secondaire au lithium, une poudre d'oxyde de silicium et une poudre de métal de lithium sont mélangées pour former un mélange, et ensuite le mélange est chauffé à une température égale ou supérieure au point de fusion de la poudre de métal de lithium afin que le métal de lithium liquide réagisse avec la poudre d'oxyde de silicium et afin de former un oxyde de silicium lithium à partir du mélange. Ensuite, l'oxyde de silicium lithium et un liant à base d'eau sont utilisés pour former un corps de matériau actif.
PCT/KR2014/002963 2013-09-30 2014-04-07 Procédé de formation d'une électrode pour une batterie secondaire au lithium WO2015046693A1 (fr)

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KR10-2013-0116504 2013-09-30
KR1020130116504A KR101527286B1 (ko) 2013-09-30 2013-09-30 리튬 이차 전지용 음극의 형성 방법

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN112751004A (zh) * 2021-01-04 2021-05-04 澳门大学 LixSi复合材料及其制备方法和锂离子电池负极材料
CN114672713A (zh) * 2022-04-21 2022-06-28 胜华新能源科技(东营)有限公司 含锂金属硅的制备方法、含锂金属硅、含锂SiO及其应用

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CN111370693B (zh) * 2020-03-24 2022-12-27 洛阳联创锂能科技有限公司 一种高首次效率硅氧锂负极材料的制备方法
KR102557600B1 (ko) * 2022-04-21 2023-07-20 싱화 엠페렉스 테크놀로지 (동잉) 씨오., 엘티디. 리튬 함유 금속 실리콘의 제조 방법, 리튬 함유 금속 실리콘, 리튬 함유 SiO 및 그 응용

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WO2012176039A1 (fr) * 2011-06-24 2012-12-27 Toyota Jidosha Kabushiki Kaisha Matériau actif d'électrode négative et procédé de production d'un matériau actif d'électrode négative

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112751004A (zh) * 2021-01-04 2021-05-04 澳门大学 LixSi复合材料及其制备方法和锂离子电池负极材料
CN112751004B (zh) * 2021-01-04 2024-05-07 澳门大学 LixSi复合材料及其制备方法和锂离子电池负极材料
CN114672713A (zh) * 2022-04-21 2022-06-28 胜华新能源科技(东营)有限公司 含锂金属硅的制备方法、含锂金属硅、含锂SiO及其应用
CN114672713B (zh) * 2022-04-21 2022-09-16 胜华新能源科技(东营)有限公司 含锂金属硅的制备方法、含锂金属硅、含锂SiO及其应用
WO2023201767A1 (fr) * 2022-04-21 2023-10-26 胜华新能源科技(东营)有限公司 Procédé de préparation d'un métal au silicium contenant du lithium, métal au silicium contenant du lithium, sio contenant du lithium et son utilisation

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KR101527286B1 (ko) 2015-06-09

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