WO2015004705A1 - Matériau actif d'électrode positive pour des batteries secondaires au lithium-ion - Google Patents

Matériau actif d'électrode positive pour des batteries secondaires au lithium-ion Download PDF

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Publication number
WO2015004705A1
WO2015004705A1 PCT/JP2013/068591 JP2013068591W WO2015004705A1 WO 2015004705 A1 WO2015004705 A1 WO 2015004705A1 JP 2013068591 W JP2013068591 W JP 2013068591W WO 2015004705 A1 WO2015004705 A1 WO 2015004705A1
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WIPO (PCT)
Prior art keywords
ion secondary
positive electrode
active material
electrode active
lithium ion
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PCT/JP2013/068591
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English (en)
Japanese (ja)
Inventor
小西　宏明
章 軍司
孝亮 馮
翔 古月
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株式会社 日立製作所
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Priority to PCT/JP2013/068591 priority Critical patent/WO2015004705A1/fr
Publication of WO2015004705A1 publication Critical patent/WO2015004705A1/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
    • H01M4/36—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
    • H01M4/485—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
    • H01M4/52—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

  • the present invention relates to a positive electrode active material for a lithium ion secondary battery, a method for producing the same, and a lithium ion secondary battery using the same.
  • the problem with electric vehicles is that the energy density of the driving battery is low and the travel distance for one charge is short. Therefore, there is a demand for an inexpensive secondary battery with high energy density.
  • Lithium ion secondary batteries have a higher energy density per weight than secondary batteries such as nickel hydrogen batteries and lead batteries, but in order to meet the demands of electric vehicles, it is necessary to further increase the energy density. In order to realize high energy density of the battery, it is necessary to increase the energy density of the positive electrode and the negative electrode, and high capacity of the active material is required.
  • Layered solid solution is a positive electrode active material that can be expected to have a high capacity.
  • Patent Document 1 describes a positive electrode material in which a lithium composite oxide having a layered layered rock salt type crystal structure of a hexagonal system and a lithium manganese oxide having a spinel structure belonging to a space group R-3m is mixed.
  • the composition formula Li a M1 b M2 c O d (M1 is Mn, Ni, 2 or more elements including at least Mn of Co, M2 is Al, Ti, Mg, of B, at least one Element, 1.1 ⁇ a ⁇ 1.3, 0.7 ⁇ b + c ⁇ 1.1, 0 ⁇ c ⁇ 0.a> b + c) and at least a portion of the surface of the positive electrode material
  • a covering layer including the third element as a constituent element while covering, the capacity retention rate at the time of cycling is improved.
  • the positive electrode material disclosed in Patent Document 1 can obtain a high capacity, but the irreversible capacity is large because the content of Mn is large. Since the battery needs a negative electrode matched to the charge capacity of the positive electrode, when using a positive electrode active material having a large irreversible capacity, a negative electrode having a capacity corresponding to the first large charge capacity is required. However, since the discharge capacity that can actually be used is smaller than the charge capacity, the unit weight and the capacity per unit volume decrease as the amount of the negative electrode increases. Therefore, an object of the present invention is to provide a layered solid solution positive electrode active material having a small irreversible capacity and a high discharge capacity.
  • ⁇ Positive electrode active material> When using a lithium ion secondary battery for an electric vehicle, it is required that the energy density is high, the travel distance per charge is long, and the life is long. In the lithium ion secondary battery, this characteristic is closely related to the positive electrode active material. In order to improve the energy density of the battery, it is required to increase the capacity of the positive electrode active material.
  • the positive electrode active material for a lithium ion secondary battery according to the present invention is a particle containing Li, Ni, and Mn.
  • the particle has an inner portion and a surface portion, and the surface portion is a range of 1/10 of the particle diameter from the surface of the particle, and the inner portion is a portion other than the surface portion of the particle.
  • FIG. 2 shows the structure of the particle according to the present invention.
  • 11 is the inside
  • 12 is the surface layer.
  • the inside of the particle has the composition formula Li x Ni a Mn b M c O 2 (1 ⁇ x ⁇ 1.2, 0.2 ⁇ a ⁇ 0.4, 0.4 ⁇ b ⁇ 0.6, c ⁇ 0.
  • M is a transition metal element such as Al or Mg).
  • M is an additive or an impurity contained at a composition ratio of 0.02 or less, and does not greatly affect the capacity and irreversible capacity of the positive electrode active material. By satisfying the above composition, high capacity can be achieved in the potential range of 3.0 to 4.6 V.
  • X in the composition formula represents the proportion of Li in Li x Ni a Mn b M c O 2 . If x is less than 1, the amount of Li contributing to the reaction is reduced and a high capacity can not be obtained. On the other hand, when x is larger than 1.2, the crystal lattice becomes unstable and the discharge capacity is reduced.
  • a represents the content ratio (atomic weight ratio) of Ni of the positive electrode active material. If a is smaller than 0.2, the content of Ni, which is mainly responsible for charge and discharge, decreases, so the capacity decreases. On the other hand, when a is larger than 0.4, the valence number of Ni increases, the charge / discharge capacity involving Ni decreases, and a high capacity can not be obtained.
  • the positive electrode active material according to the present invention contains Li, Ni and Mn as transition metals, it does not contain expensive Co.
  • the positive electrode active material in the present embodiment has an advantage of low cost in addition to high energy density.
  • the positive electrode active material according to the present invention is characterized in that the atomic ratio of Li to Ni and Mn (Li / (Ni + Mn)) in the surface layer portion is lower than the internal Li / (Ni + Mn).
  • the irreversible capacity can be reduced because the content ratio of Li to Ni and Mn in the surface layer portion is lower than the content ratio of Li to Ni and Mn inside.
  • the initial charge / discharge curve of the conventional layered solid solution positive electrode active material is shown in FIG.
  • the vertical axis represents voltage
  • the horizontal axis represents capacity
  • 13 is a charge curve
  • 14 is a discharge curve.
  • Li in the surface layer can be lost by surface treatment with an acid.
  • the method of deficient Li in the surface layer is not limited to this, and the Li content in the surface layer may be lower than the internal Li content.
  • the positive electrode active material according to the present invention is characterized in that the surface layer portion contains the additive metal element M ′.
  • the surface layer portion having a smaller content of Li than the inside of the particles is devoid of Li 2 O and becomes active. In the activated part, the decomposition reaction of Li salt which is an electrolyte is likely to occur. Therefore, by covering the active part of the surface layer with the phase containing M ', it is possible to improve the capacity retention rate upon cycling.
  • M ' is a metal element which does not exist in the inside of the particle, and examples thereof include Mg, Fe, Zn, Al, Mo and the like. These may coat the surface layer as an oxide.
  • the content of M ′ is characterized in that it is 1 to 5% by mass ratio to the positive electrode active material. If the content of M 'is less than 1%, there is no effect on the improvement of the capacity retention rate during cycling. On the other hand, when the content is more than 5%, the resistance becomes high, and the content of Li, Ni, and Mn in the positive electrode active material decreases, so the capacity decreases.
  • the positive electrode active material according to the present invention can be produced by a method generally used in the technical field to which the present invention belongs. For example, it can be produced by mixing and firing compounds containing Li, Ni, and Mn in appropriate proportions. The composition of the positive electrode active material can be appropriately adjusted by changing the ratio of the compound to be mixed.
  • Examples of the compound containing Li include lithium acetate, lithium nitrate, lithium carbonate, lithium hydroxide, lithium oxide and the like.
  • Examples of the compound containing Ni include nickel acetate, nickel nitrate, nickel carbonate, nickel sulfate, nickel hydroxide and the like.
  • As a compound containing Mn, manganese acetate, manganese nitrate, manganese carbonate, manganese sulfate, manganese oxide etc. can be mentioned, for example.
  • composition of the positive electrode material can be determined by, for example, elemental analysis by inductively coupled plasma (ICP) or the like, and elemental analysis from the surface to the inside by Auger analysis.
  • ICP inductively coupled plasma
  • the lithium ion secondary battery according to the present invention is characterized by containing the above-mentioned positive electrode active material.
  • a lithium ion secondary battery with high energy density can be obtained. Since the battery requires an amount of the negative electrode matched to the charge capacity of the positive electrode, when using a positive electrode active material having a large irreversible capacity, a negative electrode having a capacity corresponding to the first large charge capacity is required. However, since the discharge capacity that can actually be used is smaller than the charge capacity, the larger amount of the negative electrode results in wasting the negative electrode.
  • the lithium ion secondary battery according to the present invention can be preferably used, for example, for an electric vehicle.
  • the lithium ion secondary battery is composed of a positive electrode containing a positive electrode active material, a negative electrode containing a negative electrode active material, a separator, an electrolytic solution, an electrolyte and the like.
  • the negative electrode active material is not particularly limited as long as it can absorb and release lithium ions.
  • Materials generally used in lithium ion secondary batteries can be used as the negative electrode material.
  • graphite, lithium alloy and the like can be exemplified.
  • a separator those generally used in lithium ion secondary batteries can be used.
  • a microporous film or non-woven fabric made of polyolefin such as polypropylene, polyethylene, and a copolymer of propylene and ethylene can be exemplified.
  • the electrolytic solution and the electrolyte those generally used in lithium ion secondary batteries can be used.
  • the electrolytic solution diethyl carbonate, dimethyl carbonate, ethylene carbonate, propylene carbonate, vinylene carbonate, methyl acetate, ethyl methyl carbonate, methyl propyl carbonate, dimethoxyethane and the like can be exemplified.
  • the electrolyte LiClO 4, LiPF 6, LiBF 4, LiAsF 6, LiSbF 6, LiCF 3 SO 3, LiC 4 F 9 SO 3, LiCF 3 CO 2, Li 2 C 2 F 4 (SO 3) 2, LiN (CF 3 SO 2) 2, LiC (CF 3 SO 2) can be exemplified 3 or the like.
  • the lithium ion secondary battery 10 includes an electrode group including a positive electrode 1 having a positive electrode active material coated on both sides of a current collector, a negative electrode 2 having a negative electrode active material coated on both sides of the current collector, and a separator 3.
  • the positive electrode 1 and the negative electrode 2 are wound via the separator 3 to form a wound electrode group.
  • the wound body is inserted into the battery can 4.
  • the negative electrode 2 is electrically connected to the battery can 4 via the negative electrode lead piece 6.
  • a sealing lid 7 is attached to the battery can 4 via a packing 8.
  • the positive electrode 1 is electrically connected to the sealing lid 7 through the positive electrode lead piece 5.
  • the wound body is insulated by the insulating plate 9.
  • the electrode group may not be a wound body shown in FIG. 1, and may be a laminate in which the positive electrode 1 and the negative electrode 2 are stacked via the separator 3.
  • ⁇ Preparation of positive electrode active material Lithium carbonate, nickel carbonate and manganese carbonate were mixed in a ball mill to obtain a precursor. The obtained precursor was calcined at 500 ° C. for 12 hours in the air to obtain a lithium transition metal oxide. The obtained lithium transition metal oxide was pelletized and then fired at 850 to 1050 ° C. for 12 hours in the air. The fired pellets were crushed in an agate mortar and classified with a 45 ⁇ m sieve to obtain a positive electrode active material.
  • the following two-step method was used as the surface treatment of the obtained positive electrode active material.
  • the positive electrode active material was acid-treated to deplete Li in the surface layer.
  • the positive electrode active material was added to the acidic solution and stirred while heating at 100 to 130.degree. Thereafter, it was heated at 200 to 400 ° C., and after the temperature dropped, it was washed with purified water.
  • an acidic solution nitric acid, hydrochloric acid, sodium sulfate, ammonium sulfate etc. can be mentioned.
  • the surface part lacking Li was covered with a phase containing an additive metal element.
  • the positive electrode active material after the first-step treatment was placed in a solution containing the elemental species to be coated, and stirred while heating at 100 to 130.degree. Thereafter, the resultant was heated at 300 to 600 ° C. to obtain a surface-coated positive electrode active material.
  • a solution containing an additive metal element a solution in which magnesium acetate, iron acetate, zinc acetate, aluminum lactate, molybdic acid and the like are dissolved in purified water or citric acid can be mentioned.
  • composition of the positive electrode active material used in each example and comparative example is shown in Table 1.
  • a positive electrode was produced using 18 types of positive electrode active materials produced as mentioned above, and 18 types of trial manufacture batteries were produced.
  • the positive electrode active material, the conductive agent, and the binder were uniformly mixed to prepare a positive electrode slurry.
  • the positive electrode slurry was applied onto a 20 ⁇ m thick aluminum current collector foil, dried at 120 ° C., and compression molded by a press so that the electrode density was 2.2 g / cm 3 to obtain an electrode plate. Thereafter, the electrode plate was punched into a disk shape having a diameter of 15 mm to produce a positive electrode.
  • the negative electrode was produced using metallic lithium.
  • a non-aqueous electrolytic solution one in which LiPF 6 was dissolved at a concentration of 1.0 mol / L in a mixed solvent of ethylene carbonate and dimethyl carbonate at a volume ratio of 1: 2 was used.
  • the charge and discharge test was performed on the prototype battery.
  • the charging was constant current constant voltage charging (CC-CV mode), and the upper limit voltage was 4.6V.
  • the discharge was constant current discharge (CC mode), and the lower limit voltage was 2.5V.
  • the charge / discharge current was equivalent to 0.05 C, and the charge cutoff current was equivalent to 0.005 C.
  • a value obtained by dividing the discharge capacity in the area of 4.6 to 3.0 V by the discharge capacity in the area of 4.6 to 3.0 V in the comparative example 1 is defined as a discharge capacity ratio. The results are shown in Table 2.
  • the irreversible capacity ratio is lower and the capacity retention ratio is higher than in Comparative Example 1. Since the positive electrode active materials of Examples 1 to 11 were subjected to the surface treatment, the content ratio of Li to Ni and Mn in the surface layer portion is low, and the surface layer portion contains the additive metal element. Therefore, the irreversible capacity can be reduced and the discharge capacity can be improved by using the positive electrode active material in which the surface layer portion contains an additive metal element, which has a lower Li content in the surface layer than the internal Li content.
  • Example 2 has a smaller irreversible capacity ratio than Comparative Example 6.
  • the positive electrode active material of Example 2 has a structure in which the surface treatment with acid is performed and Li in the surface layer is lost, while the positive electrode active material of Comparative Example 6 is not treated with acid, so the surface layer is Li is not deficient. Therefore, it was found that the irreversible capacity can be reduced by using the positive electrode active material in which the Li content to the internal Ni and Mn is lower than the Li content to the Ni and Mn in the surface layer.
  • Example 1 When Example 1 is compared with Comparative Example 7, Example 1 has a larger capacity retention ratio than Comparative Example 7.
  • the positive electrode active material of Example 1 contains the additive metal element in the surface layer portion, but the surface layer portion of the positive electrode active material of Comparative Example 7 is not coated. Therefore, in Comparative Example 7, the capacity retention ratio was reduced. Therefore, it was found that the particle surface can be protected and the cycle characteristics can be improved by including the metal element not present inside in the surface layer portion.
  • the discharge capacity ratio of Examples 1 to 4 is higher than the discharge capacity ratio of Comparative Examples 2 to 4. This is because the composition of the positive electrode active material of Comparative Examples 2 to 4 is not included in the range of 1 ⁇ x ⁇ 1.2, 0.2 ⁇ a ⁇ 0.4, 0.4 ⁇ b ⁇ 0.6. It is for.
  • Comparative Example 2 since the amount of Li of the positive electrode active material is small, the capacity is reduced and the irreversible capacity is high.
  • Comparative Example 3 since the amount of Li of the positive electrode active material was too large, the crystal lattice became unstable and the capacity decreased. In Comparative Example 4, the capacity decreased because the amount of Ni of the positive electrode active material was too large.
  • the irreversible capacity can be reduced and the discharge capacity can be improved by covering the surface layer portion with a phase containing a metal element that is not present inside the particles after depleting Li in the surface layer portion.
  • cycle characteristics can be improved.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'invention porte sur un matériau actif d'électrode positive pour des batteries secondaires au lithium-ion, qui est caractérisé par le fait qu'il est constitué de particules qui contiennent du lithium, du nickel et du manganèse et est également caractérisé par le fait que : chacune desdites particules possède un intérieur et une couche de surface ; la composition des intérieurs de particule peut être représentée par la formule de composition LixNiaNnbMcO2 (avec 1 < x ≤ 1,2, 0,2 ≤ a ≤ 0,4, 0,4 ≤ b ≤ 0,6, c ≤ 0,02, a + b + c = 0,8, et M représentant un élément de métal de transition) ; le rapport atomique du lithium sur le nickel et le manganèse dans les couches de surface est inférieur au rapport atomique du lithium sur le nickel et le manganèse dans les intérieurs de particule ; et les couches de surface contiennent un élément de métal ajouté. Cette invention rend possible le fait de fournir un matériau actif d'électrode positive pour des batteries secondaires au lithium-ion ayant une capacité de décharge élevée et une capacité irréversible faible.
PCT/JP2013/068591 2013-07-08 2013-07-08 Matériau actif d'électrode positive pour des batteries secondaires au lithium-ion WO2015004705A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015130273A (ja) * 2014-01-07 2015-07-16 日立金属株式会社 リチウムイオン二次電池用正極活物質、それを用いたリチウムイオン二次電池用正極及びリチウムイオン二次電池、並びに、リチウムイオン二次電池用正極活物質の製造方法
WO2022237184A1 (fr) * 2021-05-08 2022-11-17 蜂巢能源科技股份有限公司 Matériau d'électrode positive exempt de cobalt, son procédé de préparation et son application

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003500318A (ja) * 1999-05-15 2003-01-07 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフトング 金属酸化物で被覆されたリチウム混合酸化物粒子
JP2012129166A (ja) * 2010-12-17 2012-07-05 Samsung Sdi Co Ltd リチウムイオン二次電池
JP2012138197A (ja) * 2010-12-24 2012-07-19 Asahi Glass Co Ltd リチウムイオン二次電池用の正極活物質、正極、リチウムイオン二次電池、および、リチウムイオン二次電池用正極活物質の製造方法
JP2012142154A (ja) * 2010-12-28 2012-07-26 Sony Corp リチウムイオン二次電池、電動工具、電動車両および電力貯蔵システム
JP2012169066A (ja) * 2011-02-10 2012-09-06 Asahi Glass Co Ltd リチウムイオン二次電池用の正極活物質の製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003500318A (ja) * 1999-05-15 2003-01-07 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフトング 金属酸化物で被覆されたリチウム混合酸化物粒子
JP2012129166A (ja) * 2010-12-17 2012-07-05 Samsung Sdi Co Ltd リチウムイオン二次電池
JP2012138197A (ja) * 2010-12-24 2012-07-19 Asahi Glass Co Ltd リチウムイオン二次電池用の正極活物質、正極、リチウムイオン二次電池、および、リチウムイオン二次電池用正極活物質の製造方法
JP2012142154A (ja) * 2010-12-28 2012-07-26 Sony Corp リチウムイオン二次電池、電動工具、電動車両および電力貯蔵システム
JP2012169066A (ja) * 2011-02-10 2012-09-06 Asahi Glass Co Ltd リチウムイオン二次電池用の正極活物質の製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015130273A (ja) * 2014-01-07 2015-07-16 日立金属株式会社 リチウムイオン二次電池用正極活物質、それを用いたリチウムイオン二次電池用正極及びリチウムイオン二次電池、並びに、リチウムイオン二次電池用正極活物質の製造方法
WO2022237184A1 (fr) * 2021-05-08 2022-11-17 蜂巢能源科技股份有限公司 Matériau d'électrode positive exempt de cobalt, son procédé de préparation et son application

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