WO2019078563A1 - Casette pour cuire un matériau actif d'électrode positive de batterie secondaire au lithium et son procédé de fabrication - Google Patents

Casette pour cuire un matériau actif d'électrode positive de batterie secondaire au lithium et son procédé de fabrication Download PDF

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Publication number
WO2019078563A1
WO2019078563A1 PCT/KR2018/012137 KR2018012137W WO2019078563A1 WO 2019078563 A1 WO2019078563 A1 WO 2019078563A1 KR 2018012137 W KR2018012137 W KR 2018012137W WO 2019078563 A1 WO2019078563 A1 WO 2019078563A1
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WIPO (PCT)
Prior art keywords
mgo
powder
sagger
present
average particle
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PCT/KR2018/012137
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English (en)
Korean (ko)
Inventor
유지훈
박정식
성대용
최원석
황지훈
김용석
최요한
Original Assignee
엘지전자 주식회사
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Priority to KR1020207004761A priority Critical patent/KR102652593B1/ko
Priority to CN201880067482.9A priority patent/CN111225889A/zh
Publication of WO2019078563A1 publication Critical patent/WO2019078563A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C04B35/053—Fine ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron

Definitions

  • the present invention relates to the improvement of the lifetime of a fireproof container for firing a cathode active material of a lithium secondary battery using a material which has low reactivity with lithium and has high strength and thermal shock resistance compared to existing commercial fireplaces.
  • the cathode active material used for the lithium secondary battery is composed of Li, Co, Mn, Ni, etc., and the raw material is buried in a fireproof container and fired at 400 to 1000 ° C. At this time, the Li and Co compounds are melted and penetrate into the pores of the inner wall and react with the constituents to cause cracking and peeling. The quality of the cathode material is deteriorated by the reactant in the peeled inner shell, and when the inner shell is broken due to cracking, the cathode material may deteriorate in performance when it is introduced into a subsequent process.
  • An object of the present invention is to improve the service life of a firebox, which is a plastic container of a lithium ion battery cathode active material.
  • the present invention provides a lithium secondary battery for cathode active material, which comprises 70 to 99.5 at.% Of MgO and 0.5 to 30 at.% Of Al2O3, and has a porosity of 10% I will provide my wallet.
  • the strength of the inner shell may be greater than or equal to 600 MPa.
  • the present invention includes a step of mixing a MgO powder and an Al 2 O 3 powder to prepare a mixed powder, molding the mixed powder into a predetermined shape to produce a molded body, and sintering the molded body at a temperature of 1550 to 1700 ° C And the mixed powder is composed of 70 to 99.5 at.% Of MgO and 0.5 to 30 at.% Of Al2O3.
  • the present invention also provides a method of manufacturing an inner shell for firing a lithium secondary battery cathode active material.
  • the MgO powder may be a mixture of two kinds of powders having different average particle diameters.
  • the average particle diameter of any one of the two kinds of powders may be 27 to 33 mu m and the average particle diameter of the other one may be 3 to 8 mu m.
  • the Al2O3 powder may have an average particle diameter of 0.5 to 10 mu m.
  • the average particle size of the MgO powder and the average particle size of the Al2O3 powder may be the same.
  • the MgO may be dead burnt MgO or molten MgO.
  • the strength and the thermal shock resistance of the existing firefly are increased, and the reactivity with lithium is lowered, so that the firefly is not damaged even after the firing is repeated 100 times or more.
  • the inner wall according to the present invention has a durability 3 times higher than that of the conventional inner wall.
  • FIG. 1 is a conceptual diagram showing a sintering process of a lithium ion battery cathode active material.
  • Figs. 2A and 2B are photographs of samples used for evaluating the performance of the fireproof glove according to the present invention.
  • Figs. 3A to 3C are SEM photographs of an inner fire wall according to the present invention.
  • FIG. 4 is a photograph of a conventional inner fire coat after being repeatedly fired 30 times.
  • FIG. 5 is a photograph of the inner fire coat according to the present invention taken after firing 100 times.
  • the lithium secondary battery cathode active material is composed of a mixture of Li and at least one of Co, Ni, Mn, and Fe.
  • the mixture is calcined in an inner shell to prepare a cathode active material of a lithium secondary battery.
  • the composition of the inner shell was composed of a mixture of Al 2 O 3 (main component), SiO 2 , and MgO.
  • the inner fire coat is peeled off at about 30 times of firing and can not be reused anymore.
  • the present invention provides an inner shell composed of 70 to 99.5 at.% MgO and 0.5 to 30 at.% Al 2 O 3 .
  • MgO is a major constituent of the fire coat according to the present invention. Since MgO has a very low reactivity with Li, it is possible to prevent the firefly and lithium from reacting during repeated firing.
  • the MgO contained in the inner protective layer according to the present invention is 70 to 99.5 at.%.
  • the other components of the inner furnace are made of Al 2 O 3 .
  • Al 2 O 3 serves to facilitate the porosity control by lowering the sintering temperature for the manufacture of fireproofing. Specifically, Al 2 O 3 is added in an amount of 0.5 to 30 at.%. When the content of Al 2 O 3 is less than 0.5 at.%, The effect of lowering the sintering temperature is insufficient. When the content of Al 2 O 3 is more than 30 at.%, The reactivity with Li is increased and the lifetime of the inner shell decreases.
  • MgO and Al 2 O 3 of at.% Being based on the total of the number of MgO and Al 2 O 3 by mole.
  • Additives such as binders can be added in the manufacture of fireproofs, but they are not included in the finished fireproofing because they are all removed during the sintering process.
  • SiC, cordierite, mullite and the like may be further added to control the sintering temperature and increase the thermal expansion coefficient and strength.
  • SiC, cordierite, mullite and the like may be further added to control the sintering temperature and increase the thermal expansion coefficient and strength.
  • the additives are not essential.
  • the MgO powder dispersion prepared by the atmospheric oxidation method can be applied to the surface of the inner shell to be dense.
  • the coating layer formed in this manner is not essential.
  • the sintering temperature for producing an inner protective layer is 1550 to 1700 ° C. It is easy to control the porosity at the sintering temperature.
  • the porosity of the inner shell according to the present invention is preferably 10% or less.
  • the porosity of the inner shell In order to allow the cathode active material to be fired more than 100 times, the porosity of the inner shell must be 10% or less.
  • the average size of the pores is preferably 10 ⁇ or less.
  • MgO powder and Al 2 O 3 powder are mixed to prepare a mixed powder.
  • the MgO powder may be a mixture of two powders having different average particle diameters.
  • the two types of powders may be mixed in a ratio of 7: 3, 5: 5, or 3: 7.
  • the average particle diameter of any one of the two kinds of powders may be 27 to 33 mu m and the average particle diameter of the other one may be 3 to 8 mu m. Accordingly, the present invention reduces the porosity of the inner shell.
  • the present invention is not limited thereto, and the MgO powder may be composed of one kind of powder.
  • the average particle diameter of the MgO powder may be 2 to 4 ⁇ ⁇ .
  • the average particle diameter of the Al 2 O 3 powder may be 0.5 to 10 ⁇ m.
  • the mean particle size of Al 2 O 3 powder exceeds 10 ⁇ m, there is a problem that the increase in porosity of the hwagap.
  • the average particle diameter of the MgO powder and the average particle diameter of the Al 2 O 3 powder may be equal to each other.
  • the mixed powder of MgO and Al 2 O 3 is made of a mixture of the said MgO and Al 2 O 3 as a sludge state can be produced in such a way as to evaporate water.
  • Moisture can react with MgO in the sludge state, which can adversely affect the hardness of the fire wall.
  • the MgO may be Dead Burnt MgO or fused MgO.
  • An additive such as a binder may be added during the production of the molded article.
  • the additive to be added in the production of the molded article is a well-known technology, and a detailed description thereof will be omitted. Since the additive is an organic material, it is all removed during the sintering of the fireproof glove, and is no longer left in the finished fireproof glove.
  • the components of the inner shell used in the performance comparison experiment (hereinafter, comparative example) consisted of 70 at.% Al 2 O 3 , 19 at.% SiO 2 , 10 at.% MgO and other components.
  • the specimen includes a circular specimen having a predetermined thickness (FIG. 2A) and a rectangular parallelepiped specimen having an internal space (FIG. 2B).
  • the rectangular parallelepiped-shaped specimen has a shape similar to that of an actual inner shell.
  • a circular specimen is referred to as a coin sample
  • a rectangular parallelepiped specimen is referred to as Lab. It is called a scale sample.
  • composition of the specimen used in the performance evaluation described below is shown in Table 1 below.
  • the inner shell according to the present invention has much higher strength than the conventional shell shell, the possibility of breakage during firing of the cathode active material is lowered.
  • a cathode material containing lithium was placed on each sample, and then the temperature was raised to 800 ° C at a rate of 10 ° C / min and maintained at 800 ° C for one hour. Thereafter, it was cooled by an air cooling method for 30 minutes or more.
  • the lifetime evaluation was performed under pressure conditions taking into consideration the actual weight of the cathode material. After repeated evaluation of the lifetime described above, changes in the sample were observed. Observation results are shown in Table 4 below.
  • the inner shell has a porosity of at least 10% .
  • the strength and the thermal shock resistance of the existing firefly are increased, and the reactivity with lithium is lowered, so that the firefly is not damaged even after the firing is repeated 100 times or more.
  • the inner wall according to the present invention has a durability 3 times higher than that of the conventional inner wall.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

La présente invention concerne une casette pour cuire un matériau actif d'électrode positive de batterie secondaire au lithium, la casette comprenant de 70 à 99,5 % atomique de MgO et de 0,5 à 30 % atomique d'Al2O3 et a une porosité de 10 % ou moins. Selon la présente invention, la casette présente une meilleure résistance et une résistance aux chocs thermiques accrue par rapport à une casette classique et a une réactivité réduite avec le lithium, et par conséquent ne se casse pas même après avoir été cuite une centaine de fois ou plus de manière répétée. Compte tenu du fait qu'une casette classique est cassée après avoir été cuite environ 30 fois, la casette selon la présente invention présente une durabilité au moins 3 fois supérieure à celle de la casette classique.
PCT/KR2018/012137 2017-10-17 2018-10-15 Casette pour cuire un matériau actif d'électrode positive de batterie secondaire au lithium et son procédé de fabrication WO2019078563A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020207004761A KR102652593B1 (ko) 2017-10-17 2018-10-15 리튬이차전지 양극활물질 소성용 내화갑 및 그 제조 방법
CN201880067482.9A CN111225889A (zh) 2017-10-17 2018-10-15 锂二次电池正极活性物质烧成用匣钵及其制造方法

Applications Claiming Priority (2)

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US201762573668P 2017-10-17 2017-10-17
US62/573,668 2017-10-17

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CN112430082A (zh) * 2020-12-15 2021-03-02 湖南仁海科技材料发展有限公司 一种氧化锌匣钵及其制备方法
CN112811886A (zh) * 2021-01-16 2021-05-18 陕西科技大学 一种电池匣钵及其制备方法
CN114031407A (zh) * 2021-12-13 2022-02-11 湖南太子新材料科技有限公司 一种用于锂电池正极材料的碳化硅匣钵及其制备方法

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CN113603469B (zh) * 2021-08-04 2022-12-16 江苏晶邦新型材料有限公司 一种复合尖晶石莫来石陶瓷耐火材料及其制备方法
KR20230168569A (ko) 2022-06-07 2023-12-14 주식회사 에코프로비엠 전구 물질 소성용 내화갑

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CN112811886A (zh) * 2021-01-16 2021-05-18 陕西科技大学 一种电池匣钵及其制备方法
CN114031407A (zh) * 2021-12-13 2022-02-11 湖南太子新材料科技有限公司 一种用于锂电池正极材料的碳化硅匣钵及其制备方法

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KR102652593B1 (ko) 2024-04-01
CN111225889A (zh) 2020-06-02
KR20200058383A (ko) 2020-05-27

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