WO2013132996A1 - リチウム二次電池用負極活物質およびその製造方法 - Google Patents

リチウム二次電池用負極活物質およびその製造方法 Download PDF

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Publication number
WO2013132996A1
WO2013132996A1 PCT/JP2013/053837 JP2013053837W WO2013132996A1 WO 2013132996 A1 WO2013132996 A1 WO 2013132996A1 JP 2013053837 W JP2013053837 W JP 2013053837W WO 2013132996 A1 WO2013132996 A1 WO 2013132996A1
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Prior art keywords
negative electrode
lithium secondary
active material
electrode active
secondary battery
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PCT/JP2013/053837
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English (en)
French (fr)
Japanese (ja)
Inventor
晃二 久幸
雅司 坂口
忠利 黒住
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昭和電工株式会社
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Priority to CN201380004284.5A priority Critical patent/CN103999271B/zh
Publication of WO2013132996A1 publication Critical patent/WO2013132996A1/ja

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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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/068—Flake-like particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/05—Light metals
    • B22F2301/054—Alkali metals, i.e. Li, Na, K, Rb, Cs, Fr
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M4/04—Processes of manufacture in general
    • 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 negative electrode active material for a lithium secondary battery and a method for producing the same, and more specifically, a negative electrode active material for a non-aqueous electrolyte secondary battery capable of reversibly occluding and releasing Li ions in large quantities and the production thereof.
  • the nonaqueous electrolyte secondary battery includes a secondary battery using a nonaqueous electrolyte obtained by dissolving an electrolyte in an organic solvent, and a secondary battery using a nonaqueous electrolyte such as a polymer electrolyte or a gel electrolyte. .
  • Lithium secondary batteries such as lithium ion batteries and lithium polymer batteries have a high energy density and are not only used as main power sources for mobile communication devices and portable electronic devices, but also for large-scale power storage. It is also attracting attention as a power source and an on-vehicle power source.
  • a negative electrode of such a lithium secondary battery conventionally, those formed from various carbon materials such as graphite and carbon having a low crystallinity have been widely used.
  • a negative electrode made of a carbon material has a low usable current density and an insufficient theoretical capacity.
  • graphite which is one of the carbon materials, has a theoretical capacity of only 372 mAh / g, and therefore a higher capacity is desired.
  • a negative electrode active material made of a material other than metal Li which is a substance having a discharge capacity larger than that of a general-purpose carbon material.
  • elements such as Sn, Si and Ag, nitrides, oxides and the like of these can occlude Li ions to form an alloy with Li ions, and the occlusion amount is much larger than various carbon materials. It is known to show a value.
  • a negative electrode active material is an alloy of two or more phases composed of a metal that easily stores and releases Li ions and a metal that does not store and release, and the metal that does not store and release does not store and release Li ions.
  • a negative electrode active material intended to suppress the expansion / contraction of the negative electrode during discharge and the cracking or pulverization of the negative electrode due to expansion / contraction has been proposed.
  • Patent Document 1 discloses a raw material melt consisting of a Li ion storage phase ⁇ and a phase ⁇ made of an intermetallic compound or a solid solution of an element constituting the Li ion storage phase ⁇ and another element and having a selected composition.
  • An anode active material having a structure rapidly quenched and solidified by an atomizing method, a roll quenching method, or the like is described.
  • Patent Document 2 discloses Ag, Al, Au, Ca, Cu, Fe, In, Mg, Pd, Pt, Y Zn, Ti, V, Cr, Mn, Co, Ni, Y, Zr, Nb, Mo, Hf, Ta, W and an A component that is at least one element selected from the group consisting of rare earth elements, and Ga, A negative electrode made of a composite powder formed by mixing a raw material consisting of a B component, which is at least one element selected from the group consisting of Ge, Sb, Si and Sn, and performing mechanical alloying treatment Substances have been described.
  • the object of the present invention is to solve the above-described problems, and to increase the amount of occlusion / release of Li ions, thus increasing the charge / discharge capacity and reducing the capacity decrease due to repeated charge / discharge.
  • An object of the present invention is to provide a negative electrode active material for a lithium secondary battery and a method for producing the same, which can achieve a longer cycle life.
  • the present invention comprises the following aspects in order to achieve the above object.
  • a negative electrode active material for a lithium secondary battery having a size that can be measured and having a powder specific surface area of 0.3 m 2 / g or more by the BET method.
  • Powder is formed by cutting aluminum foil with a thickness of 0.15 mm or less to form particles, and each particle constituting the powder is passed through a sieve having a mesh size of 0.1 mm (based on JIS Z8801-1).
  • a method for producing a negative electrode active material for a lithium secondary battery characterized in that the specific surface area of the powder according to the BET method is 0.3 m 2 / g or more.
  • a negative electrode for a lithium secondary battery in which a mixed material containing a negative electrode active material, a conductive additive, and a binder described in any one of 1) to 9) above is attached on a current collector.
  • a lithium secondary battery comprising the negative electrode described in 19) above, a separator, and a positive electrode for a lithium secondary battery.
  • the present invention also includes the following aspects.
  • the negative active material for a lithium secondary battery comprises a powder that is an aggregate of particles formed by cutting an aluminum foil having a thickness of 0.15 mm or less.
  • the size is such that it can pass through a sieve with a mesh size of 0.1 mm (based on JIS Z8801-1), and the specific surface area of the powder by the BET method is 0.3 m 2 / g or more.
  • the specific surface area of the powder formed is increased. Accordingly, the volume change of the negative electrode active material during charging / discharging is reduced, and the volume change of the negative electrode active material during charging / discharging is increased.
  • Separation of substances from conductive aids and binders can be effectively suppressed, and capacity reduction due to repeated charging and discharging is reduced, and the cycle life of lithium secondary batteries is extended. Will be possible.
  • the reason is estimated as follows. That is, when Li ions are alloyed with Al, a compound containing Li ions is formed on the surface of the particles by preferential reaction from the surface of the particles, but the specific surface area of the powder by the BET method is 0. If it is 3 m ⁇ 2 > / g or more, the compound containing many Li ions will be formed in the surface of particle
  • the lithium secondary battery including the negative electrode formed from the negative electrode active materials 1) to 9) is more than the lithium secondary battery including the negative electrode formed from the negative electrode active materials made of various carbon materials.
  • a large amount of Li ions can be occluded / released, and the charge / discharge capacity is increased.
  • the volume change at the time of charging / discharging of the lithium secondary battery using the negative electrode formed from the negative electrode active material is further effectively reduced. be able to.
  • a powder is prepared by cutting an aluminum foil having a thickness of 0.15 mm or less to form particles, and each particle constituting the powder is sieved with a sieve having a mesh size of 0.1 mm (JIS Z8801). -1), and the specific surface area of the powder by the BET method is only 0.3 m 2 / g or more, so that a negative electrode active material for a lithium secondary battery can be easily manufactured. can do.
  • the negative electrode active materials 2) to 9) can be easily produced.
  • FIG. 1 is a schematic vertical sectional view showing an apparatus for cutting an aluminum foil to form a powder that becomes a negative electrode active material for a lithium secondary battery according to the present invention.
  • 1 is a partially cutaway front view showing a lithium secondary battery having a negative electrode formed using a negative electrode active material for a lithium secondary battery according to the present invention.
  • FIG. 1 shows particles constituting the negative electrode active material for a lithium secondary battery according to the present invention
  • FIG. 2 shows an apparatus for cutting an aluminum foil to form a powder that becomes a negative electrode active material for a lithium secondary battery according to the present invention
  • FIG. 3 shows an example of a lithium secondary battery having a negative electrode formed using the negative electrode active material for a lithium secondary battery according to the present invention.
  • a negative electrode active material for a lithium secondary battery is made of powder which is an aggregate of particles formed by cutting an aluminum foil having a thickness of 0.15 mm or less, and each particle has a sieve having an opening of 0.1 mm (JIS (Based on Z8801-1), and the specific surface area of the powder by the BET method is 0.3 m 2 / g or more.
  • “foil” means that the thickness is 0.006 to 0.2 mm as defined in JIS.
  • “Powder” means an aggregate of particles having a maximum dimension of 1 mm or less, as defined in JIS Z2500.
  • the reason why the thickness of the aluminum foil used is limited to 0.15 mm is that when the thickness of the aluminum foil exceeds 0.15 mm, it becomes difficult to cut and the production efficiency decreases.
  • the aluminum foil to be used is preferably made of Al having a purity of 99% by mass or more, and is preferably made of Al having a purity of 99.9% by mass or more. This is for increasing the amount of insertion / extraction of Li ions to / from the negative electrode made of the formed negative electrode active material. In particular, when composed of Al having a purity of 99.9% by mass or more, the initial charge / discharge capacity of the lithium secondary battery using the negative electrode formed of the negative electrode active material can be increased, and the capacity by repeating charge / discharge can be increased. Reduction can be reduced.
  • the purity of the aluminum foil represents the balance obtained by subtracting the total amount of Fe, Si and Cu from 100% by mass, as defined in JIS H4170.
  • the powder which is an aggregate of particles formed by cutting the aluminum foil, includes particles of various shapes, but when the aluminum foil having a thickness of 0.15 mm or less is cut, the foil is divided. As a result, a new surface is formed and a stretched portion is formed by bending, resulting in an increase in specific surface area.
  • the particle (1) has a shape as shown in FIG.
  • the particles constituting the powder serving as the negative electrode active material for the lithium secondary battery may be formed by cutting the aluminum foil and pulverizing it by a method in which a compressive stress is applied.
  • the particles may be formed by cutting the aluminum foil and subjecting it to chemical dissolution treatment using acid or alkali. Further, the particles may be formed by cutting the aluminum foil, pulverizing it by a method in which a compressive stress is applied, and then performing a chemical dissolution treatment using an acid or an alkali.
  • the size of the particles is limited to a size that can pass through a sieve having an aperture of 0.1 mm (based on JIS Z8801-1). This is because when mixed with the binder, the paste does not form an appropriate paste, and coating on the current collector becomes difficult.
  • the size of each particle is preferably such that it can pass through a sieve having an aperture of 0.045 mm (based on JIS Z8801-1), and the projected circumference equivalent circle diameter is 0.010 mm or less. More preferably, it is desirable that the projected circumference circle equivalent diameter is 0.005 mm or less.
  • the size of each particle is preferably a size that can pass through a sieve having an opening of 0.045 mm (based on JIS Z8801-1), and a sieve having an opening of 0.010 mm (based on JIS Z8801-1). ) Is more preferable, and it is desirable that the size be able to pass through a sieve having an aperture of 0.005 mm (based on JIS Z8801-1).
  • the specific surface area by the BET method of the powder which is an aggregate of the particles, is limited to 0.3 m 2 / g or more, because the amount of occlusion / release of Li ions to the negative electrode made of the formed negative electrode active material is increased. It is to do.
  • the specific surface area is preferably 0.5 m 2 / g or more.
  • the specific surface area by the BET method is determined by a known method as follows. That is, the solid substance and the gas present around it attract each other by van der Waals force when rapidly cooled, so measure the amount of adsorbed gas and calculate the surface area of the solid by substituting it into the BET equation. can do.
  • the specific surface area of the powder is determined by the BET method using nitrogen gas as the adsorption gas, helium as the carrier gas, and liquid nitrogen as the coolant.
  • nitrogen gas which is a carrier gas
  • helium which is a carrier gas
  • the nitrogen gas concentration in the mixed gas is 29.8%.
  • Conditions such as the thickness of the aluminum foil, the size of the particles, and the specific surface area of the powder by the BET method include the amount of Li ions occluded on the surface of the powder particles formed by cutting the aluminum foil, and the negative electrode active material. It is determined from the viewpoint of absorbing the expansion of the negative electrode during charging of the lithium secondary battery including the negative electrode and the contraction of the negative electrode during discharging.
  • a method of cutting finely with a blade is preferable, and the method of tearing or knocking may cause the opening to the particle surface of the formed powder to be crushed Therefore, it is not preferable.
  • a method of finely cutting using a blade there is a method of using an apparatus including a movable blade and a fixed blade, rotating the movable blade at a high speed, and cutting with the fixed blade. In this case, it is possible to adjust the size of the particles by arranging a screen having a large number of sieves below the movable blade and the fixed blade and appropriately adjusting the size of the sieves.
  • FIG. 2 schematically shows a specific example of an apparatus for cutting an aluminum foil.
  • the housing (21) of the cutting device (20) is provided with a cutting chamber (22) and a powder recovery chamber (23) located below the cutting chamber (22).
  • the housing (21) is provided with a foil inlet (24) facing the cutting chamber (22) and a powder recovery port (25) facing the powder recovery chamber (23).
  • the lids (26) and (27) can be opened and closed freely.
  • a plurality of rotations attached to the rotating body (28) at intervals in the rotating direction of the rotating body (28) and the rotating body (28) A rotary cutting machine (30) having a blade (29) is installed.
  • a plurality of fixed blades (31) are attached to the housing (21) so that the front end portion is desired in the cutting chamber (22). Then, by rotating the rotating body (28), the aluminum foil is cut by the rotating blade (29) and the fixed blade (31).
  • a screen (32) having a plurality of sieves is arranged between the cutting chamber (22) and the powder recovery chamber (23) in the housing (21) of the cutting device (20).
  • the screen (32) comprises a sieve (based on JIS Z8801-1) having an aperture of 0.1 mm, preferably 0.045 mm, more preferably 0.010 mm, and desirably 0.005 mm.
  • the foil inlet (24) is closed by the lid (26), and the rotating body (28) is rotated.
  • the fixed blade (31) With the fixed blade (31), the aluminum foil is cut until it becomes particles of a size passing through the screen (32), and the particles passing through the screen (32) are put into the powder recovery chamber (23). enter. Thereafter, the lid (27) is opened and the powder is taken out from the powder collection chamber (23). In this way, a negative electrode active material is obtained.
  • the negative electrode active material is used for, for example, a coin-type lithium secondary battery (10) as shown in FIG.
  • the coin-type lithium secondary battery (10) is sandwiched between a negative electrode (12), a positive electrode (13) facing the negative electrode (12), and a negative electrode (12) and a positive electrode (13) in a case (11).
  • the separator (14) and a non-aqueous electrolyte (not shown) are enclosed.
  • the negative electrode (12) is obtained by adhering a mixture (16) containing a negative electrode active material, a conductive additive and a binder on a current collector (15).
  • a current collector for example, a rolled copper foil or a copper foil such as an electrolytic copper foil is used.
  • a conductive auxiliary agent ketjen black or acetylene black is used, but it is not limited to this.
  • the binder polyvinylidene fluoride is used, but is not limited thereto.
  • the positive electrode (13) for example, a material made of LiCoO 2 is used as an active material, and a mixture of the active material, a conductive additive and a binder is attached on a current collector made of aluminum foil.
  • the present invention is not limited to this.
  • the initial charge / discharge capacity of the lithium secondary battery (10) is increased, and the capacity reduction due to repeated charge / discharge is reduced.
  • the negative electrode active material according to the present invention is used in a coin-type lithium secondary battery.
  • the present invention is not limited to this, and known lithium secondary batteries such as a square type, a cylindrical type, and a laminate type are used. Used for secondary batteries.
  • Example 1 A commercially available aluminum foil made of Al having a purity of 99.9% by mass with a thickness of 0.12 mm was shredded with a shredder apparatus, and then a screen made of a sieve (based on JIS Z8801-1) having an opening of 0.045 mm ( The negative electrode active material made of powder was pulverized by a pulverizer shown in FIG. The particles in the obtained negative electrode active material have a size that can pass through a sieve having an aperture of 0.045 mm (based on JIS Z8801-1), and the specific surface area of the powder by the BET method is 0.6 m 2 / g. It was.
  • EC ethylene carbonate
  • DMC dimethyl carbonate
  • Example 2 A commercially available aluminum foil made of Al having a purity of 99.9% by mass with a thickness of 0.12 mm was shredded with a shredder apparatus, and then a screen made of a sieve (based on JIS Z8801-1) having an opening of 0.045 mm ( The powder was pulverized by the pulverizer shown in FIG. The particles in the obtained powder have a size that can pass through a sieve having an aperture of 0.045 mm (based on JIS Z8801-1).
  • the powder particles obtained as described above were subjected to a chemical dissolution treatment in 5N HCl at a liquid temperature of 60 ° C. for 40 minutes to produce a negative electrode active material.
  • the specific surface area of the powder constituting the obtained negative electrode active material by the BET method was 1.1 m 2 / g.
  • EC ethylene carbonate
  • DMC dimethyl carbonate
  • Comparative Example 1 (volume ratio)) was dissolved in 1 mol / liter LiPF 6 as an electrolyte, and a coin-type model battery (CR2032 type) was produced in a dry box having an atmosphere with a dew point of ⁇ 50 ° C. or lower.
  • Comparative Example A commercially available aluminum foil made of Al having a purity of 99.9% by mass and having a thickness of 0.12 mm was shredded by a shredder apparatus, and then pulverized by a ball mill, and made of a powder that is an aggregate of flat particles.
  • a negative electrode active material was made.
  • the particles in the obtained negative electrode active material have a size that can pass through a sieve having an aperture of 0.050 mm (based on JIS Z8801-1), and the specific surface area of the powder by the BET method is 0.07 m 2 / g. It was.
  • EC ethylene carbonate
  • DMC dimethyl carbonate
  • the model battery was charged at a constant current of 0.2 mA / cm 2 until reaching 1 V, rested for 10 minutes, and then discharged at a constant current of 0.2 mA / cm 2 until it reached 0 V. This was defined as one cycle, and charging / discharging was repeated to examine the discharge capacity.
  • Table 1 shows the number of cycles and the discharge capacity of the model batteries produced in Examples 1 and 2 and the comparative example.
  • the model batteries produced in Examples 1 and 2 had a higher initial discharge capacity than the model batteries produced in the comparative examples, and a decrease in discharge capacity after 100 cycles. It can be seen that the sufficient value is maintained. Therefore, in the model battery manufactured in the example, the cycle life is extended as compared with the model battery manufactured in the comparative example.
  • the negative electrode active material for a lithium secondary battery according to the present invention is suitably used for a negative electrode of a lithium secondary battery, and it is possible to achieve a long cycle life of the lithium secondary battery.

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  • Engineering & Computer Science (AREA)
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PCT/JP2013/053837 2012-03-05 2013-02-18 リチウム二次電池用負極活物質およびその製造方法 WO2013132996A1 (ja)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03252052A (ja) * 1990-02-28 1991-11-11 Sanyo Electric Co Ltd 電池
JPH03294405A (ja) * 1990-04-11 1991-12-25 Energy Conversion Devices Inc 微粉砕した水素吸蔵合金材料からなる負極の連続的製造方法
JPH10241684A (ja) * 1997-02-27 1998-09-11 Sanyo Electric Co Ltd 非水電解質電池
JP2011187387A (ja) * 2010-03-10 2011-09-22 Gs Yuasa Corp 鉛蓄電池用負極板
WO2012073815A1 (ja) * 2010-11-30 2012-06-07 昭和電工株式会社 リチウム二次電池用負極活物質およびその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001332255A (ja) * 2000-03-16 2001-11-30 Sanyo Electric Co Ltd リチウム二次電池用負極
CN101645500B (zh) * 2009-09-08 2011-10-26 无锡欧力达新能源电力科技有限公司 碳基嵌渗硫材料的制备和以此为正极活性材料的铝二次电池

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03252052A (ja) * 1990-02-28 1991-11-11 Sanyo Electric Co Ltd 電池
JPH03294405A (ja) * 1990-04-11 1991-12-25 Energy Conversion Devices Inc 微粉砕した水素吸蔵合金材料からなる負極の連続的製造方法
JPH10241684A (ja) * 1997-02-27 1998-09-11 Sanyo Electric Co Ltd 非水電解質電池
JP2011187387A (ja) * 2010-03-10 2011-09-22 Gs Yuasa Corp 鉛蓄電池用負極板
WO2012073815A1 (ja) * 2010-11-30 2012-06-07 昭和電工株式会社 リチウム二次電池用負極活物質およびその製造方法

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