CN104835938A - Preparation method of lithium ion battery anode slurry - Google Patents
Preparation method of lithium ion battery anode slurry Download PDFInfo
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- CN104835938A CN104835938A CN201510188238.6A CN201510188238A CN104835938A CN 104835938 A CN104835938 A CN 104835938A CN 201510188238 A CN201510188238 A CN 201510188238A CN 104835938 A CN104835938 A CN 104835938A
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000006256 anode slurry Substances 0.000 title abstract 3
- 239000002002 slurry Substances 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000006258 conductive agent Substances 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000010405 anode material Substances 0.000 claims abstract description 4
- 239000006257 cathode slurry Substances 0.000 claims description 28
- 239000007773 negative electrode material Substances 0.000 claims description 19
- 239000011230 binding agent Substances 0.000 claims description 18
- 239000000853 adhesive Substances 0.000 claims description 17
- 230000001070 adhesive effect Effects 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 20
- 239000008367 deionised water Substances 0.000 abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000007767 bonding agent Substances 0.000 abstract 4
- 238000007865 diluting Methods 0.000 abstract 1
- 238000004898 kneading Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 239000011149 active material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910052493 LiFePO4 Inorganic materials 0.000 description 4
- 239000012895 dilution Substances 0.000 description 4
- 238000010790 dilution Methods 0.000 description 4
- 239000000428 dust Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- H01M4/04—Processes of manufacture in general
-
- 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
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a lithium ion battery anode slurry. The preparation method comprises the following steps: firstly, diluting a bonding agent with a certain amount of deionized water, adding a part of anode material into the diluted bonding agent solution, and stirring to obtain a primary slurry; secondly, adding a conductive agent into the primary slurry, and stirring to obtain a secondary slurry; and lastly, adding the remaining anode anode material and deionized water into the secondary slurry, and stirring for a certain period of time to obtain the anode slurry. A pure powder mixing process is omitted, and the bonding agent is diluted firstly and then powder is added into the diluted bonding agent solution in a slurry preparation process, so that the problems of powder flying and the like caused by pure powder stirring are solved, and the slurry making efficiency is increased. Compared with an existing slurry combining process, the method has the advantages that the slurry has higher solid content in a kneading process, and a better dispersion effect can be achieved.
Description
Technical field
The invention belongs to technical field of lithium-ion battery, be specifically related to a kind of preparation method of lithium ion battery cathode slurry.
Background technology
Lithium ion battery has the advantages such as operating voltage is high, energy density is high, non-environmental-pollution, is widely used at present in daily life.Lithium ion battery generally comprises positive and negative electrode pole piece, barrier film, electrolyte etc.Time prepared by electrode plates, first by active material (LiFePO4, graphite etc.), conductive agent (conductive black, acetylene black etc.), binding agent (LA132, PVDF, CMC, SBR) and solvent (NMP, H
2o) be mixed together and make electrode slurry, then it is coated in collection liquid surface on request, obtain pole piece through super-dry.
The preparation of slurry is the critical process of lithium battery production link, and the uniformity coefficient of slurry mixing is directly connected to preparation technology and the battery performance of follow-up each operation.Cathode size generally includes graphite, conductive agent, binding agent and solvent etc.Traditional method slurry preparation method first binding agent and solvent is mixed, and adds conductive agent and stir obtained conducting resinl, in conducting resinl, then add active material stir, and finally adds solvent adjustment viscosity and obtain the slurry being applicable to be coated with.Because conductive agent belongs to low polarity lipophilicity substance, disperse comparatively difficulty in an aqueous medium.In addition, when adopting traditional handicraft to close slurry, the general solid content of slurry is on the low side, causes the dispersion effect of slurry poor.And whole preparation process is consuming time longer.
For overcoming the above problems, roughly flow process is as follows generally to have employed new slurry-stirring process at present: first conductive agent and active material are carried out premixed and obtain powder mixture, in mixture, then adds binder solution stir, finally obtained slurry.This technique is more and more applied.But adopt the method for powder premixed, occur a large amount of points of dust from flying at the preparation initial stage of slurry, produce environment and personnel on the one hand and do not measure impact, the powder loss caused due to dust from flying on the other hand also have impact on the consistency of slurry.
Therefore, work out a kind of preparation method of lithium ion battery cathode slurry, while guaranteeing that its solid content is high, reduce powder in its preparation process and fly upward, and improve its dispersiveness, the development being prepared by lithium ion battery to industry is significant.
Summary of the invention
In order to overcome the defect of prior art, object of the present invention provides a kind of preparation method of lithium ion battery cathode slurry that is simple efficient, that fly upward without powder.
To achieve these goals, the technical solution used in the present invention is as follows:
Prepared by a kind of method of lithium ion battery cathode slurry, concrete operation step is:
1) negative electrode active material powder body material, conductive agent and adhesive is got; The mass ratio of negative electrode active material powder body material, electric agent, adhesive is (85 ~ 96): (2 ~ 9): (2 ~ 6);
2) in adhesive, add solvent, after mixing, obtain binder solution;
3) part negative electrode active material powder body material is added step 2) in the binder solution prepared, stir, obtain elementary slurry;
4) conductive agent is added step 3) in the elementary slurry prepared, stir, obtain secondary slurries;
5) remaining negative electrode active material powder body material is added step 4) in the secondary slurries prepared, stir, add solvent adjustment viscosity and obtain the lithium ion battery cathode slurry that solid content is 50 ~ 70%;
Wherein step 3) and step 5) in the mass ratio of negative electrode active material powder body material be (1 ~ 2): 1.
Described negative electrode active material powder body material is one or more the mixing in Delanium, native graphite, lithium titanate anode material.
Described adhesive is aqueous binder LA132.
Described conductive agent is at least one in conductive black SP, KS-6.
Step 3) described in stir time be 30 ~ 60min.
Step 4) described in stir time be 60 ~ 240min.
Step 3), step 4) and step 5) in speed of agitator be not more than 30r/min.
In slurry preparation process, step 3) in be not more than 30r/min revolution speed stir 30 ~ 60min obtain elementary slurry, step 4) in be not more than 30r/min revolution speed stir 60 ~ 240min obtain secondary slurries, step 5) in add and stir 60min with the revolution speed being not more than 30r/min before solvent after, add solvent to be not more than the revolution speed of 30r/min, the rotational velocity of 1500r/min stirs 60min, obtains the lithium ion battery cathode slurry that solid content is 50 ~ 70%.
Lithium ion battery cathode slurry of the present invention, adopt the binder solution first preparing dilution, get the binder solution that amount of activated material adds dilution again, add conductive agent again, the preparation method of remaining active material prepares, and lithium ion battery cathode slurry solid content of the present invention is high, and conductive agent is added in the mixed serum of the binder solution of part negative electrode active material and dilution, improve the dissolubility of conductive agent, and then make the particle diameter of cathode size little, be easy to stably dispersing.
The preparation method of lithium ion battery cathode slurry of the present invention, the present invention adopts initial stage wet mixing, high solids content is mediated, and then the operating procedure that dilution is stirred prepares cathode size, namely adhesive and solvent is first added at the initial stage of closing slurry, and then add part negative electrode active material and conductive agent, finally add remaining active material, eliminate the process of simple powder mixing, avoid and be dry mixed the powder caused and fly upward, and the powder after being dry mixed, after adding adhesive and solvent, a large amount of powders increases the load of equipment, need longer incorporation time just can stir, the present invention adopts active material to add in batches, and cancel the method for simple powder mixing, both ensure that high solids content was mediated, improve the solid content of cathode size, alleviate apparatus of load again, shorten incorporation time, improve pulping efficiency.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
The present embodiment lithium ion battery cathode slurry, negative electrode active material powder body material is LiFePO4, and conductive agent is the mixture of SP and KS-6, and adhesive is LA132, and mass ratio is: Delanium: SP:KS-6:LA132=92:3:2:3.
The present embodiment lithium ion battery cathode slurry is prepared by following methods and obtains, and the method concrete operation step is as follows:
1) example takes Delanium, SP, KS-6 and LA132 in mass ratio;
2) adhesive is added in deionized water, obtain binder solution;
3) step 2 is added by 1/2 of Delanium total amount) in the binder solution prepared, the revolution speed with 25r/min in double planetary mixer stirs 60min respectively, obtains elementary slurry;
4) SP and KS-6 all being added step 3 successively) in the elementary slurry prepared, the revolution speed with 25r/min in double planetary mixer stirs 90min respectively, obtains secondary slurries;
5) remaining 1/2 LiFePO4 is added step 4) in the secondary slurries prepared, with the revolution speed 60min of 25r/min in double planetary mixer, finally add deionized water, the cathode size of obtained solid content 60% stir 60min with the rotational velocity of the revolution speed of 10r/min, 1500r/min in double planetary mixer after.
Embodiment 2
The present embodiment lithium ion battery cathode slurry, negative electrode active material powder body material is native graphite, and conductive agent is SP, and adhesive is LA132, and mass ratio is native graphite: SP:LA132=93:3.5:3.5.
The present embodiment lithium ion battery cathode slurry is prepared by following methods and obtains, and the method concrete operation step is as follows:
1) example takes native graphite, SP and LA132 in mass ratio;
2) adhesive is added in deionized water, obtain binder solution;
3) step 2 is added by 1/2 of native graphite total amount) in the binder solution prepared, the revolution speed with 25r/min in double planetary mixer stirs 30min respectively, obtains elementary slurry;
4) SP all being added step 3) in the elementary slurry prepared, the revolution speed with 25r/min in double planetary mixer stirs 120min respectively, obtains secondary slurries;
5) remaining 1/2 native graphite is added step 4) in the secondary slurries prepared, with the revolution speed 60min of 25r/min in double planetary mixer, finally add deionized water, the cathode size of obtained solid content 65% stir 60min with the rotational velocity of the revolution speed of 10r/min, 1500r/min in double planetary mixer after.
Embodiment 3
The present embodiment lithium ion battery cathode slurry, negative electrode active material powder body material is LiFePO4, and conductive agent is SP, and adhesive is LA32, and mass ratio is lithium titanate: SP:KS-6: LA132=85:5:4:6.
The present embodiment lithium ion battery cathode slurry is prepared by following methods and obtains, and the method concrete operation step is as follows:
1) example takes lithium titanate, SP, KS-6 and LA132 in mass ratio;
2) adhesive is added in deionized water, obtain binder solution;
3) step 2 is added by 2/3 of lithium titanate total amount) in the binder solution prepared, the revolution speed with 30r/min in double planetary mixer stirs 30min respectively, obtains elementary slurry;
4) SP all being added step 3) in the elementary slurry prepared, the revolution speed with 25r/min in double planetary mixer stirs 60min respectively, obtains secondary slurries;
5) remaining 1/3 lithium titanate is added step 4) in the secondary slurries prepared, with the revolution speed 60min of 25r/min in double planetary mixer, finally add deionized water, the cathode size of obtained solid content 70% stir 60min with the rotational velocity of the revolution speed of 10r/min, 1500r/min in double planetary mixer after.
Comparative example 1
Lithium ion battery cathode slurry formula is Delanium: SP:KS-6:LA132=92%:3%:2%:3%, preparation method is: 1) first diluted by adhesive LA132, then add conductive agent SP and KS-6 successively and stir 60min respectively, then deionized water is added, with the 5r/min that revolves round the sun in double planetary mixer, the speed of rotation 1800r/min stirs 120min, obtained conducting resinl; 2) divided by Delanium and progressively add for three times in the conducting resinl prepared, revolution speed 25r/min stirs 30min respectively.Add deionized water, with the 5r/min that revolves round the sun in double planetary mixer, the speed of rotation 1800r/min stirs 90min, finally the cathode size of obtained solid content 60%.
Comparative example 2
Lithium ion battery cathode slurry formula is native graphite: SP:LA132=93%:3.5%:3.5%, preparation method is: part negative electrode active material and conductive agent SP are carried out mix and blend 30min, then adds adhesive and partial solvent and stirs 120min with the revolution speed of 25r/min and obtain elementary slurry.The negative electrode active material of remainder and solvent are added and stirs 60min with the revolution speed of 25r/min, then stir 60min further with the speed of the 5r/min that revolves round the sun, rotation 1800r/min, finally the cathode size of obtained solid content 65%.
Detect the embodiment of the present invention 1,2,3, the particle diameter of lithium ion battery cathode slurry prepared with comparative example 1, measurement result is as shown in table 1.
The particle diameter test result of table 1 embodiment and comparative example
Shown by the testing result shown in table 1, slurry particle diameter prepared by the embodiment of the present invention 1 and embodiment 2 is significantly less than comparative example 1 and comparative example 2, illustrate that the particle diameter of lithium ion battery cathode slurry prepared by this employing inventive method is little, the degree that is uniformly dispersed is good, and slurry is more stable.
Claims (7)
1. a preparation method for lithium ion battery cathode slurry, its preparation process is as follows:
1) negative electrode active material powder body material, conductive agent and adhesive is got; The mass ratio of negative electrode active material powder body material, electric agent, adhesive is (85 ~ 96)): (2 ~ 9): (2 ~ 6);
2) in adhesive, add solvent, after mixing, obtain binder solution;
3) part negative electrode active material powder body material is added step 2) in the binder solution prepared, stir and obtain elementary slurry;
4) conductive agent is added in elementary slurry prepared by step 3), stir and obtain secondary slurries;
5) remaining negative electrode active material powder body material is added in secondary slurries prepared by step 4), stir, add solvent adjustment viscosity and obtain the lithium ion battery cathode slurry that solid content is 50 ~ 70%.
2. the preparation method of a kind of lithium ion battery cathode slurry as claimed in claim 1, is characterized in that: the negative electrode active material powder body material described in step 1) is one or more the mixing in Delanium, native graphite, lithium titanate anode material.
3. the preparation method of a kind of lithium ion battery cathode slurry as claimed in claim 1, is characterized in that: in step 3) and step 5), the mass ratio of negative electrode active material powder body material is (1 ~ 2): 1.
4. the preparation method of a kind of lithium ion battery cathode slurry as claimed in claim 1, is characterized in that: the conductive agent described in step 1) is at least one in conductive black SP, KS-6.
5. the preparation method of a kind of lithium ion battery cathode slurry as claimed in claim 1, is characterized in that: the time of stirring described in step 3) is 30 ~ 60min.
6. the preparation method of a kind of lithium ion battery cathode slurry as claimed in claim 1, is characterized in that: the time of stirring described in step 4) is 60 ~ 240min.
7. the preparation method of a kind of lithium ion battery cathode slurry as claimed in claim 1, is characterized in that: in step 3), step 4) and step 5), speed of agitator is not more than 30r/min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510188238.6A CN104835938A (en) | 2015-04-20 | 2015-04-20 | Preparation method of lithium ion battery anode slurry |
| PCT/CN2015/098493 WO2016169289A1 (en) | 2015-04-20 | 2015-12-23 | Method for preparing lithium ion battery negative electrode slurry |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510188238.6A CN104835938A (en) | 2015-04-20 | 2015-04-20 | Preparation method of lithium ion battery anode slurry |
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| CN201510188238.6A Pending CN104835938A (en) | 2015-04-20 | 2015-04-20 | Preparation method of lithium ion battery anode slurry |
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| WO2016169289A1 (en) * | 2015-04-20 | 2016-10-27 | 田东 | Method for preparing lithium ion battery negative electrode slurry |
| CN108461703A (en) * | 2018-02-23 | 2018-08-28 | 安徽益佳通电池有限公司 | A kind of preparation method of lithium ion battery electrode sizing agent |
| CN110690412A (en) * | 2019-10-22 | 2020-01-14 | 合肥国轩高科动力能源有限公司 | A kind of ternary lithium ion battery positive electrode sheet and its preparation method and battery |
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