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WO2018151566A2 - Matériau actif d'électrode positive pour batterie secondaire au lithium - Google Patents

Matériau actif d'électrode positive pour batterie secondaire au lithium Download PDF

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Publication number
WO2018151566A2
WO2018151566A2 PCT/KR2018/002018 KR2018002018W WO2018151566A2 WO 2018151566 A2 WO2018151566 A2 WO 2018151566A2 KR 2018002018 W KR2018002018 W KR 2018002018W WO 2018151566 A2 WO2018151566 A2 WO 2018151566A2
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WIPO (PCT)
Prior art keywords
active material
positive electrode
electrode active
surface portion
secondary battery
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Ceased
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PCT/KR2018/002018
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English (en)
Korean (ko)
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WO2018151566A3 (fr
Inventor
조성우
최창민
오지우
정희원
최수안
전상훈
안지선
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L&F Co Ltd
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L&F Co Ltd
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Publication of WO2018151566A2 publication Critical patent/WO2018151566A2/fr
Publication of WO2018151566A3 publication Critical patent/WO2018151566A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • H01M4/366—Composites as layered products
    • 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
    • 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
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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

  • It relates to a positive electrode active material for a lithium secondary battery.
  • a battery generates electric power by using an electrochemical reaction material for the positive electrode and the negative electrode.
  • Representative examples of such a battery include a lithium secondary battery that generates electrical energy by a change in a chemical potential (chemi ca l potent i al) when lithium silver is intercalated / deintercalated at a positive electrode and a negative electrode.
  • the lithium secondary battery is manufactured by using a material capable of reversible intercalation / deintercalation of lithium ions as a positive electrode and a negative electrode active material, and filling an organic electrolyte or a polymer electrolyte between the positive electrode and the negative electrode.
  • a lithium composite metal compound is used as a cathode active material of a lithium secondary battery, and composite metal oxides such as LiCo0 2 , LiMn 2 0 4 , LiNi0 2 , and LiMn0 2 have been studied.
  • Mn-based positive electrode active materials such as the positive electrode active material LiMn 2 0 4 , LiMn0 2 is easy to synthesize, relatively inexpensive, has the best thermal stability compared to other active materials when overcharged, and has a low environmental pollution attractive material Although it has a disadvantage, the capacity is small.
  • LiCo0 2 has good electrical conductivity and high cell voltage of about 3.7V. Stability and discharge capacity are also excellent. It is a representative cathode active material that is currently commercialized and commercially available. However, since LiCo0 2 is expensive, it takes up more than 30% of the battery price, which leads to a problem of low price competitiveness. In addition, LiNi0 2 exhibits the highest discharge capacity of battery characteristics among the cathode active materials mentioned above, but has a disadvantage in that it is difficult to synthesize. In addition, the high oxidation state of nickel causes a decrease in battery and electrode life, and there is a problem of severe self discharge and inferior reversibility. In addition, it is having difficulty in commercialization due to incomplete stability.
  • Such nickel-based positive electrode active material is now replacing the various core metal products are coming out.
  • the surface of the particles serving as cores has been remodeled in various forms in order to generate a positive electrode active material, improve lifetime, and improve rate characteristics.
  • the application of the metal element is basically a trade-off form in which the initial capacity is necessarily accompanied with a decrease in initial capacity.
  • the cathode material particles have various compositions and sizes depending on the application. It can be changed in morphology, which has not yet been derived in terms of optimized surface treatments.
  • the metal that may be included in the metal oxide layer surface-treated in the positive electrode active material for a real secondary battery is Mg, Al, Co, K, Na, Ca, Si, Ti, It suggests the formation technology of two or more multi-layers containing different metals selected from the group consisting of Sn, V, Ge, Ga, B, As and Zr, but only mentions the difference in the presence or absence of surface treatment. , Composition or morphology . If there is a change, it is not known what change should be made also in the aspect of surface treatment.
  • a lithium composite oxide core In one embodiment of the present invention, a lithium composite oxide core; And. A surface portion located on the surface of the core portion, wherein the surface portion includes an A1 element and an M element, and M represents Mg, Ti, Ca, W, B, Ba. Zr, or a combination thereof, and the surface portion of the element provides a cathode active material for a rechargeable lithium battery that satisfies the following formula (1).
  • Y is the total amount of A1 and M in the surface portion
  • X is the BET specific surface area value of the positive electrode active material
  • C is the minimum value of the total amount of Al, B, and M in the surface portion
  • A is for the X and Y Slope
  • a and C may satisfy a range of 1.5 ⁇ A / C ⁇ 3.
  • the element of the surface portion may satisfy the content of Equation 2 below.
  • Y is the amount of A1 in the surface portion
  • X is the BET specific surface area value of the positive electrode active material
  • C is the minimum value of ' A ⁇ in the surface portion
  • A is the slope with respect to the X' and Y '
  • the element of the surface portion may satisfy the content of Equation 3 below.
  • Y ′′ is the amount of M in the surface portion
  • X is the BET specific surface area value of the positive electrode active material
  • C ′′ is the minimum value of M in the surface portion
  • a ′′ is the slope for the X ′′ and Y ′ ,
  • X may be 0 m 2 / g ⁇ X ⁇ 4 m 2 / g.
  • the lithium composite oxide core may include Ni, Co, and Mn.
  • the lithium composite oxide core may include a dopant which is Zr, Ti, Al, Mg, V, Zn, Mo, V, Cr, Fe, Sr, or a combination thereof.
  • the core including the core particles within the through-pores, hollow, solid, or son combinations, and wherein the surface portion of the through hole of the core, the pore, hollow, solid, or a combination thereof: be present both on the surface Can be.
  • the total content of A1 and M in the surface portion may be 1000 ppm to 2500 ppm.
  • the content of A1 and M in the surface portion may satisfy the ratio L5 ⁇ A1 / M ⁇ 4.
  • the BET specific surface area of the cathode active material may satisfy 0.1 to 1.2 niVg.
  • the element M includes B (boron) and B, and additionally Mg, Ti, Ca, W, Ba, Zr. Or a combination thereof. .
  • 1 is a trend line graph of content data according to an embodiment of the present invention.
  • a lithium composite oxide core In one embodiment of the present invention, a lithium composite oxide core; And a surface portion located on the surface of the core portion, wherein the surface portion includes A1 and B, and may further include element M, which is Mg, Ti, Ca, W, B, Ba, Zr, or a combination thereof. And, the element of the surface portion provides a positive electrode active material for a lithium secondary battery that satisfies the content of the following formula (1).
  • Y is the total amount of A 1 and B and the element M in the surface portion,.
  • X is a BET specific surface area value of the positive electrode active material
  • C is the minimum value of the total amount of A1, B and M in the surface portion
  • A is a creeper.
  • the A is the slope, that is, the rate of change of the Y value when the X value changes, and since the Y value is a positive integer, when the A value is large, the Y value also increases. Report the BET value as X. When the total content of the surface treatment element is viewed as Y, it can be seen that Y increases according to A.
  • the BET value of the cathode material may be obtained by multiplying A according to Equation (1) and adding the minimum value C.
  • C can be 600 ⁇ C ⁇ 1000.
  • the minimum value is preferably in the range of 1.5 ⁇ A / C ⁇ 3 in relation to the slope, which is another increase in the surface treatment content.
  • 600 ⁇ C ⁇ 1000 is preferred.
  • the positive electrode active material according to the embodiment of the present invention may appropriately adjust the content of the surface treatment element of the surface portion according to the ratio of the BET specific surface area, thereby providing a positive electrode active material having improved cycle characteristics.
  • the specific surface area by BET in the active material is directly related to the area where Li ions are redoxed through the electrolyte, and ultimately, it is an index used to improve energy density.
  • BETs vary in the level of application depending on the use of the active material, which is usually controlled by the size and shape of the particles.
  • the construction of surface treatment conditions that can be considered for the adjustment of BET can be said to be appropriate for the change in the use of the cathode material.
  • the reaction area with the electrolyte increases, so the surface treatment area for suppressing side reactions must also increase. At this time, the surface treatment content should be applied differently depending on the treatment elements.
  • the surface treatment consists of a multi-element application comprising A1 and B as elements and optionally including one or more elements selected from Mg, Ti, Ca, W, B, Ba, Zr.
  • A1 may form an oxide form or diffuse into the bulk of the mother particles by combining with surrounding oxygen at the surface treatment reaction temperature.
  • the A 1 -containing oxide insulator may be formed on the surface portion of the mother particles, or may exist in a concentration gradient in the inner direction from the surface portion. At this time, it may serve as a dopant substituted for the transition metal in the bulk of the matrix or may be located between grain boundaries.
  • B may react with the surrounding L i to form an ion conductor or form an oxide.
  • a 1 to form a non-conductor serves to reduce the surrounding electron conductivity serves to suppress the reaction with the electrolyte.
  • the surface treatment content of A 1 and B may vary depending on the BET.
  • BET increases The total amount of surface treatment increases with the increase of A1.
  • the content increases with BET, but the degree of increase is not greater than the increase rate of A1. This is because the sensitivity of the decrease in discharge capacity is greater than that of A1 in the Examples and Comparative Examples.
  • the element of M may further include one or more elements selected from Mg, Ti, Ca, W, Ba, Zr. They may vary in form depending on the firing temperature during surface treatment, but basically form oxides. They can be used differently depending on the application. For example, Mg. In the case of Ca, it is substituted with Li in the surface filling of the mother particles to prevent cationic mixing (Cat i on Mi x) due to N i divalent, or in the case of W and Ba, it may be used in connection with particle strength.
  • Ti and Zr mainly recognize the function as an insulator, and the inventors recognize.
  • the element of the surface portion may satisfy the content of Equation 2 below.
  • X is a BET specific surface area value of the positive electrode active material
  • A is the degree of change of A 'content as the BET changes.
  • a 'and C' are 1400 ⁇ A ' ⁇ 1650, respectively. 300 ⁇ C ⁇ 500.
  • the element of the surface portion may satisfy the content of Equation 3 below.
  • Y ' is the amount of ⁇ in the surface portion
  • X is a BET specific surface area value of the positive electrode active material
  • a ′′ is the slope with respect to X ′′ and Y ′′.
  • a ', and C may be 100 ⁇ A" ⁇ 150, 300 ⁇ C " ⁇ 500, respectively.
  • X may be 0 m 2 / g ⁇ X ⁇ 4 m 2 / g. This refers to the commercialized BET range and can be selected according to the characteristics of the desired positive electrode active material.
  • the lithium composite oxide core is Ni. Co, and Mn.
  • the lithium composite oxide core is Zr, Ti, Al, Mg, V, Zn, Mo. V. Cr, Fe, Sr, or combinations thereof. Dopant for the improvement of the structural characteristics of the positive electrode active material. Appropriately applicable.
  • the core is. Through-holes, pores, hollows in the core particles. Solid, or a combination thereof, and the surface portion may all be present on the surface of the through-hole, pores, hollows, solids, or a combination thereof of the core.
  • the core may be a one body of a single primary particle form.
  • the total content of A1 and B in the surface portion may be 1000 ppm to 5000 ppm. This range may be adjusted according to the correlations of Equations 1 to 3, but the present invention is not limited to the above ranges.
  • A1 and M eg, B
  • 1.5 ⁇ A1 / M ⁇ 4 weight ratio can be satisfied.
  • the BET specific surface area of the cathode active material may satisfy 0.1 to 2.0 mVg.
  • nickel cobalt manganese hydroxide powder, Zr0 2 powder, and Ti0 2 powder were dry mixed.
  • the molar ratio of nickel: cobalt: manganese and nickel cobalt manganese hydroxide: Zr: Ti in the nickel cobalt manganese hydroxide was satisfied to satisfy the conditions of the active materials shown in Tables 1 to 4 above.
  • the dry mixture was calcined so that the Zr0 2 powder and the Ti0 2 powder were uniformly attached to the particle surface of the composite transition metal hydroxide.
  • the core obtained by the above process, A1 (0H) 3 powder, and 3 ⁇ 40 3 powder were dry mixed.
  • the mixed weight ratio at this time satisfied each active material condition of Tables 1-4.
  • a positive electrode slurry was prepared by adding to 5.0 wt%.
  • the positive electrode slurry was applied to a thin film of aluminum (A1), which is a positive electrode current collector having a thickness of 20 to 40 / zm, vacuum dried, and roll pressed to prepare a positive electrode.
  • Li-metal was used as the negative electrode.
  • a half cell of a coin cell type was prepared using Li PF6EC: DMC (l: lvol%).
  • Example 6 205.51 80.98% Comparative Example 1-1 167.88 87.38%
  • Comparative Example 2 has a smaller A 1 group compared to the Example, the initial capacity is similar to the Example, but as the BET proceeds higher it can be seen that the cycle characteristics do not reach the level of the Example. This means that the cycle characteristics may also increase if the A 1 content increases with the increase of BET.
  • Comparative Example 3 is to increase the group of A 1 than the embodiment level to ensure the cycle characteristics can be expected, but the higher the BET it can be seen that the reduction of the discharge capacity is remarkable. .

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

Abstract

La présente invention concerne un matériau actif d'électrode positive pour une batterie secondaire au lithium, et fournit un matériau actif d'électrode positive pour une batterie secondaire au lithium, le matériau actif d'électrode positive comprenant : un noyau d'oxyde composite de lithium ; et une partie surface située sur une surface de la partie noyau, la partie surface contenant un élément Al et un élément M ; M représentant Mg, Ti, Ca, W, B, Ba, Zr ou une combinaison de ceux-ci ; et les éléments de la partie surface satisfaisant au contenu de l'équation 1 ci-dessous : [Équation 1] Y = AX + C. Dans l'équation 1, Y est la quantité totale d'Al et de M dans la partie surface ; X est une valeur de la surface spécifique BET du matériau actif d'électrode positive ; C est la valeur minimale de la quantité totale d'Al, de B et de M dans la partie surface ; A est la pente pour X et Y ; 1500 < A < 1800 ; et 600 < C < 1000.
PCT/KR2018/002018 2017-02-16 2018-02-19 Matériau actif d'électrode positive pour batterie secondaire au lithium Ceased WO2018151566A2 (fr)

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KR1020170020845A KR20180094567A (ko) 2017-02-16 2017-02-16 리튬 이차 전지용 양극 활물질
KR10-2017-0020845 2017-02-16

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KR102701052B1 (ko) 2018-12-10 2024-09-02 주식회사 엘지에너지솔루션 고-니켈 양극 활물질, 그 제조 방법, 이를 포함하는 양극 및 리튬이차전지
KR102558390B1 (ko) * 2020-10-26 2023-07-24 주식회사 에코프로비엠 양극 활물질 및 이를 포함하는 리튬 이차전지

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KR101785266B1 (ko) * 2013-01-18 2017-11-06 삼성에스디아이 주식회사 복합양극활물질, 이를 채용한 양극 및 리튬전지, 및 그 제조방법
KR101609544B1 (ko) * 2013-03-26 2016-04-06 주식회사 엘 앤 에프 리튬 이차 전지용 양극 활물질 및 이를 이용한 리튬 이차 전지
KR20150100406A (ko) * 2014-02-25 2015-09-02 삼성에스디아이 주식회사 양극 활물질, 그 제조방법, 이를 포함하는 리튬 이차 전지용 양극 및 이를 채용한 리튬 이차 전지
KR101576274B1 (ko) * 2014-05-28 2015-12-09 국립대학법인 울산과학기술대학교 산학협력단 리튬 이차전지용 양극 활물질, 이들의 제조방법, 및 이를 포함하는 리튬 이차전지
KR101747140B1 (ko) * 2014-08-29 2017-06-14 주식회사 엘 앤 에프 리튬 이차 전지용 니켈계 복합 산화물, 및 이를 포함하는 리튬 이차 전지

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KR20180094567A (ko) 2018-08-24

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