WO2020184125A1 - 非水電解質蓄電素子及び蓄電装置 - Google Patents

非水電解質蓄電素子及び蓄電装置 Download PDF

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WO2020184125A1
WO2020184125A1 PCT/JP2020/006687 JP2020006687W WO2020184125A1 WO 2020184125 A1 WO2020184125 A1 WO 2020184125A1 JP 2020006687 W JP2020006687 W JP 2020006687W WO 2020184125 A1 WO2020184125 A1 WO 2020184125A1
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negative electrode
active material
electrode active
aqueous electrolyte
power storage
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French (fr)
Japanese (ja)
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理史 ▲高▼野
健太 上平
智典 加古
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GS Yuasa International Ltd
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GS Yuasa International Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/44—Methods for charging or discharging
    • 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
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • 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 non-aqueous electrolyte power storage element and a power storage device.
  • Non-aqueous electrolyte secondary batteries represented by lithium ion secondary batteries are widely used in electronic devices such as personal computers and communication terminals, automobiles, etc. due to their high energy density.
  • the non-aqueous electrolyte secondary battery generally has a pair of electrodes electrically separated by a separator and a non-aqueous electrolyte interposed between the electrodes, and transfers ions between the two electrodes. It is configured to charge and discharge.
  • capacitors such as lithium ion capacitors and electric double layer capacitors are also widely used as non-aqueous electrolyte power storage elements other than non-aqueous electrolyte secondary batteries.
  • the positive electrode and the negative electrode of such a non-aqueous electrolyte power storage element usually have a layer structure in which an active material layer is laminated on a conductive base material.
  • aluminum is generally used as the positive electrode base material and copper is generally used as the negative electrode base material because it does not corrode with respect to the potentials of the positive electrode and the negative electrode.
  • it has been studied to use aluminum as a negative electrode base material, which is more flexible, easier to handle, and less costly than copper.
  • 0.1V vs It is known that the alloying reaction of aluminum and lithium occurs at a low potential near Li / Li + .
  • the present invention has been made based on the above circumstances, and an object of the present invention is to suppress alloying of aluminum as a negative electrode base material with lithium even when charged at a high rate at a high temperature. It is an object of the present invention to provide a non-aqueous electrolyte storage element capable of producing a non-aqueous electrolyte storage element, and a power storage device including such a non-aqueous electrolyte storage element.
  • the non-aqueous electrolyte power storage element made to solve the above problems includes a negative electrode base material made of aluminum and a negative electrode active material layer laminated on the negative electrode base material and containing non-graphicular carbon. It is a non-aqueous electrolyte power storage element having a negative electrode having a negative electrode and a non-aqueous electrolyte containing a lithium salt, and having a density of the negative electrode active material layer of 0.9 g / cm 3 or more and 1.2 g / cm 3 or less.
  • the power storage device is a power storage device including the non-aqueous electrolyte power storage element and a control unit that controls charging of the non-water electrolyte power storage element with a current amount in a range including 3C or more. ..
  • a non-aqueous electrolyte storage element capable of suppressing alloying of aluminum as a negative electrode base material with lithium even when charged at a high rate at a high temperature, and such a non-aqueous electrolyte storage element.
  • a power storage device including an element can be provided.
  • FIG. 1 is a schematic view showing a power storage device according to an embodiment of the present invention and a state in which the power storage device is mounted on a vehicle.
  • FIG. 2 is an external perspective view showing a non-aqueous electrolyte secondary battery according to an embodiment of the non-aqueous electrolyte power storage device of the present invention.
  • FIG. 3 is a graph showing the negative electrode potentials of the batteries of Examples and Comparative Examples in a fully charged state.
  • FIG. 4 is a linear sweep voltammogram of aluminum foil measured in an experimental example.
  • the non-aqueous electrolyte power storage element comprises a negative electrode base material made of aluminum, a negative electrode laminated on the negative electrode base material and having a negative electrode active material layer containing non-graphicular carbon, and a lithium salt. It is a non-aqueous electrolyte power storage element that comprises a non-aqueous electrolyte and has a density of the negative electrode active material layer of 0.9 g / cm 3 or more and 1.2 g / cm 3 or less.
  • the non-aqueous electrolyte power storage element has the above configuration, it is possible to suppress alloying of aluminum as a negative electrode base material with lithium even when charged at a high rate at a high temperature.
  • the reason for this is not clear, but the following is presumed.
  • the density of the negative electrode active material layer is less than 0.9 g / cm 3 , the contact between the non-graphitic carbons which are the negative electrode active materials and the contact between the non-graphitable carbon and the negative electrode base material are insufficient, and the resistance The increase increases the overvoltage.
  • the density of the negative electrode active material layer exceeds 1.2 g / cm 3 , it is difficult for the non-aqueous electrolyte to sufficiently penetrate into the negative electrode active material layer, and the overvoltage becomes large due to the lack of the non-aqueous electrolyte inside the negative electrode active material layer. Become. In particular, when charging at a high rate, the overvoltage tends to increase. When the overvoltage becomes large in this way, the negative electrode potential tends to fall below the alloying potential in a state close to full charge.
  • the density of the negative electrode active material layer is 0.9 g / cm 3 or more and 1.2 g / cm 3 or less, so that it is high at high temperature. Even if the battery is charged at a rate, the negative electrode potential is unlikely to fall below the alloying potential, and it is presumed that alloying with lithium is suppressed. As described above, according to the non-aqueous electrolyte storage element, the alloying of aluminum of the negative electrode base material with lithium is suppressed, so that the performance deterioration of the non-aqueous electrolyte storage element can be suppressed.
  • the "aluminum negative electrode base material” means that the material of the negative electrode base material is pure aluminum or an aluminum alloy.
  • non-graphitic carbon refers to a carbon material having an average lattice spacing (d 002 ) of the (002) plane measured by a wide-angle X-ray diffraction method before charging / discharging or in a discharged state of 0.340 nm or more.
  • the “discharged state” here means that the open circuit voltage is 0.7 V or more in a unipolar battery using a negative electrode containing a carbon material as a negative electrode active material as a working electrode and metallic lithium as a counter electrode. To say.
  • the open circuit voltage is substantially the same as the potential of the negative electrode containing the carbon material with respect to the oxidation-reduction potential of lithium.
  • the open circuit voltage is 0.7 V or more
  • the potential of the negative electrode is 0.7 V (vs. Li / Li + ) or more
  • the carbon material which is the negative electrode active material can be stored and discharged by charging and discharging. It means that sufficient lithium ions are released.
  • the "density" of the negative electrode active material layer means a value obtained by dividing the mass of the negative electrode active material layer by the apparent volume of the negative electrode active material layer.
  • the apparent volume refers to the volume including the void portion, and can be obtained as the product of the average thickness and the area of the negative electrode active material layer.
  • the negative electrode further has a conductive layer provided between the negative electrode base material and the negative electrode active material layer, and the conductive layer is a region on the negative electrode base material on which the negative electrode active material layer is laminated. It is preferable to cover the whole.
  • the density of the negative electrode active material layer is preferably 1.0 g / cm 3 or more and 1.1 g / cm 3 or less.
  • the negative electrode potential at the upper limit voltage of the non-aqueous electrolyte power storage element is 0.3 V vs. It is preferably Li / Li + or more.
  • the negative electrode potential at the upper limit voltage is 0.3 V vs.
  • the "upper limit voltage for use” means the highest voltage if there is a description of the working voltage range in the instruction manual of the non-aqueous electrolyte power storage element. If there is no instruction manual or the like, it means a voltage value controlled so as not to rise further by a control device or the like of a non-aqueous electrolyte power storage element. Further, in the method of confirming the "negative electrode potential at the upper limit voltage for use", first, in the non-aqueous electrolyte power storage element, the amount of electricity to be charged when the upper limit voltage for use is set from the state of the predetermined voltage scheduled to be disassembled is specified.
  • the non-aqueous electrolyte power storage element is disassembled under a predetermined voltage state, the specified charging electricity amount is charged by a unipolar test using the disassembled negative electrode, and the open circuit potential after charging is measured. Determine the negative electrode potential at the upper limit voltage.
  • the non-aqueous electrolyte storage element is preferably for a power source having a function of being charged by regenerative energy. Since a power source having a function of being charged by regenerative energy, such as a power source for a hybrid electric vehicle, is charged at a high rate, alloying with lithium is likely to occur when aluminum is used as a negative electrode base material. Therefore, even if the negative electrode base material is charged at a high rate, the non-aqueous electrolyte power storage element capable of suppressing the alloying of aluminum of the negative electrode base material with lithium has a function of being charged by such regenerative energy. When used as a power source, it has great advantages.
  • the power storage device is a power storage device including the non-aqueous electrolyte power storage element and a control unit that controls charging of the non-water electrolyte power storage element with a current amount in a range including 3C or more. Since the power storage device includes the non-aqueous electrolyte power storage element according to the embodiment of the present invention, the negative electrode base material can be alloyed with lithium of aluminum even when charging is performed at a high rate of 3C or more. It can be suppressed. Therefore, the power storage device can suppress the deterioration of the performance of the power storage device even if the power storage device is repeatedly charged at a high rate.
  • 1C is a current value at which the amount of electricity when the non-aqueous electrolyte storage element is energized with a constant current for 1 hour is the same as the nominal capacity of the non-aqueous electrolyte storage element, and is "3C". Is a current value three times that value.
  • the non-aqueous electrolyte power storage element has a positive electrode, a negative electrode, and a non-aqueous electrolyte.
  • a non-aqueous electrolyte secondary battery will be described as an example of the non-aqueous electrolyte power storage element.
  • the positive electrode and the negative electrode usually form electrode bodies that are alternately superposed by stacking or winding through a separator.
  • the electrode body is housed in a battery container, and the non-aqueous electrolyte is filled in the battery container.
  • the non-aqueous electrolyte is interposed between the positive electrode and the negative electrode.
  • the battery container a known metal battery container, resin battery container, or the like that is usually used as a battery container for a non-aqueous electrolyte secondary battery can be used.
  • the positive electrode has a positive electrode base material and a positive electrode active material layer arranged directly on the positive electrode base material or via an intermediate layer such as a conductive layer.
  • the positive electrode base material has conductivity.
  • conductive means that the volume resistivity is measured according to JIS-H-0505 (1975 years) is not more than 10 7 ⁇ ⁇ cm, and "non-conductive” means that the volume resistivity is 10 7 ⁇ ⁇ cm greater.
  • metals such as aluminum, titanium, tantalum, and stainless steel or alloys thereof are used. Among these, aluminum and aluminum alloys are preferable from the viewpoint of balance of potential resistance, high conductivity and cost.
  • examples of the form of forming the positive electrode base material include foil, a vapor-deposited film, and the like, and foil is preferable from the viewpoint of cost. That is, aluminum foil and aluminum alloy foil are preferable as the positive electrode base material. Examples of aluminum or aluminum alloy include A1085, A1N30, and A3003 specified in JIS-H-4000 (2014).
  • the positive electrode active material layer contains a positive electrode active material.
  • the positive electrode active material layer is usually formed from a so-called positive electrode mixture containing a positive electrode active material.
  • the positive electrode active material layer contains optional components such as a conductive agent, a binder (binder), a thickener, and a filler, if necessary.
  • Examples of the positive electrode active material include composite oxides represented by Li x MO y (M represents at least one kind of transition metal) (Li x CoO 2 having a layered ⁇ -NaFeO type 2 crystal structure, Li x NiO 2). , Li x MnO 3 , Li x Ni ⁇ Co ⁇ Mn (1- ⁇ - ⁇ ) O 2, etc., Li x Mn 2 O 4 , Li x Ni ⁇ Mn (2- ⁇ ) O 4, etc. with spinel type crystal structure, etc.
  • Li x MO y M represents at least one kind of transition metal
  • Li w Me x (XO y ) z (Me represents at least one kind of transition metal, X represents, for example, P, Si, B, V, etc.)
  • Polyanion compounds LiFePO 4 , LiMnPO 4 , LiNiPO) 4 , LiCoPO 4 , Li 3 V 2 (PO 4 ) 3 , Li 2 MnSiO 4 , Li 2 CoPO 4 F, etc.).
  • the elements or polyanions in these compounds may be partially substituted with other elements or anion species.
  • one of these compounds may be used alone, or two or more of these compounds may be mixed and used.
  • Li x Ni ⁇ Co ⁇ Mn (1- ⁇ - ⁇ ) O 2 having a layered ⁇ -NaFeO type 2 crystal structure and containing at least Ni, Co, and Mn.
  • examples thereof include a lithium transition metal composite oxide represented by.
  • x is more than 0 and 1.3 or less, and may be 1.
  • ⁇ and ⁇ are each more than 0, and the sum of ⁇ and ⁇ is less than 1.
  • ⁇ , ⁇ and (1- ⁇ - ⁇ ) may be, for example, 0.1 or more and 0.8 or less, and may be 0.3 or more and 0.5 or less, respectively.
  • lithium transition metal composite oxide examples include LiNi 1/3 Co 1/3 Mn 1/3 O 2 , LiNi 3/5 Co 1/5 Mn 1/5 O 2 , and LiNi 1/2 Co 1/5 Mn. Examples thereof include 3/10 O 2 , LiNi 1/2 Co 3/10 Mn 1/5 O 2 , LiNi 8/10 Co 1/10 Mn 1/10 O 2 .
  • the lower limit of the content of the positive electrode active material in the positive electrode active material layer is preferably 70% by mass, more preferably 80% by mass.
  • the upper limit of this content for example, 99% by mass is preferable, and 95% by mass is more preferable.
  • the content (grain amount) of the positive electrode active material per unit area in the positive electrode active material layer is, for example, 3 mg / cm 2 or more and 20 mg / cm 2 or less.
  • the content (weighting amount) per unit area of the positive electrode active material is the amount in one layer laminated on one surface of the positive electrode base material. The same applies to the content (weight) per unit area of the negative electrode active material described later.
  • the conductive agent is not particularly limited as long as it is a conductive material that does not adversely affect the battery performance.
  • a conductive agent include natural or artificial graphite; carbon black such as furnace black, acetylene black, and Ketjen black; metal; conductive ceramics and the like.
  • the shape of the conductive agent include powder and fibrous.
  • the content of the conductive agent in the positive electrode active material layer can be, for example, 1% by mass or more and 10% by mass or less.
  • binder examples include fluororesins (polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), etc.), thermoplastic resins such as polyethylene, polypropylene, and polyimide; ethylene-propylene-diene rubber (EPDM), sulfonated EPDM, and styrene butadiene. Elastomers such as rubber (SBR) and fluororubber; polysaccharide polymers and the like can be mentioned.
  • the content of the binder in the positive electrode active material layer can be, for example, 1% by mass or more and 10% by mass or less.
  • the thickener examples include polysaccharide polymers such as carboxymethyl cellulose (CMC) and methyl cellulose.
  • CMC carboxymethyl cellulose
  • the content of the thickener in the positive electrode active material layer can be, for example, 0.1% by mass or more and 5% by mass or less.
  • the positive electrode active material layer may not contain a thickener.
  • the filler is not particularly limited as long as it does not adversely affect the battery performance.
  • the main component of the filler include polyolefins such as polypropylene and polyethylene, silica, alumina, zeolite, and glass.
  • the content of the filler in the positive electrode active material layer can be, for example, 0.1% by mass or more and 5% by mass or less.
  • the positive electrode active material layer may not contain a filler.
  • the average thickness of the positive electrode active material layer is, for example, 10 ⁇ m or more and 100 ⁇ m or less.
  • the conductive layer of the positive electrode is a coating layer on the surface of the positive electrode base material, and includes conductive particles such as carbon particles to reduce the contact resistance between the positive electrode base material and the positive electrode active material layer.
  • the positive electrode conductive layer can be formed, for example, by a composition containing a conductive agent used for the positive electrode active material layer and the same as those exemplified as the binder.
  • the negative electrode has a negative electrode base material and a negative electrode active material layer arranged directly on the negative electrode base material or via a conductive layer.
  • the negative electrode base material is made of aluminum. That is, the material of the negative electrode base material is aluminum or an aluminum alloy. The content of aluminum in the negative electrode base material is, for example, 95% by mass or more, preferably 99% by mass or more. An oxide film may be formed on the surface of the negative electrode base material.
  • Aluminum foil and aluminum alloy foil are preferable as the negative electrode base material. Specific examples of the aluminum and the aluminum alloy are the same as those exemplified for the positive electrode base material.
  • the negative electrode active material layer contains non-graphitic carbon that functions as a negative electrode active material.
  • the negative electrode active material layer is usually formed from a so-called negative electrode mixture containing a negative electrode active material.
  • the negative electrode mixture contains optional components such as a conductive agent, a binder, a thickener, and a filler, if necessary.
  • a conductive agent, a binder, a thickener, and a filler the same one as that of the positive electrode active material layer can be used.
  • non-graphitizable carbon contained in the negative electrode active material layer examples include non-graphitizable carbon (hard carbon) and easily graphitizable carbon (soft carbon), and non-graphitizable carbon is preferable.
  • non-graphitizable carbon examples include a calcined phenol resin, a calcined furan resin, and a calcined furfuryl alcohol resin.
  • easily graphitizable carbon examples include coke and pyrolyzable carbon.
  • the non-graphitizable carbon refers to a carbon material having d 002 of 0.36 nm or more and 0.42 nm or less.
  • the non-graphitizable carbon usually has a property that it is difficult to form a graphite structure having three-dimensional stacking regularity among non-graphitizable carbons.
  • the graphitizable carbon refers to a carbon material having d 002 of 0.34 nm or more and less than 0.36 nm.
  • the graphitizable carbon usually has a property that a graphite structure having a three-dimensional stacking regularity can be easily formed among non-graphitizable carbons.
  • the negative electrode active material may further contain a negative electrode active material other than non-graphitic carbon.
  • examples of such other negative electrode active materials include graphite; metals or metalloids such as Si and Sn; metal oxides such as Si oxides and Sn oxides or metalloid oxides; polyphosphate compounds and the like.
  • the lower limit of the content of non-graphitic carbon with respect to the total negative electrode active material is preferably 90% by mass, more preferably 95% by mass, and even more preferably 99% by mass. As described above, by increasing the content of non-graphitic carbon in the negative electrode active material, the negative electrode potential can be easily controlled, and the alloying of aluminum of the negative electrode base material with lithium can be further suppressed.
  • the upper limit of this content may be 100% by mass.
  • the lower limit of the non-graphitable carbon content in the negative electrode active material layer is preferably 80% by mass, more preferably 90% by mass, and even more preferably 95% by mass.
  • the upper limit of this content for example, 99% by mass is preferable, and 98% by mass is more preferable.
  • the content of the conductive agent in the negative electrode active material layer can be, for example, 0.1% by mass or more and 5% by mass or less.
  • the negative electrode active material layer may not contain a conductive agent.
  • the content of the binder in the negative electrode active material layer can be, for example, 0.5% by mass or more and 5% by mass or less.
  • the content of the thickener in the negative electrode active material layer can be, for example, 0.1% by mass or more and 3% by mass or less.
  • the content of the filler in the negative electrode active material layer can be, for example, 0.1% by mass or more and 5% by mass or less.
  • the negative electrode active material layer may not contain a filler.
  • the lower limit of the density of the negative electrode active material layer is 0.9 g / cm 3 , preferably 0.95 g / cm 3 , and more preferably 1.0 g / cm 3 .
  • the upper limit of the density is 1.2 g / cm 3, preferably 1.15 g / cm 3, more preferably 1.1 g / cm 3, more preferably 1.05 g / cm 3.
  • the density of the negative electrode active material layer can be adjusted by, for example, the particle size of non-graphitable carbon, the pressure of the press during molding of the negative electrode active material layer, and the like.
  • the content (grain amount) of the negative electrode active material in the negative electrode active material layer per unit area is, for example, 3 mg / cm 2 or more and 20 mg / cm 2 or less.
  • the average thickness of the negative electrode active material layer is, for example, 30 ⁇ m or more and 200 ⁇ m or less.
  • the conductive layer of the negative electrode (negative electrode conductive layer) is a coating layer on the surface of the negative electrode base material, and is provided between the negative electrode base material and the negative electrode active material layer.
  • the negative electrode conductive layer can reduce the contact resistance between the negative electrode base material and the negative electrode active material layer and suppress the increase in resistance, and as a result, the alloying of aluminum of the negative electrode base material with lithium can be reduced.
  • the negative electrode conductive layer should cover 95% or more of the region on the negative electrode base material on which the negative electrode active material layer is laminated. It is preferable that the entire region on the negative electrode base material on which the negative electrode active material layer is laminated is covered. That is, it is preferable that each component constituting the negative electrode active material layer such as non-graphitic carbon is not in contact with the negative electrode base material.
  • the negative electrode conductive layer can be formed by, for example, a composition containing a conductive agent and a binder.
  • the conductive agent used in the negative electrode conductive layer include those similar to those exemplified as the conductive agent used in the positive electrode active material layer, and carbon particles such as graphite and carbon black are preferable.
  • the content of the conductive agent in the negative electrode conductive layer can be, for example, 20% by mass or more and 60% by mass or less.
  • binder used for the negative electrode conductive layer examples include those exemplified as the binder used for the positive electrode active material layer, and cellulosic binders, chitosan binders and acrylic binders are preferable. These binders are less likely to swell with respect to a non-aqueous electrolyte (non-aqueous electrolyte solution), exhibit good conductivity, and can effectively suppress the alloying of aluminum as a negative electrode base material with lithium. ..
  • the cellulosic binder and the chitosan binder may be a cellulose derivative or a chitosan derivative that has been hydroxyalkylated, carboxyalkylated, sulfate esterified, or the like.
  • examples of the cellulose derivative include carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and the like. These may be salts.
  • Acrylic binders include polyacrylic acid, polymethacrylic acid, polyitaconic acid, poly (meth) acryloyl morpholine, poly N, N-dimethyl (meth) acrylamide, poly N, N-dimethylaminoethyl (meth) acrylate, and poly N. , N-Dimethylaminopropyl (meth) acrylamide, polyglycerin (meth) acrylate and the like.
  • the content of the binder in the negative electrode conductive layer can be, for example, 40% by mass or more and 80% by mass or less.
  • the negative electrode conductive layer may be formed by plating a metal that does not substantially react with lithium.
  • a woven fabric, a non-woven fabric, a porous resin film, or the like As the material of the separator, for example, a woven fabric, a non-woven fabric, a porous resin film, or the like is used. Among these, a porous resin film is preferable from the viewpoint of strength, and a non-woven fabric is preferable from the viewpoint of liquid retention of a non-aqueous electrolyte.
  • a porous resin film is preferable from the viewpoint of strength
  • a non-woven fabric is preferable from the viewpoint of liquid retention of a non-aqueous electrolyte.
  • polyolefins such as polyethylene and polypropylene are preferable from the viewpoint of strength
  • polyimide and aramid are preferable from the viewpoint of oxidative decomposition resistance.
  • a composite separator having a porous resin film and an inorganic porous layer may be used.
  • Non-aqueous electrolytes include lithium salts.
  • the non-aqueous electrolyte is usually a non-aqueous electrolyte solution containing a lithium salt as an electrolyte salt and a non-aqueous solvent for dissolving the electrolyte salt.
  • the non-aqueous electrolyte may be a solid electrolyte or the like.
  • Lithium salts include inorganic lithium salts such as LiPF 6 , LiPO 2 F 2 , LiBF 4 , LiClO 4 , LiN (SO 2 F) 2 , LiSO 3 CF 3 , LiN (SO 2 CF 3 ) 2 , LiN (SO 2). C 2 F 5 ) 2 , LiN (SO 2 CF 3 ) (SO 2 C 4 F 9 ), LiC (SO 2 CF 3 ) 3 , LiC (SO 2 C 2 F 5 ) 3 and other fluorinated hydrocarbon groups Examples thereof include lithium salts having. Among these, an inorganic lithium salt is preferable, and LiPF 6 is more preferable.
  • the upper limit is not particularly limited, but is preferably 2.5 mol / L, more preferably 2 mol / L, and even more preferably 1.5 mol / L.
  • the non-aqueous electrolyte may contain an electrolyte salt other than the lithium salt.
  • an electrolyte salt include sodium salt, potassium salt and the like.
  • the electrolyte salt may be substantially composed of only a lithium salt.
  • the content ratio of the lithium salt in the electrolyte salt is preferably 90 mol% or more, more preferably 99 mol% or more.
  • non-aqueous solvent a known non-aqueous solvent usually used as a non-aqueous solvent for a general non-aqueous electrolyte for a power storage element can be used.
  • the non-aqueous solvent include cyclic carbonates, chain carbonates, esters, ethers, amides, sulfones, lactones, nitriles and the like. Among these, it is preferable to use at least cyclic carbonate or chain carbonate, and it is more preferable to use cyclic carbonate and chain carbonate in combination.
  • the volume ratio of the cyclic carbonate to the chain carbonate is not particularly limited, but is, for example, 5:95 or more and 50:50 or less. Is preferable.
  • cyclic carbonate examples include ethylene carbonate (EC), propylene carbonate (PC), butylene carbonate (BC), vinylene carbonate (VC), vinylethylene carbonate (VEC), chloroethylene carbonate, fluoroethylene carbonate (FEC), and difluoroethylene carbonate.
  • EC ethylene carbonate
  • PC propylene carbonate
  • BC butylene carbonate
  • VC vinylene carbonate
  • VEC vinylethylene carbonate
  • FEC fluoroethylene carbonate
  • difluoroethylene carbonate difluoroethylene carbonate
  • styrene carbonate catechol carbonate
  • 1-phenylvinylene carbonate 1,2-diphenylvinylene carbonate and the like
  • PC is preferable.
  • chain carbonate examples include diethyl carbonate (DEC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), diphenyl carbonate and the like, and among these, EMC is preferable.
  • the negative electrode potential at the upper limit voltage of the non-aqueous electrolyte power storage element is 0.3 V vs. It is preferably Li / Li + or more. With this setting, the negative electrode potential does not easily fall below the alloying potential even when charging at a high temperature, and the alloying of aluminum of the negative electrode base material with lithium can be more sufficiently suppressed.
  • the upper limit of the negative electrode potential at this operating upper limit voltage is not particularly limited, and for example, 0.5 V vs. It may be Li / Li + or less, and 0.4 V vs. It may be Li / Li + or less.
  • the closed circuit potential of the negative electrode at the upper limit voltage of use is 0.3 V vs. It is preferably used under the condition of Li / Li + or more. With this setting, the negative electrode potential does not easily fall below the alloying potential even when charged at a high rate under high temperature, and the alloying of aluminum as the negative electrode base material with lithium is further sufficiently suppressed. Can be done.
  • the upper limit of the closed circuit potential of the negative electrode at this operating upper limit voltage is not particularly limited, and for example, 0.5 V vs. It may be Li / Li + or less, and 0.4 V vs. It may be Li / Li + or less.
  • the negative electrode potential at the upper limit voltage of use can be adjusted by designing the capacitance of the positive electrode and the negative electrode. For example, it can be adjusted by adjusting the type of each active material of the positive electrode and the negative electrode and the ratio of the content (weight of basis weight) of each active material per unit area.
  • the positive electrode active material is a lithium transition metal composite oxide represented by Li x Ni ⁇ Co ⁇ Mn (1- ⁇ - ⁇ ) O 2
  • the negative electrode active material is non-graphitic carbon.
  • the mass ratio (P / N) of the content (P) of the positive electrode active material per unit area in the positive electrode active material layer and the content (N) of the negative electrode active material in the negative electrode active material layer per unit area is 0. It is preferably .75 or more and 1.30 or less, and more preferably 0.80 or more and 1.25 or less.
  • the positive electrode active material is a polyanion compound (LiFePO 4 or the like) and the negative electrode active material is non-graphographic carbon
  • the content (P) of the positive electrode active material per unit area in the positive electrode active material layer and the negative electrode active material layer is preferably 0.68 or more and 1.30 or less, and more preferably 0.80 or more and 1.25 or less.
  • the non-aqueous electrolyte storage element can be used in the same field as the conventional non-aqueous electrolyte storage element, but among them, it can be used as a power source (storage element) having a function of being charged and discharged by regenerative energy.
  • Power supplies that have the function of being charged and discharged by regenerative energy include hybrid electric vehicle (HEV) power supplies, electric vehicle (EV) power supplies, plug-in hybrid vehicle (PHEV) power supplies, other vehicle power supplies, and train power supplies. And so on.
  • HEV hybrid electric vehicle
  • EV electric vehicle
  • PHEV plug-in hybrid vehicle
  • the method for producing the non-aqueous electrolyte power storage element is not particularly limited, and known methods can be combined.
  • the non-aqueous electrolyte power storage element includes, for example, an electrode body in which positive electrodes and negative electrodes are produced, a non-aqueous electrolyte is prepared, and positive electrodes and negative electrodes are laminated or wound alternately via a separator. It can be produced by a production method including forming, accommodating a positive electrode and a negative electrode (electrode body) in a battery container, and injecting the non-aqueous electrolyte into the battery container. The above injection can be performed by a known method. After injection, a non-aqueous electrolyte secondary battery (storage element) can be obtained by sealing the injection port.
  • a negative electrode having a negative electrode active material layer having a predetermined density can also be produced by a conventionally known method. Specifically, it can be obtained by laminating the negative electrode active material layer directly on the negative electrode base material or via the conductive layer.
  • the laminating of the negative electrode active material layer can usually be performed by applying a negative electrode mixture.
  • the negative electrode mixture is usually a paste containing each component of the negative electrode active material layer and a dispersion medium (solvent).
  • the dispersion medium water or an organic solvent such as N-methylpyrrolidone (NMP) may be appropriately selected and used.
  • the coating of the negative electrode mixture can be performed by a known method. Usually, after coating, the coating film is dried to volatilize the dispersion medium.
  • the coating film in the thickness direction.
  • the press can be performed using a known device such as a roll press.
  • the conductive layer can also be formed, for example, by applying a paste for forming the conductive layer and drying it.
  • the power storage device 100 includes the non-aqueous electrolyte secondary battery 1 according to the non-aqueous electrolyte power storage element embodiment of the present invention and the non-aqueous electrolyte secondary battery. It is provided with a control unit 102 that controls charging / discharging of 1.
  • the power storage device 100 includes a power storage unit 101 having a plurality of non-aqueous electrolyte secondary batteries 1 and a control unit 102 that charges and discharges the non-aqueous electrolyte secondary battery 1 and controls the charge and discharge. It has.
  • the control unit 102 controls the non-aqueous electrolyte secondary battery 1 to be charged / discharged at a high rate, particularly to be charged. Specifically, the control unit 102 is set to control the charging of the non-aqueous electrolyte secondary battery 1 with a current amount in a range including 3C or more. The control unit 102 may be set to control charging with a current amount in a range including 5C or more, and further 10C or more. The upper limit of the amount of electricity in charging is not particularly limited, but charging may be controlled with a current amount of 50C or less, 30C or less, or 20C or less.
  • the power storage device 100 includes the non-aqueous electrolyte secondary battery 1 according to the embodiment of the present invention, an alloy of aluminum as a negative electrode base material with lithium even when charging is performed at a high rate of 3C or more. It is possible to suppress the deterioration of the performance and the deterioration of the performance.
  • the control unit 102 and the vehicle control device 111 that controls the engine, the motor, the drive system, the electrical system, and the like are connected to the vehicle-mounted LAN and CAN. It is connected by an in-vehicle communication network 112 such as.
  • the control unit 102 and the vehicle control device 111 communicate with each other, and the power storage device 100 is controlled based on the information obtained from the communication. As a result, for example, the driving energy becomes regenerative energy during deceleration, and the non-aqueous electrolyte secondary battery 1 is charged.
  • the power storage device 100 (non-aqueous electrolyte secondary battery 1) is used as a power source having a function of being charged by regenerative energy.
  • the power storage device 100 can be mounted as a power source for automobiles such as electric vehicles, hybrid electric vehicles, and plug-in hybrid vehicles.
  • the present invention is not limited to the above-described embodiment, and can be implemented in various modifications and improvements in addition to the above-described embodiment.
  • the mode in which the power storage element is a non-aqueous electrolyte secondary battery has been mainly described, but other non-water electrolyte power storage elements may be used.
  • other non-aqueous electrolyte power storage elements include capacitors (electric double layer capacitors, lithium ion capacitors) and the like.
  • the positive electrode and the negative electrode may not be provided with the conductive layer.
  • FIG. 2 shows a schematic view of a rectangular non-aqueous electrolyte secondary battery 1 which is an embodiment of the non-aqueous electrolyte power storage element according to the present invention.
  • the figure is a perspective view of the inside of the battery container.
  • the electrode body 2 is housed in the battery container 3.
  • the electrode body 2 is formed by winding a positive electrode having a positive electrode active material and a negative electrode having a negative electrode active material through a separator.
  • the positive electrode is electrically connected to the positive electrode terminal 4 via the positive electrode lead 4'
  • the negative electrode is electrically connected to the negative electrode terminal 5 via the negative electrode lead 5'.
  • the configuration of the non-aqueous electrolyte power storage element according to the present invention is not particularly limited, and examples thereof include a cylindrical power storage element, a square power storage element (rectangular power storage element), and a flat power storage element.
  • Lithium cobalt nickel-manganese composite oxide LiCo 1/3 Ni 1/3 Mn 1/3 O 2
  • acetylene black AB
  • PVDF polyvinylidene fluoride
  • PVDF polyvinylidene fluoride
  • NMP N-methylpyrrolidone
  • This positive electrode mixture paste was applied to both sides of the aluminum foil (A1085, aluminum content 99.85% by mass) so that an uncoated portion (positive electrode active material layer non-formed region) was partially formed, and dried. ..
  • the coating amount (weighting amount) of the positive electrode active material in the positive electrode active material layer was 7.8 mg / cm 2 . Then, a roll press was performed to obtain a positive electrode.
  • the mass ratio of non-graphitizable carbon, SBR, and CMC was 97.9: 1.5: 0.6 (in terms of solid content).
  • the paste for forming the conductive layer is applied to both sides of the aluminum foil (A1N30, aluminum content 99.30% by mass) so that an uncoated portion (negative electrode active material layer non-forming region) is partially formed, and dried. As a result, a conductive layer was formed.
  • the surface of the conductive layer was coated with a negative electrode mixture paste and dried.
  • the coating amount (weighting amount) of the negative electrode active material in the negative electrode active material layer was 8.4 mg / cm 2 . Then, a roll press was performed to obtain a negative electrode.
  • the density of the negative electrode active material layer was 0.9 g / cm 3 .
  • the mass ratio (P / N) of the content (P) of the positive electrode active material per unit area in the positive electrode active material layer and the content (N) of the negative electrode active material in the negative electrode active material layer per unit area is 0. It was 9.
  • the entire region on the negative electrode base material on which the negative electrode active material layer is laminated is covered with the conductive layer.
  • the non-aqueous electrolyte is prepared by dissolving LiPF 6 in a solvent mixed so that the volume ratio of propylene carbonate, dimethyl carbonate and ethyl methyl carbonate is 30:35:35 so that the salt concentration is 1.2 mol / L. Prepared.
  • Example 1 non-aqueous electrolyte power storage element
  • Examples 2 to 4 and Comparative Examples 1 to 2 are the same as in Example 1 except that the pressure of the roll press during the production of the negative electrode is adjusted and the density of the negative electrode active material layer is changed as shown in Table 1. Obtained each battery.
  • the laminated cell was charged with a constant current (CC) at a charging current of 10 C and a charging end voltage of 3.6 V in a constant temperature bath at 25 ° C., and the closed circuit potential of the negative electrode immediately before the end of charging was measured.
  • the measurement results are taken as the negative electrode potential in the fully charged state, and are shown in Table 1 and FIG.
  • the alternating current resistance (ACR) of each battery was measured as follows. First, the battery is charged with a constant current constant voltage (CCCV) at a charging current of 1C and a charge termination voltage of 3.6V in a constant temperature bath at 25 ° C., and then a constant current (CC) is charged with a discharge current of 1C and a discharge termination voltage of 2.4V.
  • CCCV constant current constant voltage
  • CC constant current
  • Discharge was performed.
  • constant current (CC) charging was performed with a charging current of 1 C for an amount of electricity corresponding to 20% of the amount of discharged electricity.
  • the ACR of the charged battery was measured using an AC resistance meter (milliohm high tester) having a measurement frequency of 1 kHz. Table 1 shows the ACR of each battery as a relative value based on Example 3 (100%).
  • LSV Linear sweep voltammetry
  • the batteries of each example are charged at 10 C at a high temperature of 65 ° C.
  • the closed circuit potential of the negative electrode is also 0.3 V vs. The inventors have confirmed that it does not fall below Li / Li + . Therefore, in the batteries of each embodiment, the alloying of aluminum of the negative electrode base material with lithium can be suppressed even when the battery is charged at a high rate at a high temperature.
  • the present invention can be applied to a non-aqueous electrolyte power storage element used as a power source for personal computers, electronic devices such as communication terminals, automobiles, etc., particularly as a power source having a function of being charged by regenerative energy.
  • Non-aqueous electrolyte secondary battery 2 Electrode body 3 Battery container 4 Positive terminal 4'Positive lead 5 Negative terminal 5'Negative lead 100 Power storage device 101 Power storage unit 102 Control unit 110 Vehicle 111 Vehicle control device 112 Communication network

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