WO2015181940A1 - Matériau actif d'électrode négative pour batteries rechargeables au lithium-ion, et batterie rechargeable au lithium-ion - Google Patents

Matériau actif d'électrode négative pour batteries rechargeables au lithium-ion, et batterie rechargeable au lithium-ion Download PDF

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Publication number
WO2015181940A1
WO2015181940A1 PCT/JP2014/064366 JP2014064366W WO2015181940A1 WO 2015181940 A1 WO2015181940 A1 WO 2015181940A1 JP 2014064366 W JP2014064366 W JP 2014064366W WO 2015181940 A1 WO2015181940 A1 WO 2015181940A1
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Prior art keywords
lithium ion
ion secondary
active material
negative electrode
electrode active
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PCT/JP2014/064366
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English (en)
Japanese (ja)
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岡井　誠
鈴木　修一
西村　悦子
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株式会社日立製作所
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Priority to PCT/JP2014/064366 priority Critical patent/WO2015181940A1/fr
Publication of WO2015181940A1 publication Critical patent/WO2015181940A1/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
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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 ion secondary battery and a lithium ion secondary battery.
  • Graphite-based carbon materials are widely used as negative electrode active materials of lithium ion secondary batteries.
  • the stoichiometric composition when lithium is charged into graphite is LiC 6 , and its theoretical capacity can be calculated to be 372 mAh / g.
  • the silicon when the silicon is filled with lithium ions, the stoichiometric composition is Li 15 Si 4 or Li 22 Si 5 , and its theoretical capacity can be calculated to be 3577 mAh / g or 4197 mAh / g.
  • silicon is an attractive material that can store 9.6 times or 11.3 times more lithium than graphite.
  • the silicon particles when the silicon particles are filled with lithium ions, the volume expands to about 3.1 times or about 4.1 times, so that the silicon particles are mechanically broken while repeating the lithium ion charging and discharging. The destruction of the silicon particles electrically isolates the broken fine silicon particles, and the formation of a new electrochemical coating layer on the fracture surface increases the irreversible capacity and significantly reduces the charge-discharge cycle characteristics.
  • Patent Document 1 describes an example in which silicon nanoparticles are attached to the surface of dendritic carbon particles.
  • Patent Document 1 describes that the conductive material of dendritic particles to which silicon nanoparticles are attached is amorphous carbon or graphite carbon.
  • dendritic particles are amorphous carbon alone, dendritic particles can not be used as an active material, and when a nanocomposite containing dendritic particles is used for the negative electrode of a lithium ion secondary battery, a high capacity lithium ion secondary battery is obtained It may not be possible.
  • An object of the present invention is to provide a negative electrode active material for a lithium ion secondary battery capable of producing a high capacity lithium ion secondary battery.
  • a negative electrode active material for a lithium ion secondary battery comprising: a base material; and silicon nanoparticles formed on the surface of the base material, wherein the base material is a base material for forming an amorphous carbon layer and a group for forming an amorphous carbon layer
  • the base material for forming an amorphous carbon layer has an amorphous carbon layer formed on the surface of the material, and the base material for forming an amorphous carbon layer is made of an active material capable of inserting and extracting lithium ions; Negative electrode active material for lithium ion secondary batteries joined to metal materials.
  • FIG. 1 is a schematic view of a thermal vapor deposition apparatus for forming carbon-coated silicon nanoparticles on the surface of a carbon substrate. It is a scanning electron micrograph of carbon covering silicon nanoparticles formed in the surface of a carbon substrate. It is a scanning electron micrograph of carbon covering silicon nanoparticles formed in the surface of a carbon substrate. It is a scanning electron micrograph of carbon covering silicon nanoparticles formed in the surface of a carbon substrate. It is a calculation result regarding the relation between electric capacity and silicon weight ratio. It is an internal structure of the lithium ion secondary battery which concerns on one Embodiment of this invention.
  • FIG. 1 is a view schematically representing the structure of a silicon nanoparticle according to an embodiment of the present invention.
  • the negative electrode active material 1000 for a lithium ion secondary battery has a structure in which silicon nanoparticles 102 are formed on the surface of a carbon substrate 110.
  • the amorphous carbon layer 103 is formed on the surface of the graphite particles 101 (also referred to as a base for forming an amorphous carbon layer), and the silicon nanoparticles 102 are formed on the surface of the amorphous carbon layer 103.
  • the silicon nanoparticles 102 are in contact with the surface of the carbon substrate 110 via flat portions having a curvature smaller than the average curvature. In other words, the silicon nanoparticles 102 are bonded to the carbon base 110 via the amorphous carbon layer 103.
  • the carbon substrate 110 has crystallinity, and an amorphous carbon layer 103 having an amorphous structure is formed at least near the surface.
  • the carbon substrate 110 is also simply referred to as a substrate.
  • the carbon base 110 having such a structure can be easily formed by coating the surface of the graphite particle 101 with the amorphous carbon layer 103.
  • the graphite particles 101 are made of an active material capable of absorbing and desorbing lithium ions. Since the graphite particles 101 can be used as an active material, when the negative electrode active material 1000 for a lithium ion secondary battery in this example is applied to a lithium ion secondary battery, a high capacity lithium ion secondary battery can be obtained.
  • the thickness of the amorphous carbon layer 103 is desirably 1 to 100 nm, preferably 1 to 30 nm. If it is smaller than 1 nm, it is technically difficult to uniformly cover the surface of the graphite particles 101. If the thickness is larger than 100 nm, the possibility of the amorphous carbon layer 103 peeling off from the surface of the graphite particle 101 increases.
  • the silicon nanoparticles 102 can be formed on the surface of the carbon substrate 101 with high density.
  • silicon nanoparticles 102 are grown directly on the surface of the carbon substrate 110 by vapor deposition, as described later.
  • the silicon nanoparticles 102 grown on the surface slide on the crystalline carbon surface, move to aggregate, and then grow into larger and larger silicon particles 102. Do. Therefore, it is difficult to grow the silicon nanoparticles 102 at a high density.
  • the amorphous carbon layer 103 is present, the aggregation of the silicon nanoparticles 102 is unlikely to occur, and it becomes possible to form the silicon nanoparticles 102 having a relatively high diameter and a uniform diameter.
  • the silicon nanoparticles 102 are less likely to move on the amorphous carbon layer 103 than on the crystalline carbon layer.
  • the silicon nanoparticles 102 formed by the vapor deposition method have a shape bonded to the carbon base 110 through a flat surface to some extent. At the bonding interface, the carbon atom of the carbon base 110 and the silicon atom of the silicon nanoparticle 102 form a chemical bond, and the bond between the carbon base 110 and the silicon nanoparticle 102 is very strong.
  • FIG. 2 is a diagram schematically representing the structure of a silicon nanoparticle according to an embodiment of the present invention.
  • the negative electrode active material 1000 for a lithium ion secondary battery is composed of an amorphous carbon layer forming substrate 201, silicon nanoparticles 202, and an amorphous carbon layer 203.
  • Amorphous carbon layer 203 is formed on the surface of base material 201 for forming amorphous carbon layer, and silicon nanoparticles 202 are formed thereon.
  • the base 210 includes an amorphous carbon layer forming base 201 and an amorphous carbon layer 203 formed on the surface of the amorphous carbon layer forming base 201.
  • the base material 201 for forming an amorphous carbon layer it is possible to use a metal active material capable of inserting and extracting lithium ions such as silicon and tin, and various composite materials including them.
  • the amorphous carbon layer forming base material 201 is made of an active material capable of inserting and extracting lithium ions.
  • FIG. 3 is a view schematically representing the structure of silicon nanoparticles according to an embodiment of the present invention.
  • the negative electrode active material 1000 for a lithium ion secondary battery is composed of a carbon base 310, silicon nanoparticles 302, and a carbon coating layer 304.
  • silicon nanoparticles 302 are formed on the surface of the carbon substrate 310
  • a carbon coating layer 304 is formed on the surface of the silicon nanoparticles 302.
  • the carbon base 310 is composed of graphite particles 301 (base for forming an amorphous carbon layer) and an amorphous carbon layer 303.
  • the carbon substrate 310 is also simply referred to as a substrate. The only difference from the first embodiment is that the carbon coating layer 304 is formed.
  • the carbon coating layer 304 is a coating layer containing carbon as a main component, and desirably has a nanographene structure.
  • a nanographene structure In the case of having a nanographene structure, it has an electrical conductivity of 1000 S / m or more, preferably 10000 S / m or more.
  • the silicon nanoparticles 302 can be imparted with electrical conductivity, in particular, high-speed charge and discharge characteristics can be significantly improved.
  • the thickness of the carbon coating layer 304 is desirably 1 to 100 nm. If it is smaller than 1 nm, it is technically difficult to uniformly cover the surface of silicon nanoparticles. In addition, when the diameter is larger than 100 nm, the carbon covering layer 304 is likely to exfoliate from the surface of silicon nanoparticles.
  • FIG. 4 is a view schematically representing the structure of silicon nanoparticles according to an embodiment of the present invention.
  • the negative electrode active material 1000 for a lithium ion secondary battery comprises an amorphous carbon layer forming substrate 401, silicon nanoparticles 402, an amorphous carbon layer 403, and a carbon coating layer 404.
  • Amorphous carbon layer 403 is formed on the surface of a substrate 401 for forming amorphous carbon layer, silicon nanoparticles 402 are formed thereon, and a carbon coating layer 404 is formed on the surface of silicon nanoparticles 402. .
  • the only difference from the second embodiment is that the carbon coating layer 404 is formed.
  • the base 410 has an amorphous carbon layer forming base 401 and an amorphous carbon layer 403 formed on the surface of the amorphous carbon layer forming base 201.
  • the carbon coating layer 404 is a coating layer containing carbon as a main component, and desirably has a nanographene structure.
  • a nanographene structure it has an electrical conductivity of 1000 S / m or more, preferably 10000 S / m or more.
  • the thickness of the carbon coating layer 404 is desirably 1 to 100 nm. If it is smaller than 1 nm, it is technically difficult to uniformly cover the surface of the silicon nanoparticles 402. In addition, when the thickness is larger than 100 nm, the carbon covering layer 404 is likely to exfoliate from the surface of the silicon nanoparticle 402.
  • FIG. 5 is a diagram schematically representing the structure of a silicon nanoparticle according to an embodiment of the present invention.
  • the substrate 501 has a structure in which an amorphous carbon layer is coated on the surface of potato-like natural graphite.
  • the negative electrode active material 1000 for a lithium ion secondary battery has a structure in which silicon nanoparticles 502 are densely formed on the surface of a substrate 501.
  • any substrate or carbon substrate shown in Examples 1 to 4 can be used.
  • the silicon nanoparticles 502 can also form a carbon coating layer as shown in Examples 2 and 4.
  • the diameter of the silicon nanoparticles produced on the surface of the substrate is desirably 1 to 100 nm, more desirably 1 to 30 nm. If the diameter is smaller than 1 nm, the bonding strength with the substrate is weak and the possibility of peeling from the substrate is high. Also, if the diameter is larger than 100, it is likely to be broken due to mechanical strain associated with lithium ion charging and discharging.
  • the diameter is preferably 30 nm or less in order not to destroy mechanical strain caused by high-speed charge and discharge. Further, as described later, in order to realize a high electrical capacity negative electrode active material, it is necessary to increase the weight ratio of silicon. That is, it is desirable to form silicon nanoparticles on the surface of the base material as densely as possible.
  • the specific surface area of the substrate required is calculated.
  • the units are shown in square brackets.
  • the weight of one silicon nanoparticle is w.
  • the silicon nanoparticle is assumed to be a hemisphere, and its radius is r. w can be expressed by equation (1).
  • D is the density of silicon.
  • n of silicon nanoparticles formed on the surface of 1 kg of substrate can be expressed by equation (2).
  • R is a weight ratio of silicon nanoparticles.
  • the occupied area of n silicon nanoparticles is represented by equation (3), and the specific surface area of the substrate is s, and equation (4) holds when the silicon nanoparticles are closely packed.
  • FIGS. 6 and 7 show calculation results on the relationship between the specific surface area of the substrate and the radius of the silicon nanoparticles, assuming close packing.
  • R 0.20 (20 wt%)
  • FIG. 6 shows the calculation results when the radius of the silicon nanoparticles is 0 to 30 nm
  • FIG. 7 shows the results when the radius of the silicon nanoparticles is 30 to 100 nm.
  • a substrate specific surface area of 11.9 [m 2 / g] or more is necessary to achieve a weight ratio of 20 wt% of silicon.
  • a specific surface area of 1 to 8 times is required. That is, a specific surface area of 10 to 80 m 2 / g is required.
  • the specific surface area of the carbon substrate is generally as large as several hundred m 2 / g, and the electrochemical coating on the surface is The irreversible capacity associated with layer formation may be large.
  • the irreversible capacity can be suppressed by setting the specific surface area to 10 to 80 m 2 / g, preferably 20 to 40 m 2 / g as described above.
  • FIG. 8 is a schematic view of a thermal vapor deposition apparatus for forming carbon-coated silicon nanoparticles on the surface of a carbon substrate.
  • liquid silicon tetrachloride As a silicon raw material, liquid silicon tetrachloride was introduced into the reactor by bubbling with hydrogen gas.
  • the vapor pressure of silicon tetrachloride at 20 ° C. is 30 kPa, and when bubbling is introduced, the amount of silicon tetrachloride introduced is 34%. Therefore, in the case of introducing silicon tetrachloride in an amount smaller than that, it is necessary to cool the silicon tetrachloride or to provide a separate line of hydrogen gas.
  • a hydrogen line not bubbling was separately provided, joined with the bubbling line, and introduced into the reactor.
  • the procedure for the growth of carbon-coated silicon nanoparticles is as follows.
  • the reactor is made of quartz and has a diameter of 5 cm and a length of 40 cm.
  • the hydrogen line flowing at a flow rate of 200 mL / min flowing in the upper hydrogen line in FIG. 8 and the bubbling hydrogen line below closed, the growth furnace is heated from room temperature to 1000 ° C. at a rate of 10 ° C./min. did.
  • the flow rate of the upper hydrogen line was changed to 150 mL / min, and the flow rate of the hydrogen line of the lower bubbling hydrogen line was set to 50 mL / min. Under this condition, 8.5% silicon tetrachloride can be introduced.
  • the lower bubbling hydrogen line was closed, and the flow rate of the upper hydrogen line was changed to 200 mL / min and held at 1000 ° C. for 30 minutes. This makes it possible to produce silicon nanoparticles with a diameter of 30 nm on the substrate surface.
  • FIGS. 9 and 10 show scanning electron micrographs of negative electrode materials in which silicon nanoparticles are grown on the surface of amorphous carbon-coated potato-like natural graphite. It can be seen from FIGS. 9 and 10 that silicon nanoparticles can be produced at a very high density. Further, it can be seen from the enlarged photograph of FIG. 11 that the diameter of the silicon nanoparticles is 20 to 30 nm.
  • FIG. 12 shows the results of calculating the dependence of the negative electrode electric capacity on the weight ratio Si / (Si + C) of silicon to the total weight, for the negative electrode active material for lithium ion secondary batteries.
  • the weight ratio is 20% or more, particularly 40% or more, and further 80% with respect to the negative electrode active material for lithium ion secondary battery. It is desirable to contain% or more of silicon.
  • FIG. 13 is an internal structure of a lithium ion secondary battery according to an embodiment of the present invention.
  • 1401 is a positive electrode
  • 1402 is a separator
  • 1403 is a negative electrode
  • 1404 is a battery can
  • 1405 is a positive electrode current collecting tab
  • 1406 is a negative electrode current collecting tab
  • 1407 is an inner lid
  • 1408 is an internal pressure release valve
  • 1409 is a gasket
  • 1410 is a positive temperature coefficient (PTC) resistive element
  • 1411 is a battery cover.
  • the battery lid 1411 is an integrated component including an inner lid 1407, an internal pressure release valve 1408, a gasket 1409, and a positive temperature coefficient resistance element 1410.
  • the positive electrode 1401 can be manufactured by the following procedure. LiMn 2 O 4 is used as the positive electrode active material. To 85.0 wt% of the positive electrode active material, 7.0 wt% and 2.0 wt% of a graphite powder and acetylene black are added as a conductive material, respectively. Further, a solution dissolved in 6.0 wt% of polyvinylidene fluoride (hereinafter abbreviated as PVDF) and 1-methyl-2-pyrrolidone (hereinafter abbreviated as NMP) as a binder is added and mixed by a planetary mixer. Further, the bubbles in the slurry are removed under vacuum to prepare a homogeneous positive electrode mixture slurry.
  • PVDF polyvinylidene fluoride
  • NMP 1-methyl-2-pyrrolidone
  • This slurry is uniformly and evenly applied on both sides of a 20 ⁇ m thick aluminum foil using a coater. After application, it is compression molded by a roll press so that the electrode density is 2.55 g / cm 3 . This is cut with a cutting machine to produce a positive electrode 1401 having a thickness of 100 ⁇ m, a length of 900 mm, and a width of 54 mm.
  • the negative electrode 1403 can be manufactured by the following procedure.
  • the negative electrode active material the negative electrode active material for a lithium ion secondary battery in the present invention such as the negative electrode active material for a lithium ion secondary battery in any of FIGS. 1 to 5 can be used.
  • a solution of 5.0 wt% of PVDF dissolved in NMP as a binder is added to 95.0 wt% of the negative electrode active material. It is mixed with a planetary mixer, and bubbles in the slurry are removed under vacuum to prepare a homogeneous negative electrode mixture slurry. This slurry is uniformly and uniformly applied on both sides of a 10 ⁇ m-thick rolled copper foil with a coating machine.
  • the electrode is compression molded by a roll press to an electrode density of 1.3 g / cm 3 . This is cut with a cutting machine to produce a negative electrode 1303 having a thickness of 110 ⁇ m, a length of 950 mm, and a width of 56 mm.
  • the positive electrode current collecting tab 1405 and the negative electrode current collecting tab 1406 are ultrasonically welded to the positive electrode 1401 and the uncoated part (current collector plate exposed surface) of the negative electrode 1403 which can be manufactured as described above.
  • the positive electrode current collection tab 1405 can be an aluminum lead piece, and the negative electrode current collection tab 1406 can be a nickel lead piece.
  • a separator 1402 made of a porous polyethylene film with a thickness of 30 ⁇ m is inserted into the positive electrode 1401 and the negative electrode 1403, and the positive electrode 1401, the separator 1402, and the negative electrode 1403 are wound.
  • the wound body is housed in a battery can 1404, and the negative electrode current collection tab 1406 is connected to the can bottom of the battery can 1404 by a resistance welder.
  • the positive electrode current collection tab 1405 is connected to the bottom surface of the inner lid 1407 by ultrasonic welding.
  • a non-aqueous electrolyte is injected.
  • the solvent of the electrolytic solution is, for example, composed of ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC), and there is a volume ratio of 1: 1: 1 or the like.
  • the electrolyte is LiPF 6 at a concentration of 1 mol / L (about 0.8 mol / kg). Such an electrolytic solution is dropped from above the wound body, and the battery lid 1411 is crimped and sealed in the battery can 1404 to obtain a lithium ion secondary battery.

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

Abstract

L'invention concerne un matériau actif d'électrode négative pour batteries rechargeables au lithium-ion, qui permet la production d'une batterie rechargeable au lithium-ion ayant une grande capacité. Le matériau actif d'électrode négative pour batteries rechargeables au lithium-ion comprend une base et des nanoparticules de silicium formées sur la surface de la base. La base comprend une base pour formation de couche de carbone amorphe et une couche de carbone amorphe qui est formée sur la surface de la base pour formation de couche de carbone amorphe. La base pour formation de couche de carbone amorphe est constituée d'un matériau actif qui est apte à absorber et à désorber des ions lithium. Les nanoparticules de silicium sont liées à la base de carbone par l'intermédiaire de la couche de carbone amorphe.
PCT/JP2014/064366 2014-05-30 2014-05-30 Matériau actif d'électrode négative pour batteries rechargeables au lithium-ion, et batterie rechargeable au lithium-ion WO2015181940A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004146292A (ja) * 2002-10-28 2004-05-20 Japan Storage Battery Co Ltd 非水電解質二次電池
JP2006504234A (ja) * 2002-10-23 2006-02-02 イドロ−ケベック グラファイトを基材とし、少なくとも一層の連続層または不連続層で被覆された核を含む粒子、それらの製法及び使用
JP2009181767A (ja) * 2008-01-30 2009-08-13 Tokai Carbon Co Ltd リチウム二次電池の負極材用複合炭素材料及びその製造方法
JP2012099452A (ja) * 2010-11-04 2012-05-24 Samsung Sdi Co Ltd ２次電池用負極活物質およびこれを含むリチウム２次電池
JP2013084601A (ja) * 2011-10-05 2013-05-09 Samsung Sdi Co Ltd 負極活物質及び該物質を採用したリチウム電池
JP2014067639A (ja) * 2012-09-26 2014-04-17 Mitsubishi Chemicals Corp 非水系二次電池用炭素材料、非水系二次電池用負極及び非水系二次電池

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006504234A (ja) * 2002-10-23 2006-02-02 イドロ−ケベック グラファイトを基材とし、少なくとも一層の連続層または不連続層で被覆された核を含む粒子、それらの製法及び使用
JP2004146292A (ja) * 2002-10-28 2004-05-20 Japan Storage Battery Co Ltd 非水電解質二次電池
JP2009181767A (ja) * 2008-01-30 2009-08-13 Tokai Carbon Co Ltd リチウム二次電池の負極材用複合炭素材料及びその製造方法
JP2012099452A (ja) * 2010-11-04 2012-05-24 Samsung Sdi Co Ltd ２次電池用負極活物質およびこれを含むリチウム２次電池
JP2013084601A (ja) * 2011-10-05 2013-05-09 Samsung Sdi Co Ltd 負極活物質及び該物質を採用したリチウム電池
JP2014067639A (ja) * 2012-09-26 2014-04-17 Mitsubishi Chemicals Corp 非水系二次電池用炭素材料、非水系二次電池用負極及び非水系二次電池

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