CN102593415A - Preparation method for positive electrode of lithium ion battery - Google Patents
Preparation method for positive electrode of lithium ion battery Download PDFInfo
- Publication number
- CN102593415A CN102593415A CN2012100551363A CN201210055136A CN102593415A CN 102593415 A CN102593415 A CN 102593415A CN 2012100551363 A CN2012100551363 A CN 2012100551363A CN 201210055136 A CN201210055136 A CN 201210055136A CN 102593415 A CN102593415 A CN 102593415A
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- lithium ion
- preparation
- collector
- ion cell
- cell positive
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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
Abstract
The invention provides a preparation method for the positive electrode of a lithium ion battery, and the method is characterized by comprising the following steps of: first, conducting pretreatment on a current collector of the lithium ion battery; then loading a catalyst on the current collector; then employing a chemical vapor deposition method for in-situ growth of carbon nanotubes and carbon nanofibers on the current collector of the lithium ion battery; and finally blending the positive electrode material into a pasty slurry, which is then directly applied on aluminum foil with the carbon nanotubes and carbon nanofibers through blade coating, thus obtaining the positive electrode of the lithium ion battery. The method of the invention is mainly used for manufacturing the positive electrode of a lithium ion battery.
Description
Technical field
The present invention relates to nano material and technical field of lithium ion, specifically, relate to the CNT or the anodal preparation method of carbon nano-fiber of lithium ion battery.
Background technology
Lithium rechargeable battery is as a kind of novel green high-capacity secondary power supply; Be widely used in the modern digital products such as mobile phone, notebook computer, camera; Yet along with the expansion of lithium ion battery to fields such as electric automobiles, the research and development of the high-power battery group of high current charge-discharge become researcher research focus.Wherein, the development that has height ratio capacity, high power charging-discharging ability, stable performance, a positive electrode that cost is low remains studies difficult point now.
Positive electrode commonly used has cobalt acid lithium (LiCoO
2), LiMn2O4 (LiMn
2O
4), lithium nickelate (LiNiO
2), LiFePO4 (LiFePO
4) and nickle cobalt lithium manganate (LiNi1/3Co1/3Mn1/3O
2) etc.Generally all there is the problem of poor electric conductivity in they, have hindered the development of high-multiplying-power battery.In active material, add conductive agents such as conductive carbon black, acetylene black, CNT, carbon nano-fiber and can significantly improve its conductivity, especially CNT has characteristics such as accurate one-dimentional structure, excellent mechanical performances, high conductivity, high-termal conductivity and receives much concern.Grant number is that CN101335347B discloses through means such as ball milling, air-flow preliminary treatment, acidification, esterification treatment and in positive electrode, adds CNT; But; Because the nano-meter characteristic of CNT causes its surface energy very big; Be easy to reunite; Only depend on physical methods such as ultrasonic dispersion, ball milling to be difficult to guarantee the dispersing uniformity of CNT, the method for chemical modifications such as other acidifying, esterification can not fundamentally solve the dispersion problem of CNT, so CNT is failed at the inner three-dimensional net structure that connects continuously that forms of electrode material; Limited that carbon is received, the giving full play to of mitron performance, thereby also be difficult to effectively improve the conductivity of positive electrode and the ability of fast charging and discharging.
Publication number is a kind of method at positive active material surface in situ carbon nano-tube or carbon nano-fiber for CN 101527353A discloses; It is characterized in that earlier according to a certain percentage the catalyst that positive active material and carbon nano tube growth are used is made into mixed solution; After falling solvent through heating evaporation; Put into tube furnace, utilize chemical vapour deposition technique direct growth CNT or carbon nano-fiber on positive active material.This kind method can solve the dispersion problem of CNT, and production cost is low, and positive active material and CNT or carbon nano-fiber are combined into one, with LiFePO
4Compound positive electrode processes behind the half-cell first that circulation volume can reach 155mAh/g under the 0.1C multiplying power, is 143 mAh/g under the 1C multiplying power, is 112 mAh/g under the 10C multiplying power.It is thus clear that, find a kind of simple, effective method removes to solve CNT or the scattering problem of carbon nano-fiber in anode material for lithium-ion batteries is very necessary.
Summary of the invention
The present invention provide a kind of on affluxion body in lithium ion batteries in-situ growing carbon nano tube or carbon nano-fiber (CNM), and as the method for the positive pole of substrate preparation high conductivity.
Realize that technical scheme of the present invention is: the preparation method that a kind of lithium ion battery high conductivity is anodal is characterized in that it comprises the steps: at first affluxion body in lithium ion batteries to be carried out preliminary treatment; Supported catalyst on collector again; Use chemical vapour deposition technique (CVD method) in-situ growing carbon nano tube or carbon nano-fiber (CNM) on affluxion body in lithium ion batteries then; After at last positive electrode being deployed into pasty slurry there being on the aluminium foil of CNT or carbon nano-fiber (CNM) long direct blade coating, processes anode material for lithium-ion batteries.
The concrete characteristics of this programme also have, and the preliminary treatment of said collector is meant laser ablation or mechanical grinding.Destroy the oxide layer of collector outer surface on the one hand, orderly microflute is made in the exchange of convenience and catalyst on the other hand, can prepare carbon nano pipe array.
Said mechanical grinding is meant uses abrasive paper for metallograph or silicon carbide paper polishing collector, and the granularity of abrasive paper for metallograph or silicon carbide paper is 100～8 μ m.
Said silicon carbide paper polishing collector is meant that using granularity is the silicon carbide paper of 50～16 μ m, be fixed on collector on the glass plate during polishing and immerse in the deionized water, with silicon carbide paper along the direction collector of polishing.
Polish from the top down aluminium foil 5 ~ 20 times, the ethanol water ultrasonic cleaning 2～20 minutes of putting into 30～75 % then.
The use granularity is that the silicon carbide paper of 20 μ m is polished ultrasonic cleaning 5min in 50% the ethanol water 7 times.
Said on collector supported catalyst comprise the steps: to prepare the ferric nitrate (Fe (NO of 0.05～0.5mol/L
3)
3), cobalt nitrate (Co (NO
3)
2), nickel nitrate (Ni (NO
3)
2) solution; The pretreated collector that will clean up is then put into above-mentioned wherein a kind of solution and is flooded 2～5h; And it is every in the dipping process at a distance from 10～60min sonic oscillation, 3～20min.
Dipping is rinsed well with deionized water after accomplishing, and dries naturally.
In the nitrate solution of 0.1mol/L, flood 3h, and every at a distance from 30min sonic oscillation 5min.
Said affluxion body in lithium ion batteries can be a kind of in aluminium foil, Copper Foil, nickel plated steel strip and the nickel screen.
Said positive electrode can be cobalt acid lithium (LiCoO
2), LiMn2O4 (LiMn
2O
4), lithium nickelate (LiNiO
2), LiFePO4 (LiFePO
4) and nickle cobalt lithium manganate (LiNi1/3Co1/3Mn1/3O
2).
Specific embodiments of the present invention is following, and this embodiment is that example is explained orally with aluminium foil and LiFePO4, but is not limited to this:
(1) aluminium foil preliminary treatment.With thickness be 0.2mm, the high-purity aluminum foil that is of a size of 3*5 cm is fixed on the glass plate; And in the immersion deionized water, using granularity is 100～8 μ m, the silicon carbide paper of preferred 50～16 μ m; Polish from the top down aluminium foil 5 ~ 20 times; Put into the ethanol water ultrasonic cleaning 2～20 minutes of 30～75 %, preferably using granularity is the liquid honing 7 times of 20 μ m, ultrasonic cleaning 5min in 50% the ethanol water.
(2) supported catalyst.Ferric nitrate (Fe (the NO of preparation 0.05～0.5mol/L
3)
3), cobalt nitrate (Co (NO
3)
2), nickel nitrate (Ni (NO
3)
2) solution, the pretreated aluminium foil that will clean up is then put into above-mentioned wherein a kind of solution and is flooded 2～5h, and every at a distance from 10～60min sonic oscillation, 3～20min in the dipping process, preferably at the ferric nitrate (Fe (NO of 0.1mol/L
3)
3) flood 3h in the solution, and every at a distance from 30min sonic oscillation 5min.Dipping is rinsed well with deionized water after accomplishing, and dries naturally.
(3) in-situ growing carbon nano tube or carbon nano-fiber (CNM).Push tube furnace after having the aluminium foil of catalyst to put into quartz boat the load, carry out chemical vapour deposition reaction carbon nano-tube or carbon nano-fiber (CNM).
Concrete steps are for being that the heating rate with 0.5 ~ 10 ℃/min is raised to 500～800 ℃ under 95% nitrogen+5% hydrogen atmosphere at volume content; Feeding volume flow ratio then is the acetylene of 3:1～1:3 and the mist of hydrogen; Behind reaction 10～40min; Turn off acetylene and hydrogen, under high pure nitrogen atmosphere, be cooled to room temperature.
Preferably the heating rate with 2 ℃/min is raised to 750 ℃ under the hydrogen nitrogen mixed gas atmosphere, and feeding volume flow ratio then is the acetylene of 1:3 and the mist of hydrogen, reaction 20min.
The method of all carbon nano-tubes or carbon nano-fiber all is fit to this patent.
(4) be deployed into after the pasty slurry positive electrode of routine directly that blade coating has on the aluminium foil of CNT or carbon nano-fiber (CNM) long, process anode material for lithium-ion batteries.
The invention has the beneficial effects as follows directly CNT or carbon nano-fiber (CNM) are grown on the collector, with collector be an organic whole, can effectively solve the dispersion problem of CNT or carbon nano-fiber; Because CNT or carbon nano-fiber (CNM) are an organic whole with collector, can improve the transmission speed of electronics, can improve the anodal conductivity and the ability of fast charging and discharging greatly as the matrix preparation is anodal; This method has saved the pretreating process of CNT or carbon nano-fiber, so technology is simpler, production cost is lower; Because CNT or carbon nano-fiber form three-dimensional net structure on collector, specific area and specific pore volume increase, and the superincumbent adhesive force of active material increases, and therefore can reduce the binding agent consumption, thereby can further improve anodal conductivity.In the carbon nano tube growth process, activity of such catalysts is crucial, therefore keeps activity of such catalysts to help preparing the CNT of uniform diameter.Prevent to form catalyst on the one hand through supersonic oscillations and in exchange process, form metal a small bundle of straw, etc. for silkworms to spin cocoons on, cause particle to increase; On the other hand, the oscillation effect of utilizing hyperacoustic high frequency sound wave to produce produces on collector and is the active sites that dot matrix distributes, and promotes the ion-exchange between catalyst and collector, also makes that the catalyst granules in the load is orderly dot matrix distribution simultaneously.
Embodiment
Below in conjunction with embodiment the present invention is done further explanation.
Embodiment 1: thickness is 0.2mm, is of a size of 3*5 cm high-purity aluminum foil and is fixed on the glass plate; And in the immersion deionized water; Using granularity is the silicon carbide paper of 20 μ m, and the aluminium foil 7 times of polishing was from the top down put into 50% ethanolic solution ultrasonic cleaning 5 minutes; Take out aluminium foil, put into the Fe (NO of the 0.1mol/L for preparing
3)
3Flood 3h in the solution, every in the dipping process at a distance from 30min sonic oscillation 5min, take out; Naturally dry, be placed on and push in the quartz boat in the tubular react furnace, feeding volume content is 95% nitrogen+5% hydrogen; Heating rate with 2 ℃/min is raised to 750 ℃; Feeding volume flow ratio then is the acetylene of 1:3 and the mist of hydrogen, behind the reaction 20min, turns off acetylene and hydrogen; Under high pure nitrogen atmosphere, be cooled to room temperature, make the long aluminum foil current collector (CNM-Fe/Al) that CNT or carbon nano-fiber are arranged.With LiFePO
4Be deployed into pasty slurry in proportion with binding agent, directly blade coating is last at CNM-Fe/Al, and LiFePO is processed in vacuumize
4/ CNM-Fe/Al is anodal.
Embodiment 2: like embodiment 1, just selecting granularity is the silicon carbide paper of 100 μ m, the aluminium foil 3 times of polishing from the top down, and ultrasonic cleaning is 15 minutes in 30% ethanolic solution, puts into the Co (NO of the 0.05mol/L for preparing
3)
2Flood 3h in the solution, every at a distance from 60min sonic oscillation 10min, process LiFePO
4/ CNM-Co/Al is anodal.
Embodiment 3: like embodiment 1, just selecting granularity is the silicon carbide paper of 40 μ m, the aluminium foil 10 times of polishing from the top down, and ultrasonic cleaning is 5 minutes in 50% ethanolic solution, puts into the Ni (NO of the 0.3mol/L for preparing
3)
2Flood 2h in the solution, every at a distance from 30min sonic oscillation 5min, be raised to 600 ℃ with the heating rate of 10 ℃/min, feeding volume flow ratio then is the acetylene of 1:1 and the mist of hydrogen, react 20min after, process LiFePO
4/ CNM-Ni/Al is anodal.
Embodiment 4: like embodiment 1, be that high-purity nickel plated steel strip is done collector, selecting granularity is polish from the top down high-purity nickel plated steel strip 20 times of the silicon carbide paper of 32 μ m, and ultrasonic cleaning is 20 minutes in 30% ethanolic solution.Be different from embodiment 1 and be, omit the supported catalyst step, directly carbon nano-tube or carbon nano-fiber on the nickel plated steel strip collector are processed LiFePO
4/ CNM/Ni-S is anodal.
Embodiment 1-embodiment 3 conditions are fit to the Copper Foil collector equally, and embodiment 4 conditions are fit to the nickel screen collector equally, and all experiment positive electrodes are not limited only to LiFePO
4, can also be cobalt acid lithium (LiCoO
2), LiMn2O4 (LiMn
2O
4), lithium nickelate (LiNiO
2) and nickle cobalt lithium manganate (LiNi1/3Co1/3Mn1/3O
2) ternary material.
Experimental result
The positive electrode of top embodiment is made the test of having carried out chemical property behind the half-cell respectively; Test condition is done negative pole for the lithium sheet; It is that ethene carbonic ether/diethyl carbonic ether of 1:1 is an electrolyte that the LiPF6 of 1mol/L is dissolved in volume ratio; Celgard 2400 is a barrier film, 25 ℃ of room temperatures, and test result is following:
Claims (10)
1. the preparation method of a lithium ion cell positive is characterized in that it comprises the steps: at first affluxion body in lithium ion batteries to be carried out preliminary treatment; Supported catalyst on collector again; Use chemical vapour deposition technique in-situ growing carbon nano tube or carbon nano-fiber on affluxion body in lithium ion batteries then; After at last positive electrode being deployed into pasty slurry there being on the aluminium foil of CNT or carbon nano-fiber long direct blade coating, processes anode material for lithium-ion batteries.
2. the preparation method of lithium ion cell positive according to claim 1 is characterized in that the preliminary treatment of said collector is meant laser ablation or mechanical grinding.
3. the preparation method of lithium ion cell positive according to claim 2 is characterized in that said mechanical grinding is meant use abrasive paper for metallograph or silicon carbide paper polishing collector, and the granularity of abrasive paper for metallograph or silicon carbide paper is 100～8 μ m.
4. the preparation method of lithium ion cell positive according to claim 3; It is characterized in that said silicon carbide paper polishing collector is meant that using granularity is the silicon carbide paper of 50～16 μ m; Be fixed on collector on the glass plate during polishing and immerse in the deionized water, with silicon carbide paper along a direction polishing collector.
5. according to the preparation method of claim 2 or 3 or 4 described lithium ion cell positives, aluminium foil 5 ~ 20 times that it is characterized in that polishing from the top down, the ethanol water ultrasonic cleaning 2～20 minutes of putting into 30～75 % then.
6. the preparation method of lithium ion cell positive according to claim 5, it is characterized in that using granularity is the silicon carbide paper polishing 7 times of 20 μ m, ultrasonic cleaning 5min in 50% the ethanol water.
7. the preparation method of lithium ion cell positive according to claim 1, it is characterized in that said on collector supported catalyst comprise the steps: that compound concentration is the ferric nitrate of 0.05～0.5mol/L, cobalt nitrate, nickel nitrate solution; The pretreated collector that will clean up is then put into above-mentioned wherein a kind of solution and is flooded 2～5h; And it is every in the dipping process at a distance from 10～60min sonic oscillation, 3～20min.
8. the preparation method of lithium ion cell positive according to claim 7 after it is characterized in that flooding completion, rinses well with deionized water, dries naturally.
9. the preparation method of lithium ion cell positive according to claim 7 is characterized in that in the nitrate solution of 0.1mol/L, flooding 3h, and every at a distance from 30min sonic oscillation 5min.
10. the preparation method of lithium ion cell positive according to claim 1 is characterized in that said affluxion body in lithium ion batteries can be a kind of in aluminium foil, Copper Foil, nickel plated steel strip and the nickel screen.
Priority Applications (1)
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| CN2012100551363A CN102593415A (en) | 2012-03-05 | 2012-03-05 | Preparation method for positive electrode of lithium ion battery |
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|---|---|---|---|
| CN2012100551363A CN102593415A (en) | 2012-03-05 | 2012-03-05 | Preparation method for positive electrode of lithium ion battery |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102983308A (en) * | 2012-12-17 | 2013-03-20 | 中国科学院上海硅酸盐研究所 | Carbon nanotube array/nickel oxide nanoparticle coaxial composite cathode material and preparation method thereof |
| CN103852040A (en) * | 2012-11-28 | 2014-06-11 | 朴力美电动车辆活力株式会社 | Examining method of battery plate producing device and examining device thereof |
| RU2572840C2 (en) * | 2014-05-22 | 2016-01-20 | Мсд Текнолоджис Частная Компания С Ограниченной Ответственностью | Metal foil with conductive layer and manufacturing method thereof |
| CN103500838B (en) * | 2013-09-27 | 2016-06-01 | 中物院成都科学技术发展中心 | A kind of nano-carbon material air electrode for lithium air battery, preparation method and lithium-air battery thereof |
| CN106425110A (en) * | 2016-10-28 | 2017-02-22 | 深圳瑞隆新能源科技有限公司 | Manufacturing method of high-specific-surface-area current collector |
| WO2017055126A3 (en) * | 2015-09-29 | 2017-05-18 | Universite De Nantes | Electrochemical devices, with current collector having an increased resistance to corrosion |
| CN108666581A (en) * | 2018-06-29 | 2018-10-16 | 华南理工大学 | A kind of checkerboard composite current collector and preparation method thereof for lithium ion battery |
| CN108695509A (en) * | 2018-07-06 | 2018-10-23 | 重庆环纽信息科技有限公司 | High compound lithium battery anode of energy storage efficiency and preparation method thereof and lithium battery |
| CN113380978A (en) * | 2021-06-10 | 2021-09-10 | 珠海冠宇电池股份有限公司 | Flexible high-rate battery, pole piece and preparation method thereof |
| RU2758442C1 (en) * | 2020-12-08 | 2021-10-28 | Федеральное государственное бюджетное учреждение науки Институт проблем химической физики Российской Академии наук (ФГБУН ИПХФ РАН) | Composite cathode material and method for its preparation |
| CN114899409A (en) * | 2022-05-18 | 2022-08-12 | 上海瑞浦青创新能源有限公司 | Preparation method of carbon nanotube fiber current collector |
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Cited By (16)
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|---|---|---|---|---|
| CN103852040A (en) * | 2012-11-28 | 2014-06-11 | 朴力美电动车辆活力株式会社 | Examining method of battery plate producing device and examining device thereof |
| CN103852040B (en) * | 2012-11-28 | 2017-03-29 | 朴力美电动车辆活力株式会社 | The inspection method and check device of plate of battery manufacture device |
| CN102983308A (en) * | 2012-12-17 | 2013-03-20 | 中国科学院上海硅酸盐研究所 | Carbon nanotube array/nickel oxide nanoparticle coaxial composite cathode material and preparation method thereof |
| CN103500838B (en) * | 2013-09-27 | 2016-06-01 | 中物院成都科学技术发展中心 | A kind of nano-carbon material air electrode for lithium air battery, preparation method and lithium-air battery thereof |
| RU2572840C2 (en) * | 2014-05-22 | 2016-01-20 | Мсд Текнолоджис Частная Компания С Ограниченной Ответственностью | Metal foil with conductive layer and manufacturing method thereof |
| US10501861B2 (en) | 2015-09-29 | 2019-12-10 | Universite De Nantes | Electrochemical devices with current collector having an increased resistance to corrosion |
| WO2017055126A3 (en) * | 2015-09-29 | 2017-05-18 | Universite De Nantes | Electrochemical devices, with current collector having an increased resistance to corrosion |
| CN108350597A (en) * | 2015-09-29 | 2018-07-31 | 南特大学 | The electrochemical device of current-collector with corrosion resistance enhancing |
| CN108350597B (en) * | 2015-09-29 | 2020-10-23 | 南特大学 | Electrochemical device with current collector having enhanced corrosion resistance |
| CN106425110A (en) * | 2016-10-28 | 2017-02-22 | 深圳瑞隆新能源科技有限公司 | Manufacturing method of high-specific-surface-area current collector |
| CN108666581A (en) * | 2018-06-29 | 2018-10-16 | 华南理工大学 | A kind of checkerboard composite current collector and preparation method thereof for lithium ion battery |
| CN108695509A (en) * | 2018-07-06 | 2018-10-23 | 重庆环纽信息科技有限公司 | High compound lithium battery anode of energy storage efficiency and preparation method thereof and lithium battery |
| RU2758442C1 (en) * | 2020-12-08 | 2021-10-28 | Федеральное государственное бюджетное учреждение науки Институт проблем химической физики Российской Академии наук (ФГБУН ИПХФ РАН) | Composite cathode material and method for its preparation |
| CN113380978A (en) * | 2021-06-10 | 2021-09-10 | 珠海冠宇电池股份有限公司 | Flexible high-rate battery, pole piece and preparation method thereof |
| CN114899409A (en) * | 2022-05-18 | 2022-08-12 | 上海瑞浦青创新能源有限公司 | Preparation method of carbon nanotube fiber current collector |
| CN114899409B (en) * | 2022-05-18 | 2023-12-05 | 上海瑞浦青创新能源有限公司 | Preparation method of carbon nano tube fiber current collector |
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Application publication date: 20120718 |