CN104993120A - Lithium ion battery negative electrode sizing agent and preparation method thereof - Google Patents

Lithium ion battery negative electrode sizing agent and preparation method thereof Download PDF

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Publication number
CN104993120A
CN104993120A CN201510337871.7A CN201510337871A CN104993120A CN 104993120 A CN104993120 A CN 104993120A CN 201510337871 A CN201510337871 A CN 201510337871A CN 104993120 A CN104993120 A CN 104993120A
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lithium ion
ion battery
preparation
carbon fiber
silica fume
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田东
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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 lithium ion battery negative electrode sizing agent and a preparation method thereof. The lithium ion battery negative electrode sizing agent comprises lithium titanate, conductive agent, binder, thickener, solvent and dispersing agent, and is characterized by further comprising nanometer silicon powder and carbon fiber. The nanometer silicon powder and the carbon fiber are added to the negative electrode of a lithium ion battery in proportion and twined with all components such as the lithium titanate and the nanometer silicon powder conductive agent through the characteristics that the carbon fiber is high in strength, excellent in conductivity and good in thermal conductivity and has a filamentary structure, and then the effects on reinforcing the negative electrode material and increasing the conductivity are achieved. Thus, the battery capacity is improved, and the cycle life of the battery is prolonged.

Description

A kind of lithium ion battery cathode slurry and preparation method thereof
Technical field
This patent relates to a kind of lithium ion battery cathode slurry and preparation method thereof, and being specially with lithium titanate is negative material, and adds nano silica fume and the application of carbon fibre material in lithium ion battery negative.
Background technology
Since the beginning of the nineties in last century, Sony energy technology company took the lead in successfully developing the lithium ion battery using Carbon anode, lithium ion battery captures rapidly civil secondary Battery Market with the speed of average annual 15%, has become the first-selected power supply of current portable electronic equipment.The develop rapidly of lithium ion battery mainly has benefited from the contribution of electrode material, the particularly progress of negative material.What current commercial Li-ion battery negative material adopted is lithium titanate class material with carbon element, and having lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, is more satisfactory lithium ion battery negative material.
Inexpensive with it, the nontoxic and superior chemical property of material with carbon element is widely used in lithium ion battery, and state of interface and the fine structure of itself have a great impact electrode performance.At present, commercial carbon negative electrode material of lithium ion cell can be divided into lithium titanate, hard carbon and soft carbon three class, and wherein lithium titanate class material is still the main flow of lithium ion battery negative material.Lithium titanate class material with carbon element, having lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, is more satisfactory lithium ion battery negative material.But its theoretical specific capacity only has 372mAh/g, thus limit the further raising of lithium ion battery specific energy, the demand of growing high-energy Portable power source can not be met.Meanwhile, when lithium titanate is as negative material, in first charge-discharge process, form one deck solid electrolyte film (SEI) on its surface.Solid electrolyte film is the formation that react to each other such as electrolyte, negative material and lithium ion, irreversibly consumes lithium ion, is to form the main factor of of irreversible capacity; It two is in the process of Lithium-ion embeding, electrolyte easily and its be embedded in the process of moving out altogether, electrolyte is reduced, the gaseous product generated causes lithium titanate lamella to peel off, especially containing in the electrolyte of PC, lithium titanate lamella comes off new for formation interface, causes further SEI to be formed, irreversible capacity increases, and cyclical stability declines simultaneously.As lithium ion battery negative material, material with carbon element still exists that charge/discharge capacity is low, first cycle irreversible loss is large, solvent molecule intercalation and the shortcoming such as preparation cost is high altogether, and these are also the key issues solved needed in current Study on Li-ion batteries.
Li 4ti 5o 12as a kind of novel ion secondary battery cathode material lithium, compared with other business-like material, advantages such as having good cycle, do not react with electrolyte, security performance is high, charge and discharge platform is steady is one of the most excellent lithium ion battery negative material received much concern in recent years.Compared with carbon negative electrode material, lithium titanate has a lot of advantages, wherein, the deintercalation of lithium ion in lithium titanate is reversible, and lithium ion is embedding or is deviating from the process of lithium titanate, its crystal formation does not change, change in volume is less than 1%, therefore be called as " zero strain material ", can avoid causing structural damage due to the flexible back and forth of electrode material in charge and discharge cycles, thus improve cycle performance and the useful life of electrode, decrease and increase with cycle-index and bring specific capacity significantly to decay, there is the cycle performance more excellent than Carbon anode; But because lithium titanate is a kind of insulating material, its conductivity is low, thus cause the application in lithium electricity to there is the poor problem of high rate performance, lithium titanate material theoretical specific capacity is 175 mAh/g simultaneously, and actual specific capacity is greater than 160mAh/g, has the shortcomings such as gram volume is lower.
In various Novel anode material, silicon-based anode has unique advantage and potential.Silicium cathode material is in charge and discharge process, the alloys such as Li12Si7, L i13Si4, L i7Si3, L i15Si4, L i22Si5 can be formed with lithium, have high power capacity (Li22Si5, the highest 4200mAh/g), removal lithium embedded voltage low, with electrolyte reactivity is low, security performance is good etc. advantage.But violent volumetric expansion (0 ~ 300%) can occur silicon in removal lithium embedded course of reaction, thus causes destruction and the efflorescence of material structure, causes capacity to be decayed rapidly, cycle performance worsens.In addition, also there is the defects such as conductivity is low, and high rate performance is not good enough, and coulombic efficiency is lower in silicium cathode.
Silicon exceeds general 0.2V as its platform electromotive force of negative material than lithium metal, negative pole not easily occurs analysing lithium phenomenon in battery charging process.Carbon fiber has the features such as intensity is high, excellent conductivity, thermal conductivity are good simultaneously, because it has fine long filamentary structure, add in negative pole with nano silica fume simultaneously, mutually can be wound around with each components such as lithium titanate, nano silica fume conductive agents, the effect play and reinforce negative material, increasing conductivity, both coordinated, improve capacity and the cycle performance of battery.
Summary of the invention
The object of this patent is to provide a kind of lithium ion battery cathode slurry and preparation method thereof, to improve battery capacity, to improve battery cycle life.
For achieving the above object, the technical scheme that this patent adopts is: a kind of lithium titanate cathode of lithium ion battery slurry, comprise lithium titanate, conductive agent, binding agent, thickener, solvent and dispersant, it is characterized in that, also comprise nano silica fume and carbon fiber, conductive agent accounts for the 0%-3% of total solid weight, dispersant addition accounts for the 2%-10% of total solid mass fraction, nano silica fume accounts for the 2%-20% of total solid, carbon fiber accounts for the 20-80% of nano silica fume weight, described nano silica fume median particle diameter D50 scope is between 10-100nm, in described carbon fiber, straight particle diameter footpath D50 is between 10-200nm.
Described carbon fiber is hollow or solid construction.
The hollow structure of described carbon fiber is single layer hollow or multilayer hollow.
Described nano silica fume particle diameter is between 30-100nm.
Conductive agent is the one in Super-P, graphite agent, Ketjen black.
Described solvent is deionized water, binding agent is butadiene-styrene rubber, and thickener is sodium carboxymethylcellulose.
Described dispersant is ethylene glycol or glycerol.
A kind of preparation process of lithium titanate cathode of lithium ion battery slurry is as follows:
(1) take deionized water as solvent, thickener sodium carboxymethylcellulose mixer is uniformly dissolved; Pour in ball mill by the sodium carboxymethylcellulose after dissolving, add conductive agent, ball milling disperses 1 hour; Add lithium titanate, ball milling disperses 2 hours;
(2) add dispersant ethylene glycol, after ball milling disperses 10 minutes, nano silica fume and carbon fiber are added in mixing material and continue dispersion 1 hour;
(3) add butadiene-styrene rubber, ball milling disperses 1 hour, regulates slurry viscosity to 2000-3000mPas, discharging.
Nano silica fume has the feature of high power capacity, but along with very large change in volume in battery charge and discharge process, easily causes negative pole material to come off from collector, affect cycle life.This patent uses ball milling method batching, and with the use of dispersant, nano silica fume and carbon fiber are added among lithium ion battery negative in proportion, intensity is high, excellent conductivity, thermal conductivity are good to utilize carbon fiber to have, and its filamentary structure feature had, itself and each component such as lithium titanate, nano silica fume conductive agent are wound around mutually, the effect play and reinforce negative material, increasing conductivity.Thus improve battery capacity, improve battery cycle life.
Embodiment
For column type 18650 lithium ion battery, the ratio provided in this patent when cathode blending and distribution add nano silica fume and carbon fiber, comparative illustration its capacity of lithium ion battery and cycle performance are improved.In battery design, calculate positive/negative plate length by box hat filling rate 95%, embodiment and comparative example are that cathode blending mode and proportioning are illustrated.
Embodiment 1
Take deionized water as solvent, by account for mass fraction of solids be 1.5% thickener sodium carboxymethylcellulose mixer be uniformly dissolved.Pour in ball mill by the sodium carboxymethylcellulose after dissolving, add the super-P accounting for mass fraction of solids 1%, ball milling disperses 1 hour.
Add the lithium titanate accounting for mass fraction of solids 82.5%, ball milling disperses 2 hours.
Add the dispersant ethylene glycol accounting for mass fraction of solids 5%, will the nano silica fume of mass fraction of solids 5% be accounted for and account for mass fraction 2% carbon fiber and add in mixing material and continue dispersion 1 hour after ball milling disperses 10 minutes.
Add the butadiene-styrene rubber accounting for mass fraction of solids 3%, ball milling disperses 1 hour, regulates slurry viscosity to zone of reasonableness, discharging.
Comparative example 1
Take deionized water as solvent, by account for mass fraction of solids be 1.5% thickener sodium carboxymethylcellulose mixer be uniformly dissolved,
Pour in ball mill by the sodium carboxymethylcellulose after dissolving, add the super-P accounting for mass fraction of solids 3%, ball milling disperses 1 hour.
Add the lithium titanate accounting for mass fraction of solids 82.5%, ball milling disperses 2 hours.
Add the dispersant ethylene glycol accounting for mass fraction of solids 5%, after ball milling disperses 10 minutes, the nano silica fume accounting for mass fraction of solids 5% is added in mixing material and continue dispersion 1 hour.
Add the butadiene-styrene rubber accounting for mass fraction of solids 3%, ball milling disperses 1 hour, regulates slurry viscosity to zone of reasonableness, discharging.
Comparative example 2
Take deionized water as solvent, by account for mass fraction of solids be 1.5% thickener sodium carboxymethylcellulose mixer be uniformly dissolved,
Pour in ball mill by the sodium carboxymethylcellulose after dissolving, add the super-P accounting for mass fraction of solids 1%, ball milling disperses 1 hour.
Add the lithium titanate accounting for mass fraction of solids 92.5%, ball milling disperses 2 hours.
Add the dispersant ethylene glycol accounting for mass fraction of solids 5%, mass fraction 2% carbon fiber will be accounted for after ball milling disperses 10 minutes and add in mixing material and continue dispersion 1 hour.
Add the butadiene-styrene rubber accounting for mass fraction of solids 3%, ball milling disperses 1 hour, regulates slurry viscosity to zone of reasonableness, discharging.
Comparative example 3
Take deionized water as solvent, by account for mass fraction of solids be 1.5% thickener sodium carboxymethylcellulose mixer be uniformly dissolved,
Pour in ball mill by the sodium carboxymethylcellulose after dissolving, add the super-P accounting for mass fraction of solids 3%, ball milling disperses 1 hour.
Add the lithium titanate accounting for mass fraction of solids 92.5%, ball milling disperses 2 hours.
Add the butadiene-styrene rubber accounting for mass fraction of solids 3%, ball milling disperses 1 hour, regulates slurry viscosity to zone of reasonableness, discharging.
The slurry prepared by comparative example and embodiment method makes anode plate for lithium ionic cell, and assembles battery, and cycle-index when its capacity, first efficiency and capability retention 80% lists in table 1.
Table 1
Can be found by comparative example 1 and comparative example 3 contrast, in negative pole, add nano silica fume effectively can improve battery capacity, but cycle performance declines comparatively remarkable, this may be because in battery charge and discharge process, nano silica fume change in volume is larger, cause that negative material is loosely organized to come off, affect cycle performance of battery; Can be found by comparative example 2 and comparative example 3 contrast, when only adding carbon fiber in negative pole, can cycle performance of battery be improved, but battery capacity promotes little; Comparative example 1 and comparative example 1, comparative example 3 can find, add nano silica fume and carbon fiber not only can significantly improve battery capacity in battery cathode simultaneously, and its cycle performance is also highly improved.Reason is the filamentary structure feature that carbon fiber has, and each components such as itself and lithium titanate, nano silica fume, conductive agent are wound around mutually, plays and reinforces negative material, increases the effect of conductivity, thus improves battery capacity, improves the cycle life of battery.

Claims (7)

1. lithium ion battery cathode slurry and preparation method thereof, comprise lithium titanate, conductive agent, binding agent, thickener, solvent and dispersant, it is characterized in that, also comprise nano silica fume and carbon fiber, conductive agent accounts for the 0%-3% of total solid weight, dispersant addition accounts for the 2%-10% of total solid mass fraction, nano silica fume accounts for the 2%-20% of total solid, carbon fiber accounts for the 20-80% of nano silica fume weight, described nano silica fume median particle diameter D50 scope is between 10-100nm, in described carbon fiber, straight particle diameter footpath D50 is between 10-200nm, and its preparation process is as follows:
(1) added in solvent by thickener and be uniformly dissolved with mixer, pour in ball mill by the thickener after dissolving, add conductive agent, ball milling disperses 1 hour;
(2) add lithium titanate, ball milling disperses 2 hours;
(3) add dispersant, after ball milling disperses 10 minutes, nano silica fume and carbon fiber are added in mixing material and continue dispersion 1 hour;
(4) add binding agent, ball milling disperses 1 hour, regulates slurry viscosity 2000-3000mPas, discharging.
2. a kind of lithium ion battery cathode slurry according to claim 1 and preparation method thereof, is characterized in that, described carbon fiber is hollow or solid construction.
3. a kind of lithium ion battery cathode slurry according to claim 2 and preparation method thereof, is characterized in that, the hollow structure of described carbon fiber is single layer hollow or multilayer hollow.
4. a kind of lithium ion battery cathode slurry according to claim 1 and preparation method thereof, is characterized in that, described nano silica fume particle diameter is between 30-100nm.
5. a kind of lithium ion battery cathode slurry according to claim 1 and preparation method thereof, is characterized in that, described conductive agent is the one in Super-P, graphite agent, Ketjen black.
6. a kind of lithium ion battery cathode slurry according to claim 1 and preparation method thereof, is characterized in that, described solvent is deionized water, and binding agent is butadiene-styrene rubber, and thickener is sodium carboxymethylcellulose.
7. a kind of lithium ion battery cathode slurry according to claim 1 and preparation method thereof, is characterized in that, described dispersant is ethylene glycol or glycerol.
CN201510337871.7A 2015-06-18 2015-06-18 Lithium ion battery negative electrode sizing agent and preparation method thereof Pending CN104993120A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106972150A (en) * 2017-04-17 2017-07-21 上海德朗能动力电池有限公司 A kind of lithium titanate base lithium ion GND, lithium ion battery and its chemical synthesizing method
CN108281640A (en) * 2018-01-31 2018-07-13 北京国能电池科技股份有限公司 Proportioning process, based lithium-ion battery positive plate and the lithium ion battery of lithium ion battery anode glue size
CN112151756A (en) * 2020-09-14 2020-12-29 江苏塔菲尔新能源科技股份有限公司 Negative plate and battery
CN112366318A (en) * 2020-11-02 2021-02-12 横店集团东磁股份有限公司 Negative electrode slurry and preparation method and application thereof
CN115295800A (en) * 2022-10-09 2022-11-04 青岛龙迪碳材料科技有限公司 Lithium battery negative electrode material and sintering preparation method thereof

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KR20110126330A (en) * 2010-05-17 2011-11-23 삼화콘덴서공업주식회사 Active material for anode, method for manufacturing the same, and secondary battery and super capacitor including the same
CN202839843U (en) * 2012-10-17 2013-03-27 中国东方电气集团有限公司 Composite cathode of lithium ion battery
CN104681785A (en) * 2015-02-12 2015-06-03 山东精工电子科技有限公司 Lithium ion battery anode coating material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20110126330A (en) * 2010-05-17 2011-11-23 삼화콘덴서공업주식회사 Active material for anode, method for manufacturing the same, and secondary battery and super capacitor including the same
CN202839843U (en) * 2012-10-17 2013-03-27 中国东方电气集团有限公司 Composite cathode of lithium ion battery
CN104681785A (en) * 2015-02-12 2015-06-03 山东精工电子科技有限公司 Lithium ion battery anode coating material and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106972150A (en) * 2017-04-17 2017-07-21 上海德朗能动力电池有限公司 A kind of lithium titanate base lithium ion GND, lithium ion battery and its chemical synthesizing method
CN108281640A (en) * 2018-01-31 2018-07-13 北京国能电池科技股份有限公司 Proportioning process, based lithium-ion battery positive plate and the lithium ion battery of lithium ion battery anode glue size
CN108281640B (en) * 2018-01-31 2021-02-09 北京国能电池科技股份有限公司 Batching process of lithium ion battery anode slurry, lithium ion battery anode plate and lithium ion battery
CN112151756A (en) * 2020-09-14 2020-12-29 江苏塔菲尔新能源科技股份有限公司 Negative plate and battery
CN112366318A (en) * 2020-11-02 2021-02-12 横店集团东磁股份有限公司 Negative electrode slurry and preparation method and application thereof
CN115295800A (en) * 2022-10-09 2022-11-04 青岛龙迪碳材料科技有限公司 Lithium battery negative electrode material and sintering preparation method thereof

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Application publication date: 20151021