CN106602050A - Preparation method of slurry for lithium titanate battery - Google Patents
Preparation method of slurry for lithium titanate battery Download PDFInfo
- Publication number
- CN106602050A CN106602050A CN201510677353.XA CN201510677353A CN106602050A CN 106602050 A CN106602050 A CN 106602050A CN 201510677353 A CN201510677353 A CN 201510677353A CN 106602050 A CN106602050 A CN 106602050A
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- lithium titanate
- preparation
- slurry
- titanate battery
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
- H01M4/623—Binders being polymers fluorinated polymers
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of slurry for a lithium titanate battery. The method comprises the steps of (1) preparing glue, namely adding a binder and a certain amount of solvent to a stirring tank A and stirring evenly for the first time; (2) carrying out dry mixing of powder, namely adding a conductive agent and an active substance to a stirring tank B according to the designed weight proportion, carrying out full dry mixing and stirring for a certain period of time and adding a certain amount of anhydrous oxalic acid when the active substance is lithium titanate; and (3) adding the glue which is stirred for the first time in the stirring tank A to the stirring tank B and then fully stirring evenly until the viscosity of the slurry is 6,000-10,000mpa.s. Compared with the prior art, the preparation method has the beneficial effects that (1) the steps (1) and (2) of the method can be simultaneously carried out and the preparation time of the slurry can be obviously shortened; and (2) a certain amount of anhydrous oxalic acid is added to the lithium titanate slurry, so that the pH of the slurry can be improved and the long-term cycle performance of the lithium titanate battery can also be improved.
Description
【Technical field】
The present invention relates to technical field of lithium batteries, more particularly to a kind of preparation method of lithium titanate battery slurry.
【Background technology】
At present, the continuous lifting with the progress and the mankind of science and technology to new forms of energy demand, wherein having benefited from new energy
The high speed popularization of source automobile, the demand of lithium ion battery is also increasingly increasing, the requirement to the performance of battery
In continuous improvement, but most basic premise will solve its safety problem, and lithium-ion electric is further improved in addition
Pond low temperature and quick charge capability are also a big field of existing market.
There are some drawbacks in business-like graphite cathode lithium ion battery, Li dendrite is easily formed when such as overcharging,
Battery short circuit is caused, the security performance of battery is affected;When positive pole uses the material such as ternary material or cobalt acid lithium,
There is the phenomenons such as blast on fire in acupuncture, and form SEI films during negative pole first charge-discharge and cause first charge-discharge
Efficiency is low, and irreversible capacity is big;In addition material with carbon element platform is relatively low, easily causes electrolyte decomposition etc. all can cause
Potential safety hazard and service life decline and can not realize that big multiplying power is filled soon.
Lithium titanate material is zero strain material, to lithium current potential in 1.55V or so, is not likely to produce Li dendrite, is pacified
More preferably, quick charge and low temperature charging ability are strong so as to good cycle performance, security for full performance
Energy, quick charge and low temperature charging ability, there is very big market segment space, also certainly will be to fill soon in future
The first-selection of power battery, but lithium titanate material belongs to nanometer materials, and superfines, specific surface area is larger, presses
It is difficult to prepare uniform slurry according to traditional method for preparing slurry, causes pole coating effect poor, particle
Many, battery with two side terminals and stability decline, so as to cause lithium titanate battery high rate performance poor, cycle performance
It is not good.
For above the deficiencies in the prior art and defect, it is an object of the invention to provide a kind of lithium titanate battery slurry
The preparation method of material, the method process is simple, production efficiency are high, processing time is short, slurry is more uniform,
The electrical property of battery more stable, uniformity is good.
【The content of the invention】
It is an object of the invention to provide a kind of preparation side of the lithium titanate battery slurry for solving prior art defect
Method.
To achieve these goals, the invention provides a kind of preparation method of lithium titanate battery slurry, including
Following steps:
(1) prepare glue:Binding agent and a certain amount of solvent are added in agitator tank A, and is stirred for the first time
Uniformly;
(2) powder is dry-mixed:Conductive agent and active material are added in agitator tank B according to design with weight/power ratio,
Fully dry-mixed stirring certain hour, when active material is lithium titanate, need to add a certain amount of anhydrous oxalic acid;
(3) glue that completes will be for the first time stirred in agitator tank A to add in agitator tank B, is then sufficiently stirred for
Uniformly, until the viscosity of slurry is in 6000~10000mpa.s.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, the bonding in the step (1)
Agent is PVDF, and described solvent is NMP.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, first in the step (1)
Rotating speed during secondary stirring is for 10~30RPM of revolution, scattered 500~1500RPM of rotating speed, vacuum
- 0.085MPa~-0.095MPa.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, the first time of the step (1)
Mixing time is 1~2h.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, the stirring in the step (2)
Speed is for 10~20RPM of revolution, scattered 500~1500RPM of rotating speed and must not vacuumize, and ensures
Agitator tank is in sealing state.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, the stirring in the step (2)
Time is 0.5h~1.5h, and stirring stands 10~30min after terminating.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, the conduction in the step (2)
Agent is at least one in SP, KS-6, Graphene, CNT, VGCF.
Improve as a kind of the of preparation method of lithium titanate battery slurry of the present invention, the vacuum in the step (3)
The speed of stirring is 15~30RPM of revolution, scattered 1000~2000RPM of rotating speed, and vacuum is
- 0.085MPa~-0.095MPa, mixing time is 2~4h.
Compared with prior art, the preparation method of lithium titanate battery slurry of the present invention and existing conventional process techniques
Compare, have the advantages that:
1. traditional handicraft is that single pressed powder is separately added in glue, and step is complicated and powder is easily reunited, point
Dissipate uneven.
2. the step (1) of the present invention, step (2) can be carried out simultaneously, can substantially save slurry preparation time.
3. lithium titanate slurry is poor with the caking property of collector, and in lithium titanate slurry of the present invention a certain amount of nothing is added
Pasture and water acid, you can to improve the PH of slurry, the caking property of lithium titanate slurry and collector can be improved again, be carried
The long-time cycle performance of high lithium titanate battery.
【Description of the drawings】
Fig. 1 is the lithium titanate battery 4C circulation performance comparison figures of present example one and comparison example one.
【Specific embodiment】
In order that the purpose of the present invention, technical scheme and Advantageous Effects become apparent from understanding, below in conjunction with
The drawings and specific embodiments, the present invention will be described in further detail.It should be appreciated that this explanation
Specific embodiment described in book is not intended to limit the present invention just for the sake of explaining the present invention.
Embodiment one, using stirring technique of the present invention:
Positive active material in the present embodiment is nickle cobalt lithium manganate, negative electrode active material is lithium titanate, bonding
Agent is polyvinylidene fluoride (PVDF), and solvent is NMP, and conductive agent is SP and KS-6.Wherein positive pole
NCM:SP:KS-6:PVDF=91:4:1:3;Negative pole LTO:SP:KS-6:PVDF=90:4:1:5.
Prepare anode sizing agent:
(1) during the nmp solvent of 3% PVDF and 40% total amount to be added the agitator tank A of cleaning, revolution
20RPM, scattered rotating speed 1000RPM, vacuum is -0.085MPa~-0.095MPa, stirs 1.5h,
The scraper plate scraper of Teflon material is used in pilot process twice;
(2) while the KS-6 of the SP of 91% NCM and 4% and 1% is added into the agitator tank B of cleaning
In, revolution 20RPM, scattered rotating speed 800RPM must not be vacuumized, and ensure agitator tank in sealing
State, stirs 1.5h, and 15min is stood afterwards;
(3) glue in agitator tank A and remaining 60% NMP are added to into the B stirrings that stirring is completed
In tank, revolve round the sun 25RPM, scattered rotating speed 1500RPM, and vacuum is -0.085MPa~-0.095MPa
Stirring 2.5h, revolve round the sun afterwards 10RPM, scattered rotating speed 500RPM, vacuum be -0.085MPa~
- 0.095MPa, stirs slowly the qualified rear discharging of 0.5h tested viscosities.
Prepare cathode size:
(1) during the nmp solvent of 5% PVDF and 40% total amount to be added the agitator tank A of cleaning, revolution
20RPM, scattered rotating speed 1000RPM, vacuum is -0.085MPa~-0.095MPa, stirs 1.5h,
The scraper plate scraper of Teflon material is used in pilot process twice;
(2) while the KS-6 of 90% LTO, 0.9% anhydrous oxalic acid, 4% SP and 1% is added
In the agitator tank B of cleaning, revolution 20RPM, scattered rotating speed 800RPM must not be vacuumized, and be ensured
Agitator tank is in sealing state, stirs 1.5h, and 15min is stood afterwards;
(3) glue in agitator tank A and remaining 60% NMP are added to into the B stirrings that stirring is completed
In tank, revolve round the sun 25RPM, scattered rotating speed 1500RPM, and vacuum is -0.085MPa~-0.095MPa
Stirring 2.5h, revolve round the sun afterwards 10RPM, scattered rotating speed 500RPM, vacuum be -0.085MPa~
- 0.095MPa stirs slowly 0.5h discharging tested viscosities.
The slurry of above-mentioned preparation is coated, is cut, being assembled, fluid injection, standing, chemical conversion, high temperature ageing and
Lithium titanate lithium ion battery 1 is fabricated to after partial volume.
Comparative example one:Using traditional stirring technique.
For convenience of contrast properties, adopt with identical positive and negative pole material in example one in this comparative example and match somebody with somebody
Than:Positive active material is nickle cobalt lithium manganate, negative electrode active material is lithium titanate, binding agent is PVDF, molten
Agent is NMP, and conductive agent is SP and KS-6.Wherein positive pole NCM:SP:KS-6:PVDF=91:4:1:3;
Negative pole LTO:SP:KS-6:PVDF=90:4:1:5.
Prepare anode sizing agent:
(1) during the nmp solvent of 3% PVDF and 70% total amount to be added the agitator tank A of cleaning, revolution
20RPM, scattered rotating speed 1000RPM, vacuum is -0.085MPa~-0.095MPa, stirs 2h, in
Between during with the scraper plate scraper of Teflon material twice;
(2) in the agitator tank A for adding the KS-6 of 4% SP and 1%, revolution 20RPM, dispersion
Rotating speed 1500RPM, vacuum be -0.085MPa~-0.095MPa, stir 2h, iron is used in pilot process
The scraper plate scraper of fluorine dragon material is twice;
(3) in the agitator tank A for adding 91% NCM and remaining 40%NMP, revolution 20RPM,
Scattered rotating speed 1500RPM, vacuum is -0.085MPa~-0.095MPa, stirs 2.5h, middle scraper
1~2 time, stir the qualified rear discharging of 0.5h tested viscosities slowly afterwards.
Prepare cathode size:
(1) during the nmp solvent of 5% PVDF and 70% total amount to be added the agitator tank A of cleaning, revolution
20RPM, scattered rotating speed 1000RPM, vacuum is -0.085MPa~-0.095MPa, stirs 1.5h,
The scraper plate scraper of Teflon material is used in pilot process twice;
(2) it is revolution 20RPM, scattered in the agitator tank A for adding the KS-6 of 4% SP and 1%
Rotating speed 1500RPM, vacuum is -0.085MPa~-0.095MPa, stirs 2h, and iron fluorine is used in pilot process
The scraper plate scraper of imperial material is twice;
(3) the agitator tank A for adding the anhydrous oxalic acid of 90% LTO and 0.9% and remaining 40%NMP
In, revolution 20RPM, scattered rotating speed 1500RPM, vacuum is -0.085MPa~-0.095MPa, is stirred
2.5h is mixed, middle scraper 1~2 time stirs slowly afterwards the qualified rear discharging of 0.5h tested viscosities.
The slurry of above-mentioned preparation is coated, is cut, being assembled, fluid injection, standing, chemical conversion, high temperature ageing and
Lithium titanate lithium ion battery 2 is fabricated to after partial volume.
The lithium-ion electric that the lithium ion battery 1 for below making for the present embodiment makes with existing electrodes of lithium-ion batteries
The performance comparison in pond 2:
Internal resistance and circulation performance comparison:
Citing | Initial capacity (mAh) | Initial internal resistance (m Ω) | 3000 weeks capability retentions (%) of circulation |
Battery 1 | 4307 | 4.8 | 94.83 |
Battery 2 | 4300 | 5.1 | 88.26 |
Refer to shown in Fig. 1, the lithium ion battery 1 that the present embodiment makes is carried out with existing lithium ion battery
4C circulations are tested, and from test result, the stirring technique of the lithium titanate battery slurry of the present invention is compared
The lithium ion battery that traditional stirring technique makes has more preferable circulation performance.
As can be seen here, the stirring technique of lithium titanate lithium ion battery slurry of the invention, can significantly improve slurry
The dispersiveness of material, so as to it is a certain amount of reduction battery internal resistance, it is possible to improve battery cycle performance and
The uniformity of battery core.
Embodiment described above only expresses one embodiment of the present invention, and its description is more concrete and detailed,
But therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for this area
Those of ordinary skill for, without departing from the inventive concept of the premise, can also make it is some deformation and
Improve, these belong to protection scope of the present invention.
Claims (8)
1. a kind of preparation method of lithium titanate battery slurry, it is characterised in that comprise the following steps:
(1) prepare glue:Binding agent and a certain amount of solvent are added in agitator tank A, and is stirred for the first time
Uniformly;
(2) powder is dry-mixed:Conductive agent and active material are added in agitator tank B according to design with weight/power ratio,
Fully dry-mixed stirring certain hour, when active material is lithium titanate, need to add a certain amount of anhydrous oxalic acid;
(3) glue that completes will be for the first time stirred in agitator tank A to add in agitator tank B, is then sufficiently stirred for
Uniformly, until the viscosity of slurry is in 6000~10000mpa.s.
2. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
Binding agent in the step (1) is PVDF, and described solvent is NMP.
3. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
Rotating speed when first time in the step (1) stirs is 10~30RPM of revolution, scattered rotating speed 500~
1500RPM, vacuum are -0.085MPa~-0.095MPa.
4. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
The first time mixing time of the step (1) is 1~2h.
5. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
Mixing speed in the step (2) for revolution 10~20RPM, scattered 500~1500RPM of rotating speed and
Must not vacuumize, and ensure that agitator tank is in sealing state.
6. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
Mixing time in the step (2) is 0.5h~1.5h, and stirring stands 10~30min after terminating.
7. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
Conductive agent in the step (2) is at least in SP, KS-6, Graphene, CNT, VGCF
Kind.
8. the preparation method of a kind of lithium titanate battery slurry according to claim 1, it is characterised in that:
The speed of the vacuum stirring in the step (3) for revolution 15~30RPM, scattered rotating speed 1000~
2000RPM, vacuum is -0.085MPa~-0.095MPa, and mixing time is 2~4h.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107681109A (en) * | 2017-09-19 | 2018-02-09 | 合肥国轩高科动力能源有限公司 | A kind of lithium titanate battery slurry and preparation method thereof |
CN107834048A (en) * | 2017-11-24 | 2018-03-23 | 深圳市比克动力电池有限公司 | Negative electrode of lithium titanate battery slurry and preparation method thereof |
CN110165157A (en) * | 2019-04-22 | 2019-08-23 | 河南电池研究院有限公司 | A kind of uniform method for mixing of the lithium titanate slurry of carbon nanotubes |
CN110459410A (en) * | 2019-07-24 | 2019-11-15 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of super capacitor slurry and its supercapacitor prepared using super capacitor slurry |
CN112234199A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery positive electrode plate |
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CN101685861A (en) * | 2008-09-25 | 2010-03-31 | 深圳市比克电池有限公司 | Method for preparing lithium titanate cathode size |
CN102623689A (en) * | 2012-03-28 | 2012-08-01 | 重庆永通信息工程实业有限公司 | Manufacture process for lithium ion battery negative pulp adopting lithium titanate material |
CN102637905A (en) * | 2012-05-03 | 2012-08-15 | 江西省福斯特新能源有限公司 | Lithium battery manufacturing method |
CN102903930A (en) * | 2012-10-23 | 2013-01-30 | 中国科学院过程工程研究所 | Lithium ion secondary battery and preparation method thereof |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101685861A (en) * | 2008-09-25 | 2010-03-31 | 深圳市比克电池有限公司 | Method for preparing lithium titanate cathode size |
CN102623689A (en) * | 2012-03-28 | 2012-08-01 | 重庆永通信息工程实业有限公司 | Manufacture process for lithium ion battery negative pulp adopting lithium titanate material |
CN102637905A (en) * | 2012-05-03 | 2012-08-15 | 江西省福斯特新能源有限公司 | Lithium battery manufacturing method |
CN102903930A (en) * | 2012-10-23 | 2013-01-30 | 中国科学院过程工程研究所 | Lithium ion secondary battery and preparation method thereof |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107681109A (en) * | 2017-09-19 | 2018-02-09 | 合肥国轩高科动力能源有限公司 | A kind of lithium titanate battery slurry and preparation method thereof |
CN107834048A (en) * | 2017-11-24 | 2018-03-23 | 深圳市比克动力电池有限公司 | Negative electrode of lithium titanate battery slurry and preparation method thereof |
CN110165157A (en) * | 2019-04-22 | 2019-08-23 | 河南电池研究院有限公司 | A kind of uniform method for mixing of the lithium titanate slurry of carbon nanotubes |
CN110165157B (en) * | 2019-04-22 | 2022-03-18 | 河南电池研究院有限公司 | Uniform mixing method of lithium titanate slurry containing carbon nano tubes |
CN110459410A (en) * | 2019-07-24 | 2019-11-15 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of super capacitor slurry and its supercapacitor prepared using super capacitor slurry |
CN112234199A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery positive electrode plate |
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