CN101937990B - Preparation method of nano lithium iron phosphate positive slurry - Google Patents
Preparation method of nano lithium iron phosphate positive slurry Download PDFInfo
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- CN101937990B CN101937990B CN2010102931160A CN201010293116A CN101937990B CN 101937990 B CN101937990 B CN 101937990B CN 2010102931160 A CN2010102931160 A CN 2010102931160A CN 201010293116 A CN201010293116 A CN 201010293116A CN 101937990 B CN101937990 B CN 101937990B
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- 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 discloses a preparation method of nano lithium iron phosphate positive slurry, which is characterized by comprising the following steps of: (1) weighing all the following raw materials according to the weight ratio: 0.1-0.9 part of conducting material as a lithium iron phosphate active material, 0.2-1 part of binder and 10-40 parts of solvent: (2) drying all the weighed raw materials; (3) preparing the raw materials dried by the step (2) into a binder solution; (4) mixing the active substances dried in the step (2); and (5) mixing the binder solution with the active substances, stirring for 2h to prepare slurry with the viscosity of 5000-11000 cP, and sieving with a 100-mesh to 150-mesh sieve to obtain the nano lithium iron phosphate positive slurry. The adoption of the nanorized lithium iron phosphate material can increase the transfer rate of ions and electrons, and the conducting property of the material is improved.
Description
Technical field
The present invention relates to a kind of preparation method of nano-grade lithium iron phosphate anode sizing agent, and the ferric phosphate lithium cell that uses this slurry to process, lithium rechargeable battery manufacturing technology field belonged to.
Background technology
Characteristics such as LiFePO 4 material has that fail safe is good, cycle performance is excellent, environmental friendliness, raw material sources are extensive; Wherein, Lithium, iron, phosphorus all are the abundant elements of reserves on the earth, and especially the ferrous material raw material sources are wide, and are cheap; Be acknowledged as the first-selected positive electrode of lithium ion battery of new generation, become the primary study and the developing direction of main developed country in the world today.And, because self and employed electrolyte are stable under its high temperature, and have the good high-temperature cycle performance, be particularly suitable for doing electrokinetic cell.
Secondly, its relative Ni-H, the Ni-Cd battery has great advantage.Lithium iron phosphate dynamic battery has seven big advantages: one, extra long life.2000 circulation volume conservation rates are more than 80%.Two, safe in utilization; LiFePO4 has solved the security hidden trouble of cobalt acid lithium and LiMn2O4 fully; Cobalt acid lithium and LiMn2O4 can produce blast consumer's life security is constituted a threat under strong collision, even and LiFePO4 can not produce blast with the safety test of passing through strictness yet in worst traffic accident.Three, electric current fast charging and discharging greatly, under special charger, the 1.5C charging can make battery be full of in 40 minutes, and starting current can reach 2C, and lead-acid battery does not then have this performance.Four, high temperature resistant, LiFePO4 electric heating peak value can reach 350 ℃～500 ℃ and cobalt acid lithium and LiMn2O4 about 200 ℃.Five, big capacity.Six, memory-less effect.Seven, environmental protection.But the tap density of LiFeP04 positive electrode is less, waits the volume of the ferric phosphate lithium cell of capacity to be greater than lithium ion batteries such as boring sour lithium, and its ion and electronic conductivity are not good, cause the charge-discharge magnification performance not good.These have all greatly influenced LiFeP0
4Replace LiCoO
2Become anode material for lithium-ion batteries of new generation.
Mostly the preparation of present most of lithium iron phosphate positive materials is through solid phase method sintering preparation; Again it is carried out carbon and coat, with the electric conductivity of increase LiFePO4, and in fact; The LiFePO4 of solid phase method preparation promptly enables to reach smaller particle size; But carbon also can only be attached to micron-sized particle surface, and its inside still conductivity is relatively poor, thereby has determined that fundamentally its electric conductivity is relatively poor.
Summary of the invention
In order to solve above-mentioned existing problem, the purpose of this invention is to provide a kind of preparation method of nano-grade lithium iron phosphate anode sizing agent, take LiFePO 4 material through nanometerization, can improve the transfer rate of ion and electronics, thereby improve its electric conductivity.
The objective of the invention is to realize that through following technical proposals a kind of preparation method of nano-grade lithium iron phosphate anode sizing agent may further comprise the steps:
(1) takes by weighing following each raw material according to weight proportion: 8～9.5 parts of LiFePO4 active materials, 0.1～0.9 part of conductive agent, 0.2～1 part of binding agent, 10～40 parts of solvents;
(2) load weighted each raw material is carried out drying, the LiFePO4 active material is at 90～120 ℃, dry 1～3h; Binding agent is at 110～130 ℃, dry 1～3h; Conductive agent is at 180～200 ℃, dry 1～3h; Solvent N-methyl pyrrolidone uses dry molecular sieves to dewater;
(3) after each pretreatment of raw material is accomplished, preparation adhesive solution:, be heated to 40～45 ℃ and stir 1～2h with binding agent and solvent;
(4) mixing of active material: LiFePO 4 material and conductive agent are mixed mixing time 3～5h in ball grinder;
(5) last, binder solution and active material are mixed, stir 120～180min, process the slurry that viscosity is 5000～11000cP, cross 100～150 mesh sieves then, promptly get the nano-grade lithium iron phosphate anode sizing agent.
The present invention is through adopting nano lithium iron phosphate material; Material is through the primary particle nanometerization; The nano level particle that the method for offspring micronization obtains makes a micro particles be made up of many nanometer particles, and has the space to exist between the nano particle; Each nano particle is all coated by carbon like this, has increased electric conductivity greatly.
In addition, nano particle is carried out secondary granulation, make it reach micron order, improved tap density.Make the coating of pulp preparation and pole piece obtain handled easily.Therefore the slurry of processing further adds conductive agent, thereby has further improved the electric conductivity of material under the situation that existing carbon fully coats.
Lithium iron phosphate positive material of the present invention earlier with its raw material drying, is prepared the mixing of adhesive solution and active material through homogeneous phase method preparation respectively again, at last, binder solution and active material is mixed obtaining this lithium iron phosphate positive material.The inventive method can increase the electric conductivity of LiFePO4, and the LiFePO4 of homogeneous phase method preparation can reach smaller particle size, but carbon can be inner attached to micron-sized particle.Therefore, fundamentally solved the problem of original technology preparation lithium iron phosphate positive material poor electric conductivity.
Description of drawings
Fig. 1 is the charging and discharging curve of the 5C of the anode sizing agent packaged battery of preparation among the embodiment 1.
Fig. 2 is the charging and discharging curve of the 10C of the anode sizing agent packaged battery of preparation among the embodiment 1.
Embodiment
Below in conjunction with embodiment the present invention is explained further details, wherein the preparation method of red, green, blue look long-afterglow luminescent sizing agent is identical, only illustrates with the green long afterglow material.
Embodiment 1
(according to every part of 10g meter of mass fraction)
1) weight proportion by each material carries out weighing, LiFePO4 active material 80g, superconduction carbon black 1g, Kynoar 2g, N-methyl pyrrolidone 100g;
Wherein, the LiFePO4 active material is the nano ferric phosphate lithium anode material, and its tap density is greater than 1.4g/cm
3, D50 is at 10～30um.
2) load weighted each raw material is carried out drying, the LiFePO4 active material is at 90 ℃, dry 3h.Kynoar is at 110 ℃, dry 3h; The superconduction carbon black is at 180 ℃, dry 3h; Solvent N-methyl pyrrolidone uses dry molecular sieves to dewater;
3) after each pretreatment of raw material was accomplished, the preparation adhesive solution mixed Kynoar and N-methyl pyrrolidone, is heated to 40 ℃ and stirs 2h;
4) mixing of active material mixes LiFePO 4 material and superconduction carbon black mixing time 3h in ball grinder;
5) last, binder solution and active material are mixed, stir 2h, make the slurry that viscosity is 5000cP; Cross 100 mesh sieves then, obtain the nano-grade lithium iron phosphate anode sizing agent.
The present invention sees shown in Figure 1 through the charging and discharging curve effect of the 5C of the anode sizing agent packaged battery of the foregoing description 1 preparation.
The present invention sees shown in Figure 2 through the charging and discharging curve effect of the 10C of the anode sizing agent packaged battery of preparation in the foregoing description 1.
Embodiment 2
(according to every part of 10g meter of mass fraction)
1) weight proportion by each material carries out weighing, LiFePO4 active material 90g, and conductive black and superconduction carbon black be 5g (each 2.5g) altogether, Kynoar 5g, N-methyl pyrrolidone 250g;
2) load weighted each raw material is carried out drying, the LiFePO4 active material is at 120 ℃, dry 2h; Kynoar is at 115 ℃, dry 2h; Conductive black and superconduction carbon black be at 200 ℃, dry 2h; Solvent N-methyl pyrrolidone uses dry molecular sieves to dewater;
3) after each pretreatment of raw material was accomplished, the preparation adhesive solution mixed Kynoar and N-methyl pyrrolidone, is heated to 45 ℃ and stirs 1h;
4) mixing of active material mixes with the superconduction carbon black LiFePO 4 material and conductive black in ball grinder; Mixing time 4h;
5) last, binder solution and active material are mixed, stir 2h, make the slurry that viscosity is 9500cP; Cross 120 mesh sieves then, obtain the nano-grade lithium iron phosphate anode sizing agent.
Embodiment 3
(according to every part of 10g meter of mass fraction)
1) weight proportion by each material carries out weighing, LiFePO4 active material 95g, and graphite and acetylene black is 9g (each 4.5g) altogether, and polytetrafluoroethylene and Kynoar be 10g (each 5g) altogether, N-methyl pyrrolidone 400g;
2) load weighted each raw material is carried out drying, the LiFePO4 active material is at 110 ℃, dry 1h.Polytetrafluoroethylene and Kynoar be at 130 ℃, dry 1h; Graphite and acetylene black is at 200 ℃, dry 1h; Solvent N-methyl pyrrolidone uses dry molecular sieves to dewater;
3) after each pretreatment of raw material was accomplished, the preparation adhesive solution with polytetrafluoroethylene and Kynoar and the mixing of N-methyl pyrrolidone, was heated to 45 ℃ and stirs 1h;
4) mixing of active material mixes LiFePO 4 material and graphite and acetylene black in ball grinder; Mixing time 5h;
5) last, binder solution and active material are mixed, stir 2h, make the slurry that viscosity is 11000cP; Cross 150 mesh sieves then, obtain the nano-grade lithium iron phosphate anode sizing agent.
Claims (4)
1. the preparation method of a nano-grade lithium iron phosphate anode sizing agent, it is characterized in that: this method may further comprise the steps:
1) takes by weighing following each raw material according to weight proportion: 8～9.5 parts of LiFePO4 active materials, 0.1～0.9 part of conductive agent, 0.2～1 part of binding agent, 10～40 parts of solvents;
2) load weighted each raw material is carried out drying: the LiFePO4 active material is at 90～120 ℃, dry 1～3h; Binding agent is at 110～130 ℃, dry 1～3h; Conductive agent is at 180～200 ℃, dry 1～3h; Solvent uses dry molecular sieves to dewater;
3) will be through step 2) dried raw material preparation binder solution: with binding agent and solvent, be heated to 40～45 ℃ and stir 1～2h;
4) will be through step 2) dried raw material carries out active material and mixes: LiFePO4 active material and conductive agent are mixed mixing time 3～5h in ball grinder;
5) binder solution and active material are mixed, stir 2h, process the slurry that viscosity is 5000～11000cP; Cross 100～150 mesh sieves then, promptly get the nano-grade lithium iron phosphate anode sizing agent;
Said solvent is the N-methyl pyrrolidone.
2. the preparation method of a kind of nano-grade lithium iron phosphate anode sizing agent according to claim 1 is characterized in that: said LiFePO4 active material is the nano ferric phosphate lithium anode material, and its tap density is greater than 1.4g/cm
3, D50 is at 10～30um.
3. the preparation method of a kind of nano-grade lithium iron phosphate anode sizing agent according to claim 1 is characterized in that: said conductive agent is one or more in acetylene black, graphite, conductive black, the superconduction carbon black.
4. the preparation method of a kind of nano-grade lithium iron phosphate anode sizing agent according to claim 1 is characterized in that, said binding agent is one or both of Kynoar, polytetrafluoroethylene.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103400964A (en) * | 2013-07-23 | 2013-11-20 | 深圳市百纳新能源科技有限公司 | Preparation method of lithium iron phosphate electrode |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102368544B (en) * | 2011-10-28 | 2012-10-24 | 奇瑞汽车股份有限公司 | Preparation method of lithium ion battery anode slurry |
| CN102637905B (en) * | 2012-05-03 | 2015-07-08 | 江西省福斯特新能源有限公司 | Lithium battery manufacturing method |
| CN102709557B (en) * | 2012-06-05 | 2015-03-25 | 无锡合志科技有限公司 | Preparation method for anode paste of lithium iron phosphate battery |
| CN103035924B (en) * | 2012-12-31 | 2015-07-22 | 山东海特电子新材料有限公司 | Anode slurry of high-rate lithium ion battery and fabrication method of anode slurry |
| CN109346677A (en) * | 2018-10-31 | 2019-02-15 | 成都市银隆新能源有限公司 | A kind of preparation method and lithium battery of lithium battery anode slurry |
| CN109950505B (en) * | 2019-04-02 | 2022-06-28 | 上海玖银电子科技有限公司 | Lithium titanate battery slurry and preparation method thereof |
| CN115172674A (en) * | 2022-08-29 | 2022-10-11 | 吉林大学 | Lithium iron phosphate anode, preparation method and battery comprising same |
| CN117117292A (en) * | 2023-08-08 | 2023-11-24 | 湖南恒优能科技有限公司 | Low-resistance Wen Tieli battery device structure and manufacturing method thereof |
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| CN1734825A (en) * | 2005-08-08 | 2006-02-15 | 河南环宇集团有限公司 | Preparation method for high rate phosphate lithium ion battery and battery prepared thereby |
| CN101232091A (en) * | 2007-01-24 | 2008-07-30 | 比亚迪股份有限公司 | Method for preparation of lithium ion battery anode glue size and battery |
| CN101692064A (en) * | 2009-09-30 | 2010-04-07 | 彩虹集团电子股份有限公司 | LiFePO4 positive plate for testing and preparation method thereof |
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| JP4829557B2 (en) * | 2005-07-21 | 2011-12-07 | Ａｇｃセイミケミカル株式会社 | Method for producing lithium iron composite oxide |
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| CN1734825A (en) * | 2005-08-08 | 2006-02-15 | 河南环宇集团有限公司 | Preparation method for high rate phosphate lithium ion battery and battery prepared thereby |
| CN101232091A (en) * | 2007-01-24 | 2008-07-30 | 比亚迪股份有限公司 | Method for preparation of lithium ion battery anode glue size and battery |
| CN101692064A (en) * | 2009-09-30 | 2010-04-07 | 彩虹集团电子股份有限公司 | LiFePO4 positive plate for testing and preparation method thereof |
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| JP特开2007-22894A 2007.02.01 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103400964A (en) * | 2013-07-23 | 2013-11-20 | 深圳市百纳新能源科技有限公司 | Preparation method of lithium iron phosphate electrode |
| CN103400964B (en) * | 2013-07-23 | 2015-08-19 | 深圳市百纳新能源科技有限公司 | A kind of preparation method of iron phosphate lithium electrode |
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