WO2011089722A1 - 正極およびその製造方法 - Google Patents
正極およびその製造方法 Download PDFInfo
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- WO2011089722A1 WO2011089722A1 PCT/JP2010/050850 JP2010050850W WO2011089722A1 WO 2011089722 A1 WO2011089722 A1 WO 2011089722A1 JP 2010050850 W JP2010050850 W JP 2010050850W WO 2011089722 A1 WO2011089722 A1 WO 2011089722A1
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- positive electrode
- active material
- hydrophilic film
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- current collector
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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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
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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
- H01M4/04—Processes of manufacture in general
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/58—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
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/665—Composites
- H01M4/667—Composites in the form of layers, e.g. coatings
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- 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 positive electrode active material layer is formed on the hydrophilic film formed on the metal substrate, the adhesion between the positive electrode active material layer and the positive electrode current collector is increased. (Joint strength) can be improved.
- a positive electrode active material layer having an uncompressed density of 0.9 g / cm 3 to 1.5 g / cm 3 is formed on the hydrophilic film of the positive electrode current collector.
- Such an uncompressed positive electrode active material layer has a low density and has a large number of pores in the positive electrode active material layer, so that the electrolyte sufficiently permeates every corner of the positive electrode active material layer.
- the presence or absence of compression (pressing) of the positive electrode active material layer can be confirmed, for example, by measuring the surface roughness (Ra) of the positive electrode active material layer.
- the surface roughness (Ra) of the positive electrode active material layer is 3 ⁇ m or more (eg, 3 ⁇ m to 5 ⁇ m, preferably 5 ⁇ m or more). ) Can be confirmed.
- the surface roughness (Ra) may be grasped by, for example, analyzing a cross-sectional image of the positive electrode active material layer using a scanning electron microscope (SEM).
- the situation where the positive electrode active material layer obtained after drying partially lifts or peels off from the positive electrode current collector is avoided, and the adhesion between the positive electrode active material layer and the positive electrode current collector can be improved.
- the above material has high conductivity, even when a hydrophilic film made of the material is provided on the surface of the positive electrode current collector, the surface resistance of the positive electrode current collector (generated between the positive electrode active material layer and the surface current) The resistance between the positive electrode active material layer and the positive electrode current collector can be kept good by reducing the resistance.
- the hydrophilic film includes a first hydrophilic film formed on the metal substrate and a second hydrophilic film formed on the first hydrophilic film. It consists of a sex membrane.
- the second hydrophilic film is preferably a material having a higher conductivity than the first hydrophilic film.
- the first hydrophilic film is made of tungsten carbide or oxide
- the second hydrophilic film is a hydrophilic film made of carbon and having a hydrophilic surface.
- membrane is a material with better adhesiveness (bonding strength) with a metal base material (for example, aluminum foil) than a 2nd hydrophilic film
- a second hydrophilic film for example, a carbon film
- adhesion may be low and sufficient bonding strength may not be obtained.
- the first hydrophilic film for example, tungsten carbide
- the first hydrophilic film for example, tungsten carbide
- the metal substrate provided in the positive electrode current collector is made of aluminum or an aluminum alloy.
- a metal substrate made of aluminum or an aluminum alloy has a low “wetting property” with respect to an active material paste containing a polar solvent (water, N-methylpyrrolidone, etc.), so a hydrophilic film is formed on the metal substrate.
- a polar solvent water, N-methylpyrrolidone, etc.
- the method of manufacturing the said battery positive electrode suitably is provided.
- the manufacturing method is a method for manufacturing a positive electrode for a battery having a structure in which a positive electrode active material layer containing a positive electrode active material is held on a positive electrode current collector.
- the positive electrode current collector is a coating film that is formed on the surface of the metal base material constituting the main body portion of the positive electrode current collector and has a hydrophilic property than the surface of the metal base material.
- the manufacturing method of this invention apply
- a hydrophilic film is formed on the surface of the metal substrate, and then the active material paste is applied onto the hydrophilic film. Without being repelled, it becomes easy to become familiar on the positive electrode current collector (hydrophilic film). Therefore, the situation where the positive electrode active material layer obtained after drying partially lifts or peels off from the positive electrode current collector is avoided, and the adhesion between the positive electrode active material layer and the positive electrode current collector can be improved.
- a positive electrode active material layer having good adhesion can be obtained by forming a hydrophilic film on a metal substrate. Can be formed.
- a positive electrode active material layer having an uncompressed density of 0.9 g / cm 3 to 1.5 g / cm 3 can be formed.
- the production line can be made compact.
- problems such as density unevenness generated in the pressing process and damage to the positive electrode active material layer can be solved.
- an oxide film of the metal is previously formed on the surface of the metal substrate, and the surface of the metal substrate is formed before the step of forming the hydrophilic film. And a step of removing the metal oxide film formed in the step. If a metal oxide film is present on the surface of the metal substrate, the resistance between the metal substrate and the hydrophilic film may increase, and the conductivity between the metal substrate and the hydrophilic film may be impaired. According to the above method, the metal oxide film formed on the metal substrate is removed, the underlying metal surface is exposed, and the hydrophilic film is formed in direct contact with the exposed solid metal substrate. Therefore, the electrical conductivity between the metal substrate and the hydrophilic film can be made better than interposing the metal oxide film therebetween.
- the step of forming the hydrophilic film includes a step of forming a first hydrophilic film on the metal substrate and a second step on the first hydrophilic film.
- Forming a hydrophilic film For example, a hydrophilic film made of tungsten carbide or oxide may be formed as the first hydrophilic film, and a hydrophilic film made of carbon and having a hydrophilic surface may be formed as the second hydrophilic film.
- Such a battery is suitable as a battery mounted on a vehicle such as an automobile. Therefore, according to the present invention, there is provided a vehicle including any of the batteries disclosed herein (which may be in the form of an assembled battery in which a plurality of batteries are connected).
- the battery is a lithium secondary battery (typically a lithium ion battery), and the lithium secondary battery is used as a power source (typically a hybrid vehicle or an electric vehicle).
- a vehicle for example, an automobile
- a power source of the vehicle is preferable.
- FIG. 1 is a diagram showing a manufacturing flow of a positive electrode according to an embodiment of the present invention.
- FIG. 2A is a process cross-sectional view schematically showing a manufacturing process of a positive electrode according to an embodiment of the present invention.
- FIG. 2B is a process cross-sectional view schematically showing a manufacturing process of the positive electrode according to one embodiment of the present invention.
- FIG. 2C is a process cross-sectional view schematically showing the manufacturing process of the positive electrode according to one embodiment of the present invention.
- FIG. 3A is a process cross-sectional view schematically showing a manufacturing process of a positive electrode according to an embodiment of the present invention.
- FIG. 3B is a process cross-sectional view schematically showing the manufacturing process of the positive electrode according to one embodiment of the present invention.
- FIG. 4 is a cross-sectional view schematically showing a cross-sectional configuration of a positive electrode according to an embodiment of the present invention.
- FIG. 5 is a cross-sectional view schematically showing a cross-sectional configuration of a positive electrode according to another embodiment of the present invention.
- 6A is a cross-sectional view schematically showing a cross-sectional configuration of the positive electrode current collector according to Example 1.
- FIG. 6B is a cross-sectional view schematically showing a cross-sectional configuration of the positive electrode current collector according to Example 2.
- FIG. FIG. 6C is a cross-sectional view schematically showing a cross-sectional configuration of the positive electrode current collector according to Comparative Example 1.
- FIG. 6D is a cross-sectional view schematically showing a cross-sectional configuration of a positive electrode current collector according to Comparative Example 2.
- FIG. FIG. 7 is a graph showing the results (contact angle) of the wettability test for the positive electrode of each example.
- FIG. 8 is a diagram for explaining a method of measuring an electric resistance value according to the positive electrode of each example.
- FIG. 9 is a characteristic diagram showing the relationship between the battery resistance value and the contact angle according to the positive electrode of each example.
- FIG. 10 is a characteristic diagram showing the relationship between the density of the positive electrode active material layer and the battery resistance value in each example.
- FIG. 11 is a schematic view schematically showing the test battery of each example.
- an aluminum foil having a thickness of, for example, about 10 ⁇ m to 30 ⁇ m is prepared as a metal base (step S10),
- the formed metal oxide film (aluminum oxide film) is removed (step S20). Due to its characteristics, aluminum foil is immediately oxidized when exposed to the atmosphere, and therefore has an oxide film on its surface.
- a thin oxide film 13 having a thickness of about 5 nm to 10 nm is formed on the surface of the aluminum foil 12.
- the oxide film 13 formed on the surface of the aluminum foil 12 is removed to expose the metal surface made of underlying aluminum as shown in FIG. 2B, and then as shown in FIG. 2C. Further, the hydrophilic film 14 is directly formed on the exposed solid metal substrate 12.
- the hydrophilic film 14 is formed on the surface of the metal substrate 12 following the step S20 for removing the oxide film ( Step S30 shown in FIG.
- a carbide or oxide containing at least one selected from the group consisting of tungsten, tantalum, hafnium, niobium, molybdenum and vanadium as a constituent element is preferably used.
- tungsten carbide tungsten carbide
- WO 3 , W 2 C 3 and the like are exemplified as tungsten oxide.
- the tantalum carbide include TaC
- examples of the tantalum oxide include TaO 2
- the hafnium carbide include HfC and the like
- examples of the hafnium oxide include HfO 2 and the like.
- the above material has high conductivity, even when a hydrophilic film made of the material is formed on the surface of the positive electrode current collector, the surface resistance of the positive electrode current collector (generated between the positive electrode active material layer) The resistance between the positive electrode active material layer and the positive electrode current collector can be kept good by reducing the resistance.
- the electrical conductivity of the hydrophilic film for example, tungsten carbide (WC) is 17 ⁇ ⁇ cm, tantalum carbide (TaC) is 0.31 ⁇ ⁇ cm, hafnium carbide (HfC) is 0.26 ⁇ ⁇ cm, and niobium carbide (NbC).
- a known vapor deposition method for example, a physical vapor deposition method (PVD method, for example, sputtering method), a chemical vapor deposition method (CVD method, for example, plasma CVD method) or the like is preferable.
- PVD method physical vapor deposition method
- CVD method chemical vapor deposition method
- the formation of a hydrophilic film by this vapor deposition method is typically performed under reduced pressure conditions (for example, an inert gas atmosphere and a non-oxidizing gas under an inert gas atmosphere at a pressure of about 0.01 Pa to 100 Pa). And mixed gas atmosphere or air atmosphere).
- a sputtering method using a material material of the hydrophilic film as a target can be preferably employed.
- the hydrophilic film 14 By forming the hydrophilic film 14 in this manner, the positive electrode current collector 10 in which the hydrophilic film 14 is provided on the surface of the base 12 of the aluminum foil (for example, the entire range of both surfaces of the aluminum foil) is obtained. (Step S40 shown in FIG. 1). Therefore, the above steps S10 to S40 can be grasped as a method for manufacturing a positive electrode current collector or a process for preparing (manufacturing) a positive electrode current collector.
- the above active material paste is dispersed (typically dissolved) in a suitable dispersion medium with positive electrode active material powder and other positive electrode active material layer forming components (eg, conductive material and binder) used as necessary. ) And kneaded and kneaded paste-like or slurry-like electrode mixture.
- the active material paste is an aqueous paste in which an aqueous medium is used as the dispersion medium from various viewpoints such as reduction of environmental burden, reduction of material cost, simplification of equipment, reduction of waste, and improvement of handling properties. It is preferable.
- the aqueous medium water or a mixed solvent mainly containing water is preferably used.
- a solvent component other than water constituting such a mixed solvent one or more organic solvents (lower alcohol, lower ketone, etc.) that can be uniformly mixed with water can be appropriately selected and used.
- an aqueous solvent in which 80% by mass or more (more preferably 90% by mass or more, more preferably 95% by mass or more) of the aqueous solvent is water.
- a particularly preferred example is an aqueous solvent substantially consisting of water.
- the dispersion medium is not limited to an aqueous solvent, and may be a non-aqueous solvent.
- a polar solvent such as N-methylpyrrolidone (NMP) can be used.
- M in such a formula is one or more elements (typically one or more metals) including at least one metal element selected from the group consisting of Fe, Co, Ni, and Mn. Element). That is, it contains at least one metal element selected from the group consisting of Fe, Co, Ni, and Mn, but allows the presence of other minor additive elements that can be contained in small amounts (even if such minor additive elements are not present). Good.)
- a in the above formula is one or more elements selected from the group consisting of P, Si, S and V.
- This type of polyanionic compound (typically a compound having an olivine structure) is preferable because it has a high theoretical energy density and can avoid or reduce the use of expensive metal materials.
- A is P and / or Si (for example, LiFePO 4 , LiFeSiO 4 , LiCoPO 4 , LiCoSiO 4 , LiFe 0.5 Co 0.5 PO 4 , LiFe 0.5 Co 0. 5 SiO 4, LiMnPO 4, LiMnSiO 4, LiNiPO 4, LiNiSiO 4) can be cited as particularly preferred polyanionic compound.
- a positive electrode active material typically, a positive electrode active material substantially composed of a lithium-containing iron phosphate compound, which is mainly composed of an olivine-type phosphate compound containing lithium, particularly a lithium-containing iron phosphate compound (for example, LiFePO 4 ).
- a lithium-containing layered or spinel transition metal oxide lithium transition metal oxide
- lithium nickel oxide LiNiO 2
- lithium cobalt oxide LiCoO 2
- lithium manganese oxide LiMn 2 O 4
- the application of the lithium-nickel-cobalt-manganese composite oxide e.g., LiNi 1/3 Co 1/3 Mn 1/3 O 2
- the positive electrode active material is preferable.
- the active material paste may be one or more materials (other positive electrode active material layer forming components) used as a paste for forming a positive electrode active material layer in general positive electrode production. ) Can be contained as necessary.
- Representative examples of such materials include conductive materials and binders.
- carbon powder such as carbon black (acetylene black or the like), conductive metal powder such as nickel powder, or the like can be used.
- binder examples include carboxymethylcellulose (CMC), polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), polyvinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP), and styrene butadiene rubber (SBR). Etc. can be used.
- CMC carboxymethylcellulose
- PTFE polytetrafluoroethylene
- PVDF polyvinylidene fluoride
- PVDF-HFP polyvinylidene fluoride-hexafluoropropylene copolymer
- SBR styrene butadiene rubber
- the solid content concentration of the active material paste can be, for example, about 40 to 60% by mass.
- the content ratio of the positive electrode active material in the solid content is preferably at least about 50% by mass, for example, about 75 to 99% by mass. Usually, it is appropriate to set this ratio to about 80 to 95% by mass.
- the positive electrode active material may be included in a ratio of approximately 80 to 90% by mass and the conductive material in a ratio of approximately 5 to 15% by mass.
- the operation of applying (typically applying) such an active material paste 24 to the positive electrode current collector 10 uses the positive electrode current collector 10 having the surface provided with the hydrophilic film 14 as described above. Except for this point, a conventional general positive electrode for a lithium secondary battery can be produced in the same manner. For example, it is produced by applying a predetermined amount of the active material paste in layers to the positive electrode current collector from above the hydrophilic film using an appropriate coating device (slit coater, die coater, comma coater, etc.). Can be done. After coating, the coated material is dried (typically 70 ° C. to 200 ° C.) by an appropriate drying means. As a result, as shown in FIG. 3B, the positive electrode active material layer 20 is formed on the surface of the positive electrode current collector 10.
- an appropriate coating device slit coater, die coater, comma coater, etc.
- a positive electrode active material is obtained by directly applying an active material paste on a positive electrode current collector (aluminum foil) and drying it. A layer is formed.
- the positive electrode active material layer formed in this manner has low adhesion, and the positive electrode active material layer may partially lift or peel off from the positive electrode current collector. Therefore, it has been necessary to increase the adhesion (bonding strength) between the positive electrode active material layer and the positive electrode current collector by performing a press treatment.
- the positive electrode active material having good adhesion is formed by forming the hydrophilic film 14 on the metal substrate 12 and then applying the active material paste 24 on the hydrophilic film 14. Layer 20 is obtained. Therefore, the positive electrode active material layer can be formed by omitting a conventional pressing step. That is, according to the present embodiment, an uncompressed low-density positive electrode active material layer 20 can be formed by applying an active material paste on the hydrophilic film of the positive electrode current collector and drying it (see FIG. Step S60 shown in FIG. In this case, since the positive electrode can be manufactured by omitting the pressing step, the manufacturing line can be made compact. In addition, problems such as density unevenness generated in the pressing process and damage to the positive electrode active material layer can be solved. In this way, the manufacture of the positive electrode 30 according to this embodiment is completed.
- FIG. 4 schematically shows a cross-sectional structure of a positive electrode for a lithium secondary battery that is preferably manufactured by applying the positive electrode manufacturing method disclosed herein.
- the positive electrode 30 has a structure in which the positive electrode active material layer 20 including the positive electrode active material 22 is held by the positive electrode current collector 10.
- the positive electrode current collector 10 includes a metal substrate (aluminum foil) 12 constituting a main body portion of the positive electrode current collector, and a hydrophilic film 14 formed on the metal substrate. Then, on the hydrophilic film 14 of the positive electrode current collector, a low-density positive electrode active material layer 20 having an uncompressed (not subjected to press treatment) density of 0.9 g / cm 3 to 1.5 g / cm 3. Is formed.
- the hydrophilic film 14 is formed on the metal base material (aluminum foil) 12 constituting the main body portion of the positive electrode current collector, and the positive electrode active material is formed on the hydrophilic film 14. Since the material layer 20 is formed, the adhesion (bonding strength) between the positive electrode active material layer 20 and the positive electrode current collector 10 can be improved.
- An uncompressed positive electrode active material layer 20 is formed on the hydrophilic film 14 of the positive electrode current collector.
- the uncompressed positive electrode active material layer 20 has a lower density than the positive electrode active material layer that has been pressed and compressed, and has a large number of pores 26 in the positive electrode active material layer 20. The electrolyte sufficiently permeates into every corner of the active material layer.
- the density of the uncompressed positive electrode active material layer is preferably about 0.9 g / cm 3 to 1.5 g / cm 3 .
- the density of the positive electrode active material layer is too large, the number of pores 26 in the positive electrode active material layer is reduced, and the permeability of the electrolytic solution into the positive electrode active material layer is lowered, which may cause battery capacity deterioration and the like.
- high-rate discharge performance may be reduced.
- the density of the positive electrode active material layer is approximately 0.9 g / cm 3 to 1.5 g / cm 3 , for example, more preferably 0.9 g / cm 3 to 1.3 g / cm 3. .
- the positive electrode active material layer in which the density satisfies an appropriate range can be realized, for example, by appropriately selecting the material and properties of the positive electrode active material.
- the uncompressed density is 0.9 g / cm 3 to 1.5 g.
- a positive electrode having a positive electrode active material layer satisfying / cm 3 can be manufactured.
- a method of adjusting the uncompressed density to an appropriate range a method of appropriately selecting an active material paste composition and the like can be mentioned.
- the positive electrode active material layer density of uncompressed satisfy 0.9g / cm 3 ⁇ 1.5g / cm 3
- the above-described methods for adjusting the uncompressed density may be used alone or in appropriate combination.
- the presence or absence of compression (pressing) of the positive electrode active material layer can be confirmed, for example, by measuring the surface roughness (Ra) of the positive electrode active material layer.
- the positive electrode active material layer disclosed herein is an uncompressed positive electrode active material layer because the surface roughness (Ra) of the positive electrode active material layer is 3 ⁇ m or more (eg, 3 ⁇ m to 5 ⁇ m or more, eg, 5 ⁇ m). (About 10 ⁇ m).
- the surface roughness (Ra) may be grasped by, for example, analyzing a cross-sectional image of the positive electrode active material layer using a scanning electron microscope (SEM).
- a second hydrophilic film (C) made of carbon having a thickness of about 5 nm is formed on the first hydrophilic film (WC film) 14a formed in the same manner as Sample 1.
- a positive electrode current collector 10 having a film 14b was produced.
- the second hydrophilic film (C film) 14b is formed by depositing carbon under the conditions of an atmospheric pressure of 0.3 Pa, a bias voltage of 250 W, and a target current of 41 A using a general AIP (arc ion plating) apparatus. It went by.
- Samples 5 and 6 the same positive electrode current collector (WC + C film-formed product) as that of Sample 2 was used, but a positive electrode active material layer with press was formed. More specifically, in the order of samples 5 and 6, the density of the positive electrode active material layer, respectively, 1.3 g / cm 3, to prepare a by pressing so that 1.5 g / cm 3 positive electrode sheet. Further, as Samples 7 and 8, the same positive electrode current collector (untreated Al foil) as that of Sample 3 was used, but a positive electrode active material layer with press was formed. More specifically, in the order of samples 7 and 8, the density of the positive electrode active material layer, respectively, 1.3 g / cm 3, to prepare a by pressing so that 1.5 g / cm 3 positive electrode sheet.
- the electric resistance value changed greatly depending on whether or not the press was performed. Specifically, the electrical resistance value of the sample 3 without a hydrophilic film and without pressing was significantly increased as compared with the samples 7 and 8 without a hydrophilic film and with pressing. On the other hand, comparing sample 2 with a hydrophilic film and no press with samples 5 and 6 with a hydrophilic film and with a press, the electrical resistance value is 10 m ⁇ or less regardless of whether or not there is a press. Showed a low value.
- each test battery of Samples 1 and 2 having a hydrophilic film (WC film, WC + C film) is used for each test of Samples 3 and 4 having no hydrophilic film formed.
- the discharge capacity was greatly improved. The reason for this is that in Samples 1 and 2, the wettability of the positive electrode current collector with respect to the active material paste is increased due to the presence of the hydrophilic film, and the interface resistance between the positive electrode current collector and the positive electrode active material layer is reduced. It is considered that the discharge capacity is improved as compared with Samples 3 and 4.
- positive electrode sheets were prepared by changing the positive electrode active material to LiNi 1/3 Co 1/3 Mn 1/3 O 2 .
- LiNi 1/3 Co 1/3 Mn 1/3 O 2 powder as a positive electrode active material
- carbon black as a conductive material
- PVdF polyvinylidene fluoride
- NMP N-methylpyrrolidone
- the constituent elements of the wound electrode body 80 may be the same as those of the conventional wound electrode body of the lithium secondary battery except for the positive electrode sheet 30, and are not particularly limited.
- the negative electrode sheet 40 may be formed by applying a negative electrode active material layer 44 mainly composed of a negative electrode active material for a lithium secondary battery on a long negative electrode current collector 42.
- a copper foil or other metal foil suitable for the negative electrode is preferably used.
- the negative electrode active material one type or two or more types of materials conventionally used in lithium secondary batteries can be used without any particular limitation. Examples thereof include carbon-based materials such as graphite carbon and amorphous carbon, lithium-containing transition metal oxides and transition metal nitrides.
- a negative electrode active material mainly composed of a carbon-based material such as graphite carbon or amorphous carbon is exemplified.
- a separator sheet 48 As a preferred example of the separator sheet 48 used between the positive and negative electrode sheets 30 and 40, a separator sheet 48 is used.
- a porous separator sheet made of synthetic resin for example, made of polyolefin such as polyethylene
- polyolefin such as polyethylene
- the wound electrode body 80 is accommodated in the main body 52 from the upper end opening of the container main body 52 and an electrolytic solution containing an appropriate electrolyte is disposed (injected) in the container main body 52.
- the electrolyte is lithium salt such as LiPF 6, for example.
- a nonaqueous electrolytic solution obtained by dissolving a suitable amount (for example, concentration 1M) of a lithium salt such as LiPF 6 in a mixed solvent of diethyl carbonate and ethylene carbonate (for example, a mass ratio of 1: 1) can be used.
- a positive electrode for a battery including an active material layer having high electrolyte permeability and good adhesion to a positive electrode current collector.
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Abstract
Description
LiMAO4 (1)
で示される化合物が挙げられる。かかる式中のMは、Fe、Co、Ni及びMnから成る群から選択される少なくとも1種の金属元素を含む1種又は2種以上の元素(典型的には1種又は2種以上の金属元素)である。即ち、Fe、Co、Ni及びMnから成る群から選択される少なくとも1種の金属元素を含むが他の少量含有され得るマイナー添加元素の存在を許容する(かかるマイナー添加元素は存在しなくてもよい。)。また、上記式中のAは、P、Si、S及びVから成る群から選択される1種又は2種以上の元素である。
この種のポリアニオン型化合物(典型的にはオリビン構造を有する化合物)は、理論エネルギー密度が高く且つ高価な金属材料の使用を回避若しくは低減させることができるため、好ましい。上記式(1)において、AがP及び/又はSiであるもの(例えば、LiFePO4、LiFeSiO4、LiCoPO4、LiCoSiO4、LiFe0.5Co0.5PO4、LiFe0.5Co0.5SiO4、LiMnPO4、LiMnSiO4、LiNiPO4、LiNiSiO4)が特に好ましいポリアニオン型化合物として挙げられる。中でもリチウムを含有するオリビン型リン酸化合物、特にリチウム含有リン酸鉄化合物(例えばLiFePO4)を主成分とする正極活物質(典型的には、実質的にリチウム含有リン酸鉄化合物からなる正極活物質)への適用が好ましい。あるいは、リチウムニッケル酸化物(LiNiO2)、リチウムコバルト酸化物(LiCoO2)、リチウムマンガン酸化物(LiMn2O4)等の、リチウムを含有する層状またはスピネル型遷移金属酸化物(リチウム遷移金属酸化物)が挙げられる。中でも、リチウムニッケルコバルトマンガン複合酸化物(例えばLiNi1/3Co1/3Mn1/3O2)を主成分とする正極活物質への適用が好ましい。
即ち、サンプル1では、図6Aに示すように、金属基材12として、表面酸化膜が除去されたアルミニウム箔を用意し、該アルミニウム箔の片面に、厚さ約50nmの炭化タングステンからなる親水性膜(WC膜)14が形成された正極集電体10を作製した。親水性膜(WC膜)の形成は、一般的なスパッタリング装置を用いて雰囲気圧力0.3Pa、スパッタ電力1.25kWの条件で炭化タングステンをターゲットとしてスパッタリングすることにより行った。
サンプル1~4の正極集電体10のそれぞれに対し、活物質ペーストの溶媒としてN-メチルピロリドン(NMP)の液滴を付着させ、その接触角を測定した。その結果を図7および表1に示す。
続いて、サンプル1~4の各正極集電体を用いて正極シートを作製した。本例では、プレス無しの未圧縮の正極活物質層を形成した。まず、正極活物質としてのLiFePO4粉末(平均粒径30μm)と、導電材としてのカーボンブラックと、バインダとしてのポリフッ化ビニリデン(PVdF)とを、これらの材料の質量比が87:10:3となり且つ固形分濃度が約42.9質量%となるようにN-メチルピロリドン(NMP)中で混合して、活物質ペーストを調製した。この活物質ペーストを正極集電体の片面に帯状に塗布して乾燥することにより、未圧縮の正極活物質層20(厚さ約135μm)が正極集電体の片面に設けられた正極シート30を作製した。活物質ペーストの塗布量は、片面で約4mg/cm2(固形分基準)となるように調節した。また、未圧縮の正極活物質層の密度を測定したところ、約0.9g/cm3であった。
このようにして得られたサンプル1~8の正極シートの電気抵抗値を測定した。電気抵抗値の測定は図8に示す装置を用いて行った。図8に示すように、正極シート30の正極活物質層20の上に、もう一枚の正極集電体10を該正極集電体の親水性膜14と正極活物質層20とが接するように重ね合わせた。そして、一対の電圧測定端子96で挟みこみ、電圧測定端子96の上下から25kg/cm2の荷重を加えつつ、電流印加装置94から電流を流したときの電圧変化から正極シート30の電気抵抗値(mΩ)を測定した。その結果を表1および図9、図10に示す。図9は濡れ性試験で得られた接触角と電気抵抗値との関係を示した特性図であり、図10は正極活物質層の密度と電気抵抗値との関係を示している。
続いて、サンプル1~5及び7の正極シートを用いてリチウム二次電池を構築した。具体的には、上記正極シートを直径16mmの円形に打ち抜いて、正極を作製した。この正極(作用極)と、負極(対極)としての金属リチウム(直径19mm、厚さ0.02mmの金属Li箔を使用した。)と、セパレータ(直径22mm、厚さ0.02mmの多孔質ポリプロピレンシートを使用した。)とを、非水電解液とともにステンレス製容器に組み込んで、直径20mm、厚さ3.2mm(2032型)の図11に示すコインセル60(充放電性能評価用のハーフセル)を構築した。図11中、符号61は正極(作用極)を、符号62は負極(対極)を、符号63は電解液の含浸したセパレータを、符号64はガスケットを、符号65は容器(負極端子)を、符号66は蓋(正極端子)をそれぞれ示す。なお、非水電解液としては、エチレンカーボネート(EC)とジメチルカーボネート(DMC)とエチルメチルカーボネート(EMC)とを3:4:3の体積比で含む混合溶媒に支持塩としてのLiPF6を約1mol/リットルの濃度で含有させたものを用いた。その後、常法により初期充放電処理(コンディショニング)を行って試験用のリチウム二次電池を得た。
以上のようにして得られた各例の試験用リチウム二次電池のそれぞれに対して、ハイレート充放電試験を行った。具体的には、各試験用リチウム二次電池を、25℃の温度条件にて、端子間電圧が4.1Vとなるまで0.3Cの定電流で充電し、続いて合計充電時間が4時間となるまで定電圧で充電した。かかるCC-CV充電後の電池を、25℃の温度条件にて、端子間電圧が2.5Vとなるまで30Cの定電流で放電させて、30Cでの放電容量を測定した。その結果を表1および図12、図13に示す。図12は濡れ性試験で得られた接触角と放電容量との関係を示した特性図であり、図13はサンプル2,3,5,7の放電容量を示している。
サンプル9では、サンプル2と同様の正極集電体(WC+C成膜処理品)を用い、未圧縮の正極活物質層を形成した。また、サンプル10では、サンプル3と同様の正極集電体(Al未処理品)を用い、未圧縮の正極活物質層を形成した。未圧縮の正極活物質層の密度を測定したところ、約1.5g/cm3であった。また、サンプル11では、サンプル3と同様の正極集電体(Al未処理品)を用い、プレス処理を施した正極活物質層を形成した。プレス処理後の正極活物質層の密度を測定したところ、約2.0g/cm3であった。 上記得られたサンプル9~11の正極シートの電気抵抗値を、サンプル1~8と同様の方法で測定した。また、サンプル9~11の正極シートを用いてサンプル1~8と同様の方法で試験用電池を構築し、30C放電容量を測定した。その結果を表2に示す。
Claims (17)
- 正極活物質を含む正極活物質層が正極集電体上に保持された構造を有する電池用正極であって、
前記正極集電体は、
該正極集電体の本体部分を構成する金属基材と、
該金属基材の表面上に形成され、該金属基材表面よりも親水性を有する被膜であって、タングステン、タンタル、ハフニウム、ニオブ、モリブデン及びバナジウムから成る群から選択された少なくとも一種を構成元素とする炭化物若しくは酸化物からなる親水性膜、またはカーボンからなり表面が親水性である親水性膜と、
を備え、
前記正極集電体の親水性膜上に、未圧縮の密度が0.9g/cm3~1.5g/cm3である正極活物質層が形成されている、電池用正極。 - 前記正極活物質層の表面粗さ(Ra)が、3μm以上である、請求項1に記載の電池用正極。
- 前記正極活物質層は、極性溶媒を含む活物質ペーストを塗布し、乾燥させて形成されている、請求項1または2に記載の電池用正極。
- 前記親水性膜は、前記金属基材上に形成された第1親水性膜と、該第1親水性膜上に形成された第2親水性膜とから構成されている、請求項1から3の何れか一つに記載の電池用正極。
- 前記第1親水性膜は、前記第2親水性膜よりも前記金属基材との密着性がよい材料から構成され、前記第2親水性膜は、前記第1親水性膜よりも導電率が高い材料から構成されている、請求項4に記載の電池用正極。
- 前記第1親水性膜は、タングステンの炭化物または酸化物から構成され、前記第2親水性膜は、カーボンからなり表面が親水性である親水性膜である、請求項4または5に記載の電池用正極。
- 前記正極集電体が備える金属基材は、アルミニウムまたはアルミニウム合金により構成されている、請求項1から6の何れか一つに記載の電池用正極。
- 前記正極活物質は、以下の一般式:
LiMAO4 (1)
で示される化合物であって、該式中のMは、Fe、Co、Ni及びMnから成る群から選択される少なくとも1種の金属元素を含む1種又は2種以上の元素であり、式中のAは、P、Si、S及びVから成る群から選択される1種又は2種以上の元素であるポリアニオン型化合物である、請求項1から7の何れか一つに記載の電池用正極。 - 請求項1から8の何れか一つに記載の電池用正極を有する電極体と、Liイオンを含む電解液とを備えた、電池。
- 請求項9に記載の電池を搭載した車両。
- 正極活物質を含む正極活物質層が正極集電体上に保持された構造を有する電池用正極の製造方法であって、
前記正極集電体は、該正極集電体の本体部分を構成する金属基材と、該金属基材の表面上に形成され、該金属基材表面よりも親水性を有する被膜であって、タングステン、タンタル、ハフニウム、ニオブ、モリブデン及びバナジウムから成る群から選択された少なくとも一種を構成元素とする炭化物若しくは酸化物からなる親水性膜、またはカーボンからなり表面が親水性である親水性膜とを備え、以下の工程;
前記金属基材の表面上に、前記親水性膜を形成する工程:および、
前記正極集電体の親水性膜上に、極性溶媒を含む活物質ペーストを塗布し、乾燥させて、未圧縮の密度が0.9g/cm3~1.5g/cm3である正極活物質層を形成する工程:
を包含する、電池用正極の製造方法。 - 前記金属基材の表面には該金属の酸化膜が予め形成されており、
前記親水性膜を形成する工程よりも前に、前記金属基材の表面に形成された金属酸化膜を除去する工程を含む、請求項11に記載の正極製造方法。 - 前記金属酸化膜を物理的エッチングにより除去する、請求項12に記載の正極製造方法。
- 前記親水性膜を物理蒸着または化学蒸着により形成する、請求項9から13の何れか一つに記載の正極製造方法。
- 前記親水性膜を形成する工程は、前記金属基材上に第1親水性膜を形成する処理と、該第1親水性膜上に第2親水性膜を形成する処理とを含む、請求項11から14の何れか一つに記載の正極製造方法。
- 前記第1親水性膜として、タングステンの炭化物または酸化物からなる親水性膜を形成し、前記第2親水性膜として、カーボンからなり表面が親水性である親水性膜を形成する、請求項15に記載の正極製造方法。
- 前記金属基材として、アルミニウムまたはアルミニウム合金を用いる、請求項11から16の何れか一つに記載の正極製造方法。
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- 2010-01-22 KR KR1020127021863A patent/KR20120113275A/ko not_active Application Discontinuation
- 2010-01-22 WO PCT/JP2010/050850 patent/WO2011089722A1/ja active Application Filing
- 2010-01-22 US US13/521,279 patent/US20120288754A1/en not_active Abandoned
- 2010-01-22 JP JP2011550776A patent/JPWO2011089722A1/ja not_active Ceased
- 2010-01-22 CN CN2010800619933A patent/CN102714297A/zh active Pending
- 2010-01-22 EP EP10843887A patent/EP2528144A1/en not_active Withdrawn
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JP2013225471A (ja) * | 2012-03-23 | 2013-10-31 | Taiheiyo Cement Corp | 二次電池用正極活物質及びその製造方法 |
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JPWO2015159328A1 (ja) * | 2014-04-15 | 2017-04-13 | 株式会社Joled | 薄膜トランジスタ基板の製造方法 |
JP2019216055A (ja) * | 2018-06-14 | 2019-12-19 | トヨタ自動車株式会社 | 非水系二次電池用正極の製造方法 |
JP7011781B2 (ja) | 2018-06-14 | 2022-01-27 | トヨタ自動車株式会社 | 非水系二次電池用正極の製造方法 |
JP2020057584A (ja) * | 2018-09-30 | 2020-04-09 | 寧徳時代新能源科技股▲分▼有限公司Contemporary Amperex Technology Co., Limited | 集電体、極シート及び電気化学デバイス |
Also Published As
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KR20120113275A (ko) | 2012-10-12 |
JPWO2011089722A1 (ja) | 2013-05-20 |
CN102714297A (zh) | 2012-10-03 |
US20120288754A1 (en) | 2012-11-15 |
EP2528144A1 (en) | 2012-11-28 |
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