CN103872306A - Preparation method of lithium titanate negative electrode slurry - Google Patents
Preparation method of lithium titanate negative electrode slurry Download PDFInfo
- Publication number
- CN103872306A CN103872306A CN201410109865.1A CN201410109865A CN103872306A CN 103872306 A CN103872306 A CN 103872306A CN 201410109865 A CN201410109865 A CN 201410109865A CN 103872306 A CN103872306 A CN 103872306A
- Authority
- CN
- China
- Prior art keywords
- lithium titanate
- preparation
- dew point
- negative pole
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- H01M4/62—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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of lithium titanate negative electrode slurry. The preparation method comprises the following steps: lithium titanate, a conductive agent and a binding agent are baked and weighed, wherein a control range Td of an environment dew point is less than or equal to -10 DEG C; a non-ion type high molecular surfactant is added in a slurry preparation process, wherein the adding amount of the non-ion type high molecular surfactant is 0.1wt%-1wt% by taking slurry solid powder as 100%. An adding method of the non-ion type high molecular surfactant comprises the following steps: firstly, drying the lithium titanate, the conductive agent, the binding agent and the non-ion type high molecular surfactant and mixing uniformly; and adding a solvent, vacuumizing and agitating at a high speed to prepare the lithium titanate negative electrode slurry. The control range Td of the environment dew point for screening the slurry is less than or equal to -10 DEG C. The preparation method of the lithium titanate negative electrode slurry with high dispersing performance is capable of effectively improving the electric capacity of the lithium titanate.
Description
Technical field
The invention belongs to lithium-ion-power cell field, be specifically related to improve the slurry dispersive property in lithium titanate electrode production process, improve the capacitance of lithium titanate.
Background technology
At present, the development of lithium ion battery, is not only confined to engrave with oneself the 3C Product of band, more takes a broad view in military project energy storage even electric automobile market of electrodynamic type bicycle.The conventional negative pole of most is still carbon negative pole material, and material with carbon element exists some shortcomings: as it is low etc. to separate out Li dendrite, first charge-discharge efficiency.
Due to the existing potential safety hazard of material with carbon element, lithium titanate, compared with carbon negative pole material, has better chemical property and fail safe: discharge and recharge change in volume little, be called in the industry " zero strain " material, have good charge and discharge platform, good cycle; Do not react with electrolyte, do not form SEI film, first charge-discharge efficiency is higher, can reach 95% left and right; There is embedding lithium current potential high (1.55Vvs.Li/Li+), do not produce lithium dendrite arm (can not cause dendrite arm short circuit blast), there is huge commercial application prospect for negative electrode of power lithium-ion battery material, for the safety that ensures lithium battery provides the foundation, can improve cycle performance and the useful life of battery, thereby become the emphasis of current global lithium electricity industry research.
But, and even lithium titanate is as the nano level material of a kind of micron order, specific area is large, and pH value is higher, easily water suction, practice is in li-ion electrode slurry, have cohesion, agglomeration, cause its processing characteristics extreme difference, pole piece material skewness, has a strong impact on the performance of lithium titanate electrode material capacity.Therefore, finding a kind of pulping process of new lithium titanate anode material, is the problem that current people extremely pay close attention to, and meaning of the present invention is to solve negative pole batch mixing problem, brings the quality drawback in negative pole batch mixing process.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method who improves lithium titanate electrode slurry dispersive property is provided, thereby improve electrode processing characteristics, improve the capacitance of lithium titanate.
Technical scheme of the present invention is: a kind of preparation method of lithium titanate cathode size, comprises the steps:
(1) take negative pole raw material, the weight of negative pole raw material consists of: lithium titanate 84%-94%, conductive agent SUPERP4%-8%, binding agent PVDF3%-8%, add the non-ionic (polymeric surfactant) KD-1 of the 0.1%-1% of negative pole raw material total weight, control corresponding environment dew point;
(2) material step (1) being obtained is dry mixed mixing and stirring;
(3) add solvent 1-METHYLPYRROLIDONE (NMP), solvent adding amount is the 100%-180% of the weight of material that obtains of step (2), vacuumizes high-speed stirred;
(4) adopt screen cloth to filter slurry, dew point controls environment.
Further, in step (1), negative pole raw material measures after need to vacuumizing baking, and the parameter that vacuumizes baking is: vacuum degree≤-0.085Mpa, temperature 80-150 DEG C, time 5-12H.
Further, in step (1), environment dew point control criterion is Td≤-10 DEG C.
Further, in step (4), slurries filtration use screen cloth specification is 80～100 orders, corresponding environment dew point scope control Td≤-10 DEG C.
SUPERP is a kind of nano-carbon powder, and ater superfine powder has higher conductivity and oil factor, and thermal conductivity is good.Production method: adopt carbide, i.e. first electricity consumption one-tenth acetylene gas made of stones, through purifying, makes acetylene gas isolated air under 1400 DEG C of left and right high temperature carry out cracking, then through cooling, collect and obtain.Application is mainly used in the manufacture of dry cell, telecommunication facsimile transmission paper, electrophoretic primer and radio component.Also for the manufacture of vulcanie goods, the manufacture of lithium battery.
Binding agent PVDF is polyvinylidene fluoride, and non-ionic (polymeric surfactant) KD-1 is a product type, and its structure is that (a hexahydric acid low polymerization degree polymer ends is connected to C to polyesters
12the polyesters structure of alkyl).Structure is as follows:
Change lithium titanate slurry because of the high easily water absorption character of pH value, the present invention in slurry preparation process, all links in air exposure process, strictly controlled environment dew point value.Improve lithium titanate battery processing characteristics, alleviate inflatable degree.
Improve the dispersiveness of lithium titanate cathode size, need to consider following factor: 1, electrostatic stabilization 2, sterically hindered stability.The present invention adopts nmp solvent mixing lithium titanate, add a kind of non-ionic (polymeric surfactant), macromolecular compound is adsorbed in particle surface, utilizes sterically hindered stabilization, make lithium titanate cathode size form stable suspension system, reach best dispersion effect.
Brief description of the drawings
Accompanying drawing 1: lithium titanate slurry viscosity is with the variation of period of storage;
Accompanying drawing 2: lithium titanate gram volume performance.
Embodiment
A preparation method for lithium titanate cathode size, comprises the steps:
(1) after being vacuumized to baking, lithium titanate, conductive agent, binding agent weigh in proportion, lithium titanate 84%-94%, conductive agent SUPERP4%-8%, binding agent PVDF3%-8%, add the non-ionic (polymeric surfactant) KD-1 of the 0.1%-1% of negative pole raw material total weight, control corresponding environment dew point.
(2) above-mentioned material is dry mixed to mixing and stirring.
(3) add solvent 1-METHYLPYRROLIDONE (NMP), solvent adding amount is the 100%-180% of the weight of material that obtains of step (2), vacuumizes high-speed stirred.
(4) adopt screen cloth to filter slurry, dew point controls environment.
Embodiment 1
1, lithium titanate, conductive agent, binding agent are vacuumized to baking.Powder baking standard is vacuum degree≤-0.085Mpa, temperature 80-150 DEG C, time 5-12H.
2, weigh in proportion.Lithium titanate 91.5% (W/W), SUPERP5% (W/W), PVDF3% (W/W).Now to non-ionic (polymeric surfactant) KD-1 0.5% (W/W) that weigh equally.The environment dew point control criterion of weighing is Td≤-10 DEG C.
3, above-mentioned material is added to double-planet stir mixing system mix and blend 2H.
4, add 130% (W/W) nmp solvent, vacuumize high-speed stirred 8H.
5, adopt 200 eye mesh screens to filter slurry, corresponding environment dew point scope control Td≤-10 DEG C.
6, adopt Lai Bu scientific & technical corporation rotation viscometer to carry out viscosity test and follow the tracks of Stability of Slurry.
7, be made into battery (30pcs) and follow the tracks of the performance of negative pole gram volume.
Comparative example
Substantially with embodiment 1, except strengthening corresponding viscosity control, do not add non-ionic (polymeric surfactant) KD-1.
Table 1: lithium titanate slurry viscosity is with the variation of period of storage
Table 2 lithium titanate gram volume performance contrast
Claims (4)
1. a preparation method for lithium titanate cathode size, is characterized in that, comprises the steps:
(1) take negative pole raw material, the weight of negative pole raw material consists of: lithium titanate 84%-94%, conductive agent SUPER P 4%-8%, binding agent PVDF 3%-8%, add the non-ionic (polymeric surfactant) KD-1 of the 0.1%-1% of negative pole raw material total weight, control corresponding environment dew point;
(2) material step (1) being obtained is dry mixed mixing and stirring;
(3) add solvent 1-METHYLPYRROLIDONE (NMP), solvent adding amount is the 100%-180% of the weight of material that obtains of step (2), vacuumizes high-speed stirred;
(4) adopt screen cloth to filter slurry, dew point controls environment.
2. the preparation method of a kind of lithium titanate cathode size according to claim 1, it is characterized in that, in step (1), negative pole raw material measures after need to vacuumizing baking, and the parameter that vacuumizes baking is: vacuum degree≤-0.085Mpa, temperature 80-150 DEG C, time 5-12H.
3. the preparation method of a kind of lithium titanate cathode size according to claim 1, is characterized in that, in step (1), environment dew point control criterion is Td≤-10 DEG C.
4. the preparation method of a kind of lithium titanate cathode size according to claim 1, is characterized in that, in step (4), slurries filtration use screen cloth specification is 80 ~ 100 orders, corresponding environment dew point scope control Td≤-10 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410109865.1A CN103872306A (en) | 2014-03-24 | 2014-03-24 | Preparation method of lithium titanate negative electrode slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410109865.1A CN103872306A (en) | 2014-03-24 | 2014-03-24 | Preparation method of lithium titanate negative electrode slurry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103872306A true CN103872306A (en) | 2014-06-18 |
Family
ID=50910617
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410109865.1A Pending CN103872306A (en) | 2014-03-24 | 2014-03-24 | Preparation method of lithium titanate negative electrode slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103872306A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577089A (en) * | 2014-11-19 | 2015-04-29 | 山东精工电子科技有限公司 | Preparation method of lithium titanate negative-electrode slurry |
| CN104835938A (en) * | 2015-04-20 | 2015-08-12 | 田东 | Preparation method of lithium ion battery anode slurry |
| CN106602051A (en) * | 2016-12-23 | 2017-04-26 | 山东精工电子科技有限公司 | Preparation method of negative electrode slurry for lithium titanate battery |
| JP2017188203A (en) * | 2016-04-01 | 2017-10-12 | 住友金属鉱山株式会社 | Method of evaluating stability of positive electrode material slurry for lithium ion secondary battery |
| CN110707318A (en) * | 2019-08-06 | 2020-01-17 | 湖南华慧新能源股份有限公司 | Preparation method of lithium titanate battery negative electrode slurry |
| CN112467065A (en) * | 2020-11-20 | 2021-03-09 | 山东精工电子科技有限公司 | Rapid and efficient preparation method of lithium ion battery slurry, pole piece and battery thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101609881A (en) * | 2009-07-17 | 2009-12-23 | 江苏富朗特新能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN101752545A (en) * | 2008-12-03 | 2010-06-23 | 北京有色金属研究总院 | Electrode of lithium battery, preparation method of electrode and lithium battery adopting electrode |
| CN101901932A (en) * | 2010-05-17 | 2010-12-01 | 江西省福斯特新能源有限公司 | Quick-chargeable, high-security and high-multiplying-power battery and production method thereof |
| CN102130363A (en) * | 2011-01-31 | 2011-07-20 | 北京神州远望科技有限公司 | High magnification polymer lithium ion power battery and preparation method thereof |
| WO2012111547A1 (en) * | 2011-02-18 | 2012-08-23 | 株式会社 東芝 | Non-aqueous electrolyte secondary battery and method for producing same |
-
2014
- 2014-03-24 CN CN201410109865.1A patent/CN103872306A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101752545A (en) * | 2008-12-03 | 2010-06-23 | 北京有色金属研究总院 | Electrode of lithium battery, preparation method of electrode and lithium battery adopting electrode |
| CN101609881A (en) * | 2009-07-17 | 2009-12-23 | 江苏富朗特新能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN101901932A (en) * | 2010-05-17 | 2010-12-01 | 江西省福斯特新能源有限公司 | Quick-chargeable, high-security and high-multiplying-power battery and production method thereof |
| CN102130363A (en) * | 2011-01-31 | 2011-07-20 | 北京神州远望科技有限公司 | High magnification polymer lithium ion power battery and preparation method thereof |
| WO2012111547A1 (en) * | 2011-02-18 | 2012-08-23 | 株式会社 東芝 | Non-aqueous electrolyte secondary battery and method for producing same |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577089A (en) * | 2014-11-19 | 2015-04-29 | 山东精工电子科技有限公司 | Preparation method of lithium titanate negative-electrode slurry |
| CN104835938A (en) * | 2015-04-20 | 2015-08-12 | 田东 | Preparation method of lithium ion battery anode slurry |
| JP2017188203A (en) * | 2016-04-01 | 2017-10-12 | 住友金属鉱山株式会社 | Method of evaluating stability of positive electrode material slurry for lithium ion secondary battery |
| CN106602051A (en) * | 2016-12-23 | 2017-04-26 | 山东精工电子科技有限公司 | Preparation method of negative electrode slurry for lithium titanate battery |
| CN110707318A (en) * | 2019-08-06 | 2020-01-17 | 湖南华慧新能源股份有限公司 | Preparation method of lithium titanate battery negative electrode slurry |
| CN112467065A (en) * | 2020-11-20 | 2021-03-09 | 山东精工电子科技有限公司 | Rapid and efficient preparation method of lithium ion battery slurry, pole piece and battery thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105932229B (en) | A kind of preparation method of high capacity lithium ion cells cathode piece | |
| CN102522530B (en) | Nano-sulfur composite cathode material for rare earth lithium-sulfur battery, and preparation method thereof | |
| CN103872306A (en) | Preparation method of lithium titanate negative electrode slurry | |
| CN103117414B (en) | A kind of negative pole lithium titanate battery electrolyte, lithium ion battery and preparation method thereof | |
| CN106299280B (en) | Preparation method of high-capacity lithium ion battery anode slurry | |
| CN105355877B (en) | A kind of graphene metal oxide composite cathode material and preparation method thereof | |
| CN103682286B (en) | Silicon/high molecular composite microsphere and silicon-carbon composite anode material for lithium ion battery and preparation method thereof | |
| CN107026262B (en) | High-capacity spherical hard carbon negative electrode material coated with graphene on surface | |
| CN103199258A (en) | Cathode material of lithium ion battery, preparation method of cathode, and lithium ion battery | |
| CN103165869B (en) | Modification mesophase spherule negative material, lithium rechargeable battery and preparation method and application | |
| CN107845802B (en) | A kind of conducting polymer for lithium battery coats cobalt acid lithium and preparation method thereof | |
| CN104037417B (en) | A kind of modified natural graphite and preparation method thereof | |
| CN103928668B (en) | Lithium ion battery and preparation method of anode material thereof | |
| CN107910521B (en) | Ruthenium-modified carbon fluoride material, preparation and application | |
| CN103682295B (en) | A kind of lithium ion battery cathode material and its preparation method, anode plate for lithium ionic cell and lithium ion battery | |
| CN102637847A (en) | Method for preparing high-dispersity lithium battery anode and cathode slurry | |
| CN105161687B (en) | A kind of preparation method of selenium combination electrode material | |
| CN104300129A (en) | Battery, battery cathode, battery cathode material and preparation method thereof | |
| CN102881883B (en) | Ternary composite cathode material of lithium battery and preparation method of ternary composite cathode material | |
| CN104979541A (en) | Lithium titanate composite material and preparation method thereof | |
| CN106025268A (en) | Water-based lithium battery cathode slurry and preparation method thereof | |
| CN105406071B (en) | A kind of high magnification vanadium phosphate cathode material and its preparation method and application | |
| CN103833011A (en) | Graphene/carbon black composite material, preparation method and application thereof | |
| CN107732200A (en) | A kind of method that lithium ion battery negative material is prepared using photovoltaic industry waste material | |
| CN111129500A (en) | Preparation method of aqueous composite carbon nanotube conductive slurry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140618 |
|
| RJ01 | Rejection of invention patent application after publication |