CN101339995A - Preparation of lithium iron phosphate positive electrode material for lithium ion power cell - Google Patents
Preparation of lithium iron phosphate positive electrode material for lithium ion power cell Download PDFInfo
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- CN101339995A CN101339995A CNA200810150592XA CN200810150592A CN101339995A CN 101339995 A CN101339995 A CN 101339995A CN A200810150592X A CNA200810150592X A CN A200810150592XA CN 200810150592 A CN200810150592 A CN 200810150592A CN 101339995 A CN101339995 A CN 101339995A
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Abstract
The invention discloses a preparation method of a lithium iron phosphate anode material used in a lithium-ion power battery. The preparation method takes ammonium dihydrogen phosphate and lithium carbonate or lithium hydroxide or lithium acetate and ferrous oxalate or ferrous acetate or takes the lithium dihydrogen phosphate and the ferrous oxalate or ferrous acetate as raw materials, the raw materials are prepared according to the ratio of Li, P and Fe of 1:1:1 or the ratio of LiH2PO4 to Fe of 1:1, and are added with micro amount of nano-metallic oxide or metal salt. After the process of mixing by a water wet method, spraying, drying, rolling and prilling, the mixture is pre-sintered for 10 minus or plus 2 hours at the constant temperature of 300-400 DEG C and is clad with carbon for prilling after being cooled; and then after the process of mixing by the water wet method, spraying, drying, rolling and prilling, the mixture is sintered for 10 minus or plus 2 hours at the temperature of 650-800 DEG C and then is cooled to obtain the lithium iron phosphate which is made after being crashed by gas stream and being compacted. The preparation method has the prominent advantages of safe preparation process, simple operation procedure, easy realization of industrialization and stable material performance of the product.
Description
Technical field
The invention belongs to field of energy source materials, relate generally to a kind of positive electrode of lithium-ion-power cell, relate in particular to the preparation method of lithium ion battery with lithium iron phosphate positive material.
Technical background
Lithium ion battery has obtained increasing application as a kind of environment-friendly type high performance chargeable battery in various electronic products and communication tool.Thinking makes people to carrying out new planning the future of fuel-engined vehicle to the concern of environment with to energy starved.With the high energy secondary cell is the electric automobile (ElectricVehicle of power, EV) be hybrid-electric car (the Hybrid ElectricVehicle of power with fuel oil and battery, HEV) be subjected to increasing attention, this has proposed requirements such as high-performance, low cost to lithium ion battery, and then has also promoted the research to various novel electrode materials.
In novel anode material for lithium-ion batteries, LiFePO4 (LiFePO
4) have and stratiform cobalt acid lithium (LiCoO
2), lithium nickelate (LiNiO
2) and spinelle shape LiMn2O4 (LiMn
2O
4) advantage that waits material to compare favourably, table 1 has been listed the relevant comparing data of several metal materials.1997, people such as A.K.Padi are first at Padhi AK, Nanjundaswamy KS, GoodenoughJB.Phospho-olivines aspositive-electrode materials for rechargeable lithium batteries[J] .J ElectrochemSoc.1997, reported the phosphate compounds LiFePO with olivine structural among the 144:p1188-1194
4Because of its have low price, nontoxic, Environmental compatibility good, rich in mineral resources, higher specific capacity (theoretical capacity 170mAh/g, energy density 550Wh/Kg) and higher operating voltage (3.4V, with the lithium metal is negative pole), discharge and recharge to flatten and advantage such as delay, have extended cycle life, high-temperature behavior and security performance are good and cause people's extensive concern, be expected to become the main force of anode material for lithium-ion batteries of future generation.
LiFePO4 (LiFePO
4) obtained huge achievement in some developed countries such as the U.S., Japan.U.S. Valence Technology company is the earliest developer in the world, has had multiple motive-power battery to use LiFePO on its catalogue
4At present about LiFePO
4The preparation method mainly contain " carbothermic method " and " ferrous salt chemical combination method " etc.Carbothermic method is to adopt ferric iron (as Fe
2O
3) as source of iron, become the LiFePO of carbon coating by solid-phase sintering
4In solid phase synthesis, utilize material with carbon element reduction at high temperature, with the Fe in the raw material
3+Be reduced to Fe
2+, and and Li
+And PO
4 3-In conjunction with forming LiFePO
4" ferrous salt chemical combination method " is to adopt ferrous salt, lithium salts, phosphate to mix preparation at high temperature.The conditional request harshness of " carbothermic method " preparation, the time is long, and is mainly covered by the patent of the U.S. and Japan." ferrous salt chemical combination method " is that present people are to LiFePO
4Research is a kind of synthetic method of heat.Chinese patent CN200510086594.3 by people such as University of Science ﹠ Technology, Beijing Wang Xin east application discloses " a kind of microwave synthesis method of carbon-coated LiFePO 4 for lithium ion batteries ", the particular content of this method is, take by weighing lithium carbonate, ferrous oxalate and ammonium dihydrogen phosphate by stoichiometric proportion, an amount of thermal conducting agent and the organic substance that is used to carry out the carbon coating, make the abundant ground and mixed of dispersant with absolute ethyl alcohol, be pressed into bulk after drying, put into the crucible that active carbon is housed, crucible is placed the microwave field radiation heating, can make the relatively evenly LiFePO of carbon coating
4Yet this preparation method adopts alcohol as dispersant, and there is potential safety hazard in burning easily; This method adopts microwave heating simultaneously, also is difficult for carrying out industrialization production.
Several metal material related data of table 1 comparison sheet
| Cobalt Co | Nickel | Manganese Mn | Iron Fe | |
| Price than (/Fe) | 95 | 78 | 2.1 | 1 |
| Content in the earth's crust (ppm) | 25 | 75 | 950 | 50000 |
| Allow content (mg/m3) in the air | 0.1 | 1 | 5 | 10 |
| Allow content (mg/m3) in the water | 0.7 | 13.4 | 200 | 300 |
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of and be easy to realize industrialization production and adopt the water system mixing method to prepare the method for LiFePO4.
For solving the problems of the technologies described above, preparation method provided by the present invention may further comprise the steps:
(1) with ammonium dihydrogen phosphate and lithium carbonate or lithium hydroxide or lithium acetate again with ferrous oxalate or ferrous acetate according to Li: P: Fe=1: 1: 1 physical measurement is than batching, or with lithium dihydrogen phosphate and ferrous oxalate or ferrous acetate according to LiH
2PO
4: Fe=1: 1 physical measurement ratio batching, and in described batching, add micro-nano-metal-oxide or nano metal salt, constitute the doping batching thus;
(2) also adding plasma water gradually carries out ground and mixed described doping batching to be put into ball mill, sifts out abrading-ball after grinding to form pulpous state;
(3) by spray drying device slurry is become the class spherical powder, with the roll extrusion comminutor described class spherical powder is carried out the roll extrusion granulation, afterwards the granulation powder is put into the cylinder atmosphere sintering furnace, under nitrogen protection,, naturally cool to normal temperature with stove with constant temperature pre-burning 10 ± 2h of 300～400 ℃;
(4) in ball mill the granulation powder behind the sintering is carried out carbon and coat, the granulation powder after will coating is afterwards put into the cylinder atmosphere sintering furnace, with constant temperature sintering 10 ± 2h of 650～800 ℃, naturally cools to normal temperature with stove under nitrogen protection;
(5) sintered product that (4) step is produced with airslide disintegrating mill carries out comminution by gas stream, crushed products is joined plain bumper jolt ramming 30min again and obtains final LiFePO4 goods.
According to the present invention, described nano-metal-oxide can be selected titanium dioxide, zinc oxide, chromic acetate, manganese acetate, manganese carbonate, magnesium acetate or magnesium carbonate for use.
According to the present invention, describedly granulation powder behind the sintering is carried out the material that carbon coats to select acetylene black, carbon black, graphite and sucrose, glucose, carboxymethyl cellulose or polyacrylamide for use.
Beneficial effect of the present invention is embodied in the following aspects:
(1) the present invention adopts water system as dispersant, can not produce the inflammable danger that waits, and the fail safe that has not only improved technical process has also reduced production cost simultaneously.
(2) the present invention carries out the carbon coating by doped metal ion with to the granulation powder, improves the conductivity and the tap density of lithium iron phosphate positive material; In technical process, product has been carried out cylinder atmosphere sintering operation twice, thereby guaranteed that product is heated evenly, stable performance simultaneously.
(3) the present invention is by spray drying and dry method briquetting granulating working procedure, improve and improved the pattern and the tap density of lithium iron phosphate positive material, after the jolt ramming operation of postmenstruation, density can improve more than 30%, has improved the volume and capacity ratio of lithium iron phosphate positive material thus again.
Embodiment
The present invention is described in further detail below in conjunction with preferred embodiment.
The concrete processing step that the present invention prepares lithium iron phosphate positive material first preferred embodiment is:
(1) be that 99.5% lithium carbonate and content are that 99% ammonium dihydrogen phosphate and content are 99% ferrous oxalate by Li: P: Fe=1 with content: 1: 1 physical measurement is weigh batching recently, and adds the Nano titanium dioxide (TiO with rutile structure again in batching
2), its weighing is 0.2% of the total amount of batching, constitutes the batching of mixing thus;
(2) batching of will mixing joins in the SX premix ball mill, and to make the mass ratio of abrading-ball and the batching of mixing in the premix ball mill be 1.5: 1, and the ball radius of SX premix ball mill is 5～7mm; The deionization moisture that takes by weighing equal quality then joins for 3～5 times in the SX premix ball mill, and the limit adds the deionization waterside with 10 rev/mins mix at a slow speed, is mixture granularity D to no longer producing behind the gas
50≤ 1～2um, again with 100 rev/mins mix 20min fast; After sifting out abrading-ball slurry is transferred to the SM high speed ball mill, the ball radius of SM high speed ball mill is 2～3mm, and the high speed ball milling mixing 20min with 800～1000 rev/mins sifts out the abrading-ball in the slurries then;
(3) slurry is changed in the spray drying device, remove moisture content by the corresponding operation of spray drying, slurries are become to containing the class spherical powder of elements such as Li, Fe, P, then the class spherical powder is transferred in the roll extrusion comminutor, under the pressure of 5～15Mpa, carry out the roll extrusion granulation, afterwards, again the granulation powder is put into the cylinder atmosphere sintering furnace, under nitrogen protection,, and naturally cool to normal temperature with stove with 350 ℃ of constant temperature pre-burning 10 ± 2h;
(4) granulation powder behind the sintering and sucrose are added in the SX premix ball mill, the quality of sucrose be behind the sintering granulation powder quality 20%, pressing the quality sum of granulation powder and sucrose behind the sintering adds deionized water and stirs 30min with 100 rev/mins speed, after sifting out abrading-ball slurries are changed in the spray drying device, make slurries become the class spherical powder by the spray drying operation, and carry out the roll extrusion granulation once more, then the granulation powder is put into the cylinder atmosphere sintering furnace, under nitrogen protection,, and naturally cool to normal temperature with stove with 700 ℃ of constant temperature sintering 10 ± 2h;
(5) sintered product is put into airslide disintegrating mill and carried out comminution by gas stream, subsequently crushed products is joined in the plain bumper, after applying mechanical energy 30min, just obtained the high LiFePO4 goods of grain density to crushed products.
The present invention can be under the various combination of raw material, additive, covering, calcined temperature, sintering temperature, all according to the processing step of first preferred embodiment and other relevant parameter, prepare lithium iron phosphate positive material, thereby constitute a plurality of preferred embodiment of the present invention (seeing table 1 for details).What be worth proposition is that in the 7th and the 8th preferred embodiment of table 1, lithium dihydrogen phosphate and ferrous oxalate or ferrous acetate should be according to LiH
2PO
4: Fe=1: 1 physical measurement is recently prepared burden.
Claims (3)
1. the preparation method of a lithium iron phosphate positive electrode material for lithium ion power cell, it is characterized in that: this preparation method may further comprise the steps:
(1) with ammonium dihydrogen phosphate and lithium carbonate or lithium hydroxide or lithium acetate again with ferrous oxalate or ferrous acetate according to Li: P: Fe=1: 1: 1 physical measurement is than batching, or with lithium dihydrogen phosphate and ferrous oxalate or ferrous acetate according to LiH
2PO
4: Fe=1: 1 physical measurement ratio batching, and in described batching, add micro-nano-metal-oxide or nano metal salt, constitute the doping batching thus;
(2) also adding plasma water gradually carries out ground and mixed described doping batching to be put into ball mill, sifts out abrading-ball after grinding to form pulpous state;
(3) by spray drying device slurry is become the class spherical powder, with the roll extrusion comminutor described class spherical powder is carried out the roll extrusion granulation, afterwards the granulation powder is put into the cylinder atmosphere sintering furnace, under nitrogen protection,, naturally cool to normal temperature with stove with constant temperature pre-burning 10 ± 2h of 300～400 ℃;
(4) in ball mill the granulation powder behind the sintering is carried out carbon and coat, the granulation powder after will coating is afterwards put into the cylinder atmosphere sintering furnace, with constant temperature sintering 10 ± 2h of 650～800 ℃, naturally cools to normal temperature with stove under nitrogen protection;
(5) sintered product that (4) step is produced with airslide disintegrating mill carries out comminution by gas stream, crushed products is joined plain bumper jolt ramming 30min again and obtains final LiFePO4 goods.
2. the preparation method of lithium iron phosphate positive material according to claim 1, it is characterized in that: described nano-metal-oxide can be selected titanium dioxide, zinc oxide, chromic acetate, manganese acetate, manganese carbonate, magnesium acetate or magnesium carbonate for use.
3. the preparation method of lithium iron phosphate positive material according to claim 1 and 2 is characterized in that: describedly granulation powder behind the sintering is carried out the material that carbon coats can select acetylene black, carbon black, graphite and sucrose, glucose, carboxymethyl cellulose or polyacrylamide for use.
Priority Applications (1)
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|---|---|---|---|
| CNA200810150592XA CN101339995A (en) | 2008-08-12 | 2008-08-12 | Preparation of lithium iron phosphate positive electrode material for lithium ion power cell |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810150592XA CN101339995A (en) | 2008-08-12 | 2008-08-12 | Preparation of lithium iron phosphate positive electrode material for lithium ion power cell |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101867044A (en) * | 2010-06-28 | 2010-10-20 | 彩虹集团公司 | Method for preparing lithium iron phosphate material suitable for power battery |
| CN102153063A (en) * | 2011-03-31 | 2011-08-17 | 武汉工程大学 | Method for preparing lithium iron phosphate serving as battery material from brown corundum slags |
| CN102185137A (en) * | 2011-01-28 | 2011-09-14 | 厦门钨业股份有限公司 | Preparation method of multilevel-coated multivariate composite lithium iron phosphate cathode material |
| CN102275887A (en) * | 2011-01-17 | 2011-12-14 | 横店集团东磁股份有限公司 | Preparation method of high capacity high compacted density lithium iron phosphate material and product thereof |
| CN102479953A (en) * | 2010-11-25 | 2012-05-30 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery, method for manufacturing the same, and rechargeable lithium battery including the same |
| CN102482091A (en) * | 2009-09-03 | 2012-05-30 | 科莱恩金融(Bvi)有限公司 | Continuous synthesis of carbon-coated lithium-iron-phosphate |
| CN102515131A (en) * | 2011-12-23 | 2012-06-27 | 彩虹集团公司 | Process of using ferrous oxalate as iron source to prepare lithium iron phosphate in air atmosphere |
| CN102664265A (en) * | 2011-05-25 | 2012-09-12 | 淄博赛动能源材料有限公司 | Process for preparing lithium iron phosphate by using liquid phase cocrystallization and mechanical alloying |
| CN102803133A (en) * | 2009-06-24 | 2012-11-28 | 巴斯夫欧洲公司 | Process for the preparation of LiFePO4-carbon composites |
| CN103123968A (en) * | 2013-01-29 | 2013-05-29 | 中国科学院过程工程研究所 | High-performance lithium iron phosphate cathode material and preparation method of lithium iron phosphate cathode material |
| CN103500833A (en) * | 2013-10-23 | 2014-01-08 | 山东大学 | Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon |
| CN103531793A (en) * | 2013-10-23 | 2014-01-22 | 山东大学 | Method for preparing nanometer lithium iron phosphate for low temperature service |
| CN103560246A (en) * | 2013-11-25 | 2014-02-05 | 四川科能锂电有限公司 | Preparation method of positive material lithium iron phosphate of lithium ion battery |
| CN105253870A (en) * | 2015-10-20 | 2016-01-20 | 四川科能锂电有限公司 | Production process of lithium iron phosphate |
| CN108448102A (en) * | 2018-04-24 | 2018-08-24 | 方嘉城 | A kind of preparation method of high compacted density high power capacity LiFePO4 |
| CN109560281A (en) * | 2018-12-24 | 2019-04-02 | 桑顿新能源科技有限公司 | A kind of carbon-coated lithium iron phosphate positive material and preparation method thereof and lithium battery |
| CN110550615A (en) * | 2019-10-14 | 2019-12-10 | 王敏 | Preparation method of high-energy-density lithium iron phosphate |
| CN112349965A (en) * | 2020-10-14 | 2021-02-09 | 双登集团股份有限公司 | Lithium iron phosphate lithium ion battery with improved low-temperature performance and preparation method thereof |
| CN113871562A (en) * | 2021-09-28 | 2021-12-31 | 武汉科技大学 | Processing method and production line of lithium battery positive electrode material |
-
2008
- 2008-08-12 CN CNA200810150592XA patent/CN101339995A/en active Pending
Cited By (26)
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|---|---|---|---|---|
| CN102803133A (en) * | 2009-06-24 | 2012-11-28 | 巴斯夫欧洲公司 | Process for the preparation of LiFePO4-carbon composites |
| CN102482091A (en) * | 2009-09-03 | 2012-05-30 | 科莱恩金融(Bvi)有限公司 | Continuous synthesis of carbon-coated lithium-iron-phosphate |
| CN101867044A (en) * | 2010-06-28 | 2010-10-20 | 彩虹集团公司 | Method for preparing lithium iron phosphate material suitable for power battery |
| CN102479953A (en) * | 2010-11-25 | 2012-05-30 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery, method for manufacturing the same, and rechargeable lithium battery including the same |
| CN102479953B (en) * | 2010-11-25 | 2015-07-08 | 三星Sdi株式会社 | Positive active material for rechargeable lithium battery, method for manufacturing the same, and rechargeable lithium battery including the same |
| US9705132B2 (en) | 2010-11-25 | 2017-07-11 | Samsung Sdi Co., Ltd. | Olivine oxide-containing positive active material for rechargeable lithium battery with improved electro-conductivity, rate characteristics and capacity characteristics, method for manufacturing the same, and rechargeable lithium battery including the same |
| US10218001B2 (en) | 2010-11-25 | 2019-02-26 | Samsung Sdi Co., Ltd. | Olivine oxide-containing positive active material for rechargeable lithium battery with improved electro-conductivity, rate characteristics and capacity characteristics, method for manufacturing the same, and rechargeable lithium battery including the same |
| CN102275887A (en) * | 2011-01-17 | 2011-12-14 | 横店集团东磁股份有限公司 | Preparation method of high capacity high compacted density lithium iron phosphate material and product thereof |
| CN102185137A (en) * | 2011-01-28 | 2011-09-14 | 厦门钨业股份有限公司 | Preparation method of multilevel-coated multivariate composite lithium iron phosphate cathode material |
| CN102153063A (en) * | 2011-03-31 | 2011-08-17 | 武汉工程大学 | Method for preparing lithium iron phosphate serving as battery material from brown corundum slags |
| CN102153063B (en) * | 2011-03-31 | 2013-11-06 | 武汉工程大学 | Method for preparing lithium iron phosphate serving as battery material from brown corundum slags |
| CN102664265A (en) * | 2011-05-25 | 2012-09-12 | 淄博赛动能源材料有限公司 | Process for preparing lithium iron phosphate by using liquid phase cocrystallization and mechanical alloying |
| CN102515131A (en) * | 2011-12-23 | 2012-06-27 | 彩虹集团公司 | Process of using ferrous oxalate as iron source to prepare lithium iron phosphate in air atmosphere |
| CN103123968A (en) * | 2013-01-29 | 2013-05-29 | 中国科学院过程工程研究所 | High-performance lithium iron phosphate cathode material and preparation method of lithium iron phosphate cathode material |
| CN103123968B (en) * | 2013-01-29 | 2015-08-19 | 中国科学院过程工程研究所 | A kind of high-performance lithium iron phosphate cathode material and preparation method thereof |
| CN103531793A (en) * | 2013-10-23 | 2014-01-22 | 山东大学 | Method for preparing nanometer lithium iron phosphate for low temperature service |
| CN103500833B (en) * | 2013-10-23 | 2015-07-15 | 山东大学 | Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon |
| CN103500833A (en) * | 2013-10-23 | 2014-01-08 | 山东大学 | Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon |
| CN103560246B (en) * | 2013-11-25 | 2015-12-02 | 四川科能锂电有限公司 | A kind of preparation method of lithium ion battery anode material lithium iron phosphate |
| CN103560246A (en) * | 2013-11-25 | 2014-02-05 | 四川科能锂电有限公司 | Preparation method of positive material lithium iron phosphate of lithium ion battery |
| CN105253870A (en) * | 2015-10-20 | 2016-01-20 | 四川科能锂电有限公司 | Production process of lithium iron phosphate |
| CN108448102A (en) * | 2018-04-24 | 2018-08-24 | 方嘉城 | A kind of preparation method of high compacted density high power capacity LiFePO4 |
| CN109560281A (en) * | 2018-12-24 | 2019-04-02 | 桑顿新能源科技有限公司 | A kind of carbon-coated lithium iron phosphate positive material and preparation method thereof and lithium battery |
| CN110550615A (en) * | 2019-10-14 | 2019-12-10 | 王敏 | Preparation method of high-energy-density lithium iron phosphate |
| CN112349965A (en) * | 2020-10-14 | 2021-02-09 | 双登集团股份有限公司 | Lithium iron phosphate lithium ion battery with improved low-temperature performance and preparation method thereof |
| CN113871562A (en) * | 2021-09-28 | 2021-12-31 | 武汉科技大学 | Processing method and production line of lithium battery positive electrode material |
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Open date: 20090107 |