CN101420032B - Combination pulp, preparation and application thereof - Google Patents
Combination pulp, preparation and application thereof Download PDFInfo
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- CN101420032B CN101420032B CN2007101241522A CN200710124152A CN101420032B CN 101420032 B CN101420032 B CN 101420032B CN 2007101241522 A CN2007101241522 A CN 2007101241522A CN 200710124152 A CN200710124152 A CN 200710124152A CN 101420032 B CN101420032 B CN 101420032B
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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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Abstract
The invention discloses composite slurry for reducing battery polarization resistance, a manufacturing method and the application thereof. The composite slurry comprises a carbon nano tube, a water system binding agent and water; the composite slurry is mixed and stirred for 1-4 hours and is coated on the cathode of the battery. The composite slurry has the advantages of simple preparation process and capability of greatly reducing the resistance after the battery electrode is stored at a high temperature, belonging to the field of lithium secondary battery electrodes.
Description
Technical field
The present invention relates to a kind of lithium secondary battery electrode combination pulp, be specifically related to a kind of combination pulp that reduces the battery polarization impedance.The invention still further relates to the preparation method and the application thereof of above-mentioned composition coating.
Background technology
Lithium ion battery can be widely used in electronic products such as digital product, mobile phone, electric motor car.Owing to lithium ion battery easy generating electrodes polarization under hot environment causes the battery capacity loss, influenced the application of electronic product under hot environment, cause very big puzzlement to the user.Therefore, how to reduce that the polarization impedance of lithium ion battery becomes each battery manufacturer problem demanding prompt solution under the hot environment.
The main method of lithium ion battery high-temperature storage performance research is that lithium ion battery is stored special time under specific hot conditions, investigates the maintenance capacity and the recovery capability that store the back battery.Generally battery is stored 5 hours under 91 ℃ of environment, store back record discharge capacity of the cell be defined as the maintenance capacity, with after the battery charge once more discharge capacity be defined as recovery capacity after battery high-temperature stores.The capacity that first discharge capacity had more after the recovery Capacity Ratio stored is defined as reversible loss capacity.And the difference of the initial capacity before recovery capacity and the battery storage is defined as battery high-temperature storage back irreversible capacity loss.Research by each side is thought, cause the reason of irreversible capacity loss that two big classes are arranged: because the consumption of the lithium ion that various chemical reactions cause under the hot environment, this is a kind of absolute irreversible capacity loss, and because hot environment causes electrode impedance to increase, thereby cause that the polarization phenomena in the discharge process are to cause battery high-temperature to store another reason of back capacitance loss.This a part of irreversible capacity loss is not absolute irreversible, discharges with minimum electric current storing the back battery, and discharge capacity is than recovery capacity height, and these polarization phenomena that illustrated that the high temperature rear electrode causes exist.
CN1532141A discloses a kind of nano tube based high energy material and preparation method thereof, and it is the allotrope that contains carbon, as the carbon-based material of Single Walled Carbon Nanotube, and can admit the alkali metal that mixes.The reversible capacity that this material presents is between about 650mAh/g-1000mAh/g.The high power capacity of this material makes it to many application, and is attractive as the electrode material of battery.The method of described manufacture order wall carbon nano tube comprising the nano-tube material that purify to reclaim and the material of purifying is deposited on a kind of conducting base.Should cated matrix pack in a kind of electrochemical cell, and measure the material that its admittance is mixed, as the ability of a kind of alkali metal (for example lithium).
CN1588679A discloses a kind of lithium ion secondary battery anode material and preparation method thereof, lithium ion secondary battery anode material wherein contains active material and nano level conductive agent, and described conductive agent is a carbon nano-tube, carbon nano-tube is a multi-walled carbon nano-tubes, and external diameter of pipe is distributed as 5-200nm.The preparation method of this lithium ion secondary battery anode material may further comprise the steps: (1) or is contained in the solution of binding agent the ultrasonic dispersion of carbon nano-tube in water or organic solvent; (2) cobalt acid lithium, lithium nickelate, lithium nickel cobalt dioxide or spinel lithium manganese oxide anode material powder are added wherein dispersion, make uniform sizing material; (3), be coated on the collector electrode with the uniform sizing material that makes; (4) oven dry.
Above-mentioned two inventions all are to prepare conducting base (being electrode) by mix alkali-metal method in carbon nano-tube, this method just simply is blended into carbon nano-tube in the negative material, carbon nano-tube can not all be used to transport electronics, therefore can only partly improve the high-temperature storage performance of battery.
Summary of the invention
The invention provides the combination pulp that a kind of preparation technology is simple, can significantly reduce the impedance of battery electrode after high-temperature storage.
Another object of the present invention provides the preparation method of above-mentioned composition slurry.
A further object of the present invention provides the method for utilizing above-mentioned composition pulp preparation hypopolarization impedance electrodes.
For achieving the above object, it is simple and can significantly reduce the combination pulp of battery polarization impedance that the present inventor has designed a kind of preparation technology through a large amount of research and performing creative labour, and described combination pulp is to be prepared from by following components by part by weight:
Carbon nano-tube 5-15 water system binder 1 water 30-50.
Preferably, described combination pulp is to be prepared from by following components by part by weight: carbon nano-tube 5-8 water system binder 1 water 38-45.
The external diameter of pipe of described carbon nano-tube is 10-300nm, is preferably 10-40nm.
Described water system binder is a kind of or wherein several mixture in polytetrafluoroethylene, carboxymethyl propyl cellulose, polyvinyl alcohol, polyethylene glycol oxide, methylcellulose, hydroxyethylcellulose, HEMC, hydroxypropyl methylcellulose, butadiene-styrene rubber, the polyacrylate.
A kind of method for preparing described combination pulp, described method are carbon nano-tube, water system binder and water to be mixed stirred 1-4 hour, are preferably to mix and stir 1.5-2.5 hour.
A kind of method for preparing the hypopolarization impedance electrodes, comprise the steps: the battery cathode sheet after the slurry behind baking 5-15min under 60 ℃-90 ℃, at its surface-coated thickness is the described combination pulp of 4-20 micron, toasts, film-making, coiling, fluid injection, changes into, seals.
Described battery cathode sheet is a battery graphite cathode sheet.
The present inventor has gone out to prepare the method for hypopolarization impedance electrodes through a large amount of EXPERIMENTAL DESIGN, need be behind baking 5-15min under 60 ℃-90 ℃ with the battery cathode sheet after the slurry, if stoving time surpasses 15min, battery cathode sheet top layer bone dry after the slurry, bottom adhesion deficiency comes off easily; If the not enough 5min of stoving time, the battery cathode sheet top layer moisture content height after the slurry can cause the calendering of bottom during the coating of top layer.The conductivity of the carbon nano-tube that applies on the battery cathode sheet after the baking is better than graphite material; after the high-temperature storage; battery since react or particle between contact etc.; can cause further deterioration; the degree of polarization that the good electric conductivity of carbon nano-tube can reduce so cause; thereby reduce the battery capacity loss; protect electrolyte to contact simultaneously with the large tracts of land of negative pole graphite material; make the high-temperature storage stage; reduce the reaction between graphite and the electrolyte, improve battery high-temperature and store the thickness swelling that the back produces.The coating thickness of carbon nano-tube is thick more good more, if negative pole adopts carbon nano-tube entirely, effect is best, but the cost costliness is generally the 4-20 micron; If be less than 4 microns, effect is not satisfactory.
The battery of embodiment 1-10 preparation and the battery of Comparative Examples 1 preparation were deposited 5 hours under 91 ℃ of environment, measured capability retention and capacitance loss rate after two kinds of battery high-temperatures store, it the results are shown in Table 1.As can be seen from Table 1, the battery high-temperature that adds carbon nano-tube material in negative pole stores the back capability retention all more than 86%, the capacitance loss rate all is lower than 14%, expanded thickness is all below 0.6mm, and the capability retention of Comparative Examples has only 70-78%, and the capacitance loss rate is up to 30%, and expanded thickness is all above 1.0mm, that have even up to 3.8mm, so method provided by the invention is for the battery high-temperature storge quality effect that has clear improvement.
Embodiment
The capability retention after the battery high-temperature of embodiment 1-10 and Comparative Examples stores and the assay method of capacitance loss rate are as follows:
1. battery was deposited 5 hours under 91 ℃ of environment;
2. battery is all charged to 4.2V/0.1C (70mA) with 950mA and end, 700mA is discharged to 3.1V and tests its normal temperature capacity;
3. battery charge was placed 1 hour the measurement primary data at normal temperature to 4.2V; Battery is put into 91 ℃ of baking ovens, store 5h;
4. store its thickness of back test, voltage, internal resistance, residual capacity, and do three recovery capacity.
The lithium ion secondary battery anode material of embodiment 1-10 contains cobalt acid lithium and carbon nano-tube, and the consumption of described carbon nano-tube is the 1wt% of positive electrode, the external diameter 10-40nm of carbon nano-tube, and its preparation technology is a common process.
Film-making among the embodiment 1-10, coiling, fluid injection, change into, seal and be common process.
Embodiment 1
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 5 polytetrafluoroethylene 1 deionized water 40 of 10-25nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder polytetrafluoroethylene and deionized water to be mixed stirred 2 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 10min under 70 ℃ of conditions, is 10 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 110 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 2
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 11 carboxymethyl propyl celluloses 1 deionized water 50 of 15-40nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder carboxymethyl propyl cellulose and deionized water to be mixed stirred 1.5 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 5min under 90 ℃ of conditions, is 5 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 110 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 3
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 8 polyvinyl alcohol 1 deionized water 30 of 20-100nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder polyvinyl alcohol and deionized water to be mixed stirred 3 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 15min under 60 ℃ of conditions, is 20 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 8min under 105 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 4
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 15 polyethylene glycol oxides 1 deionized water 45 of 80-150nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder polyethylene glycol oxide and deionized water to be mixed stirred 4 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 12min under 80 ℃ of conditions, is 15 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 110 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 5
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 13 methylcellulose 1 deionized water 34 of 100-300nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder methylcellulose and deionized water to be mixed stirred 2.5 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 8min under 75 ℃ of conditions, is 12 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 4min under 115 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 6
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 6 hydroxyethylcelluloses 0.5 HEMC 0.5 deionized water 38 of 200-300nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder hydroxyethylcellulose and deionized water to be mixed stirred 1 hour;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 15min under 65 ℃ of conditions, is 4 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 112 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 7
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 14 hydroxypropyl methylcelluloses 1 deionized water 47 of 10-40nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder hydroxypropyl methylcellulose and deionized water to be mixed stirred 2 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 14min under 85 ℃ of conditions, is 8 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 10min under 100 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 8
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 10 butadiene-styrene rubber 0.2 Sodium Polyacrylate 0.8 deionized water 42 of 10-60nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder butadiene-styrene rubber, Sodium Polyacrylate and deionized water to be mixed stirred 3.5 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 7min under 78 ℃ of conditions, is 18 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 110 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 9
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 12 polyethylene glycol oxides 0.2 methylcellulose 0.6 polytetrafluoroethylene 0.2 deionized water 32 of 50-100nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder polyethylene glycol oxide, methylcellulose, polytetrafluoroethylene and deionized water to be mixed stirred 2 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 7min under 82 ℃ of conditions, is 16 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 110 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Embodiment 10
The weight part ratio of each component of combination pulp:
External diameter of pipe is carbon nano-tube 7 polyvinyl alcohol 0.1, hydroxyethylcellulose 0.4, HEMC polytetrafluoroethylene 0.5 deionized water 36 of 100-200nm
The preparation method of combination pulp:
Described method is carbon nano-tube, water system binder polyvinyl alcohol, hydroxyethylcellulose, HEMC polytetrafluoroethylene and deionized water to be mixed stirred 2.5 hours;
Utilize the method for above-mentioned composition pulp preparation hypopolarization impedance electrodes:
Behind baking 9min under 76 ℃ of conditions, is 13 micron described combination pulps at its surface-coated thickness with the battery graphite cathode sheet after the slurry, is to toast 5min under 110 ℃ of conditions in temperature again, carries out film-making, coiling, fluid injection then, changes into, seals.
This hypopolarization impedance electrodes and anode are prepared into battery by conventional method.
Comparative example 1
Positive and negative pole material so that embodiment 1 adopts does not add any carbon nano-tube material on the both positive and negative polarity surface, prepares burden-operation making ordinary production batteries such as slurry-film-making-coilings-fluid injection-change into-seal according to ordinary production technology.
Comparative example 2:
Positive and negative pole material so that embodiment 1 adopts does not add any carbon nano-tube material at positive pole, and with carbon nano-tube conductive agent adding the most, wherein the mass ratio of graphite, carbon nano-tube, binding agent PTFE is not 92: 5: 3, produces battery according to normal process at negative pole.
The measurement result of table 1 embodiment electrode and Comparative Examples electrode
| Battery variety | Capability retention | The capacitance loss rate | Expanded thickness/mm |
| Embodiment 1 | 92％ | 8％ | 0.4 |
| 92％ | 8％ | 0.5 | |
| 91％ | 9％ | 0.5 | |
| Embodiment 2 | 90％ | 10％ | 0.4 |
| 90％ | 10％ | 0.5 | |
| 91％ | 9％ | 0.4 | |
| Embodiment 3 | 89％ | 11％ | 0.4 |
| 91％ | 9％ | 0.3 | |
| 88％ | 12％ | 0.5 | |
| Embodiment 4 | 89％ | 11％ | 0.4 |
| 88％ | 12％ | 0.4 | |
| 98％ | 12％ | 0.5 | |
| Embodiment 5 | 89％ | 11％ | 0.5 |
| 89％ | 11％ | 0.5 | |
| 88％ | 12％ | 0.6 | |
| Embodiment 6 | 89％ | 11％ | 0.4 |
| 89％ | 11％ | 0.5 | |
| 89％ | 11％ | 0.4 | |
| Embodiment 7 | 86％ | 14％ | 0.5 |
| 87％ | 13％ | 0.6 | |
| 88％ | 12％ | 0.4 | |
| Embodiment 8 | 88％ | 12％ | 0.5 |
| 88％ | 12％ | 0.5 | |
| 87％ | 13％ | 0.6 | |
| Embodiment 9 | 89％ | 11％ | 0.4 |
| 90％ | 10％ | 0.4 | |
| 91％ | 9％ | 0.3 |
| Embodiment 10 | 88％ | 12％ | 0.6 |
| 88％ | 12％ | 0.4 | |
| 90％ | 10％ | 0.5 | |
| Comparative Examples 1 | 70％ | 30％ | 2.5 |
| 70％ | 30％ | 3.8 | |
| 71％ | 29％ | 3.5 | |
| Comparative Examples 2 | 78％ | 22％ | 1.0 |
| 78％ | 22％ | 1.2 | |
| 79％ | 21％ | 0.9 |
As can be seen from Table 1, the battery high-temperature that adds carbon nano-tube material in negative pole stores the back capability retention all more than 86%, the capacitance loss rate all is lower than 14%, expanded thickness is all below 0.6mm, and the capability retention of Comparative Examples has only 70-78%, and the capacitance loss rate is up to 30%, and expanded thickness is all above 1.0mm, that have even up to 3.8mm, so method provided by the invention is for the battery high-temperature storge quality effect that has clear improvement.
Claims (6)
1. method for preparing the hypopolarization impedance electrodes, it is characterized in that: described method comprises the steps: the anode plate for lithium ionic cell after the slurry behind baking 5-15min under 60 ℃-90 ℃, at its surface-coated thickness is 4-20 micron combination pulp, toasts, film-making, coiling, fluid injection, changes into, seals; Described combination pulp is to be prepared from by following components by part by weight:
Carbon nano-tube 5-15 water system binder 1 water 30-50.
2. the method for preparing the hypopolarization impedance electrodes according to claim 1 is characterized in that: described anode plate for lithium ionic cell is the silicon/carbon/graphite in lithium ion batteries negative plate.
3. the method for preparing the hypopolarization impedance electrodes according to claim 1 is characterized in that: described combination pulp is to be prepared from by following components by part by weight:
Carbon nano-tube 5-8 water system binder 1 water 38-45.
4. according to claim 1 or the 3 described methods that prepare the hypopolarization impedance electrodes, it is characterized in that: the external diameter of pipe of described carbon nano-tube is 10-300nm.
5. the method for preparing the hypopolarization impedance electrodes according to claim 4 is characterized in that: the external diameter of pipe of described carbon nano-tube is 10-40nm.
6. according to claim 1 or the 3 described methods that prepare the hypopolarization impedance electrodes, it is characterized in that: described water system binder is a kind of or wherein several mixture in polytetrafluoroethylene, carboxymethyl propyl cellulose, polyvinyl alcohol, polyethylene glycol oxide, methylcellulose, hydroxyethylcellulose, HEMC, hydroxypropyl methylcellulose, butadiene-styrene rubber, the polyacrylate.
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| CN2007101241522A CN101420032B (en) | 2007-10-26 | 2007-10-26 | Combination pulp, preparation and application thereof |
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| CN2007101241522A CN101420032B (en) | 2007-10-26 | 2007-10-26 | Combination pulp, preparation and application thereof |
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| CN101420032A CN101420032A (en) | 2009-04-29 |
| CN101420032B true CN101420032B (en) | 2011-12-14 |
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| US10629325B2 (en) * | 2016-06-30 | 2020-04-21 | Tatsuta Electric Wire & Cable Co., Ltd. | Silver chloride paste |
| JP6785856B2 (en) | 2016-06-30 | 2020-11-18 | タツタ電線株式会社 | Biological electrodes and methods for forming bioelectrodes |
| CN108511740A (en) * | 2017-03-13 | 2018-09-07 | 万向二三股份公司 | A kind of high-specific-capacity silicon carbon electrode coating preparation method |
| CN109713308B (en) * | 2018-12-19 | 2022-04-05 | 浙江中科立德新材料有限公司 | CNT-containing aqueous lithium battery slurry and preparation method thereof |
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| CN2538543Y (en) * | 2002-04-30 | 2003-03-05 | 虞伟达 | Aluminium frame for screen printing equipment |
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| CN2538543Y (en) * | 2002-04-30 | 2003-03-05 | 虞伟达 | Aluminium frame for screen printing equipment |
Non-Patent Citations (2)
| Title |
|---|
| 代凯 等.粘结剂对碳纳米管电剂性能的影响.《化工矿物与加工》.2005,(第5期),21-23. * |
| 刘春燕 等.纳米碳管作为锂离子电池负极材料的研究.《天津大学学报》.2001,第34卷(第1期),31-34. * |
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Effective date of registration: 20191224 Address after: 314411 Jianshe East Road, Guodian, Yanguan Town, Haining City, Jiaxing City, Zhejiang Province Patentee after: Haining Yanguan Industrial Investment Co., Ltd Address before: 518119 BYD Industrial Park, Yanan Road, Kwai Chung Town, Longgang District, Guangdong, Shenzhen Patentee before: Biyadi Co., Ltd. |
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