CN102185140A - Preparation method of nano-network conductive polymer coated lithium iron phosphate anode material - Google Patents
Preparation method of nano-network conductive polymer coated lithium iron phosphate anode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a nano-network conductive polymer coated lithium iron phosphate anode material. The preparation method is characterized in that: a surfactant is used as a template; and a conductive polymer monomer is subjected to in-situ polymerization on a lithium iron phosphate surface in a low-temperature acid solution medium and a nano-network structure is grown; and thus, the nano-network conductive polymer coated lithium iron phosphate anode material is formed. The special shape of the nano-network conductive polymer is favorable for a current carrier to be conducted among polymer aggregate particles; and the nano-network conductive polymer has high current carrier mobility ratio, and can effectively connect surfaces among lithium iron phosphate particles when coated on the lithium iron phosphate surface to form an effective conductive network, so the lithium iron phosphate conductivity is significantly improved, and the contact resistance and electrode polarization among the particles are reduced to ensure that the electrochemical performance of an electrode material is greatly improved. The preparation method has a simple process and readily-available raw materials, and is suitable for carrying out industrial large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode, belong to lithium ion battery material and preparing technical field thereof.
Background technology
Along with the progressively exhausted and biological environment of petrochemical industry resource goes from bad to worse, to save and high effect cleaning uses the energy more and more to come into one's own, lithium rechargeable battery is also so become the focus of people's concern.In lithium ion battery, positive electrode is the key factor of decision its chemical property, security performance and future thrust.LiFePO4 (LiFePO
4) as the anode material for lithium-ion batteries of new generation of tool development and application potentiality because of having abundant raw material, cheap, concern that advantages such as specific capacity is higher, working voltage platform is high, Stability Analysis of Structures, non-environmental-pollution are subjected to all circles especially.Strong covalent bond effect in the LiFePO4 makes it can keep the highly stable of crystal structure in charge and discharge process, therefore have than higher security performance of other positive electrodes such as cobalt acid lithium, LiMn2O4 and longer cycle life, make it great market prospects be arranged in the required large-sized power field of power supplies of various removable field of power supplies, particularly electric motor car.But LiFePO4 is as a kind of semiconducting compound, and the principal element that hinders its development at present is that conductivity is lower, is difficult near its theoretical capacity.
Conducting polymer has also had the semiconductor that brings because of doping or the characteristic of conductor concurrently except having the macromolecule self character.Conducting polymer has expanded to typical range of metal with the conductivity of oneself, and this is determined by its internal structure.A large amount of achievements in research shows that unique mechanism of doping effect and architectural feature make conducting polymer possess superior conduction and chemical property.That conducting polymer has is easily synthetic, conductivity is high, good stability, environment avirulence and reversible advantages such as redox characteristic, the reaction that particularly can take off lithium/embedding lithium under certain potentials.Be widely used in the research of lithium ion battery electrode material at conducting polymer in recent years, as a kind of conducting high polymers thing, it not only can improve the conductivity of inorganic material, but also can play a part conductive agent and binding agent.In addition, conducting polymer has pliable and tough mechanical performance and machinability and electrochemical redox activity, and these characteristics have determined this material to play a significant role in jacketed electrode.
In recent years, people begin to attempt conducting polymer is coated on the positive electrodes such as LiFePO4, LiMn2O4, vanadic oxide, carbon, silicon, because the coordinative role between organic substance and the inorganic matter, the material after the coating has certain raising at chemical property.(electrochemistry, Electrochemistry, 2008 such as Wang Wei; 14 volumes; May, the 2nd phase) under the argon shield condition, use the ball milling mixing method to prepare the Polyaniline Doped composite ferric lithium phosphate material, Polyaniline Doped has some improvement to electrochemical performances of lithium iron phosphate.(Chem.mater.2008 such as Goodenough, 20:7237-7241) utilize chemical polymerization that polypyrrole, polyaniline are coated on the carbon-coated LiFePO 4 for lithium ion batteries, the result shows that the electrode that is coated with conducting polymer shows best chemical property, on capacity and high rate performance, be better than far away not coat before.This is main because LiFePO4 is not good electric conductor, and conducting polymer has good electrical conductance, can reduce the contact resistance between the LiFePO4 particle.The conducting polymer pattern is graininess in the above conducting polymer coated lithium iron phosphate composite, the special pattern of nanometer network conducting polymer more helps the conduction of charge carrier between polymer poly collective particle, have higher carrier mobility, thereby have better conductivity than conductive polymer particles.In the prior art, the technology that yet there are no with nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode discloses or is used.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode, this invented technology is simple, raw material is easy to get, and preparation process is pollution-free.
The preparation method of a kind of nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode that the present invention proposes may further comprise the steps:
1, surfactant is joined is stirred to fully dissolving in 100ml 0.1～1mol/L inorganic proton acid solution, surfactant concentration is 0.1～0.5mol/L, iron phosphate powder is scattered in this solution then, and ultrasonic agitation 30～60min makes LiFePO4 fully mix with surfactant, wherein the mass ratio of LiFePO4 and surfactant is 1: 0.5～3, under the ultrasonic agitation condition, add the conducting polymer monomer, the mol ratio of conducting polymer monomer and surfactant is 1: 0.5～2, continue ultrasonic agitation 30～60min, obtain mixed liquor A;
2, mixed liquor A is cooled at-5～10 ℃; the oxidizing agent solution B that will be dissolved in the inorganic proton acid of 100ml 0.1～1mol/L under the inert gas shielding condition dropwise adds in the mixed liquor A; at-5～10 ℃ of stirring reaction 5～24h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 40～80 ℃ of vacuumize 20～48h, promptly get nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode.
Described conducting polymer is the copolymer of one or more mixtures or one or more monomers in polyaniline, polypyrrole, polythiophene, the polyoxyethylene.
Described surfactant is one or more the mixture in softex kw, hexadecyltrimethylammonium chloride, lauryl sodium sulfate, the neopelex.
The mol ratio of described conducting polymer monomer and oxidant is 1: 1～1: 3.
Described inorganic proton acid is sulfuric acid, nitric acid, hydrochloric acid, one or more mixture in phosphoric acid, perchloric acid, the acetic acid.
Described oxidant is one or more a mixture in ammonium persulfate, iron chloride, potassium permanganate, potassium bichromate, the hydrogen peroxide.
Described inert gas is the mixture of one or more gases in high-purity nitrogen, argon gas, helium, neon, krypton gas, xenon, the radon gas.
Advantage of the present invention and good effect are: the conducting polymer that (1) nanometer network conducting polymer is coated on the LiFePO4 surface can connect the surface between the LiFePO4 particle effectively, form effective conductive network, improve the LiFePO4 conductivity significantly, and reduced contact resistance and electrode polarization between the particle, thereby the high rate performance of material is improved widely; (2) cycle performance of conducting polymer self excellence and embedding lithium function, and the nanometer network conducting polymer that is coated on the LiFePO4 particle surface can prevent that LiFePO4 from directly contacting with electrolyte, reduce the generation of side reaction, suppressed the corrosion of material, restricted the generation of SEI film, the conductive polymer nanometer network configuration has improved the suppleness of electrode slice, and electrode slice is kept perfectly in cyclic process; (3) the nanometer network conducting polymer has bigger specific area at nanoscale, therefore can adsorb be suppressed at generate in the discharge process product in electrolyte dissolving and to the migration of negative pole, reduce self discharge.
Embodiment
The preparation method of nano-metal-oxide provided by the invention/Graphene doped iron lithium phosphate electrode material is as described in the summary of the invention part.The present invention will further illustrate substantive distinguishing features of the present invention and marked improvement by the description of following embodiment.
Embodiment 1
1, the 3.64g softex kw is joined is stirred to fully dissolving in the 100ml 0.1mol/L sulfuric acid solution.Then the 7.29g iron phosphate powder is scattered in this solution, and ultrasonic agitation 30min makes LiFePO4 fully mix with softex kw.Under the ultrasonic agitation condition, add the 1.8ml aniline monomer, continue ultrasonic agitation 60min, obtain mixed liquor A;
2, mixed liquor A is cooled to-5 ℃; 6.49g iron chloride is dissolved in the sulfuric acid of 100ml 0.1mol/L and forms solution B; under the nitrogen protection condition, dropwise add B in the mixed liquor A; at-5 ℃ of stirring reaction 5h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 40 ℃ of vacuumize 20h, promptly get nanometer network polyaniline coated LiFePO 4 for lithium ion batteries positive electrode.
Embodiment 2
1, the 7.29g softex kw is joined is stirred to fully dissolving in the 100ml 0.2mol/L hydrochloric acid solution.Then the 7.29g iron phosphate powder is scattered in this solution, and ultrasonic agitation 60min makes LiFePO4 fully mix with softex kw.Under the ultrasonic agitation condition, add the 0.69ml pyrrole monomer, continue ultrasonic agitation 30min, obtain mixed liquor A;
2, mixed liquor A is cooled to-2 ℃; 4.74g potassium permanganate is dissolved in the hydrochloric acid of 100ml 0.2mol/L and forms solution B; under the argon shield condition, dropwise add B in the mixed liquor A; at-2 ℃ of stirring reaction 15h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 60 ℃ of vacuumize 24h, promptly get nanometer network polypyrrole coated LiFePO 4 for lithium ion batteries positive electrode.
Embodiment 3
1, the 6.4g hexadecyltrimethylammonium chloride is joined is stirred to fully dissolving in the 100ml 0.2mol/L hydrochloric acid solution.Then the 3.2g iron phosphate powder is scattered in this solution, and ultrasonic agitation 60min makes LiFePO4 fully mix with hexadecyltrimethylammonium chloride.Under the ultrasonic agitation condition, add the 1.38ml pyrrole monomer, continue ultrasonic agitation 60min, obtain mixed liquor A;
2, mixed liquor A is cooled to 0 ℃; the 4.56g ammonium persulfate is dissolved in the hydrochloric acid of 100ml 0.2mol/L and forms solution B; under the nitrogen protection condition, dropwise add B in the mixed liquor A; at 0 ℃ of stirring reaction 24h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 60 ℃ of vacuumize 48h, promptly get nanometer network polypyrrole coated LiFePO 4 for lithium ion batteries positive electrode.
Embodiment 4
1, the 16g hexadecyltrimethylammonium chloride is joined is stirred to fully dissolving in the 100ml 1mol/L hydrochloric acid solution.Then the 5.3g iron phosphate powder is scattered in this solution, and ultrasonic agitation 60min makes LiFePO4 fully mix with hexadecyltrimethylammonium chloride.Under the ultrasonic agitation condition, add the 2ml thiophene monomer, continue ultrasonic agitation 60min, obtain mixed liquor A;
2, mixed liquor A is cooled to 10 ℃; the 4.71g ammonium persulfate is dissolved in the hydrochloric acid of 100ml 1mol/L and forms solution B; under the argon shield condition, dropwise add B in the mixed liquor A; at 10 ℃ of stirring reaction 20h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 80 ℃ of vacuumize 48h, promptly get nanometer network polythiophene coated LiFePO 4 for lithium ion batteries positive electrode.
Embodiment 5
1, the 5.77g lauryl sodium sulfate is joined is stirred to fully dissolving in the 100ml 0.1mol/L sulfuric acid solution.Then the 8.65g iron phosphate powder is scattered in this solution, and ultrasonic agitation 60min makes LiFePO4 fully mix with softex kw.Under the ultrasonic agitation condition, add the 3.6ml aniline monomer, continue ultrasonic agitation 60min, obtain mixed liquor A;
2, mixed liquor A is cooled to-2 ℃; the 9.13g ammonium persulfate is dissolved in the sulfuric acid of 100ml 0.1mol/L and forms solution B; under the nitrogen protection condition, dropwise add B in the mixed liquor A; at-2 ℃ of stirring reaction 20h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 60 ℃ of vacuumize 24h, promptly get nanometer network polyaniline coated LiFePO 4 for lithium ion batteries positive electrode.
Claims (7)
1. the preparation method of a nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode is characterized in that may further comprise the steps:
(1) surfactant is joined is stirred to fully dissolving in 100ml 0.1～1mol/L inorganic proton acid solution, surfactant concentration is 0.1～0.5mol/L, iron phosphate powder is scattered in this solution then, and ultrasonic agitation 30～60min makes LiFePO4 fully mix with surfactant, wherein the mass ratio of LiFePO4 and surfactant is 1: 0.5～3, under the ultrasonic agitation condition, add the conducting polymer monomer, the mol ratio of conducting polymer monomer and surfactant is 1: 0.5～2, continue ultrasonic agitation 30～60min, obtain mixed liquor A;
(2) mixed liquor A is cooled at-5～10 ℃; the oxidizing agent solution B that will be dissolved in the inorganic proton acid of 100ml 0.1～1mol/L under the inert gas shielding condition dropwise adds in the mixed liquor A; at-5～10 ℃ of stirring reaction 5～24h; product alternately washs to filtrate colourless with deionized water, ethanol successively; at 40～80 ℃ of vacuumize 20～48h, promptly get nanometer network conducting polymer coated LiFePO 4 for lithium ion batteries positive electrode.
2. method according to claim 1 is characterized in that: the described conducting polymer of step (1) is one or more mixture or the copolymer of one or more monomers in polyaniline, polypyrrole, polythiophene, the polyoxyethylene.。
3. method according to claim 1 is characterized in that: the described surfactant of step (1) is one or more the mixture in softex kw, hexadecyltrimethylammonium chloride, lauryl sodium sulfate, the neopelex.
4. method according to claim 1 is characterized in that: the mol ratio of described conducting polymer monomer and oxidant is 1: 1～1: 3.
5. method according to claim 1 is characterized in that: described inorganic proton acid is sulfuric acid, nitric acid, hydrochloric acid, one or more mixture in phosphoric acid, perchloric acid, the acetic acid.
6. method according to claim 1 is characterized in that: the described oxidant of step (2) is one or more a mixture in ammonium persulfate, iron chloride, potassium permanganate, potassium bichromate, the hydrogen peroxide.
7. method according to claim 1 is characterized in that: the described inert gas of step (2) is the mixture of one or more gases in high-purity nitrogen, argon gas, helium, neon, krypton gas, xenon, the radon gas.
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| CN102593444A (en) * | 2012-01-17 | 2012-07-18 | 东莞市迈科科技有限公司 | Preparation method of carbon-coated lithium titanate and product of carbon-coated lithium titanate |
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| CN108666548A (en) * | 2018-04-24 | 2018-10-16 | 中山大学 | A kind of preparation method of conductive polymer polymer poly 1,3- diacetylene-benzene coated LiFePO 4 for lithium ion batteries |
| CN110854363A (en) * | 2019-10-21 | 2020-02-28 | 珠海冠宇电池有限公司 | Modified electrode material, preparation method thereof and lithium ion battery |
| CN112290023A (en) * | 2020-10-21 | 2021-01-29 | 安徽清泉新能源科技集团有限责任公司 | Polypyrrole-doped power battery material and preparation method thereof |
| CN112582579A (en) * | 2020-12-07 | 2021-03-30 | 宁德新能源科技有限公司 | Positive electrode, electrochemical device, and electronic device |
| CN112563472A (en) * | 2020-12-16 | 2021-03-26 | 远景动力技术(江苏)有限公司 | Polymer composite lithium iron phosphate anode material and preparation method thereof |
| CN113571692A (en) * | 2021-07-21 | 2021-10-29 | 合肥国轩高科动力能源有限公司 | High-safety conductive material modified high-nickel positive electrode material and preparation method thereof |
| CN113571692B (en) * | 2021-07-21 | 2022-07-12 | 合肥国轩高科动力能源有限公司 | High-safety conductive material modified high-nickel positive electrode material and preparation method thereof |
| CN114447308A (en) * | 2022-02-10 | 2022-05-06 | 湖北亿纬动力有限公司 | Composite positive electrode material, preparation method thereof and electrochemical energy storage device |
| CN114447308B (en) * | 2022-02-10 | 2024-03-15 | 湖北亿纬动力有限公司 | Composite positive electrode material, preparation method thereof and electrochemical energy storage device |
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