WO2015098024A1 - 非水電解質二次電池用負極活物質及びその負極活物質を用いた非水電解質二次電池 - Google Patents

非水電解質二次電池用負極活物質及びその負極活物質を用いた非水電解質二次電池 Download PDF

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WO2015098024A1
WO2015098024A1 PCT/JP2014/006198 JP2014006198W WO2015098024A1 WO 2015098024 A1 WO2015098024 A1 WO 2015098024A1 JP 2014006198 W JP2014006198 W JP 2014006198W WO 2015098024 A1 WO2015098024 A1 WO 2015098024A1
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negative electrode
electrode active
sio
active material
electrolyte secondary
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PCT/JP2014/006198
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English (en)
French (fr)
Japanese (ja)
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達哉 明楽
博之 南
泰三 砂野
善雄 加藤
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三洋電機株式会社
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Priority to JP2015554530A priority Critical patent/JPWO2015098024A1/ja
Priority to CN201480071109.2A priority patent/CN105849948B/zh
Publication of WO2015098024A1 publication Critical patent/WO2015098024A1/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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 non-aqueous electrolyte secondary battery and a non-aqueous electrolyte secondary battery using the negative electrode active material.
  • SiO X Since silicon oxide represented by silicon (Si) and SiO 2 X has a higher capacity per unit volume than carbon materials such as graphite, application to a negative electrode active material is being studied. In particular, SiO X is expected to be put to practical use at an early stage because the volume expansion rate when Li is occluded during charging is smaller than that of Si.
  • Patent Document 1 discloses SiO X in which a carbon coating film is formed on the surface.
  • the non-aqueous electrolyte secondary battery using SiO X or the like as the negative electrode active material has a problem that the initial charge / discharge efficiency is poor and the capacity is greatly reduced at the beginning of the cycle as compared with the case where graphite is used as the negative electrode active material. There is.
  • the main cause of the above problem is that the volume change of SiO X or the like during charge / discharge is larger than that of graphite.
  • a large volume change of the active material is considered to cause, for example, a decrease in conductivity of the active material layer, leading to deterioration of the initial charge / discharge efficiency.
  • a negative electrode active material for a non-aqueous electrolyte secondary battery is a particulate negative electrode active material used for a non-aqueous electrolyte secondary battery, and SiO X (0.5 ⁇ X ⁇ 1.5), a carbon coating layer covering at least a part of the surface of the mother particle, and amorphous carbon particles fixed on the carbon coating layer.
  • a non-aqueous electrolyte secondary battery includes a negative electrode including the negative electrode active material, a positive electrode, a separator disposed between the positive electrode and the negative electrode, and a non-aqueous electrolyte. .
  • cycle characteristics and initial charge / discharge efficiency can be improved in a nonaqueous electrolyte secondary battery using SiO X as a negative electrode active material.
  • FIG. 3 is a first electron microscope image showing a cross section of negative electrode active material particles used in Experiment 1.
  • FIG. 3 is a second electron microscope image showing a cross section of the negative electrode active material particles used in Experiment 1.
  • FIG. 8 is a figure which shows the laser Raman spectroscopic analysis result of the negative electrode active material particle used in Experiment 1.
  • a nonaqueous electrolyte secondary battery which is an example of an embodiment of the present invention includes a positive electrode including a positive electrode active material, a negative electrode including a negative electrode active material, a nonaqueous electrolyte including a nonaqueous solvent, and a separator.
  • a positive electrode including a positive electrode active material a positive electrode active material
  • a negative electrode including a negative electrode active material a nonaqueous electrolyte including a nonaqueous solvent
  • separator As an example of the non-aqueous electrolyte secondary battery, there is a structure in which an electrode body in which a positive electrode and a negative electrode are wound via a separator and a non-aqueous electrolyte are accommodated in an exterior body.
  • the positive electrode is preferably composed of a positive electrode current collector and a positive electrode active material layer formed on the positive electrode current collector.
  • a positive electrode current collector for example, a conductive thin film, particularly a metal foil or alloy foil that is stable in the potential range of the positive electrode such as aluminum, or a film having a metal surface layer such as aluminum is used.
  • the positive electrode active material layer preferably contains a conductive material and a binder in addition to the positive electrode active material.
  • the positive electrode active material is not particularly limited, but is preferably a lithium-containing transition metal oxide.
  • the lithium-containing transition metal oxide may contain non-transition metal elements such as Mg and Al. Specific examples include lithium-containing transition metal oxides such as lithium cobaltate, olivine-type lithium phosphate represented by lithium iron phosphate, Ni—Co—Mn, Ni—Mn—Al, and Ni—Co—Al. It is done. These positive electrode active materials may be used alone or in combination of two or more.
  • carbon materials such as carbon black, acetylene black, ketjen black, graphite, and a mixture of two or more thereof can be used.
  • binder polytetrafluoroethylene, polyvinylidene fluoride, polyvinyl acetate, polyacrylonitrile, polyvinyl alcohol, and a mixture of two or more thereof can be used.
  • the negative electrode 10 preferably includes a negative electrode current collector 11 and a negative electrode active material layer 12 formed on the negative electrode current collector 11.
  • a conductive thin film particularly a metal foil or alloy foil that is stable in the potential range of the negative electrode such as copper, or a film having a metal surface layer such as copper is used.
  • the negative electrode active material layer 12 preferably contains a binder (not shown) in addition to the negative electrode active material 13.
  • a binder polytetrafluoroethylene or the like can be used as in the case of the positive electrode, but styrene-butadiene rubber (SBR), polyimide, or the like is preferably used.
  • SBR styrene-butadiene rubber
  • the binder may be used in combination with a thickener such as carboxymethylcellulose.
  • the negative electrode active material 13 includes a base particle 14 made of SiO X (0.5 ⁇ X ⁇ 1.5) and a carbon coating covering at least a part of the surface of the base particle 14.
  • a negative electrode active material 13 a having a layer 15 and amorphous carbon particles 16 fixed to the surface of the carbon coating layer 15 is used.
  • the negative electrode active material 13a may be used alone, but from the viewpoint of achieving both high capacity and improved cycle characteristics, the volume change due to charge / discharge is smaller than that of the negative electrode active material 13a. It is preferable to use a mixture with the substance 13b.
  • the negative electrode active material 13b is not particularly limited, but is preferably a carbon-based active material such as graphite or hard carbon.
  • the ratio of the negative electrode active material 13a to graphite is 1:99 to 20:80 by mass ratio. preferable. If the mass ratio is within the range, it is easy to achieve both higher capacity and improved cycle characteristics. On the other hand, when the ratio of the negative electrode active material 13a to the total mass of the negative electrode active material 13 is lower than 1% by mass, the merit of increasing the capacity by adding the negative electrode active material 13a is reduced.
  • the carbon coating layer 15 is formed on the surface of the base particles 14 made of SiO X (0.5 ⁇ X ⁇ 1.5), and the amorphous carbon particles are further formed on the surface of the carbon coating layer 15. 16 is fixed (hereinafter referred to as “negative electrode active material particles 13a”).
  • SiO X has a structure in which Si is dispersed in an amorphous SiO 2 matrix. When observed with a transmission electron microscope (TEM), the presence of dispersed Si can be confirmed.
  • the carbon coating layer 15 on the surface of the base particles 14 can improve the defect of SiO X having a low electron conductivity.
  • the amorphous carbon particles 16 fixed to the surface of 15 improve the binding force between SiO X and the binder by the anchor effect.
  • the particles fixed to the surface of the carbon coating layer 15 are amorphous carbon particles, the initial charge / discharge efficiency and the cycle characteristics are particularly improved. The reason is as follows. When carbon having high crystallinity as typified by graphite and metal fine particles are fixed to the surface of SiO X , processes such as high temperature treatment and electroless plating are required.
  • the fact that the amorphous carbon 16 is fixed to the surface of the carbon coating layer 15 means that the amorphous carbon 16 remains on the surface of the carbon coating layer 15 even when mixed with a solvent or the like when the negative electrode is manufactured. It is attached and is different from secondary aggregation.
  • the average particle diameter of the mother particles 14 is preferably 1 to 15 ⁇ m, and more preferably 4 to 10 ⁇ m.
  • the “average particle diameter” means a particle diameter (volume average particle diameter; Dv 50 ) at which the volume integrated value becomes 50% in the particle size distribution measured by the laser diffraction scattering method. Dv 50 can be measured, for example, using “LA-750” manufactured by HORIBA.
  • Dv 50 can be measured, for example, using “LA-750” manufactured by HORIBA.
  • the average particle diameter of the mother particle 14 becomes too small, the particle surface area becomes too large, the reaction amount with the electrolytic solution becomes large, and the capacity may be reduced.
  • the average particle size becomes too large, the effect of volumetric expansion of SiO X during charging increases, and the charge / discharge characteristics may deteriorate.
  • the average particle diameter of the amorphous carbon particles 16 is preferably 0.01 ⁇ m or more and 1 ⁇ m or less, and more preferably 0.05 to 0.8 ⁇ m. If the average particle diameter of the amorphous carbon particles 16 becomes too small, the unevenness on the surface of the carbon coating layer 15 on the base particles 14 becomes small, and the anchor effect tends to be insufficient. On the other hand, if the average particle size becomes too large, the number of amorphous carbon particles 16 fixed on the carbon coating layer 15 is limited, and the anchor effect tends to be insufficient.
  • the amorphous carbon particles 16 are greater than 0% by mass and 15% by mass or less, more preferably 2% by mass or more and 8% by mass or less with respect to the mother particle 14. If the amount of the amorphous carbon particles 16 is too small relative to the base particles 14, the unevenness formed on the surface of the carbon coating layer 15 on the base particles 14 is reduced, and a sufficient anchor effect tends not to be obtained. On the other hand, if the amount is too large, the amount of amorphous carbon occupied in the active material increases, and the capacity tends to decrease.
  • carbon black As the carbon material in the carbon coating layer 15, carbon black, acetylene black, ketjen black, graphite, and a mixture of two or more thereof can be used as in the conductive material of the positive electrode active material layer.
  • the carbon coating layer 15 covers 50% or more and 100% or less, preferably 100%, of the surface of the mother particle 14.
  • the surface of the mother particle 14 is covered with the carbon coating layer 15 when the surface of the mother particle 14 is at least 1 nm thick when the particle cross section is observed by SEM. It is covered.
  • the average thickness of the carbon coating layer 15 is preferably 1 to 200 nm and more preferably 5 to 100 nm in consideration of ensuring conductivity and diffusibility of Li + into SiO X or the like as the mother particle 14. Moreover, it is suitable for the coating layer 15 to have a substantially uniform thickness over the whole area.
  • the average thickness of the carbon coating layer 15 can be measured by cross-sectional observation of the negative electrode active material particles 13a using a scanning electron microscope (SEM), a transmission electron microscope (TEM), or the like.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • the ratio of the carbon coating layer to SiO X is desirably 10% by mass or less.
  • the carbon coating layer 15 can be formed by using a general method such as a CVD method, a sputtering method, or a plating method (electrolytic / electroless plating).
  • a general method such as a CVD method, a sputtering method, or a plating method (electrolytic / electroless plating).
  • the coating layer 15 made of a carbon material is formed on the surface of the SiO X particles by the CVD method, for example, the SiO x particles and the hydrocarbon gas are heated in the gas phase, and the hydrocarbon gas is thermally decomposed. The resulting carbon is deposited on the SiO X particles.
  • the hydrocarbon gas methane gas or acetylene gas can be used.
  • the negative electrode active material 13a preferably has a BET specific surface area of 1 to 30 m 2 / g, more preferably 5 to 30 m 2 / g. If the BET specific surface area becomes too small, the unevenness of the SiO X particles is not sufficiently formed, and a sufficient anchor effect tends not to be obtained. On the other hand, when the BET specific surface area becomes too large, the amount of the binder adhering to the SiO X surface becomes too large, and the dispersibility of the binder is lowered, and the negative electrode adhesion tends to be lowered.
  • an aqueous solution containing an organic acid catalyst and SiO X particles including the carbon coating layer are mixed, and then hydrolyzed and polymerized at 80 to 120 ° C. After the reaction, water can be evaporated and heat treatment can be performed at 500 to 800 ° C.
  • a lithium compound may be mixed.
  • the organic acid catalyst include citric acid, malic acid, tartaric acid, lactic acid, and glycolic acid.
  • the lithium compound include LiOH, Li 2 CO 3 , LiF, and LiCl.
  • SiO X constituting the mother particle 14 may contain lithium silicate (Li 4 SiO 4 , Li 2 SiO 3 , Li 2 Si 2 O 5 , Li 8 SiO 6, etc.) in the particle.
  • lithium silicate Li 4 SiO 4 , Li 2 SiO 3 , Li 2 Si 2 O 5 , Li 8 SiO 6, etc.
  • Non-aqueous electrolyte examples include LiClO 4 , LiBF 4 , LiPF 6 , LiAlCl 4 , LiSbF 6 , LiSCN, LiCF 3 SO 3 , LiCF 3 CO 2 , LiAsF 6 , LiB 10 Cl 10 , lower aliphatic carboxylic acid.
  • Lithium, LiCl, LiBr, LiI, chloroborane lithium, borates, imide salts, and the like can be used.
  • LiPF 6 is preferably used from the viewpoints of ion conductivity and electrochemical stability.
  • One electrolyte salt may be used alone, or two or more electrolyte salts may be used in combination. These electrolyte salts are preferably contained at a ratio of 0.8 to 1.5 mol with respect to 1 L of the nonaqueous electrolyte.
  • non-aqueous electrolyte solvent for example, a cyclic carbonate, a chain carbonate, a cyclic carboxylic acid ester or the like is used.
  • cyclic carbonate examples include propylene carbonate (PC) and ethylene carbonate (EC).
  • chain carbonate examples include diethyl carbonate (DEC), ethyl methyl carbonate (EMC), and dimethyl carbonate (DMC).
  • DEC diethyl carbonate
  • EMC ethyl methyl carbonate
  • DMC dimethyl carbonate
  • examples of the cyclic carboxylic acid ester include ⁇ -butyrolactone (GBL) and ⁇ -valerolactone (GVL).
  • a non-aqueous solvent may be used individually by 1 type, and may be used in combination of 2 or more type.
  • separator a porous sheet having ion permeability and insulating properties is used.
  • the porous sheet include a microporous thin film, a woven fabric, and a nonwoven fabric.
  • material of the separator polyolefin such as polyethylene and polypropylene is suitable.
  • the ratio of the carbon film having a film thickness of 1 nm or more on the surface of each SiO X particle was calculated from the ratio of the sum of the interface lengths of the carbon film having a film thickness of 1 nm or more and SiO X to the outer peripheral length of SiO X in the particle cross section .
  • the average value of the ratio of the carbon coating on the surface of 30 SiO X particles was calculated as the carbon coverage.
  • FIG. 4 shows an SEM image obtained by atomizing and dispersing SiO X particles after heat treatment and water washing in a solvent using TK fill mix (manufactured by PRIMIX Corporation). Since SiO X whose surface is coated with amorphous carbon has been atomized and dispersed, the amorphous carbon exists on the surface of the coated carbon film. It was judged that it was fixed on the surface of the coated carbon film, not secondary aggregation or simple adhesion.
  • FIG. 5 shows a laser Raman spectroscopic analysis of carbonaceous matter (hereinafter referred to as ⁇ ) on the surface of the SiO X particles after heat treatment and water washing, measured using a Raman spectroscope ARAMIS (manufactured by Shimadzu Corporation). A Raman spectrum considered to be a mixed system of two or more species was observed.
  • ⁇ a laser Raman spectroscopic analysis of carbonaceous matter
  • ARAMIS manufactured by Shimadzu Corporation
  • FIGS. 5 to 7 the saddle between the G-band and D-band intensity of the (minimum) is defined as I V, compares the I V / I G value for alpha, the spectral interpretation went. Smoothing was performed as appropriate, and the base line was linearly approximated at 800 to 1900 cm ⁇ 1 .
  • FIG. 8 shows a graph of each I V / I G value.
  • FIG. 8 shows that ⁇ is made of a mixed component of ⁇ and ⁇ . Therefore, it was confirmed that the carbon fixed on the SiO X whose surface was coated with carbon was amorphous carbon having low crystallinity.
  • SiO X and PAN polyacrylonitrile
  • NMP N-methyl-2-pyrrolidone
  • This was stirred using a mixer (Primics, Robomix) to prepare a negative electrode mixture slurry.
  • the negative electrode mixture slurry was applied on one surface of a copper foil such that the mass per lm 2 of the negative electrode mixture layer was 25 g / m 2 .
  • this was dried at 105 ° C. in the atmosphere and rolled to prepare a negative electrode.
  • the filling density of the negative electrode mixture layer was 1.50 g / ml.
  • an electrode body was produced using the above negative electrode with a Ni tab attached to the outer periphery, a lithium metal foil, and a polyethylene separator disposed between the negative electrode and the lithium metal foil.
  • This electrode body was put in a battery casing made of aluminum laminate, and a non-aqueous electrolyte was injected into the battery casing, and then the battery casing was sealed to prepare a battery A1.
  • Example 2 A battery A2 was produced in the same manner as in Experiment 1 except that the amount of citric acid added was 0.18 mol.
  • Example 3 Battery A2 was produced in the same manner as in Experiment 1 except that the amount of citric acid added was 0.25 mol.
  • Example 4 Similar to Experiment 1 above, except that untreated SiO X was used as SiO X as the negative electrode active material (that is, SiO X having no amorphous carbon particles on the carbon coating was used). Battery Z was produced. A BET specific surface area of the SiO X particles was measured using a TriStar II3020, it was 5m 2 / g. A cross-sectional SEM image of the SiO X particles is shown in FIG. The small particles in FIG. 9 are highly crystalline carbon particles, which remain without forming a layer when the carbon coating layer 15 is formed.
  • the amorphous carbon particles are not formed on the carbon coating film on the surface of the SiO X particles, a sufficient anchor effect cannot be obtained between the active material particles and the binder, and the adhesion between the active materials is low. It is thought that it fell.
  • the carbon coating film is formed on the surface of the SiO X particles, and the amorphous carbon particles are fixed on the carbon coating film, so that anchors are provided between the active material particles and the binder. It is considered that sufficient unevenness was obtained on the particle surface to obtain the effect, and the adhesion between the active materials was improved.

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PCT/JP2014/006198 2013-12-25 2014-12-12 非水電解質二次電池用負極活物質及びその負極活物質を用いた非水電解質二次電池 WO2015098024A1 (ja)

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CN201480071109.2A CN105849948B (zh) 2013-12-25 2014-12-12 非水电解质二次电池用负极活性物质以及使用该负极活性物质的非水电解质二次电池

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WO2016035274A1 (ja) * 2014-09-01 2016-03-10 三洋電機株式会社 非水電解質二次電池用負極活物質
WO2017085908A1 (ja) * 2015-11-18 2017-05-26 信越化学工業株式会社 負極活物質、混合負極活物質材料、非水電解質二次電池用負極、リチウムイオン二次電池、負極活物質の製造方法、及びリチウムイオン二次電池の製造方法
JP2017168406A (ja) * 2016-03-18 2017-09-21 信越化学工業株式会社 非水電解質二次電池負極活物質、負極及び電池の製造方法
CN108463910A (zh) * 2016-01-07 2018-08-28 信越化学工业株式会社 负极活性物质及其制造方法、非水电解质二次电池用负极、锂离子二次电池及其制造方法
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US11075369B2 (en) 2015-09-24 2021-07-27 Lg Chem, Ltd. Negative electrode active material for lithium secondary battery and method of preparing the same
WO2017085908A1 (ja) * 2015-11-18 2017-05-26 信越化学工業株式会社 負極活物質、混合負極活物質材料、非水電解質二次電池用負極、リチウムイオン二次電池、負極活物質の製造方法、及びリチウムイオン二次電池の製造方法
JP2017097955A (ja) * 2015-11-18 2017-06-01 信越化学工業株式会社 負極活物質、混合負極活物質材料、非水電解質二次電池用負極、リチウムイオン二次電池、負極活物質の製造方法、及びリチウムイオン二次電池の製造方法
US11430980B2 (en) 2015-11-18 2022-08-30 Shin-Etsu Chemical Co., Ltd. Negative electrode active material, mixed negative electrode active material, negative electrode for nonaqueous electrolyte secondary battery, lithium ion secondary battery, production method of negative electrode active material, and production method of lithium ion secondary battery
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JP2017168406A (ja) * 2016-03-18 2017-09-21 信越化学工業株式会社 非水電解質二次電池負極活物質、負極及び電池の製造方法
WO2020262436A1 (ja) * 2019-06-28 2020-12-30 三洋電機株式会社 二次電池用負極活物質、及び二次電池

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