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WO2014092347A1 - Matériau actif d'électrode négative pour batterie secondaire au lithium et batterie secondaire utilisant celui-ci - Google Patents

Matériau actif d'électrode négative pour batterie secondaire au lithium et batterie secondaire utilisant celui-ci Download PDF

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Publication number
WO2014092347A1
WO2014092347A1 PCT/KR2013/010438 KR2013010438W WO2014092347A1 WO 2014092347 A1 WO2014092347 A1 WO 2014092347A1 KR 2013010438 W KR2013010438 W KR 2013010438W WO 2014092347 A1 WO2014092347 A1 WO 2014092347A1
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Prior art keywords
secondary battery
active material
negative electrode
electrode active
alloy
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Ceased
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PCT/KR2013/010438
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English (en)
Korean (ko)
Inventor
김향연
배영산
임혜민
성민석
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Iljin Electric Co Ltd
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Iljin Electric Co Ltd
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Publication date
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Publication of WO2014092347A1 publication Critical patent/WO2014092347A1/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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/134—Electrodes based on metals, Si or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—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
    • H01M4/386—Silicon or alloys based on silicon
    • 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 secondary battery using the same, and more particularly, to a negative electrode active material for a lithium secondary battery having a high charge and discharge capacity and an excellent capacity retention rate, and a secondary battery using the same.
  • Lithium metal is used as a negative electrode active material of a conventional lithium battery.
  • a carbon-based material is used as a negative electrode active material instead of lithium metal because a short circuit of the battery occurs due to dendrite formation. .
  • Examples of the carbon-based active material include crystalline carbon such as graphite and artificial graphite, and amorphous carbon such as soft carbon and hard carbon.
  • crystalline carbon such as graphite and artificial graphite
  • amorphous carbon such as soft carbon and hard carbon.
  • Graphite is typically used as the crystalline carbon, and has a theoretical limit capacity of 372 mAh / g, which has a high capacity, and is used as a negative electrode active material.
  • the graphite or carbon-based active material has a rather high theoretical capacity, it is only about 380 mAh / g, and there is a problem in that the above-described negative electrode cannot be used in the development of a high capacity lithium battery in the future.
  • a negative electrode active material based on metals or intermetallic compounds.
  • lithium batteries using metals or semimetals such as aluminum, germanium, silicon, tin, zinc, and lead as negative electrode active materials have been studied.
  • Such a material has a high energy density and high energy density, and can absorb and release more lithium ions than a negative electrode active material using a carbon-based material, thereby manufacturing a battery having a high capacity and a high energy density.
  • Pure silicon for example, is known to have a high theoretical capacity of 4017 mAh / g.
  • the cycle characteristics are deteriorated, and it is still an obstacle to practical use.
  • the silicon is used as a lithium occlusion and emission material as a negative electrode active material, it is interposed between the active materials due to the volume change in the charging and discharging process. This is because a decrease in conductivity or a phenomenon in which the negative electrode active material peels from the negative electrode current collector occurs. That is, the silicon, etc. included in the negative electrode active material occludes lithium by charging and expands to about 300 to 400% by volume, and when lithium is discharged, the inorganic particles shrink.
  • Repeating such a charge / discharge cycle may cause electrical insulation due to cracking of the negative electrode active material, and thus has a problem in that it is used in a lithium battery because the life is sharply reduced.
  • Korean Laid-Open Patent Publication No. 2004-0063802 relates to a "negative active material for lithium secondary batteries, a manufacturing method thereof, and a lithium secondary battery", which uses a method of eluting a metal after alloying another metal such as silicon and nickel.
  • Patent No. 2004-0082876 relates to "Method for Producing Porous Silicon and Nano-Sized Silicon Particles and Application to Cathode Material for Lithium Secondary Battery", and heat treatment by mixing a silicon precursor such as alkali metal or alkaline earth metal in powder state and silicon dioxide. Later, the technique of eluting with an acid was disclosed.
  • the patents may improve the initial capacity retention rate due to the buffering effect due to the porous structure.
  • the porous silicon particles having low conductivity are used, if the particles are not nano-sized, the conductivity between the particles may be lowered at the time of manufacturing the electrode. There is a problem that the retention characteristics are lowered.
  • a negative electrode active material for a lithium secondary battery in which the electrical change does not easily occur due to a small volume change during charge and discharge.
  • Another object of the present invention is to provide a negative electrode active material for a lithium secondary battery excellent in initial efficiency and capacity retention characteristics.
  • the present invention provides an anode active material for a lithium secondary battery, characterized in that the amorphous crystallinity of the microcrystalline region of the matrix (Matrix) in the alloy is 30% or more as an alloy consisting of the formula (1).
  • the present invention provides a negative electrode active material for a lithium secondary battery, characterized in that the transition metal is selected from the group consisting of Al, Cu, Ti and Fe.
  • the present invention also provides a secondary battery comprising a cathode and an electrolyte including a cathode and an anode active material according to the present invention.
  • the present invention provides a secondary battery in which the positive electrode comprises a thiolated intercalation compound, an inorganic sulfur or a sulfur compound.
  • the present invention also provides a secondary battery in which the electrolyte contains a non-aqueous organic solvent and a lithium salt.
  • the present invention also provides a secondary battery having a cylindrical shape, a horn shape, a coin shape, or a pouch shape.
  • the negative electrode active material for a lithium secondary battery according to the present invention has an effect of extending the service life because the electrical change does not occur because the volume change is small during charge and discharge when used in the secondary battery.
  • the negative electrode active material for a lithium secondary battery according to the present invention has an excellent initial efficiency and capacity retention characteristics when used in a secondary battery.
  • the negative electrode active material for a lithium secondary battery according to the present invention has an effect that the amount of voltage and current is maintained substantially constant even when repeated charging and discharging when used in the secondary battery.
  • Figure 1 shows the SEM measurement results of the negative electrode active material according to an embodiment of the present invention.
  • Figure 2 shows the XRD measurement results of the negative electrode active material according to an embodiment of the present invention.
  • Figure 3 shows the amorphousness measurement of the negative electrode active material according to an embodiment of the present invention.
  • Figure 4 shows the charge and discharge capacity of the negative electrode active material according to an embodiment of the present invention.
  • 5 is a charge and discharge cycle repeated up to 50 times at 0.5C of a battery manufactured using a negative electrode active material according to an embodiment of the present invention, the capacity change according to the cycle is measured.
  • the present invention provides an anode active material for a secondary battery, characterized in that the amorphous crystallinity is 30% or more in the microcrystalline region of the matrix (Matrix) in the alloy as an alloy of the formula (1).
  • the microcrystalline region is present on the matrix of the alloy, and the presence of the microcrystalline region allows lithium to be diffused more easily than the crystalline region mainly.
  • the ratio of the presence of the microcrystalline region may be represented through the degree of amorphousness, and when the amorphous region is formed on the matrix, it may be suppressed in the volume expansion during charging of the secondary battery in applying it as a negative electrode active material of the secondary battery.
  • the present invention is characterized in that at least 30% of the degree of amorphousness of the microcrystalline region on the matrix (Matrix).
  • the amorphousness of the microcrystalline region is 30% or more, thereby facilitating the diffusion of lithium.
  • the amorphous phase on the matrix is 30% or more, when the secondary battery is used as a negative electrode active material, it can be seen that volume expansion is suppressed during charging.
  • the transition metal is preferably selected from one or more from the group consisting of Al, Cu, Ti and Fe.
  • Figure 1 shows the SEM measurement results of the negative electrode active material according to an embodiment of the present invention
  • Figure 2 shows the XRD measurement results of the negative electrode active material according to an embodiment of the present invention.
  • Amorphization degree of the microcrystals in the range of ° ⁇ 100 ° to 30 to 45%, thereby having an effect that the volume expansion is suppressed when the alloy is charged in the secondary battery.
  • the amorphousness is 30 to 45%, volume expansion is suppressed so that electrical insulation is hardly generated.
  • Calculation of the degree of amorphousness used in the present invention is as follows, the expression can be obtained by looking at the area to measure the degree of amorphousness of FIG.
  • the high degree of amorphousness may be interpreted to mean that there are many microcrystalline regions, and thus, a buffering function may be performed in the microcrystalline region during charging to block a factor in which lithium ions may accumulate and expand in volume. It becomes possible.
  • the method for preparing the negative electrode active material of the present invention is not particularly limited, and for example, various fine powder production techniques known in the art (gas atomizer method, centrifugal gas atomizer method, plasma atomizer method, rotary electrode method, Mechanical alignment, etc.) may be used.
  • gas atomizer method centrifugal gas atomizer method, plasma atomizer method, rotary electrode method, Mechanical alignment, etc.
  • Si and the components constituting the matrix may be mixed, the mixture may be melted by an arc melting method or the like, and then applied to a single roll quench solidification method in which the melt is sprayed onto a rotating copper roll to prepare an active material. have.
  • the method applied in the present invention is not limited to the above method, and if a sufficient quenching speed can be obtained in addition to the single-roll quenching solidification method, the fine powder production technique (gas atomizer method, centrifugal gas atomizer method) presented above. , Plasma atomizer method, rotary electrode method, mechanical aligning method, and the like.
  • a secondary battery may be manufactured using a negative electrode active material according to an embodiment of the present invention, and the positive electrode of the secondary battery may include a ritated intercalation compound, and also inorganic sulfur (S8). Also, elemental sulfur and sulfur compounds may be used.
  • the kind of electrolyte included in the secondary battery of the present invention is not particularly limited either, and general means known in the art may be employed.
  • the electrolyte may include a non-aqueous organic solvent and a lithium salt.
  • the lithium salt may be dissolved in an organic solvent to serve as a source of lithium ions in the battery and to promote the movement of lithium ions between the positive electrode and the negative electrode.
  • lithium salts examples include LiPF 6 , LiBF 4 , LiSbF 6 , LiAsF 6 , LiCF 3 SO 3 , LiN (CF 3 SO 2 ) 3 , Li (CF 3 SO 2 ) 2 N, LiC 4 F 9 SO 3 , LiClO 4 , LiAlO 4 , LiAlCl 4 , LiN (C x F 2x + 1 SO 2 ) (C y F 2y + 1 SO 2 ), where x and y are natural numbers, LiCl, LiI, and lithium It includes the one or more kinds of bisoxalate borate (lithium bisoxalate borate) or the like as a supporting electrolyte salt.
  • the concentration of lithium salt in the electrolyte which can vary depending on the application, is typically used within the range of 0.1M to 2.0M.
  • the organic solvent serves as a medium to move ions involved in the electrochemical reaction of the battery, for example, benzene, toluene, fluorobenzene, 1,2-difluorobenzene, 1, 3-difluorobenzene, 1,4-difluorobenzene, 1,2,3-trifluorobenzene, 1,2,4-trifluorobenzene, chlorobenzene, 1,2-dichlorobenzene, 1, 3-dichlorobenzene, 1,4-dichlorobenzene, 1,2,3-trichlorobenzene, 1,2,4-trichlorobenzene, iodobenzene, 1,2-diiobenzene, 1, 3-diiobenzene, 1,4-diiobenzene, 1,2,3-triiobenzene, 1,2,4-triiobenzene, fluorotoluene, 1,2-difluorotoluene , 1,3-di
  • the secondary battery of the present invention may further include conventional elements such as a separator, a can, a battery case or a gasket, and the specific types thereof are not particularly limited.
  • the secondary battery of the present invention may be manufactured in a conventional manner and shape in the art, including such elements.
  • Examples of the shape that the secondary battery of the present invention may have include a cylindrical shape, a horn shape, a coin shape, or a pouch shape, but are not limited thereto.
  • the method for preparing the negative electrode active material of the present invention is not particularly limited, and for example, various fine powder production techniques known in the art (gas atomizer method, centrifugal gas atomizer method, plasma atomizer method, rotary electrode method, Mechanical alignment, etc.) may be used.
  • gas atomizer method centrifugal gas atomizer method, plasma atomizer method, rotary electrode method, Mechanical alignment, etc.
  • Si and the components constituting the matrix were mixed, the mixture was melted by an arc melting method or the like, and then applied to a single roll quench solidification method in which the melt was sprayed onto a rotating copper roll to prepare an active material.
  • the method applied in the present invention is not limited to the above method, and if a sufficient quenching speed can be obtained in addition to the single-roll quenching solidification method, the fine powder manufacturing technique (gas atomizer method, centrifugal gas atomizer method, plasma method) presented above. It can also be manufactured by the atomizer method, the rotating electrode method, the mechanical etching method and the like.
  • a composite alloy was prepared in which the transition metal was Cu 65.40 Ni 25.69 Cu 8.91 in the Si x Ni y M z alloy, and the degree of amorphousness of the alloy was measured. In preparing, it was used as a negative electrode active material.
  • Example 2 It carried out similarly to Example 1 except having set the transition metal as Ti in Si x Ni y M z alloy, and set it as Si 65.41 Ni 25.69 Ti 8.90 .
  • Example 2 It carried out similarly to Example 1 except having set the transition metal to Fe in the alloy of Si x Ni y M z to Si 65.40 Ni 25.69 Fe 8.91 .
  • Example 2 It carried out similarly to Example 1 except having set the transition metal to Al in Si x Ni y M z alloy, and set it as Si 65.40 Ni 25.70 Al 8.90 .
  • Si 60 Fe 14 Al 26 was prepared. At this time, Si 60 Fe 14 Al 26 was prepared and used as a negative electrode active material.
  • Si x Ni y M z of a transition in the alloy and the metal of Fe was carried out in the same manner as in Example 1 except that Si 45 Ni 25 Fe 30.
  • Example 2 The same procedure as in Example 1 was carried out except that Si 48 Ni 30 Al 22 was prepared using Al as a transition metal in the alloy of Si x Ni y M z .
  • SEM Scanning Electron Microscopy
  • the Si phase was uniformly dispersed and precipitated on the matrix.
  • Cu k ⁇ -ray XRD measurements were performed on the negative active materials prepared in Examples 1 to 4, and the results are shown in FIG. 2.
  • the measurement angle was set at 20 degrees to 100 degrees, and the measurement speed was set at 5.7 degrees per minute.
  • Coin-shaped secondary batteries were prepared using the negative electrode active materials prepared in Examples 1 to 4 and Comparative Examples 1 to 4, and after the charge and discharge evaluations, the results are shown in FIG. 4.
  • the mixing ratio of the active material, the conductive agent (Super P-based conductive agent), and the binder (PI-based binder) is 77: 15: 2: 6 (active material: additive: conductive agent: binder). It was prepared as possible. Charged and discharged after performing once at 0.5C for the prepared electrode plate was measured, as shown in Table 1 below.
  • the amorphousness measurement can be obtained by using the formula of the amorphousness degree using the XRD pattern of the alloy.
  • the volume expansion factor may be reduced.
  • the degree of amorphousness was less than 30%, and thus, it is judged that the volume expansion is higher than that of the Examples.
  • Charge and discharge was repeated 50 times at 0.5C and measured, and the result is as shown in FIG.
  • the charge and discharge method was performed according to the charge and discharge method for the active material for a lithium secondary battery generally known in the art.

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

Abstract

La présente invention concerne un matériau actif d'électrode négative pour une batterie secondaire au lithium et une batterie secondaire utilisant celui-ci, et plus particulièrement, fournit un matériau actif d'électrode négative pour une batterie secondaire au lithium et une batterie secondaire utilisant celui-ci, le matériau actif comprenant un alliage représenté par la formule chimique (1) SixNiyMz (dans la formule 50≤x≤90, 1≤y≤49, 1≤z≤49, x+y+z=100, x, y et z étant chacun des pourcentages atomiques, et m étant un métal de transition), et le degré d'amorphisation d'une région microcristalline sur la matrice dans l'alliage étant d'au moins 30 %.
PCT/KR2013/010438 2012-12-12 2013-11-18 Matériau actif d'électrode négative pour batterie secondaire au lithium et batterie secondaire utilisant celui-ci Ceased WO2014092347A1 (fr)

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KR20120144153A KR101492973B1 (ko) 2012-12-12 2012-12-12 리튬 이차 전지용 음극활물질 및 이를 이용한 이차전지
KR10-2012-0144153 2012-12-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018225971A1 (fr) * 2017-06-07 2018-12-13 한국생산기술연구원 Matériau actif d'anode destiné à une batterie secondaire au lithium, anode destinée à une batterie secondaire au lithium, et batterie secondaire au lithium comprenant une telle anode

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101762773B1 (ko) * 2015-05-06 2017-07-28 공문규 리튬 이차 전지용 음극 활물질
KR102527633B1 (ko) 2023-03-17 2023-04-28 성재욱 리튬 이차전지용 음극 활물질, 이의 제조방법 및 상기 음극 활물질을 포함하는 리튬 이차전지

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001338646A (ja) * 2000-05-26 2001-12-07 Sanyo Electric Co Ltd リチウム二次電池用負極
KR20050090220A (ko) * 2004-03-08 2005-09-13 삼성에스디아이 주식회사 리튬 이차 전지용 음극 활물질, 그의 제조 방법 및 그를포함하는 리튬 이차 전지
KR20060074808A (ko) * 2004-12-27 2006-07-03 삼성에스디아이 주식회사 리튬 이차 전지
KR20080009269A (ko) * 2005-03-23 2008-01-28 파이오닉스 가부시키가이샤 리튬이차전지용 음극 활물질 입자와 음극 및 그들의 제조방법

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001338646A (ja) * 2000-05-26 2001-12-07 Sanyo Electric Co Ltd リチウム二次電池用負極
KR20050090220A (ko) * 2004-03-08 2005-09-13 삼성에스디아이 주식회사 리튬 이차 전지용 음극 활물질, 그의 제조 방법 및 그를포함하는 리튬 이차 전지
KR20060074808A (ko) * 2004-12-27 2006-07-03 삼성에스디아이 주식회사 리튬 이차 전지
KR20080009269A (ko) * 2005-03-23 2008-01-28 파이오닉스 가부시키가이샤 리튬이차전지용 음극 활물질 입자와 음극 및 그들의 제조방법

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018225971A1 (fr) * 2017-06-07 2018-12-13 한국생산기술연구원 Matériau actif d'anode destiné à une batterie secondaire au lithium, anode destinée à une batterie secondaire au lithium, et batterie secondaire au lithium comprenant une telle anode

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KR20140080578A (ko) 2014-07-01

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