CN101591012A - A kind of preparation method who is used for lithium ion battery anode material lithium iron phosphate - Google Patents
A kind of preparation method who is used for lithium ion battery anode material lithium iron phosphate Download PDFInfo
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- CN101591012A CN101591012A CNA2008101130350A CN200810113035A CN101591012A CN 101591012 A CN101591012 A CN 101591012A CN A2008101130350 A CNA2008101130350 A CN A2008101130350A CN 200810113035 A CN200810113035 A CN 200810113035A CN 101591012 A CN101591012 A CN 101591012A
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Abstract
The present invention relates to a kind of anode material for lithium ion battery method preparing phosphate iron lithium.With the compound of the compound of metal iron powder, lithium, phosphorus according to atomic ratio Li: Fe: P=(0.95～1.1): prepare burden at 1: 1, the presoma that adds carbon or carbon again, uniform mixing is 1～20 hour in medium, dry then, granulation, in inert atmosphere, handled 1～20 hour under 300 ℃～500 ℃ conditions again, be then to synthesize 5～36 hours under 600 ℃～850 ℃ conditions, obtain lithium iron phosphate positive material.The present invention uses cheap metal iron powder to be starting material, adds carbon or carbon matrix precursor, carries out the method for mechanical pelleting, effectively improved the tap density of iron lithium phosphate, improved its conductivity, prepared positive electrode material, characteristic such as specific storage height, cycle performance are good, good rate capability.The method preparation technology that the present invention prepares iron lithium phosphate is simple, and is workable, easy realization of large-scale production.
Description
Technical field
The present invention relates to a kind of lithium ion battery anode material lithium iron phosphate (LiFePO that is used for
4) the preparation method, belong to the anode material for lithium-ion batteries preparing technical field.
Background technology
Since nineteen ninety Sony corporation of Japan exploitation lithium ion battery, the research and development of positive electrode material just are subjected to people's attention.The positive electrode material of answering the commercialization lithium ion battery to use at present is mainly the embedding lithium transition-metal oxide, comprises that cobalt acid lithium, lithium nickelate, lithium manganate etc. are.Wherein, the most widely used cobalt acid lithium material because of its scarcity of resources, cost an arm and a leg, shortcoming such as poor safety performance developed its application in high capacity cell.Aboundresources, the widespread use that the lithium manganate material capacity that the prices of raw and semifnished materials are cheap is lower, the high temperature cyclic performance difference has limited this kind material.Lithium nickelate does not still obtain widespread use because of its preparation difficulty, poor heat stability and safety performance etc.Compare with the anode material for lithium-ion batteries (cobalt acid lithium, lithium manganate, nickle cobalt lithium manganate ternary system etc.) of present practicality, iron lithium phosphate is a kind of compound of olivine structural, cheap, environmental friendliness, specific storage height, cycle performance and advantages such as thermostability is fabulous, security height are enriched in the source, be considered to the most potential s-generation anode material for lithium-ion batteries, has vast potential for future development at the accumulation energy type lithium-ions battery, the particularly fast-developing lithium ion powered battery preferred system of positive electrode material.
Method preparing phosphate iron lithium mainly contains high temperature solid phase synthesis and low temperature liquid phase synthesis method.In the high temperature solid phase synthesis there be typical method, ferrous iron organic compound with costliness is the high temperature synthetic method of presoma, even ferrous iron also can be oxidized in this method because under inert atmosphere protection, synthetic product purity is not high, and tap density is lower; With the ferric iron is the carbothermic method of presoma, and generated time is long, and energy consumption is higher.Low temperature liquid phase synthesis method advantage is that the raw material mixing can reach the molecular level level, but the product crystallization degree is not high, and there are the mixing phenomenon in Fe and Li, still need at high temperature to handle, and make complicated process of preparationization, are not suitable for large-scale production.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of lithium ion battery anode material lithium iron phosphate, this method preparation technology is simple, preparation cost is low, be easy in industrial enforcement, prepared product purity height, chemical property is good.
To achieve these goals, the present invention takes following technical scheme.
A kind of preparation method who is used for lithium ion battery anode material lithium iron phosphate may further comprise the steps:
With the compound of the compound of metal iron powder, phosphorus, lithium according to atomic ratio Li: Fe: P=(0.95-1.1): prepare burden at 1: 1, add the presoma of carbon or carbon again, uniform mixing is 1～20 hour in medium, and is dry then.Dried mixture adds the granulation of granulating agent mechanically mixing; mixture after the granulation is placed in the high temperature shaft furnace; under 1～30 liter/minute protection of inert gas; under 300 ℃～500 ℃ conditions, to handle 1～20 hour under 1～15 ℃/minute the temperature rise rate; continue then to heat up and after under 600 ℃～850 ℃ conditions synthetic 5～36 hours, reduce to room temperature, make lithium ion battery olivine structure lithium iron phosphate positive electrode material.
The compound of said phosphorus is one or more mixtures in monometallic, Lin acid Qing Er , Lin Suan Er Qing , Trilithium phosphate, the tertiary iron phosphate.
The compound of said lithium is one or more mixtures in lithium hydroxide, Quilonum Retard, monometallic, Trilithium phosphate, the Lithium Acetate.
Said carbon is graphite, acetylene black, and carbon matrix precursor is one or more in polyethylene, polyoxyethylene glycol, polyvinyl alcohol and the sugar, and add-on accounts for 1～30wt% of gross weight.Gross weight described here is the gross weight of raw material, i.e. the gross weight of the compound of the compound of iron powder, lithium, phosphorus and carbon or carbon matrix precursor.
Said carbon matrix precursor is the organic or macromolecular compound that can be decomposed into carbon class material through pyrolysis.
Said medium is that water, ethanol, acetone, propyl carbinol, n-propyl alcohol, Virahol, second are fine, one or more mixtures in the thanomin.
Said granulating agent is one or more the mixture in polyvinyl alcohol, polyacrylamide, Viscotrol C, the water, and add-on is with respect to 1～10wt% of raw material gross weight.Here said raw material gross weight, the i.e. gross weight of the compound of the compound of iron powder, lithium, phosphorus and carbon or carbon matrix precursor.
Said drying temperature is 50 ℃～200 ℃.The exsiccant time is as the criterion so that liquid medium is vapored away.
It is raw material that the present invention adopts iron powder, adds the presoma of carbon or carbon in starting material, and mechanical pelleting has reduced synthesis temperature, has accelerated heat transfer, mass transfer process.In reaction process, the reaction that exists for of carbon provides good reducing atmosphere, has obtained purity height, the good iron lithium phosphate product of chemical property; The LiFePO that adopts the bigger metal iron powder of density to make
4The material tap density is higher (by 1.1g/cm
3Bring up to 1.3g/cm
3More than), the specific storage height; Moreover, become nucleation centre with metal iron powder, can obtain the metal iron powder of controllable granularity and narrow particle size distribution by the meticulous control of wet processing, utilize the inheritance of pyroreaction, be convenient to from the granularity and the size-grade distribution of raw material control finished product; Starting material wide material sources used in the present invention, be easy to get, pollution-free, cost is low; Processing method technology is simple, workable, easy realization of large-scale production, the prepared iron lithium phosphate of the present invention shows excellent chemical property as lithium ion cell positive, the anode material for lithium-ion batteries of preparing is widely used in fields such as electronics, electromobile, has broad application prospects.
Description of drawings
Fig. 1 is the sem photograph by the LiFePO 4 material of embodiment 1 preparation.
Fig. 2 is the crystallogram by the LiFePO 4 material of embodiment 1 preparation.
Fig. 3 is that voltage range is 2.2V～4.25V by the first charge-discharge graphic representation of the LiFePO 4 material test cell of embodiment 1 preparation, and electrolytic solution is 1M (mol/L) LiPF
6/ EC+DMC (1: 1), charge-discharge magnification are 0.1C.
Fig. 4 is that voltage range is 2.2V～4.25V by the cycle performance figure of the prepared lithium ion battery of embodiment 1, and electrolytic solution is 1M (mol/L) LiPF
6/ EC+DMC (1: 1), charge-discharge magnification are 0.1C.
Fig. 5 is assembled into charging and discharging curve under the charge-discharge magnifications different behind the 10Ah high-power lithium ion power cell by embodiment 1 prepared lithium ion battery material, discharge-rate is respectively 1C, 6C, 10C, 20C, voltage range 2.2V～4.25V, electrolytic solution are 1M (mol/L) LiPF
6/ EC+DMC (1: 1).
Embodiment
The gross weight of said raw material is meant the compound of iron powder, lithium, the compound of phosphorus and the gross weight of carbon or carbon matrix precursor in the following embodiments.For example, " with 0.5 mole iron powder; 0.5 mole Lin Suan Er Qing , 0.55 mole lithium hydroxide, the glucose that accounts for raw material gross weight 5% mix "; The weight of glucose wherein be iron powder; Lin Suan Er Qing , lithium hydroxide and glucose the raw material gross weight 5%.
With 0.5 mole iron powder, 0.5 mole monometallic, the sucrose that accounts for raw material gross weight 8% mixes and put into the rod milling jar, with ethanol is medium, thorough mixing is 5 hours on rod mill, dry down at 80 ℃, the polyvinyl alcohol solution mechanical stirring granulation of dried mixture with respect to raw material gross weight 5wt%, mixture after the granulation is put into shaft furnace, under 5 liters/minute argon gas atmosphere, being warming up to 300 ℃ with 6 ℃/minute speed handled 10 hours, 700 ℃ of following Synthetic 2s 0 hour, reduce to room temperature then and obtain iron lithium phosphate then.Record the tap density 1.43g/cm of synthetic materials
3Fig. 1 is synthetic product LiFePO
4Stereoscan photograph, as can be seen from Figure, the granularity of synthetic product is substantially less than 2 microns.Fig. 2 is synthetic product LiFePO
4XRD figure, XRD analysis result shows, prepared product LiFePO
4Powder has single olivine-type crystalline structure, does not observe impurity peaks, the product purity height.
Make electrode with 1 synthetic positive electrode material of embodiment according to following method:
Take by weighing prepared iron lithium phosphate respectively with 83: 10: 7 mass ratioes: binding agent PVDF (polyvinylidene difluoride (PVDF)): acetylene black is coated on the two sides of aluminium foil after mixing the furnishing pulpous state, at air drying, makes electrode.Counter electrode is formed test cell for the lithium tinsel.Electrolytic solution is 1M (mol/L) LiPF
6/ EC+DMC etc., EC are NSC 11801, and DMC is a methylcarbonate.Charging and discharging currents density 0.1C, discharging and recharging upper and lower limit voltage is 2.2～4.25V.The continuous current tester that computerizeds control carries out electrochemistry capacitance and loop test.Fig. 3 presses the first charge-discharge curve of 0.1C multiplying power at the battery of 2.2～4.25V voltage range for respective battery, and as seen from the figure, institute's synthetic product has the favorable charge-discharge voltage platform about 3.4V, and reversible specific capacity is 157mAh/g.Fig. 4 is the cycle performance of battery under the 0.1C multiplying power, and as seen from the figure, institute's synthetic material has good cycle performance, and through 25 circulations, capacity attenuation is very little.Fig. 5 is assembled into discharge curve under the charge-discharge magnifications different behind the 10Ah high-power lithium ion power cell for institute's synthetic material, and as seen from the figure, capacity attenuation is not clearly when 1C, 6C, 10C, illustrates that the heavy-current discharge performance of synthetic materials is better.
Embodiment 2
Iron powder with 0.5 mole, 0.5 the Lin Suan Er Qing of mole, 0.55 mole lithium hydroxide, the glucose that accounts for raw material gross weight 5% mix and put into the rod milling jar, with water is medium, thorough mixing is 12 hours on rod mill, 120 ℃ of of of of of of dry down at, the polyacrylamide solution mechanical stirring granulation of dried mixture with respect to raw material gross weight 10wt%, put into shaft furnace after the granulation, under 10 liters/minute argon gas atmosphere, 350 ℃ of of of of 10 ℃/minute of of of of of of with of of of being warming up to speed handled, 20 hours, 700 ℃ of of of of of of of following Synthetic 2s 4 hours, reduce to room temperature and obtain iron lithium phosphate then.The tap density that records iron lithium phosphate is 1.38g/cm3, equally the method according to embodiment 1 is prepared into electrode slice, is assembled into behind the battery with the rate charge-discharge of 0.1C, and the mensuration reversible capacity is 153mAh/g.
Embodiment 3
Iron powder with 0.5 mole, 0.26 the Quilonum Retard of mole, 0.5 the Lin of mole acid Qing Er , account for the polyethylene mixing of raw material gross weight 20% and put into the rod milling jar, with ethanol is medium, thorough mixing is 5 hours on rod mill, 80 ℃ of of of of of of dry down at, the Viscotrol C solution mechanical stirring granulation of dried mixture with respect to raw material gross weight 3wt%, after the granulation this miscellany is put into shaft furnace, under 10 liters/minute argon gas atmosphere, 400 ℃ of of of of 10 ℃/minute of of of of of of with of of of being warming up to speed handled, 15 hours, 750 ℃ of of of of of of of following Synthetic 2s 4 hours, reduce to room temperature then and obtain iron lithium phosphate then.The tap density that records iron lithium phosphate is 1.41g/cm3, prepare electrode slice by the method for embodiment 1, be assembled into behind the test cell with the rate charge-discharge of 0.1C, reversible capacity is 155mAh/g.
Embodiment 4
Iron powder with 0.5 mole, 0.5 the monometallic of mole, the acetylene black that accounts for raw material gross weight 10% are mixed and are put into the rod milling jar, with ethanol is medium, thorough mixing is 8 hours on rod mill, dry down at 80 ℃, the polyvinyl alcohol solution mechanical stirring granulation of dried mixture with respect to raw material gross weight 8wt%, after the granulation this miscellany is put into shaft furnace, under 8 liters/minute nitrogen atmosphere, being warming up to 350 ℃ with 12 ℃/minute speed handled 10 hours, 800 ℃ of following Synthetic 2s 0 hour, reduce to room temperature then and obtain iron lithium phosphate then.The tap density that records iron lithium phosphate is 1.36g/cm
3, prepare electrode slice by the method for embodiment 1, be assembled into behind the test cell with the rate charge-discharge of 0.1C, reversible capacity is 151mAh/g.
Claims (8)
1, a kind of preparation method who is used for lithium ion battery anode material lithium iron phosphate is characterized in that:
1) with the compound of the compound of metal iron powder, lithium, phosphorus according to atomic ratio Li: Fe: P=(0.95～1.1): prepare burden at 1: 1, add the precursor of carbon or carbon again, uniform mixing is 1～20 hour in medium, and is dry then;
2) dried miscellany adds granulating agent, mechanical stirring granulation;
3) mixture after the above-mentioned granulation is put in the shaft furnace; flow velocity be the 1-30 liter/minute protection of inert gas under heat-treat; temperature rise rate is 1～15 ℃/minute; be warming up under 300 ℃～500 ℃ conditions thermal treatment 1～20 hour; continue then to be warming up under 600 ℃～850 ℃ conditions and synthesized 5～36 hours; reduce to room temperature then, obtain lithium iron phosphate positive material.
2, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1 is characterized in that: the compound of described lithium is one or more mixtures in lithium hydroxide, Quilonum Retard, Trilithium phosphate, the monometallic.
3, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1 is characterized in that:the compound of described phosphorus is one or more mixtures in monometallic, Lin acid Qing Er , Lin Suan Er Qing , Trilithium phosphate, the tertiary iron phosphate.
4, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1, it is characterized in that: described carbon is graphite, acetylene black, carbon matrix precursor is one or more in polyethylene, polyoxyethylene glycol, polyvinyl alcohol and the sugar, and add-on accounts for 1～30wt% of gross weight.
5, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1 is characterized in that: described medium is that water, ethanol, acetone, propyl carbinol, n-propyl alcohol, Virahol, second are fine, one or more mixtures in the thanomin.
6, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1 is characterized in that: described granulating agent is polyvinyl alcohol, polyacrylamide, Viscotrol C, one or more of water, and add-on accounts for 1～10wt% of gross weight.
7, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1 is characterized in that: described drying temperature is 50 ℃～200 ℃.
8, the preparation method who is used for lithium ion battery anode material lithium iron phosphate according to claim 1 is characterized in that: described shielding gas is a kind of of high pure nitrogen, high-purity argon gas, or its mixed gas.
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| CN103137968A (en) * | 2011-11-30 | 2013-06-05 | 北京有色金属研究总院 | Positive electrode composite material for lithium ion batteries and preparation method thereof |
| CN103151521A (en) * | 2013-02-22 | 2013-06-12 | 中国科学院过程工程研究所 | Positive electrode material of lithium ion battery and preparing method thereof |
| CN103985862A (en) * | 2014-04-14 | 2014-08-13 | 江苏中欧材料研究院有限公司 | Synthetic method of high vibration compaction high specific capacity phosphatic positive pole material |
| CN104300110A (en) * | 2014-09-23 | 2015-01-21 | 中南大学 | Preparation method of lithium manganese phosphate-lithium vanadium phosphate composite |
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| CN108706564A (en) * | 2018-04-24 | 2018-10-26 | 江西省金锂科技股份有限公司 | A kind of preparation method of high-pressure solid lithium ion battery anode material lithium iron phosphate |
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| CN1255888C (en) * | 2004-05-20 | 2006-05-10 | 上海交通大学 | Method for preparing lithiumion cell positive material iron-lithium phosphate |
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| US9742006B2 (en) | 2013-01-10 | 2017-08-22 | Lg Chem, Ltd. | Method for preparing lithium iron phosphate nanopowder coated with carbon |
| CN103151521A (en) * | 2013-02-22 | 2013-06-12 | 中国科学院过程工程研究所 | Positive electrode material of lithium ion battery and preparing method thereof |
| CN103151521B (en) * | 2013-02-22 | 2015-12-23 | 中国科学院过程工程研究所 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN103985862A (en) * | 2014-04-14 | 2014-08-13 | 江苏中欧材料研究院有限公司 | Synthetic method of high vibration compaction high specific capacity phosphatic positive pole material |
| CN104300110A (en) * | 2014-09-23 | 2015-01-21 | 中南大学 | Preparation method of lithium manganese phosphate-lithium vanadium phosphate composite |
| CN106957049A (en) * | 2017-05-09 | 2017-07-18 | 东北大学 | A kind of method for preparing nanoscale lithium manganese phosphate |
| CN108529584A (en) * | 2018-04-24 | 2018-09-14 | 江西省金锂科技股份有限公司 | The preparation method of high-density lithium iron phosphate positive material |
| CN108706564A (en) * | 2018-04-24 | 2018-10-26 | 江西省金锂科技股份有限公司 | A kind of preparation method of high-pressure solid lithium ion battery anode material lithium iron phosphate |
| CN113745503A (en) * | 2021-08-04 | 2021-12-03 | 北京泰丰先行新能源科技有限公司 | Preparation method of high-compaction lithium iron phosphate cathode material |
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Effective date of registration: 20160321 Address after: 101407 Beijing Yanqi Yanqi Economic Development Zone Huairou District Road No. 3 Patentee after: GUOLIAN AUTOMOBILE POWER CELL INSTITUTE CO., LTD. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |