CN101867044A - Method for preparing lithium iron phosphate material suitable for power battery - Google Patents
Method for preparing lithium iron phosphate material suitable for power battery Download PDFInfo
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- CN101867044A CN101867044A CN201010211088A CN201010211088A CN101867044A CN 101867044 A CN101867044 A CN 101867044A CN 201010211088 A CN201010211088 A CN 201010211088A CN 201010211088 A CN201010211088 A CN 201010211088A CN 101867044 A CN101867044 A CN 101867044A
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- lithium
- phosphate
- lifepo4
- iron
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- 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
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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 method for preparing a lithium iron phosphate material suitable for a power battery. In the method, lithium iron phosphate is taken as a substrate and the lithium iron phosphate material is prepared by mixing and sintering by a hydrothermal method, wherein the lithium iron phosphate consists of lithium salt, iron salt and phosphate; the mole ratio of lithium to iron to phosphorus is 1:1:1; the lithium salt is lithium carbonate, lithium hydroxide or lithium fluoride; the iron salt is iron acetate, ferrous chloride or iron hydroxide; and the phosphate is lithium dihydrogen phosphate, ammonium dihydrogen phosphate or triammonium phosphate. The lithium iron phosphate prepared by the method of the invention has high purity and specific capacity. Moreover, a synthesizing process of the invention has the advantages of simpleness, practicability, safety, reliability, low production cost, high yield and environmental friendliness.
Description
Technical field:
The invention belongs to the anode material for lithium-ion batteries field, relate in particular to a kind of LiFePO 4 material that is applicable to electrokinetic cell and preparation method thereof.
Background technology:
From eighties of last century since the latter stage nineties, olivine-type LiFePO
4The research of positive electrode causes numerous researchers' concern.LiFePO4 has high theoretical capacity (170mAh/g), high working voltage (voltage platform about 3.5V), suitable mass density (3.64g/cm
3), self discharge is little, LiFePO under low current density
4In Li
+Almost can 100% embed/take off embedding, have extended cycle life, good cycle, memory-less effect, cheap, Heat stability is good, advantage such as environmentally friendly, be expected to become anode material for lithium-ion batteries of new generation.
Lithium ion battery is widely used in the middle of the various electronic equipments, as notebook computer, in machine battery, digital camera, portable lighting equipment etc.Simultaneously, it also is used to electric tool, electric bicycle and electric automobile.Along with the consumption gradually of world petroleum resource, and society improves gradually to requirement on environmental protection, and electric motor car has obtained unprecedented opportunity to develop, as electric vehicle power sources, is the direction of electric motor car development with lithium ion battery.
In lithium ion battery, positive electrode occupies important status, also is the emphasis of current lithium ion battery development.In traditional positive electrode, the advantage of cobalt acid lithium is that energy height, good cycle, preparation are simple, technology maturation, Technological adaptability are good, and shortcoming is that price is too high, poor safety performance; The advantage of LiMn2O4 is a low price, and shortcoming is that cycle performance and high-temperature behavior have much room for improvement; / 2nd materials that partly substitute cobalt with manganese and nickel be a kind of LiMn2O4 and cobalt acidity can with the material of price compromise, its cobalt content can not fall very lowly, and the price of nickel is very high, so its cost performance is undesirable; And the LiFePO4 cost is low, aboundresources, good cycle, is desirable anode material for lithium-ion batteries.
LiFePO
4Positive electrode also has very big shortcoming, and its ion and electronic conductivity are not good, causes the charge-discharge magnification performance not good, and this shortcoming has greatly influenced LiFePO
4Replace LiCoO
2Become anode material for lithium-ion batteries of new generation, and LiFePO
4This shortcoming of positive electrode can overcome by the preparation ultra-fine grain, by increasing the material specific area, promotes being in contact with one another or the coated with conductive charcoal between the particle, can improve LiFePO
4The electric conductivity of positive electrode.But new problem thereupon appears again, increase along with specific area, the amount that is coated with required bonding agent and solvent also increases greatly, brought very big difficulty for the coating of pole piece, and after pole piece is prepared into electric core or battery, be easy to occur falling the material phenomenon, so, the present ubiquity coating of LiFePO 4 material difficult problem.
The people such as J.B.6oodenough of U.S. Texas university in 1999 obtain the patent right of the lithium battery anode LiFePO 4 material of US Patent No.591382, with 0.05mA/cm
2Low discharging current, capacity is 110mAh/g, reaches the theoretical capacity of 170mAh/g far away, reason is that LiFePO4 electronics and ionic conductivity are low.Be head it off, people such as N.Ravet and M.Armand adopt carbon coating, method metal-doped and that phosphate potential substitutes to improve the LiFePO4 conductivity greatly.The Yet-Ming Chiang of Massachusetts Institute Technology in 2002 etc. applies for a patent US2004/005265A1, the above metal ion of doping+divalent can increase substantially electronic conductivity in the lithium position, thereby improved the multiplying power property of LiFePO4, more than provided fundamental basis for the application in the power lithium-ion battery.
Sony company adopts Li
3PO and Fe
3(PO)
2-8H
2O is a raw material, adds amorphous carbon black or charcoal LiFePO4 primary particle ball milling together, in preparing LiFePO4 below 600 ℃.This method biggest advantage is to have only water to discharge in the tail gas, the productive rate height, but need preparation ferrous phosphate LiFePO4 primary particle earlier, and also if other elements that mix need to add in addition in proportion the balance that phosphoric acid could keep each element metering ratio.
Based on pyrocarbon thermal reduction synthetic technology, the cheap ferric iron sources such as di-iron trioxide of U.S. Valence Technology Inc. company, it is excessive to add weight ratio 100% when raw material mix, and is prepared LiFePO4 in ferric iron by the amorphous carbon black that carbon black is reduced to ferrous consumption.
Prior art generally adopts solid phase method or wet chemical method to prepare positive active material LiFePO
4, for example CN 1401559A discloses a kind of LiFePO4 (LiFePO
4) the preparation method, this method is the even back high-temperature calcination of lithium salts, ferrous salt and phosphate ground and mixed, the calcining back that finishes adds the conductive agent ground and mixed and makes LiFePO4.But when adopting solid phase method, various solid constituents are difficult to fully mix, therefore in the iron phosphate lithium positive pole active material that obtains various compositions especially conductive agent disperse inhomogeneously, directly influence the conductivity of positive active material.
Summary of the invention:
The object of the invention is to overcome the shortcoming that LiFePO4 purity is not high, specific capacity is lower, conductivity is bad of existing method preparation, provide a kind of raw material sources abundant, cheap, synthesis technique is simple, safe and reliable, production cost is low, productive rate is high, non-environmental-pollution, product have the preparation method of better chemical property.
The invention provides a kind of preparation method who is applicable to the high-density spherical ferric lithium phosphate of electrokinetic cell, comprise the steps:
(1) preparation nano-scale lithium iron phosphate primary particle: according to the mol ratio of lithium, iron, phosphorus is that 1: 1: 3 ratio is the mixed solution of 6.9-7.1 with lithium salts, molysite and phosphate preparation soluble in water respectively pH scope, this mixed solution is carried out the oil bath heating, gelatinous precipitate through in the isolated by filtration solution repeatedly obtains the LiFePO4 primary particle;
(2) spraying forms offspring: use spraying machine to spray, obtain the LiFePO4 second particle;
(3) LiFePO4 sintering: the LiFePO4 second particle is placed in the nitrogen environment,, obtains being shaped as spherical LiFePO 4 material through high-temperature roasting.
The oil bath heating-up temperature is 100-130 ℃ in the described step (1), and be 1-2 hour heating time.
Described lithium salts is lithium carbonate, lithium hydroxide, lithium fluoride; Described molysite is ferrous acetate, ferric nitrate, iron hydroxide; Described phosphate is lithium dihydrogen phosphate, ammonium dihydrogen phosphate, triammonium phosphate.
The spray parameters inlet temperature that described step (2) is set is 100-150 ℃, and outlet temperature is 50-100 ℃; According to percentage by weight, the liquid solid content of LiFePO4 second particle is 5-15%.
The temperature of high-temperature roasting is 400-800 ℃ in the described step (3), and roasting time is 4-8 hour.
This method is to be matrix with the lithium iron phosphate, sintering forms to adopt hydro thermal method to mix also, described particulate is formed the composite lithium iron phosphate second particle, and the LiFePO4 second particle is spherical in shape, and this method is to improve the tap density and the volume and capacity ratio of material by the spheroidization of LiFePO4 particle.
The LiFePO4 precipitation that hydro thermal method of the present invention makes should be cleaned and isolated by filtration repeatedly, filters the method that adopts decompress filter and reduces disengaging time.
The present invention adopts hydro thermal method, and reason is if adopt solid phase method, and various solid constituents are difficult to fully mix, therefore in the iron phosphate lithium positive pole active material that obtains various compositions especially conductive agent disperse inhomogeneously, influence the conductivity of positive active material.Hydro thermal method can finely be avoided this deficiency of solid phase method, and various solid constituents can evenly disperse, and makes LiFePO 4 material have good conductive capability.
Description of drawings:
Fig. 1 is sem photograph (SEM) figure of the LiFePO4 of preparation in the embodiment of the invention 1;
Fig. 2 is sem photograph (SEM) figure of the LiFePO4 of preparation in the embodiment of the invention 2;
Fig. 3 is sem photograph (SEM) figure of the LiFePO4 of preparation in the embodiment of the invention 3.
Embodiment:
Below in conjunction with accompanying drawing the present invention is done and to describe in further detail:
A kind of preparation method who is applicable to the LiFePO 4 material that electrokinetic cell is used comprises the steps:
(1). preparation nano-scale lithium iron phosphate primary particle
According to three kinds of salt ratios is P: Fe: Li=1: 1: 1 ratio, take by weighing three kinds of medicines and soluble in water respectively, and utilize magnetic stirring apparatus to stir, and the PH scope of measurement solution is about 7.Pour into through the solution after fully stirring and to carry out the oil bath heating in the round-bottomed flask, temperature remains on 100-130 ℃, and through 1-2 hour heating, precipitation was formed on the bottom, through isolated by filtration repeatedly, obtains the LiFePO4 primary particle.
(2). spraying forms offspring
Use spraying machine to spray, the setting spray parameters is: inlet temperature 100-150 ℃, outlet temperature 50-100 ℃, through experiment repeatedly, spray parameters obtains the LiFePO4 second particle and be shaped as sphere, and particle size is even in this scope, and fine powder content is low.
(3). the LiFePO4 sintering
The LiFePO4 second particle is placed the atmosphere tube type stove, in nitrogen environment, through 400-800 ℃ high-temperature roasting 4-8 hour, obtain lithium iron phosphate positive material.
The present invention is 5-15% (the LiFePO4 second particle of spraying is the mixture of liquid and solid, and wherein solid accounts for the 5-15% of mixture) to the liquid solid content of the LiFePO4 second particle that the nano-grade lithium iron phosphate primary particle is sprayed.
Embodiment 1:
Utilize assay balance accurately to take by weighing 149g (NH respectively
4)
3PO
4, 91.5g FeCl
225g LiF, then it is dissolved in respectively in the 500ml water, utilize magnetic stirring apparatus fully to dissolve and mix, stirred about 20 minutes, reagent dissolves fully, solution becomes homogeneous solution, and perusal solution does not have the visible crystals particle, utilize the soda acid indicator to measure acidity and alkalinity, the pH value should be 7, at this moment, and under the effect of mechanical agitation slurry (rotating speed=400 rev/min), successively three kinds of solution that prepare are poured in the big round bottom flask while stirring, utilize 120 ℃ of oil baths (this laboratory use silicone oil) heating 2h down, in heating, utilize mechanical agitator (rotating speed=400 rev/min) to stir, solid to drag cleans repeatedly and filters, and finally obtains the LiFePO4 primary particle.
The LiFePO4 primary particle sprayed obtains the LiFePO4 second particle, and the spray parameters of setting spraying machine is: 130 ℃ of inlet temperatures, 60 ℃ of outlet temperatures obtain the LiFePO4 second particle.
Place tube furnace to carry out roasting the LiFePO4 second particle, in tube furnace, feed the mist of 90% nitrogen and 10% hydrogen, be warmed up to 800 ℃, keep temperature 6h with the speed of 2 ℃/min, then stove is naturally cooled to room temperature, obtain spherical LiFePO 4 material.
LiFePO 4 material is carried out SEM detect, we can find out that LiFePO4 offspring particle diameter is even from Fig. 1, and segmentation is few, and particle is spherical, can effectively increase tap density.
Embodiment 2:
Utilize assay balance accurately to take by weighing 14.9g (NH respectively
4)
3PO
4, 9.15g FeCl
2, 2.5g LiF, then it is dissolved in respectively in the 50ml water, utilize magnetic stirring apparatus fully to dissolve and mix, stirred about 20 minutes, reagent dissolves fully, solution becomes homogeneous solution, and perusal solution does not have the visible crystals particle.Utilize the soda acid indicator to measure acidity and alkalinity, the pH value should be 7, at this moment, under the effect of mechanical agitation slurry (rotating speed=400 rev/min), successively three kinds of solution that prepare are poured in the big round bottom flask while stirring, utilize 120 ℃ of oil baths (silicone oil is used in this laboratory) heating 2h down, in heating, utilize mechanical agitator (rotating speed=400 rev/min) to stir, the solid of drag is cleaned repeatedly and filters, finally obtain the LiFePO4 primary particle.
The LiFePO4 primary particle sprayed obtains the LiFePO4 second particle, and the spray parameters of setting spraying machine is: 130 ℃ of inlet temperatures, 60 ℃ of outlet temperatures obtain the LiFePO4 second particle.
Place tube furnace to carry out roasting the LiFePO4 second particle, in tube furnace, feed the mist of 90% nitrogen and 10% hydrogen, be warmed up to 800 ℃, keep temperature 6h with the speed of 2 ℃/min, then stove is naturally cooled to room temperature, obtain spherical LiFePO 4 material.
LiFePO 4 material is carried out SEM detects, from Fig. 2 we LiFePO4 offspring particle diameter is even as can be seen, fine powder is few, particle be a sphere, can effectively increase tap density.
Embodiment 3:
Utilize assay balance accurately to take by weighing 1490g (NH respectively
4)
3PO
4, 915g FeCl
2, 250g LiF, then it is dissolved in respectively in the 5000ml water, utilize magnetic stirring apparatus fully to dissolve and mix, stirred about 20 minutes, reagent dissolves fully, solution becomes homogeneous solution, and perusal solution does not have the visible crystals particle.Utilize the soda acid indicator to measure acidity and alkalinity, the pH value should be 7, at this moment, in mechanical agitation slurry (rotating speed=400 rev/min) effect down, successively three kinds of solution that prepare are poured in the big round bottom flask while stirring, utilized oil bath (silicone oil is used in this laboratory) to heat 2h down for 120 ℃, in heating, utilize mechanical agitator (rotating speed=400 rev/min) to stir, the solid of drag is cleaned repeatedly and filters, finally obtain the LiFePO4 primary particle.
The LiFePO4 primary particle sprayed obtains the LiFePO4 second particle, and spraying machine is set spray parameters, 100 ℃ of inlet temperatures, and 50 ℃ of outlet temperatures obtain the LiFePO4 second particle.
Place tube furnace to carry out roasting the LiFePO4 second particle, in tube furnace, feed the mist of 90% nitrogen and 10% hydrogen, be warmed up to 600 ℃, keep temperature 6h with the speed of 2 ℃/min, stove naturally cools to room temperature, obtains spherical LiFePO 4 material.
LiFePO 4 material is carried out SEM detects, from Fig. 3 we LiFePO4 offspring particle diameter is even as can be seen, segmentation is few, particle be a sphere, can effectively increase tap density.
Above content is to further describing that the present invention did in conjunction with concrete preferred implementation; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by claims of being submitted to.
Claims (5)
1. a method for preparing lithium iron phosphate material that is applicable to electrokinetic cell is characterized in that, comprises the steps:
(1) preparation nano-scale lithium iron phosphate primary particle: according to the mol ratio of lithium, iron, phosphorus is that 1: 1: 1 ratio is the mixed solution of 6.9-7.1 with lithium salts, molysite and phosphate preparation soluble in water respectively pH scope, this mixed solution is carried out the oil bath heating, gelatinous precipitate through in the isolated by filtration solution repeatedly obtains the LiFePO4 primary particle;
(2) spraying forms offspring: use spraying machine to spray, obtain being shaped as spherical LiFePO4 second particle;
(3) LiFePO4 sintering: the LiFePO4 second particle is placed in the nitrogen environment,, obtains being shaped as spherical LiFePO 4 material through high-temperature roasting.
2. method according to claim 1 is characterized in that: the oil bath heating-up temperature is 100-130 ℃ in the described step (1), and be 1-2 hour heating time.
3. method according to claim 1 is characterized in that: described lithium salts is lithium carbonate, lithium hydroxide, lithium fluoride; Described molysite is ferrous acetate, ferric nitrate, iron hydroxide; Described phosphate is lithium dihydrogen phosphate, ammonium dihydrogen phosphate, triammonium phosphate.
4. method according to claim 5 is characterized in that: the spray parameters inlet temperature that described step (2) is set is 100-150 ℃, and outlet temperature is 50-100 ℃; According to percentage by weight, the liquid solid content of LiFePO4 second particle is 5-15%.
5. method according to claim 1 is characterized in that: the temperature of high-temperature roasting is 400-800 ℃ in the described step (3), and roasting time is 4-8 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441274A (en) * | 2013-09-04 | 2013-12-11 | 江苏元景锂粉工业有限公司 | Method for preparing high-density high-power spherical lithium iron phosphate positive material |
| CN114620701A (en) * | 2022-02-23 | 2022-06-14 | 贵州新天鑫化工有限公司 | Preparation method of nanoscale lithium iron phosphate |
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| CN101081695A (en) * | 2007-06-27 | 2007-12-05 | 上海电力学院 | Preparation method of doped modified ferric phosphate lithium |
| CN101121509A (en) * | 2007-07-23 | 2008-02-13 | 河北工业大学 | Hydro-thermal synthetic preparation method for lithium ion battery anode material lithium iron phosphate |
| CN101339995A (en) * | 2008-08-12 | 2009-01-07 | 中国兵器工业第二一三研究所 | Preparation of lithium iron phosphate positive electrode material for lithium ion power cell |
| CN101475157A (en) * | 2009-01-21 | 2009-07-08 | 武汉大学 | Preparation of lithium iron phosphate nano composite microsphere |
| CN101746742A (en) * | 2008-12-11 | 2010-06-23 | 中国电子科技集团公司第十八研究所 | Method for preparing lithium ion battery anode material spherical LiFePO4 |
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2010
- 2010-06-28 CN CN201010211088A patent/CN101867044A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081695A (en) * | 2007-06-27 | 2007-12-05 | 上海电力学院 | Preparation method of doped modified ferric phosphate lithium |
| CN101121509A (en) * | 2007-07-23 | 2008-02-13 | 河北工业大学 | Hydro-thermal synthetic preparation method for lithium ion battery anode material lithium iron phosphate |
| CN101339995A (en) * | 2008-08-12 | 2009-01-07 | 中国兵器工业第二一三研究所 | Preparation of lithium iron phosphate positive electrode material for lithium ion power cell |
| CN101746742A (en) * | 2008-12-11 | 2010-06-23 | 中国电子科技集团公司第十八研究所 | Method for preparing lithium ion battery anode material spherical LiFePO4 |
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| 《电化学 》 20081231 王思敏 等 《纳米级LiFePO4材料的水热模板法合成及其性能研究》 365-368 1－5 , 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103441274A (en) * | 2013-09-04 | 2013-12-11 | 江苏元景锂粉工业有限公司 | Method for preparing high-density high-power spherical lithium iron phosphate positive material |
| CN114620701A (en) * | 2022-02-23 | 2022-06-14 | 贵州新天鑫化工有限公司 | Preparation method of nanoscale lithium iron phosphate |
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Application publication date: 20101020 |