WO2021100198A1 - Batterie secondaire au lithium et son procédé de fabrication - Google Patents
Batterie secondaire au lithium et son procédé de fabrication Download PDFInfo
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- WO2021100198A1 WO2021100198A1 PCT/JP2019/045810 JP2019045810W WO2021100198A1 WO 2021100198 A1 WO2021100198 A1 WO 2021100198A1 JP 2019045810 W JP2019045810 W JP 2019045810W WO 2021100198 A1 WO2021100198 A1 WO 2021100198A1
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- lithium
- positive electrode
- electrolyte
- secondary battery
- lithium secondary
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
- H01M10/0585—Construction or manufacture of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Definitions
- the present invention relates to a lithium secondary battery and a method for manufacturing the same.
- Lithium-ion secondary batteries that use lithium-ion insertion / removal reactions are widely used as secondary batteries with high energy density in various electronic devices, automobile power supplies, and power storage applications. Research and development of electrode materials and electrolyte materials are underway for the purpose of improving the performance and reducing the cost.
- Non-Patent Document 1 Flexible batteries are reported, for example, in Non-Patent Document 1.
- the battery is reported to be thin, bendable, and exhibit a discharge capacity of approximately 250 ⁇ Ah / g with a current density of 0.1 mA / cm 2.
- a lithium secondary battery that is thin and can be bent is being studied.
- battery materials that transmit visible light have also been reported.
- a battery that transmits visible light has a low energy density, it is necessary to use a large amount of battery material, and the current situation is that it has not been put into practical use.
- a battery that has transparency and flexibility for visible light has a high output voltage, and has a high energy density can be put into practical use, it is possible to greatly expand the design and application range of IoT devices. There is a problem that the battery does not exist.
- the present invention has been made in view of this problem, and an object of the present invention is to provide a lithium secondary battery having a high output voltage and a method for manufacturing the same, which has both transparency and flexibility for visible light.
- the lithium secondary battery according to one aspect of the present invention includes a positive electrode containing a substance formed on a flexible transparent film substrate and capable of inserting and removing lithium ions, and a transparent electrolyte having lithium ion conductivity.
- the positive electrode comprises a metallic lithium formed on a flexible transparent film substrate, a lithium-containing substance, and a negative electrode formed of either a metal capable of inserting and removing ions, and the positive electrode is made of LiCoPO4X or Li2CoPO4X.
- the gist is that halogen was added to X.
- the method for manufacturing a lithium secondary battery according to one aspect of the present invention is a positive electrode film formation in which a positive electrode containing a substance capable of inserting and removing lithium ions formed on a flexible transparent film substrate is formed.
- a lithium secondary battery having a high output voltage and a method for manufacturing the same, which has both transparency and flexibility for visible light.
- FIG. 1 It is a schematic diagram which shows the basic structure of the lithium secondary battery which concerns on this embodiment. It is a flowchart which shows the procedure for manufacturing the lithium secondary battery shown in FIG. It is a figure which shows an example of charge / discharge characteristics of the lithium secondary battery shown in FIG. It is a figure which shows an example of the charge / discharge cycle characteristic of the lithium secondary battery shown in FIG. It is a figure which shows an example of the light transmission characteristic of the lithium secondary battery shown in FIG.
- FIG. 1 is a schematic view showing a basic configuration of a lithium secondary battery according to the present embodiment.
- 1 (a) is a plan view
- FIG. 1 (b) is a side view.
- hatching is provided so that the laminated layers can be easily seen.
- the flexible positive electrode side transparent film substrate 4 and the negative electrode side transparent film substrate 5 having visible light transmission are sandwiched between the laminated films 7 and laminated.
- the films 7 are heat-bonded to each other.
- the positive electrode 1, the electrolyte 2, and the negative electrode 3 are laminated and arranged in the laminated film 7.
- the positive electrode terminal 8 is located on the outside of the laminated film 7 from one short side of the positive electrode side transparent film substrate 4, and the negative electrode terminal 9 is located on the outside of the laminated film 7 from one short side of the negative electrode side transparent film substrate 5. It is protruding. Voltage and current can be taken out from between the positive electrode terminal 8 and the negative electrode terminal 9.
- the positive electrode terminal 8 and the negative electrode terminal 9 may be an extension of the transparent electrode film 6 described later, or may be made of metal.
- the lithium secondary battery 100 has a configuration in which a positive electrode 1, an electrolyte 2, and a negative electrode 3 are laminated.
- the positive electrode 1 is formed on a transparent conductive film 6 formed on the entire surface of the flexible positive electrode side transparent film substrate 4 facing the negative electrode 3 with a predetermined thickness of a substance capable of inserting and removing lithium ions. Is formed.
- the negative electrode 3 contains a substance capable of inserting and removing lithium ions on the transparent conductive film 6 formed on the entire surface of the flexible negative electrode side transparent film substrate 5 facing the positive electrode 1. It is formed by forming a film with a predetermined thickness.
- the positive electrode side transparent film substrate 4 and the negative electrode side transparent film substrate 5 are made of, for example, polyethylene terephthalate (PET) or polypropylene (PP).
- PET polyethylene terephthalate
- PP polypropylene
- the visible light transmittance of PET and PP is about 90%.
- the positive electrode side transparent film substrate 4 and the negative electrode side transparent film substrate 5 may be made of the same material or may be made of different materials.
- the positive electrode 1 and the negative electrode 3 are arranged so as to face each other with the electrolyte 2 interposed therebetween.
- the electrolyte 2 a conventional organic electrolyte containing lithium ions or an aqueous electrolyte can be used.
- a solid electrolyte such as a polymer electrolyte containing lithium ions can also be used as long as it transmits visible light.
- a separator (not shown) may be included between the positive electrode 1 and the negative electrode 3.
- the light-transmitting separator include polyethylene (PE), polypropylene (PP), and an ion exchange membrane.
- the separator may be impregnated with the electrolyte 2.
- the organic electrolyte or the aqueous electrolyte may be impregnated with the polymer electrolyte or the like.
- both electrodes may be arranged so as to be in contact with them.
- the lithium secondary battery 100 has a positive electrode 1 formed on the positive electrode side transparent film substrate 4 and containing a substance capable of inserting and removing lithium ions, and lithium ion conductivity.
- the transparent electrolyte 2 is provided with a negative electrode 3 formed of a substance capable of dissolving and precipitating lithium or inserting and removing lithium ions on the negative electrode side transparent film substrate 5.
- FIG. 2 is a flowchart showing a procedure for manufacturing the lithium secondary battery 100 according to the present embodiment. A method for manufacturing the lithium secondary battery 100 will be described with reference to FIG.
- each of the positive electrode side transparent film substrate 4 and the negative electrode side transparent film substrate 5 is cut into a predetermined size (step S1).
- the sizes of the positive electrode side and the negative electrode side transparent film substrates 4 and 5 are, for example, 100 mm in length ⁇ 50 mm in width.
- the thickness is, for example, 0.1 mm.
- the transparent conductive film 6 on the positive electrode 1 side is formed (step S2).
- the transparent conductive film 6 is formed on the surface of the positive electrode side transparent film substrate 4.
- the transparent conductive film 6 is formed of ITO (Indium Tin Oxide).
- the transparent conductive film 6 was coated with ITO to a thickness of 150 nm by an RF sputtering method. Sputtering was carried out using an ITO (5wt% SnO 2 ) target with an RF output of 100 W while flowing argon (1.0 Pa).
- a positive electrode 1 is formed on the transparent electrode film 6 (step S3).
- the positive electrode 1 for example, lithium cobalt oxide (Li2CoPO4F), which is a material of Experimental Example 1 described later, is formed into a film with a thickness of 100 nm by an RF sputtering method (step S3).
- the film formation of the positive electrode 1 was carried out using a ceramic target of Li2CoPO4F, the flow partial pressure ratio of argon and oxygen was 3: 1, the total gas pressure was 3.7 Pa, and the RF output was 800 W.
- the transparent conductive film 6 on the negative electrode 3 side is formed (step S4).
- the transparent electrode film 6 on the negative electrode 3 side is the same as that on the positive electrode 1 side.
- the negative electrode 3 is formed (step S5).
- the negative electrode 3 is formed by forming a film of lithium titanate (Li4Ti5O12), which is a material of, for example, Experimental Example 1 described later, to a thickness of 100 nm by an RF sputtering method.
- the film formation of the negative electrode 3 was carried out using a ceramic target of Li4Ti5O12, the flow partial pressure ratio of argon and oxygen was 3: 1, the total gas pressure was 4.0 Pa, and the RF output was 700 W.
- the size of the positive electrode 1 and the negative electrode 3 is, for example, 90 mm in length ⁇ 50 mm in width.
- the size of the bipolar film is smaller than that of the transparent electrode film 6.
- the bipolar transparent electrode film 6 formed as described above has a portion protruding with a length of 10 mm in length.
- the relevant portions are used as the positive electrode terminal 8 and the negative electrode terminal 8 leaving a range of 10 mm in length ⁇ 10 mm in width so that they do not face each other.
- the positive electrode side transparent film substrate 4 and the transparent electrode film 6, and the negative electrode side transparent film substrate 5 and the transparent electrode film 6 are other than the electrode terminals.
- a range of 10 mm in length x 40 mm in width is cut out.
- Electrolyte 2 is an organic electrolytic solution prepared by dissolving 1 mol / L of lithium bistrifluoromethanesulfonylimide (LiTFSI) as a lithium salt in polyvinyl fluoride (PVdF) powder and propylene carbonate (PC), which are binders, and a dispersion medium.
- the weight ratio of tetrahydrofuran (THF) as a 1: 9: mixed solution at 10 at a dew point of -50 ° C. or less of the dry air, and stirred for 1 hour at 60 ° C., poured 50ml solution in a Petri dish of 200 mm phi, 50 ° C.
- Electrolyte 2 having a transparent film having a thickness of 1 ⁇ m was prepared by vacuum drying in the above for 12 hours.
- the battery is assembled (step S8).
- the positive electrode side transparent film substrate 4 on which the positive electrode 1 is formed, the negative electrode side transparent film substrate 5 on which the negative electrode 3 is formed, and the electrolyte 2 are laminated so that the positive electrode 1 and the negative electrode 3 face each other with the electrolyte 2 interposed therebetween.
- the thickness of the hot-pressed battery is about 400 ⁇ m.
- a positive electrode 1 containing a substance capable of inserting and removing lithium ions formed on a flexible transparent film substrate is formed.
- Positive electrode film formation step S3 electrolyte formation step S7 for forming a transparent electrolyte having lithium ion conductivity, and a metal formed on a flexible transparent film substrate, which is capable of inserting and removing lithium or lithium ions.
- the positive electrode forming step S3 forms Li2CoPO4F.
- the lithium secondary battery 100 manufactured by the above manufacturing method was evaluated by performing the following charge / discharge test and charge / discharge cycle test.
- the charge / discharge test was performed using a general charge / discharge system (for example, Hokuto Denko: SD8 charge / discharge system).
- a general charge / discharge system for example, Hokuto Denko: SD8 charge / discharge system.
- the current density per effective area of the positive electrode 1 was energized at 1 ⁇ A / cm 2 , and the final charging voltage was 4.5 V.
- the discharge conditions were a current density of 1 ⁇ A / cm 2 and a discharge end voltage of 2.5 V.
- the charge / discharge test was performed in a constant temperature bath at 25 ° C. (the atmosphere is a normal atmosphere).
- FIG. 3 is a diagram showing an example of charge / discharge characteristics measured in the charge / discharge test.
- the horizontal axis of FIG. 3 is the capacity [mAh], and the vertical axis is the battery voltage [V].
- the broken line shows the charging characteristic and the solid line shows the discharging characteristic.
- the charge / discharge cycle test is a test that evaluates the deterioration of the discharge capacity by repeating charging / discharging.
- FIG. 4 is a diagram showing a characteristic example of the charge / discharge cycle test.
- the horizontal axis of FIG. 4 is the number of cycles, and the vertical axis is the discharge capacity [mAh]. As shown in FIG. 4, it shows a characteristic that the discharge capacity decreases when the charge / discharge cycle is repeated.
- a battery produced by changing the amount of positive electrode material of the lithium secondary battery 100 according to the present embodiment as shown in the following experimental example was evaluated by the above charge / discharge test and charge / discharge cycle test. An experimental example will be described before the evaluation result.
- Li2CoPO4F which is the amount of positive electrode material in Experimental Example 1, is composed of the raw materials reagents lithium cobalt oxide (LiCoPO4: High Purity Chemistry Co., Ltd.) and lithium fluoride (LiF: Fuji Film Wako Pure Chemical Industries, Ltd.). Weighed so that the molar ratio of F was 1: 1 and crushed and mixed well in a dairy pot. Then, the obtained mixture was filled in a crucible and prepared by heating at 780 ° C. for 24 hours in an argon atmosphere using an electric furnace.
- LiCoPO4F which is the amount of positive electrode material in Experimental Example 2
- Co F of cobalt phosphate
- LiF Fuji Film Wako Pure Chemical Industries, Ltd.
- Li2CoPO4Cl which is the amount of positive electrode material in Experimental Example 3, is composed of lithium cobalt oxide (LiCoPO4: High Purity Chemistry Co., Ltd.) and lithium chloride (LiCl: Fuji Film Wako Pure Chemical Industries, Ltd.) as raw materials. Weighed so that the molar ratio was 1: 1 and crushed and mixed well in a dairy pot. Then, the obtained mixture was filled in a crucible and heated at 550 ° C. for 36 hours in an argon atmosphere using an electric furnace.
- LiCoPO4Cl which is the amount of positive electrode material in Experimental Example 4, is made by using cobalt phosphate (CoPO4: High Purity Chemistry Co., Ltd.) and lithium chloride (LiCl: Fuji Film Wako Pure Chemical Industries, Ltd.) as raw materials in Co: F. Weighed so that the molar ratio was 1: 1 and crushed and mixed well in a dairy pot. Then, the obtained mixture was filled in a crucible and heated at 550 ° C. for 36 hours in an argon atmosphere using an electric furnace.
- Li2CoPO4Br which is the amount of positive electrode material in Experimental Example 5, is composed of the raw materials reagents lithium cobalt oxide (LiCoPO4: High Purity Chemistry Co., Ltd.) and lithium bromide (LiBr: Fuji Film Wako Pure Chemical Industries, Ltd.). Weighed so that the molar ratio of F was 1: 1 and crushed and mixed well in a dairy pot. Then, the obtained mixture was filled in a crucible and heated at 480 ° C. for 48 hours in an argon atmosphere using an electric furnace.
- LiCoPO4Br which is the amount of positive electrode material in Experimental Example 6, is a Co: F of cobalt phosphate (CoPO4: High Purity Chemistry Co., Ltd.) and lithium bromide (LiBr: Fuji Film Wako Pure Chemical Industries, Ltd.), which are the raw materials. Weighed so that the molar ratio was 1: 1 and crushed and mixed well in a dairy pot. Then, the obtained mixture was filled in a crucible and heated at 480 ° C. for 48 hours in an argon atmosphere using an electric furnace.
- Li2CoPO4Br which is the amount of positive electrode material in Experimental Example 7, is composed of the raw materials reagents lithium cobalt oxide (LiCoPO4: High Purity Chemistry Co., Ltd.) and lithium iodide (LiI: Fuji Film Wako Pure Chemical Industries, Ltd.). Weighed so that the molar ratio of F was 1: 1 and crushed and mixed well in a dairy pot. Then, the obtained mixture was filled in a crucible and prepared by heating at 400 ° C. for 72 hours in an argon atmosphere using an electric furnace.
- LiCoPO4I which is the amount of positive electrode material in Experimental Example 8, is a Co: F of cobalt phosphate (CoPO4: High Purity Chemistry Co., Ltd.) and lithium iodide (LiI: Fuji Film Wako Pure Chemical Industries, Ltd.), which are the raw materials. Weighed so that the molar ratio was 1: 1 and crushed and mixed well in a mortar. Then, the obtained mixture was filled in a crucible and prepared by heating at 400 ° C. for 72 hours in an argon atmosphere using an electric furnace.
- the amount of the positive electrode material in Experimental Examples 1 to 8 above is a lithium oxide obtained by adding a halogen to X of LiCoPO4X or Li2CoPO4X.
- LiCoPO4F LiCoPO4F
- Experimental Example 4 LiCoPO4Cl
- Experimental Example 6 LiCoPO4Br
- Experimental Example 8 LiCoPO4I, respectively. Is called halogen. Therefore, LiCoPO4X is a lithium oxide in which halogen is added to X.
- Li2CoPO4F Li2CoPO4F
- Experimental Example 3 Li2CoPO4Cl
- Experimental Example 5 Li2CoPO4Br
- Experimental Example 7 Li2CoPO4Br.
- Li2CoPO4X is a lithium oxide in which halogen is added to X.
- a polymer electrolyte was used as the electrolyte 2 of Experimental Examples 1 to 8.
- the material of the negative electrode is lithium titanate (Li4Ti5O12).
- Table 1 shows the results of evaluating the lithium secondary batteries of Experimental Examples 1 to 8 by the above evaluation method.
- the average discharge voltage of the lithium secondary batteries of Experimental Examples 1 to 8 according to this embodiment is 4.0 V.
- the average discharge capacity retention rate in the 20th cycle is 94%.
- the lithium secondary batteries of Experimental Examples 1 to 8 had a high output voltage and showed practical characteristics.
- Experimental Example 9 is a lithium secondary battery in which the electrolyte 2 of Experimental Example 1 is changed from a polymer electrolyte to an organic electrolyte.
- Table 2 is a table showing the evaluation results of Experimental Examples 1 and 9.
- FIG. 5 is a diagram showing the light transmission characteristics of the lithium secondary battery 100 according to the present embodiment.
- the horizontal axis of FIG. 5 is the wavelength of light [nm], and the vertical axis is the transmittance of light [%].
- the broken line indicates the light transmission characteristic of the negative electrode side transparent film substrate 5 including the negative electrode 3.
- the alternate long and short dash line shows the light transmission characteristics of the positive electrode side immediate film substrate 4 including the positive electrode 1.
- the solid line shows the light transmission characteristics of the entire lithium secondary battery 100.
- the lithium secondary battery 100 transmits light as a whole in the visible light wavelength range (translation 380 nm to 780 nm). It transmits about 36% of light at a wavelength of 600 nm.
- the lithium secondary battery 100 has a high output voltage, a stable charge cycle characteristic, and a light transmission characteristic.
- the present invention it is possible to provide a lithium secondary battery having a high output voltage and a method for manufacturing the same, which has both transparency and flexibility for visible light.
- the present invention is not limited to the above embodiment, and can be modified within the scope of the gist thereof.
- Negative electrode terminal 100 Lithium secondary battery
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Abstract
La présente invention comprend : une électrode positive 1 formée sur un substrat de film transparent souple et comprenant une substance qui permet l'insertion et la désorption d'ions lithium ; un électrolyte 2 qui est transparent et qui présente une conductivité d'ions lithium ; et une électrode négative 3 formée sur un substrat de film transparent souple et constituée d'un métal qui permet l'insertion et la désorption de lithium métallique ou d'ions lithium. L'électrode positive 1 est un oxyde de lithium dans lequel un halogène est ajouté à X dans LiCoPO4X ou dans Li2CoPO4X. L'électrolyte 2 est un électrolyte polymère qui est transparent aux ions lithium.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2003229126A (ja) * | 2002-02-01 | 2003-08-15 | Sangaku Renkei Kiko Kyushu:Kk | 非水電解質二次電池用電極活物質、それを含む電極及び電池 |
JP2008146917A (ja) * | 2006-12-07 | 2008-06-26 | Nippon Synthetic Chem Ind Co Ltd:The | 全固体型リチウム二次電池 |
JP2012526376A (ja) * | 2009-06-25 | 2012-10-25 | ノキア コーポレイション | ナノ構造可撓性電極およびこれを使用するエネルギー貯蔵デバイス |
KR20140074266A (ko) * | 2014-05-26 | 2014-06-17 | 한국전기연구원 | 유연성 투명 전지의 제조 방법 |
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- 2019-11-22 WO PCT/JP2019/045810 patent/WO2021100198A1/fr active Application Filing
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JP2003229126A (ja) * | 2002-02-01 | 2003-08-15 | Sangaku Renkei Kiko Kyushu:Kk | 非水電解質二次電池用電極活物質、それを含む電極及び電池 |
JP2008146917A (ja) * | 2006-12-07 | 2008-06-26 | Nippon Synthetic Chem Ind Co Ltd:The | 全固体型リチウム二次電池 |
JP2012526376A (ja) * | 2009-06-25 | 2012-10-25 | ノキア コーポレイション | ナノ構造可撓性電極およびこれを使用するエネルギー貯蔵デバイス |
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