WO2005006469A1 - 集電構造体及び電極構造体 - Google Patents
集電構造体及び電極構造体 Download PDFInfo
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- WO2005006469A1 WO2005006469A1 PCT/JP2004/010110 JP2004010110W WO2005006469A1 WO 2005006469 A1 WO2005006469 A1 WO 2005006469A1 JP 2004010110 W JP2004010110 W JP 2004010110W WO 2005006469 A1 WO2005006469 A1 WO 2005006469A1
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- current collecting
- substrate
- electrode
- active material
- electrode active
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/66—Current collectors
- H01G11/68—Current collectors characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/66—Current collectors
- H01G11/70—Current collectors characterised by their structure
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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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- 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
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- H—ELECTRICITY
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- 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
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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- 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
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
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- 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
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/663—Selection of materials containing carbon or carbonaceous materials as conductive part, e.g. graphite, carbon fibres
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
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- H01M4/665—Composites
- H01M4/667—Composites in the form of layers, e.g. coatings
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- H—ELECTRICITY
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- H01M4/661—Metal or alloys, e.g. alloy coatings
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/664—Ceramic materials
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/669—Steels
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- H—ELECTRICITY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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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
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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
- Y02E60/13—Energy storage using capacitors
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Definitions
- the present invention relates to a current collecting structure and an electrode structure of an electric component such as a battery and a capacitor.
- a current collecting structure and an electrode structure of an electric component such as a battery and a capacitor use a binder for bonding a current collecting substrate, a conductive additive, and an electrode active material.
- the conductivity and durability were not good.
- An object of the present invention is to obtain a current collecting structure and an electrode structure having good electric conductivity and ionic conductivity. Another object of the present invention is to obtain a current collecting structure and an electrode structure having good durability. Another object of the present invention is to provide a battery and a capacitor with good performance.
- the present invention resides in a current collecting structure, comprising: a current collecting substrate; and a carbon material formed on the current collecting substrate without using a binder. Further, the present invention provides a current collecting structure, comprising: a current collecting substrate; and a rod-shaped, sponge-shaped, or fiber-shaped carbon material formed on the current collecting substrate. It is in. Further, the present invention is an electrode structure, comprising: the current collecting substrate according to any one of the above; and an electrode active material formed on a surface of the carbon material. Further, the present invention resides in an electrode structure comprising: a current collecting substrate; and an electrode active material formed on the current collecting substrate without using a binder. The present invention also resides in an electrode structure including a current collecting substrate and a rod-shaped, sponge-shaped, or fiber-shaped electrode active material formed on the current collecting substrate. Detailed description of the invention
- Electrodes for electrical components such as batteries and capacitors
- Electrodes of electrical components such as batteries and capacitors (electric double-layer capacitors, electric double-layer capacitors) are capable of transferring electricity to or from ions, or of attracting ions.
- the electrode structure of the positive electrode of the battery has LiMn O
- Electrode active material which electrode active material is used and in the case of a negative electrode structure, graphite or hard carbon Which electrode active material is used.
- an electrode active material having a high surface area capable of adhering a large amount of ions such as lithium on the current collecting structure is used.
- An electrolyte substance and a separator (if necessary) are placed between the electrode structures to produce a secondary battery or capacitor.
- the current collecting substrate is a part of the positive electrode and the negative electrode of an electric component such as a battery or a capacitor, and takes in and out of electricity and supports the electrode.
- the current-collecting substrate can be made of a conductive material such as aluminum or copper, which can conduct electricity, or made of ceramic or glass to which a conductive material such as metal or carbon is attached, or a holding material such as stainless steel. Can be used.
- a conductive material such as aluminum or copper, which can conduct electricity, or made of ceramic or glass to which a conductive material such as metal or carbon is attached, or a holding material such as stainless steel.
- the current collecting substrate for example, an aluminum thin film or a copper thin film can be used.
- a material in which a layer or film is formed by depositing a carbon material such as graphite on the surface of ceramic or glass, or a material in which a metal such as aluminum or copper is formed can be used.
- the carbon material is a substance containing carbon as a main component.
- the fender lightning structure is a lightning ⁇ that is one of the lightning poles of the thunderbolt, and the lightning fever is the lightning pole of the thunderbolt. Since a layer of graphite was formed on a board, a carbon layer was formed on the board without using a binder. , .M is a rod, a sponge, a fiber, etc., which has a lot of internal space.) Tk ik. Ik ⁇ ⁇ m.m G. Without using an adhesive.
- the formation of the carbon material is performed by obtaining a prescribed shape such as adhesion, deposition, bonding, and the like.
- a method of forming a carbon material formed by growing is to form a layer or film of a carbon material by a bran method, or
- the carbon material which is controlled to the shape of a bran according to the conditions of the bran, in the form of a rod, sponge, or fiber, adheres to a certain board for lightning strike without using an adhesive, or ⁇ !
- hard carbon, soft carbon, or any of these is used in addition to graphite in addition to the ⁇ -group material.
- the rod shape, sponge shape, or fiber shape refers to a state in which a carbon material is formed on a substrate with a different porosity. That is, the rod shape, sponge shape, or fiber shape refers to a state in which the carbon material has a porosity on the substrate like seabed seaweed or seaweed.
- Rod is a carbon material that protrudes above the chubby, for example the density of the layers is 1. 4gZcm 3, spongy is a carbon material that protrudes upward thinner than rod, for example density is 0.
- the fiber shape is a carbon material protruding more narrowly, for example, having a density of 0.4 g / cm 3 .
- the density of a general layer or film is, for example, 2.4 gZcm 3 . These density values are merely examples and are set arbitrarily.
- the rod shape can be called a rod shape, the sponge shape can be called a chain shape, and the fiber shape can be called a thread shape.
- the carbon material protruding in the shape of a rod, sponge, or fiber preferably has a higher density (lower porosity) near the current collecting substrate and a lower density (higher porosity) above.
- a higher density lower porosity
- higher porosity higher density
- higher porosity lower density
- higher porosity higher porosity
- the electrode structure is obtained by forming at least an electrode layer made of an electrode active material and a conductive material on a current collecting substrate.
- An electrode structure is formed by forming an electrode active material on the surface of a carbon material, such as a rod-shaped, sponge-shaped, or fiber-shaped current collector structure (hereinafter, also referred to as a branched or branched state), to collect electricity.
- a porous electrode layer is formed on a substrate.
- An electrode active material such as a water droplet or a sphere is formed on the surface of the current collecting structure without using an adhesive (binder). Forming is to obtain a fixed state such as adhesion, fixation, and bonding, for example, by growing.
- the average particle size of the electrode active material formed on the surface of the carbon material is preferably 2 ⁇ m (m) or less, more preferably 1 ⁇ m or less, for example, submicron.
- the average particle size of 1-2 microns is the limit of the pulverization process, and an active material smaller than the limit should be formed on the surface of the carbon material.
- the electrode structure is also provided on a current collecting substrate in the form of a rod, a sponge, or a fiber (hereinafter, referred to as a fiber).
- a porous electrode active material having a space inside such as a branched or branched state is formed, and a conductive material is formed thereon.
- the formation method is performed by various methods and conditions.
- An electrode active material such as water droplets or spheres is formed on the current collecting substrate without using an adhesive (binder).
- a conductive material such as graphite is formed on the surface of an electrode active material formed on a current collecting substrate to produce an electrode structure.
- the conductive material is formed in a particle shape or a fiber shape on the surface of the electrode active material.
- the conductive material is also formed on the current collecting substrate in the form of particles or fibers.
- the conductive material is formed on a current collecting substrate which is not covered with the electrode active material. Alternatively, it is formed at high density on the surface of the electrode active material near the current collecting substrate.
- the conductive material is formed over a current collecting substrate that is not covered with the electrode active material, and is formed at a high density on the surface of the electrode active material near the current collecting substrate. With these configurations, the electric resistance can be reduced.
- an electrode structure having a small specific resistance can be obtained, and a high-rate battery can be obtained.
- an electrode structure having high ionic conductivity and high electrical conductivity can be obtained.
- the electrode structure is not affected by the change with time of the binder, so that a long-life electrode structure can be obtained.
- ceramic or glass can be used as the current collecting substrate, a long-lasting and highly durable electrode structure can be obtained.
- an electrode structure with less elasticity due to a temperature change can be obtained.
- treatment at a high temperature becomes possible, manufacturing of the electrode structure can be facilitated, and electrode structures having various structures can be obtained.
- electrolytes such as nonflammable and non-toxic
- the electrolyte can be in various states such as liquid and solid.
- the electrolyte penetrates into the electrode structure, and the electrode active material, the electrolyte, and the conductive material are in a state of high conductivity both electrically and ionically.
- a conductive material such as a rod, a sponge, or a fiber, and an electrode active material are formed on a current-collecting substrate in an arbitrary shape and an arbitrary thickness as an electrode layer having a gap
- an electric capacity is obtained.
- Batteries and capacitors having a large size can be manufactured. With this configuration, the air gap
- the porosity can be arbitrarily adjusted, for example, a porosity of 40% or more can be obtained.
- the conductive material can be formed of node carbon or soft carbon, the electrical characteristics of the electrode structure can be variously changed.
- a conductive material in the form of particles or fibers is formed on the surface of the electrode active material, and the conductive material is not covered with the electrode active material. Some of them have been formed, some have a conductive material formed at high density in the electrode active material near the current collecting substrate, and some have an electrolyte material in the space between the electrode active materials.
- the description “without using an adhesive (binder)” means that the adhesive force of the adhesive (binder) is substantially reduced in forming the current collecting structure and the electrode structure.
- the electrode active material exchanges ions, and there are many materials depending on the type of battery.
- the positive electrode active materials include LiCoO, LiNiO, and LiMnO.
- the negative electrode active material examples include metals such as a carbon-based material and lithium metal.
- a high surface area material can be used as the electrode active material of the capacitor.
- activated carbon obtained by activating a carbon material by a steam activation method, a molten KOH activation method, or the like is preferable.
- the fuel electrode and air electrode of a fuel cell such as PAFC and PEFC can be formed of a sponge-like porous material, for example, a porous carbon structure.
- the electrode of the fuel cell holds a catalyst such as platinum on such a porous material.
- a porous substance, for example, porous carbon can be formed into a sponge shape by a vapor deposition method, which can ensure durability and a strong supporting force, and can also increase the durability of a fuel cell.
- a catalyst such as platinum can be formed on the porous material in various shapes such as a granular shape and a dot shape as in the case of vapor deposition of the electrode active material.
- Carbon self-assembly is used, for example, in nanotechnology, and a structure having voids therein can be obtained by directional interaction without using an adhesive (binder). Thereby, it is possible to form carbon (graphite) or an electrode active material in the form of a rod, a sponge, or a fiber on the current collecting substrate so as to have voids therein.
- the molecular epitaxy method involves irradiating a heated substrate with a molecular beam, for example, to grow a crystal. Artificially, it is not possible to use an adhesive (binder) in a shape intended for a small size structure of about 20 nanometers. Can be crafted. By using this technique, rod-like, sponge-like, or fiber-like carbon (graphite) or an electrode active material can be formed on the current collecting substrate so as to have voids therein.
- Vapor deposition is capable of forming substances on various substrates in a chemical composition, a layer structure, and a thickness, a droplet shape, a spherical shape such as a spherical shape. Also, vapor deposition can provide a high vapor deposition rate.
- a method of depositing a thin film includes providing a substantially evacuated processing chamber with a vapor containing at least one selected gas phase component under various conditions. The vapor is condensed on the heated substrate and forms a liquid phase deposit by maintaining the temperature of the substrate below the condensation temperature of the components and above the sublimation temperature of the gas phase components.
- the vapor material is deposited on the substrate as a substantially constant thickness liquid layer due to the wettability of the substrate surface as a solid layer as in conventional thermal sputtering. . Therefore, it sufficiently adheres to the substrate and ensures the uniformity of the thickness of the deposited material. After cooling, the liquid deposit solidifies. By changing the conditions of vapor deposition variously, vapor deposition of various shapes becomes possible.
- the term "sublimation temperature” refers to the maximum temperature at which a phase deposit can be obtained directly from a matched vapor. The liquid component is then cooled, forming a solid phase layer of the desired substance.
- the present vapor deposition enables vapor deposition without chemically changing a raw material. Forces that are available for one raw material It is possible to provide more than one phase component.
- Two or more phases The components are, for example, a plurality of phase components produced by co-evaporating at least two reagent materials, or those condensed on a substrate.
- the condensed reagent components can react with the liquid phase on the substrate surface after being condensed.
- the present deposition is applicable to depositing a wide variety of layers including thin films of metals, semiconductors, and non-metallic inorganic substances. Useful for forming solid electrolytes and electrodes for batteries. In addition, it can be used for fuel cells and other electromagnetically active (active) devices
- the individual components with the appropriate molecular ratios in the solid are transferred to a heating device such as a furnace. Can be melted. The melt is desirably agitated. Agitation can be performed using a cavitation stirrer.
- a heating device such as a furnace.
- the melt is desirably agitated. Agitation can be performed using a cavitation stirrer.
- the particles can be ground to a size of less than 100 m to form a powder suitable for evaporation.
- the vapor is condensed on the heated substrate by maintaining the temperature of the substrate below the condensation temperature of the gas phase components to form a liquid phase deposit.
- the processing chamber walls are preferably maintained at a temperature sufficient to avoid deposition on the walls, because the deposition of evaporated material on the reactor chamber walls reduces the deposition rate on the substrate. This is because the fine particles may be mixed in the vapor deposition layer. For example, film flakes deposited on process chamber walls can result in particulate mixing in the deposited film. Therefore, it is preferable to set the temperature of the processing chamber and the substrate so as to condense the liquid on the substrate which is on the processing chamber wall. Thus, the temperature of the chamber walls is maintained above the vapor condensation temperature, while the substrate is maintained below the vapor condensation temperature.
- the resulting structure of the solid film that is formed depends on the cooling rate of the deposition liquid. Select the cooling rate according to the particles and the intended use of the particles. As the cooling rate increases, generally The structure of the deposited layer changes from crystalline to microcrystalline, amorphous-crystalline, and amorphous. As used herein, the term non-crystalline refers to a structure having localized microcrystals arranged in a substantially non-crystalline matrix.
- microcrystalline and amorphous crystalline structures exhibit a highly homogeneous chemical composition and sufficient electrochemical properties such as ionic conductivity and electrochemical activity.
- the electrochemical properties of solid electrolyte membranes based on molybdenum oxide based force materials and eutectic oxide and sulfide oxides are microcrystalline and non-crystalline structures, respectively.
- a high value of the force sword inherent energy and a high value of the electrolyte conductivity were exhibited. It is possible to provide the electrodes and the electrolyte material in this manner for making batteries that utilize thick and multi-layered films to deposit and include electrode films deposited on the electrolyte film.
- FIG. 6 discloses a general deposition system 100 employed to deposit materials utilizing vapor condensation.
- the deposition system 100 can include a dosing device 110, a processing chamber 120 having an adjustable working chamber volume, and a valve 20 that allows for separation of the substrate from other portions of the working chamber. Reduction of the working chamber volume during the evaporative Z condensation process may increase the vapor density and vapor condensation rate of the substrate. Evaporation Z The increase in working chamber volume with the valve closed after the condensation process is completed can be used to reduce the temperature of the deposited film material resulting from adiabatic expansion and increase the solidification rate of the film material It is possible to do.
- the cavitation stirring of the melt in the evaporator can be used in conjunction with a system that corrects the composition of the steam.
- a system that corrects the composition of the steam For example, when heavy and light elements evaporate together, it is desirable to correct the vapor composition because the respective elements that make up the vapor have different agility and partial pressure.
- One or more additional evaporation or inlet gas systems should be used in conjunction with the main evaporator to add steam with one or more components, increase the partial pressure of this component, and correct the steam composition. Is possible.
- the electrical resistance of the vapor depends on the nature of the composition. In this case, high By measuring the current between the two specific electrodes at a voltage (eg, 500 V) and correcting as described above, it is possible to control the composition of the vapor “in situ”.
- a voltage eg, 500 V
- This method allows the production of thin films of different materials on various substrates, such as metal substrates, ceramic substrates, etc., and substantially avoids segregation in the heating bath and provides high homogeneity. It provides a composition of the gas composition.
- the vacuum condensation method involves evaporating at least one solid source material
- the resulting thickness, structural homogeneity, physical and chemical properties of the deposited film are primarily: It turns out that it depends on the parameters.
- the parameters are: (1) the temperature of the evaporator, (2) the temperature of the vapor of the vaporized substance, (3) the pressure and density of the vapor of the vaporized substance, (4) the temperature and state of the substrate surface, (5) There is a deposition rate of the condensed film material and (6) a cooling rate of the condensed film material.
- the desired membrane material component is generally delivered as a powder 3 into the dosing device and is delivered to the processing chamber via a chute 4 using a dosing-dollar 2.
- Dispensing-One dollar 2 can be controlled by the electromagnetic lever 1.
- the processing chamber is heated by a heating device 6 such as a resistance heating element that can be protected by a shield 7.
- An inert gas such as argon, can be sent through the cane 5 directed to the substrate 12 side.
- a second inlet for inert gas via pipe 8 can be installed to allow any gas to flow through the deposited film material.
- the preheated gas can also be sent into the chamber via pipe 21.
- the substrate can be heated by the heater 11.
- the temperature of the substrate can be monitored by thermocouple 13.
- a vacuum valve 20 is provided to enable the reactor chamber to be evacuated.
- the outer compartment 15 of the processing chamber is preferably expandable and contractible so that the volume of the processing chamber can be changed.
- the evaporator 17 is capable of melting and evaporating one or more components to be evaporated. [0037]
- the temperature profile of the evaporator can be adjusted to ensure pre-drying and outgassing of the feedstock. When increasing the vapor density, the evaporation rate can be reduced. This decrease can be corrected by increasing the corresponding temperature of the evaporator. However, too rapid a temperature increase at the start of the process can lead to the formation of macroscopic droplets.
- macroscopic droplets indicate that there was insufficient adhesion to the substrate during condensation on the substrate.
- macroscopic droplets are useful when applied to the final stage of the process, and condensation on already formed film material will result in the condensation of that film material.
- the specific area can be increased.
- an increased specific membrane area can be useful in battery applications because it enhances the force sword or electrochemical properties of the solid electrolyte.
- the temperature profile shown in FIG. 7 includes three stages. The third stage, at temperatures up to 2000 ° C, is where evaporation occurs. The first low temperature stage at 100 ° C-150 ° C is the drying stage. The intermediate stage between 900 and 1100 ° C is the deaeration stage. The third stage, at temperatures up to 2000 ° C, is where evaporation occurs.
- the temperature of the vapor determines the kinetic energy of the atoms and molecules of the vapor.
- E 3Z2kT
- the temperature near where the substrate is deposited is low.
- the phase corresponding to the substrate temperature is located in the region of the stable liquid phase 320 at the pressure P. Therefore,
- This vapor deposition is to generate vapor condensation on the substrate.
- the vapor density and related thermodynamic parameters are determined by the rate of evaporation of the starting material and the rate of condensation on the substrate.
- vapor condensation on the substrate will generally be initiated at a higher pressure compared to its equilibrium value (located on the diagram line). This is because the vapors must reach the required degree of supersaturation when moving to a condensed state.
- An independent temperature control system is preferably provided for controlling the temperature of the evaporator and the substrate. The temperature control system is preferably controlled and adjusted by a computer.
- An independent temperature control system for the evaporator and the substrate makes it possible to maintain the desired temperature distribution in the working chamber substantially independent of the spray rate.
- forced cooling can utilize forced cooling to solidify the liquid more quickly.
- an inert gas jet can be used to cool the liquid to be deposited.
- the structure of the solid formed generally depends on the cooling rate. As the cooling rate increases, the crystallinity generally decreases.
- the crystal structure is generally formed at a maximum cooling rate of 2 KZs. Is done. Increasing the cooling rate from approximately 5 KZs to 7 KZs generally leads to the formation of a eutectic particulate structure.
- Amorphous crystalline structures are composed of extremely dispersed crystalline phases with a wide, homogeneous amorphous domain and can include different types of solid solutions.
- the present vapor deposition can be used for the purpose of forming a layer structure different from the structure of the initial raw material.
- the initial material typically utilizes a eutectic composition that exhibits a melting temperature in the range of 800 ° C to 1000 ° C.
- a condensed thin liquid layer material is first formed and solidified under controlled cooling. Controlled cooling can be performed with a forced gas such as argon injection.
- the substrate temperature and cooling rate are selected to form an amorphous-crystalline structure with enhanced ionic conductivity at room temperature.
- Such a structure enables a 500-1000fold (fold) increase in the ionic conductivity of the electrolyte, which creates vacancies on the interface between crystalline phases inserted in the amorphous matrix. It is thought to occur.
- Various studies have been reported on intercalated phases that increase the conductivity of solid electrolytes, such as aluminum, silicon oxide, lithium halides, and mechanical mixing of silver and copper. See, for example, Wagner Jr., J. B. in: C. A. C. A. C. Sequeira, A. Hooper, Sequeira, and A. Hooper, Solid State Batteries, Matinus Nijhof f Publishing, Dordrecht, 1985, p. 77.
- This deposition can enhance this effect because the micropores and other macroscopic defects are minimal. Calo, this effect can be enhanced by adding ion migration along the vacancies between the closest planes of the crystal lattice.
- the cooling treatment can be adjusted based on the desired layer properties.
- forced gas cooling eg, Ar
- the gas can be directed toward the substrate. This makes it possible to prevent thermal decomposition of the layer. If a high cooling rate is required to form the desired deposited layer force amorphous crystalline structure, the cooling jet can be directed toward the deposited layer. If high thermal stresses are known to develop, the jet can be directed to both sides of the deposited layer.
- the deposition rate can be increased by reducing the volume of the processing chamber. Reduced processing chamber volume can increase vapor density and increase deposition rate.
- Multi-layer deposition of the same or different materials can be achieved by using a cyclic 'multi-step process.
- the evaporator can be filled with the desired source, the source to be evaporated, and the vapor condensed on the substrate.
- the processing chamber can be evacuated.
- the evaporator can be refilled with the same or different raw materials, and the above steps are repeated.
- a refilling step is not required.
- Cyclic processes can be used to produce relatively thick layers (eg,> 20 m), and if a non-optimal cooling process results in a substantial crystalline structure, one-step deposition and In comparison, it has a microcrystalline structure or an amorphous-crystalline structure. Relatively thick layers can be produced, and each cycle uses a cyclic process in which only the thin layers are rapidly cooled to retain microcrystalline or amorphous crystals.
- cooling In general, effective cooling of relatively thick layers (eg,> 20 m) obtained by a one-step deposition method involves inherent difficulties. Cooling follows after deposition of substantially the entire thickness of the layer. Because many materials, including most electrolyte and electrode materials, exhibit low thermal conductivity, the cooling rate required to form an amorphous crystalline structure is simply Obtained with a thin outer surface of the layer. Removal of heat inside the layer is inefficient, with the result that a crystalline (eg, polycrystalline) structure is generally formed throughout the material. During the multilayer cyclic deposition process, multiple cooling and deposition steps are used, with cooling occurring after each thin layer deposition. As a result, cooling is more efficient than conventional cooling processes.
- the vapor condensate obtained by performing the cooling process creates a composite layer (for example, force sword Z solid electrolyte) having sufficient adhesion between the respective layers. If interval deposition is used for one or more layers, not only sufficient intra-layer deposition but also extra-layer deposition will be sufficient.
- melt agitation can be useful because the evaporation process power is primarily driven by the surface force of the melt. If large amounts of material are evaporated, convection in the liquid will not have enough time for the highest evaporation rate to compensate for the lack of components on the melt surface.
- the adhesion of the deposited layer generally depends on the state of the specific substrate surface. By pre-cleaning the surface of the substrate before vapor deposition, the adhesion can be enhanced. For example, solution cleaning, ion beam and plasma treatments known in the art can be used.
- Pulse deposition can be used in some cases to produce a layer with improved surface smoothness.
- pulse deposition a portion of the desired layer thickness is deposited, The deposition process is suspended for a period, and then another layer is deposited.
- Pulsed deposition can be achieved using a shutter that can separate the evaporated vapor from the processing chamber. For example, the shutter can be opened for a short time when the vapor reaches a predetermined temperature and the processing chamber walls and the substrate reach a desired temperature. If the shirt is properly sealed, the pressure will increase near the heater. As a result, the flow of deposition material will be directed to the substrate.
- one or more gases can be sent to the processing chamber during the deposition process containing the desired additional components, before cooling the substrate.
- the gas is preheated to a desired temperature, such as the temperature of a reactor chamber.
- Thin additional metal layers such as Cu, Au, Pt, Al, Al-Li alloys or Li layers having a thickness of up to approximately 5 ⁇ m, may be deposited on the surface of the deposited layer. Is possible.
- This layer can be used to determine the properties of the layer formed from the vapor condensation process. To this end, the electrical resistance (expressed in ohm-cm) between the substrate and the metallic layer can be measured via the layer formed by the vapor condensation process. is there. If the measured resistance is lower than the value calculated from the specific conductivity and the size of the layer geometry, it is assumed that a layer with a high porosity is present and that there is a high Z or defect concentration. (See Figure 8).
- the low electrical resistance due to the use of this deposition is due to sufficient adhesion to solid electrolytes and force sword materials, and results in the deposited metal passing through perforated macrocracks and other defects in the layer. It is thought to occur as This reduces local shorts and, in general, reduces the electrical resistance of the layer.
- FIG. 9 shows an example of a current collecting structure in which a graphite current collecting layer is formed by vapor deposition on an aluminum current collecting substrate.
- the deposition conditions were changed variously.
- FIG. 10, FIG. 11, and FIG. 12 are examples of a current collecting structure in which rod-like, sponge-like, and fiber-like graphite current collecting layers are formed by vapor deposition on a current collecting substrate.
- Figure 10 (B) Figure 12 (B) is all 2000x magnification. It is a large photograph (SEM photograph). As described above, a current collecting structure having a graphite having a high porosity can be obtained, and the function of a conductive additive can also be obtained.
- FIG. 1 and 2 show examples of electrode active material structures in which an electrode active material is formed on a current-collecting substrate.
- FIG. 1 shows an example in which an electrode active material is formed in a dot shape on a current collecting substrate by vapor deposition
- FIG. 2 shows an example in which a rod-shaped, sponge-shaped, or fiber-shaped electrode active material is formed. The deposition conditions were varied.
- Figure 1 (B) Figure 2 (B) shows the spinel LiMn O electrode active material (white area).
- FIG. 2 shows that an electrode active material structure having a high porosity electrode active material can be obtained.
- FIG. 3 is a schematic diagram of an electrode structure having the electrode layer thus formed
- FIG. 4 shows an electrode structure in which a fiber-like graphite is formed.
- Figure 4 (B) shows the electrode active material surface of spinel LiMnO.
- FIG. 4 is an example of an electrode structure obtained by forming a fiber-like graphite on a current collecting substrate surface.
- Fig. 4 (B) is an enlarged photograph (SEM photograph) of 4000 times.
- an electrode structure having a high porosity can be obtained without using an adhesive.
- an electrolyte material such as a liquid or a solid enters the electrode structure, and the electrode active material, the electrolyte material, and the conductive material are brought into a state of high conductivity both electrically and ionically.
- Fig. 5 (A) shows a diagram in which a conductive material (shaded layer on the substrate surface) is formed on a V-collecting substrate covered with an electrode active material
- Fig. 5 (B) Shows a diagram in which a conductive material (hatched portion of the electrode active material on the substrate surface) is formed at high density on the surface of the electrode active material near the current collecting substrate.
- FIGS. 13 (A) to 13 (C) are schematic diagrams of electrode structures in which a granular electrode active material is formed by vapor deposition on the rod-shaped, sponge-shaped, or fiber-shaped graphite surfaces of the current collecting structure.
- FIG. 14 (B) is an example of an electrode structure obtained by forming particles having a spinel structure of lithium manganese oxide on the rod-like graphite of FIG. 14 (A) by vapor deposition.
- Fig. 14 (B) is a 2000 times enlarged photograph (SEM photograph), in which the granular substance is a particle having a spinel structure.
- an electrode structure having an electrode layer with a high porosity can be obtained by vapor deposition without using an adhesive (binder). This allows sufficient electrolyte to penetrate the electrode structure
- the electrode active material, the electrolyte, and the graphite become electrically and ionically highly conductive.
- the alloy current collecting substrate was formed into a fiber-like shape using a vapor deposition technique.
- This positive electrode structure is composed of LiMn O and carbon and has a diameter of 16 mm and a thickness of about 10 m.
- FIG. 17 shows a cross-sectional structure of the positive electrode structure.
- the lower black band 400 is the current collecting substrate of A1.
- a porous current-collecting layer is formed on the current-collecting substrate, which also acts as a carbon material.
- FIG. 17 shows the carbon material, the electrode active material, and the voids on the current collecting substrate.
- a Li alloy was used for the negative electrode structure.
- the electrolyte is LiPF
- FIG. 15 shows the measurement data of the battery. From FIG. 15, it can be seen that a high discharge rate of 100 C or more can be obtained. It is possible to extract about 20 times more current than conventional lithium secondary batteries.
- the positive electrode structure of the lithium ion battery 2 As the positive electrode structure of the lithium ion battery 2, the same one as in the lithium ion battery 1 was used. This was put into a beaker together with the negative electrode structure and the electrolyte, to produce a battery.
- a Li alloy was used for the negative electrode structure.
- the electrolyte used is LiPF with a solution resistance of 19 ⁇ .
- FIG. 16 shows the data. This data was measured using a test method called the cyclic voltammetry (CV) method, based on the response of the electrode.
- CV cyclic voltammetry
- FIG. 1 is a diagram of an electrode active material structure in which an electrode active material is formed on a current collecting substrate.
- FIG. 2 is a diagram of a sponge-like or fiber-like electrode active material structure in which an electrode active material is formed on a current collecting substrate.
- FIG. 3 is a schematic diagram of an electrode structure in which granular graphite is formed on an electrode active material formed on a current collecting substrate.
- FIG. 4 is a diagram of an electrode structure in which fiber-like graphite is formed on an electrode active material formed on a current collecting substrate.
- FIG. 5 is a schematic diagram of an electrode structure in which a graphite is formed near a current collecting substrate and an electrode active material is further formed.
- FIG. 6 is a schematic diagram of a vapor deposition device.
- FIG. 7 is a graph showing temperature characteristics of solid electrolyte deposition.
- FIG. 8 is a schematic diagram illustrating thermodynamics of steam.
- FIG. 9 is a diagram of a current collecting structure in which a graphite layer is formed on a current collecting substrate.
- FIG. 10 is a view of a current collecting structure on which rod-shaped graphite is formed.
- FIG. 11 is a view of a current collecting structure in which sponge-like graphite is formed.
- FIG. 12 is a diagram of a current collecting structure on which fiber-like graphite is formed.
- FIG. 13 is a schematic diagram of an electrode structure in which an electrode active material is formed on a graphite, sponge, or fiber graphite surface.
- FIG. 14 is a diagram of an electrode structure in which an electrode active material is formed on a rod-shaped graphite surface.
- FIG. 15 is a view showing a discharge rate of a battery pack and a cell.
- FIG. 16 is a diagram showing the responsivity of the electrode of the battery beaker. 1.
- Cell vertical axis: iZmA, horizontal axis: EZVvslMLi + Z Li).
- FIG. 17 is a SEM photograph of an electrode structure.
- Electromagnetic lever 2: Dosing- $, 3: Powder, 4: Chute, 5: Pipe, 6: Heating device, 7: Shield, 8: Pipe, 11: Heater, 12: Substrate, 13: Thermocouple ( Thermocouple), 14: shutter, 15: outer compartment of processing chamber, 17: evaporator, 18: heater, 20: vacuum valve, 21: pipe, 100: evaporation system, 110: dosing device, 120: processing channel , 310: gas phase, 320: liquid phase, 400: aluminum foil, 410: porous electrode layer.
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US10/565,128 US20060175704A1 (en) | 2003-07-15 | 2004-07-15 | Current collecting structure and electrode structure |
JP2005511587A JPWO2005006469A1 (ja) | 2003-07-15 | 2004-07-15 | 集電構造体及び電極構造体 |
EP04747576A EP1662592A4 (en) | 2003-07-15 | 2004-07-15 | ELECTRICITY STRUCTURE AND ELECTRON STRUCTURE |
CN2004800201147A CN1823439B (zh) | 2003-07-15 | 2004-07-15 | 集电结构体以及电极结构体 |
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JP2003274990 | 2003-07-15 | ||
JP2003-274990 | 2003-07-15 | ||
JP2003-296689 | 2003-08-20 | ||
JP2003296689 | 2003-08-20 | ||
JP2004-206268 | 2004-07-13 | ||
JP2004206268 | 2004-07-13 |
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PCT/JP2004/010110 WO2005006469A1 (ja) | 2003-07-15 | 2004-07-15 | 集電構造体及び電極構造体 |
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US (1) | US20060175704A1 (ja) |
EP (1) | EP1662592A4 (ja) |
JP (1) | JPWO2005006469A1 (ja) |
CN (1) | CN1823439B (ja) |
WO (1) | WO2005006469A1 (ja) |
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JP2006261399A (ja) * | 2005-03-17 | 2006-09-28 | Ricoh Elemex Corp | 蓄電デバイス |
JP2006278239A (ja) * | 2005-03-30 | 2006-10-12 | Sharp Corp | リチウム二次電池、リチウム二次電池用正極板及びそれらの製造方法 |
JP4550640B2 (ja) * | 2005-03-30 | 2010-09-22 | シャープ株式会社 | リチウム二次電池、リチウム二次電池用正極板及びそれらの製造方法 |
US7972731B2 (en) * | 2006-03-08 | 2011-07-05 | Enerl, Inc. | Electrode for cell of energy storage device and method of forming the same |
JP2008270092A (ja) * | 2007-04-24 | 2008-11-06 | Toyota Motor Corp | 非水電解質電池用集電体、非水電解質電池用集電体の製造方法及び非水電解質電池 |
JP2009163989A (ja) * | 2008-01-07 | 2009-07-23 | Sumitomo Electric Ind Ltd | リチウム電池、リチウム電池用正極およびその製造方法 |
KR20110100275A (ko) * | 2008-12-12 | 2011-09-09 | 어플라이드 머티어리얼스, 인코포레이티드 | 하이브리드 나노―탄소 층을 갖는 삼차원 배터리 |
KR101657146B1 (ko) * | 2008-12-12 | 2016-09-13 | 어플라이드 머티어리얼스, 인코포레이티드 | 하이브리드 나노―탄소 층을 갖는 삼차원 배터리 |
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US20060175704A1 (en) | 2006-08-10 |
EP1662592A4 (en) | 2008-09-24 |
CN1823439A (zh) | 2006-08-23 |
EP1662592A1 (en) | 2006-05-31 |
CN1823439B (zh) | 2013-07-17 |
JPWO2005006469A1 (ja) | 2007-09-20 |
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