CN101955175A - Industrial preparation method for lithium iron phosphate - Google Patents
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Abstract
The invention belongs to an energy material, and particularly relates to a method for preparing a lithium iron phosphate anode material suitable to be used by a power type lithium ion battery and the like by using PVP (polyvinylpyrrolidone) as a dispersant and a carbon source at the same time in an aqueous solution. The method comprises the following steps of: weighing a lithium source compound, an iron source compound and a phosphorus source compound in a weight ratio, adding the compounds into water, adding a proper amount of PVP into the mixture, grinding the mixture for certain time, drying the mixture, transferring the obtained precursor into an atmosphere protection furnace, treating the precursor for certain time at a high temperature under inert atmosphere, and cooling the product to obtain the lithium iron phosphate. By observing, one-time particles are uniform and fine, and the first discharge capacity is 157.6mAh/g. The method has the advantages of low energy consumption, high grinding efficiency and environment-friendly and pollution-free production process, and is an excellent method for synthesizing a green new energy source material. The prepared material has the advantages of uniform particle size distribution, good circulating stability and prominent magnification performance, and is a battery anode material suitable for high-capacity energy storage equipment such as substations and the like and large-sized mobile equipment such as electric automobiles and the like.
Description
Technical field:
The invention belongs to green energy resource material technology field, particularly relate to lithium ion battery ferrousphosphate lithium material and manufacture method thereof.
Background technology:
Lithium ion battery compare with the traditional chemical power supply have high-voltage, heavy body, memory-less effect, advantage such as self-discharge is few and high-temperature behavior is good, generally paid attention to by people.And since the last century the nineties, all adopted LiCoO more than 90% as the positive electrode material of commercialization lithium ion battery
2, but Co content is limited, costs an arm and a leg, and toxicity is big, and the potential safety hazard of existence is also outstanding day by day, and a kind of novel secondary chemical sources of electric energy of an urgent demand occurs.LiNiO
2Once be considered to substitute LiCoO
2, but himself having the preparation difficulty, the shortcoming of cycle life and poor heat stability also exists certain potential safety hazard in addition; The LiMn of spinel shape
2O
4Safe, be easy to synthesize, but the J-T effect of self is difficult to overcome, cycle performance difference especially high temperature cyclic performance is bad, has directly restricted its application in the power cell field.
J.B.Goodenough group successfully synthesized the iron lithium phosphate with olivine structural in 1997, proposed and had proved that it has the lithium of being in arrears with performance, proposed in U.S. Pat A 5,910,382, with LiFePO
4As positive pole material of secondary lithium battery.As anode material for lithium-ion batteries, it is abundant, cheap that iron lithium phosphate has synthesis material, nontoxic, environmental friendliness own, the higher (170mAhg of theoretical specific capacity
-1), excellent heat stability, characteristics such as good cycle, this allows the lot of domestic and foreign investigator that it is felt more concern.Yet LiFePO
4Than LiCoO
2And LiMn
2O
4Low density (3.7g/em
3) can to influence energy capacity of battery to a certain extent close; Along with Li
+Be in arrears with FePO
4/ LiFePO
4The generation of two-phase interface and variation cause the ion of LiFePO 4 material and electronic conductivity low.Low electronic conductivity and lithium ion rate of diffusion are to make LiFePO
4Become the biggest obstacle of anode material for lithium-ion batteries of new generation.In order to overcome this defective, domestic and international research person do a lot of work, and quite effective.M.Armand etc. disclose LiFePO in U.S. Pat A 6,514,640
4Carry out the iron position and mix, thereby conductivity of electrolyte materials is improved; Patent USA 6,528,033 and the CN200410017382.5 method that all adopts carbon to coat improved the apparent specific conductivity of iron lithium phosphate, thereby improved the chemical property of material to a certain extent.
Except these two kinds of methods, the control particle grain size also is to improve the effective ways of material electrochemical performance, in the process of lapping of precursor, along with particle size reduction, surface-area increases, and is easy to generate reunion, this moment, plant capacity mainly was used to break the particle of these reunions, and particle size reduction is not made contributions, thereby caused the waste of energy, need to add an amount of dispersion agent and improve plant factor.The inorganic powder dispersion agent mainly comprises three kinds of inorganic dispersant, organic dispersing agent and macromolecule dispersing agents, and this non-ionic water-soluble polymer of polyvinylpyrrolidone belongs to a kind of of macromolecule dispersing agent.The adding of PVP can the homodisperse precursor, and improved mill efficiency greatly, PVP is dispersed in precursor particle periphery as carbon source simultaneously, and carbon evenly is coated on around the iron lithium phosphate particle, the iron lithium phosphate particulate is grown up played effective interception.The LiFePO 4 particle crystal grain that obtains of sintering is tiny like this, narrow distribution range, and the Physical Processing performance is good, especially is fit to be applied to the power cell field.
Summary of the invention:
The present invention is directed to problems such as existing lithium ion anode material LiFePO 4 energy consumption height, efficient when industrial production are low, a kind of industrial production process of LiFePO 4 is provided.
The object of the invention provides a kind of preparation method who is fit to simultaneously the LiFePO 4 of anode material that power-type lithium ion battery etc. uses in aqueous solvent with PVP (polyvinylpyrrolidone) as dispersion agent as the preparation of carbon source.This method low-carbon environment-friendly, energy consumption is little, efficient is high, is fit to suitability for industrialized production.
The industrial production process of a kind of LiFePO 4 provided by the invention is as follows:
Take by weighing Li source compound, Fe source compound, P source compound, carbon source by certain stoichiometric ratio, be added to ball milling in the aqueous solvent that contains the finite concentration dispersion agent respectively.Ball milling certain hour after drying slurry, and the exsiccant precursor is transferred in the inert atmosphere protection stove feeds protection of inert gas, the pyroprocessing through certain program obtains lithium ferrous phosphate as anode material of lithium ion battery after the cooling.
The industrial production process of above-mentioned a kind of LiFePO 4 as preferably, describedly takes by weighing Li source compound, Fe source compound, P source compound, carbon source by certain stoichiometric ratio, wherein takes by weighing Li: Fe=(0.9～1.1) in molar ratio: 1; Fe: P=(0.9～1): 1; Fe: C=1: (0.5～2).
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, described Fe: the C=1 that takes by weighing in molar ratio: C is meant carbon in the carbon source and the carbon sum in the dispersion agent in (0.5～2).
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, described Li source compound can be one or more in the lithium salts such as lithium hydroxide, Quilonum Retard, lithium acetate, lithium oxalate, monometallic; Described Fe source compound can be one or more in the molysite such as ferric oxide, Ferrox, ferrous phosphate, tertiary iron phosphate; Described P source compound can be one or more in the phosphoric acid salt such as primary ammonium phosphate, Trilithium phosphate, monometallic, ferrous ammonium phosphate, tertiary iron phosphate; Described carbon source can be carbohydrates such as fructose, glucose, sucrose, maltose, water-soluble polymer dispersants such as polyvinylpyrrolidone, one or more of materials such as graphite, acetylene black.
The industrial production process of above-mentioned a kind of LiFePO 4 as preferably, describedly is added to ball milling in the aqueous solvent that contains the finite concentration dispersion agent, is PVP as the material of dispersion agent.
The industrial production process of above-mentioned a kind of LiFePO 4 as preferably, describedly is added to ball milling in the aqueous solvent that contains the finite concentration dispersion agent, and the concentration that dispersion agent adds is 3.5～35g/L
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, described aqueous solvent is a deionized water.
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, described ball milling certain hour, this scope is mill speed 300～1500r/min, time 2～12h.
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, the temperature of described dry slurry is 80～120 ℃.
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, described feeding protection of inert gas, the inert atmosphere of feeding can be that nitrogen, argon gas or nitrogen are argon-mixed.
The industrial production process of above-mentioned a kind of LiFePO 4, as preferably, the pyroprocessing of the certain program of described process specifically refers to following program:
(1) temperature rise rate with 2～10 ℃/min rises to 350～450 ℃, and behind insulation 4～10h, the temperature rise rate with 2～10 ℃/min is warming up to 650～750 ℃ again, and insulation 8～20h obtains lithium ferrous phosphate as anode material of lithium ion battery after the cooling.
(2) temperature rise rate with 2～10 ℃/min rises to 350～450 ℃, insulation 4～10h postcooling, dry grinding 2～8h, go into stove once more and feed rare gas element, temperature rise rate with 2～10 ℃/min is warming up to 650～750 ℃, insulation 8～20h obtains lithium ferrous phosphate as anode material of lithium ion battery after the cooling.
The present invention proposes a kind of preparation method who is fit to simultaneously the LiFePO 4 of anode material that power-type lithium ion battery etc. uses in aqueous solvent with PVP (polyvinylpyrrolidone) as dispersion agent as the preparation of carbon source.This method makes the precursor homodisperse, and mill efficiency is improved, being adsorbed in around the precursor of dispersion agent simultaneously, and the carbon when making sintering evenly is coated on around the particle, helps generating the less and uniform LiFePO 4 of high purity and particle.
Description of drawings:
Fig. 1 presses the X-ray diffracting spectrum of the prepared LiFePO 4 of embodiment 1.
Fig. 2 presses the stereoscan photograph of the prepared LiFePO 4 of embodiment 1.
Fig. 3 presses the transmission electron microscope photo of the prepared ferrousphosphate lithium material of embodiment 1.
Fig. 4 presses the loading capacity first of the prepared ferrousphosphate lithium material of embodiment 1.
Fig. 5 presses the circulation discharge performance figure of the prepared ferrousphosphate lithium material of embodiment 1.
Embodiment:
Embodiment 1
Taking by weighing 6.65g lithium hydroxide, 29.61g tertiary iron phosphate, 4.40g polyvinylpyrrolidone is added in the 125g water; move to baking oven behind the rotating speed ball milling 2h with 300r/min; temperature is 80 ℃ in the baking oven; move to process furnace after the oven dry; logical Ar protection in the process furnace; be warming up to 350 ℃ with 2 ℃/min, be warming up to 650 ℃ with 2 ℃/min behind the insulation 4h, insulation 8h postcooling obtains ferrous phosphate doping lithium anode material.The assembling button cell carries out electrochemical property test to the iron phosphate powder positive electrode material: anode pole piece is pressed LiFePO
4: the mixed of acetylene black: PTFE (tetrafluoroethylene)=75: 20: 5 evenly back compressing tablet is made.With pole piece in 80 ℃ of vacuum-drying 12h.Counter electrode is a metal lithium sheet, and barrier film is polypropylene porous film (Celgard-2400), and electrolytic solution is 1.0mol/LliPF
6/ EC/DMC.Button cell assembles in being full of the glove box of Ar.Battery performance test voltage range 2.4～4.2V.Fig. 1 is the XRD diffractogram of sample, and sample 1 has kept olivine structural as seen from the figure.Fig. 2 is the SEM photo of sample 1, and is tiny from scheming visible sample particle homogeneous.Fig. 3 is the TEM photo of sample 1, from scheming successfully to have coated the thin carbon of one deck around the visible sample.Fig. 4 is the first circle charge/discharge capacity of sample 1, and sample head is put 157.6mAh/g, near the theoretical capacity of LiFePO 4.Fig. 5 is the circulation volume figure of sample 1, and from scheming sample discharge 137.6mAh/g behind visible the 50th cycle, the sample capacity conservation rate is 88%.
Embodiment 2
Taking by weighing 16.47g monometallic, 12.65g ferric oxide, 5g glucose and 0.315g polyvinylpyrrolidone is added in the 100g water, move to baking oven behind the rotating speed ball milling 6h with 600r/min, temperature is 100 ℃ in the baking oven, moves to process furnace after the oven dry, logical N in the process furnace
2-Ar gas mixture protection is warming up to 400 ℃ with 6 ℃/min, and insulation 6h takes out dry grinding 2h after being cooled to room temperature, moves to and continues logical N in the stove
2-Ar gas mixture is protected and is warming up to 700 ℃ with 6 ℃/min, and insulation 10h cooling obtains ferrous phosphate doping lithium anode material.The assembling button cell carries out electrochemical property test to the iron phosphate powder positive electrode material: anode pole piece is pressed LiFePO
4: the mixed of acetylene black: PTFE (tetrafluoroethylene)=75: 20: 5 evenly back compressing tablet is made.With pole piece in 80 ℃ of vacuum-drying 12h.Counter electrode is a metal lithium sheet, and barrier film is polypropylene porous film (Celgard-2400), and electrolytic solution is 1.0mol/LliPF
6/ EC/DMC.Button cell assembles in being full of the glove box of Ar.Battery performance test voltage range 2.4～4.2V.Put 145mAh/g headed by the electrochemistry capacitance of sample.
Embodiment 3
Take by weighing 6.12kg monometallic, 29.61kg tertiary iron phosphate, 3kg sucrose and 0.315g polyvinylpyrrolidone and be added in the 105kg water, behind the rotating speed ball milling 12h with 1200r/min, make spraying drying with 120 ℃, move to process furnace after the drying, logical N in the process furnace
2Protection is warming up to 450 ℃ with 10 ℃/min, and insulation 10h is cooled to and takes out dry grinding 6h after the room temperature, moves to continue logical N in the stove
2Protection also is warming up to 750 ℃ with 10 ℃/min, and insulation 20h cooling obtains ferrous phosphate doping lithium anode material.The assembling button cell carries out electrochemical property test to the iron phosphate powder positive electrode material: anode pole piece is pressed LiFePO
4: the mixed of acetylene black: PTFE (tetrafluoroethylene)=75: 20: 5 evenly back compressing tablet is made.With pole piece in 80 ℃ of vacuum-drying 12h.Counter electrode is a metal lithium sheet, and barrier film is polypropylene porous film (Celgard-2400), and electrolytic solution is 1.0mol/L1iPF
6/ EC/DMC.Button cell assembles in being full of the glove box of Ar.Battery performance test voltage range 2.4～4.2V.Put 150mAh/g headed by the electrochemistry capacitance of sample.
Claims (11)
1. the industrial production process of a LiFePO 4 is characterized in that comprising following concrete steps:
(1) preparation of precursor is to take by weighing Li source compound, Fe source compound, P source compound, carbon source by certain stoichiometric ratio, is added to ball milling in the aqueous solvent that contains the finite concentration dispersion agent respectively;
(2) ball milling certain hour after drying slurry, and the exsiccant precursor is transferred in the inert atmosphere protection stove feeds protection of inert gas, the pyroprocessing through certain program obtains lithium ferrous phosphate as anode material of lithium ion battery after the cooling.
2. the industrial production process of LiFePO 4 as claimed in claim 1 is characterized in that taking by weighing Li source compound, Fe source compound, P source compound, carbon source by certain stoichiometric ratio, wherein takes by weighing Li: Fe=(0.9～1.1) in molar ratio: 1; Fe: P=(0.9～1): 1; Fe: C=1: (0.5～2).
3. the industrial production process of LiFePO 4 as claimed in claim 2 is characterized in that taking by weighing in molar ratio Fe: C=1: the C in (0.5～2) is meant carbon in the carbon source and the carbon sum in the dispersion agent.
4. as the industrial production process of one of them described LiFePO 4 of claim 1-3, it is characterized in that described Li source compound is one or more in the lithium salts such as lithium hydroxide, Quilonum Retard, lithium acetate, lithium oxalate, monometallic; Described Fe source compound is one or more in the molysite such as ferric oxide, Ferrox, ferrous phosphate, tertiary iron phosphate; Described P source compound is one or more in the phosphoric acid salt such as primary ammonium phosphate, Trilithium phosphate, monometallic, ferrous ammonium phosphate, tertiary iron phosphate; Described carbon source is carbohydrates such as fructose, glucose, sucrose, maltose, water-soluble polymer dispersants such as polyvinylpyrrolidone, one or more of materials such as graphite, acetylene black.
5. the industrial production process of LiFePO 4 as claimed in claim 4 is characterized in that described dispersion agent is PVP.
6. the industrial production process of LiFePO 4 as claimed in claim 5 is characterized in that, is added to ball milling in the aqueous solvent that contains the finite concentration dispersion agent, and the concentration that dispersion agent adds is 3.5～35g/L.
7. the industrial production process of LiFePO 4 as claimed in claim 6 is characterized in that, described aqueous solvent is a deionized water.
8. the industrial production process of LiFePO 4 as claimed in claim 7 is characterized in that, the ball milling certain hour, and this scope is mill speed 300～1500r/min, time 2～12h.
9. the industrial production process of LiFePO 4 as claimed in claim 8 is characterized in that, the temperature of dry slurry is 80～120 ℃.
10. the industrial production process of LiFePO 4 as claimed in claim 9 is characterized in that, feeds protection of inert gas, and the inert atmosphere of feeding is that nitrogen, argon gas or nitrogen are argon-mixed.
11. the industrial production process as one of them described LiFePO 4 of claim 5-10 is characterized in that, the pyroprocessing of the certain program of process comprises concrete following program:
(1) temperature rise rate with 2～10 ℃/min rises to 350～450 ℃, and behind insulation 4～10h, the temperature rise rate with 2～10 ℃/min is warming up to 650～750 ℃ again, and insulation 8～20h obtains lithium ferrous phosphate as anode material of lithium ion battery after the cooling;
(2) temperature rise rate with 2～10 ℃/min rises to 350～450 ℃, insulation 4～10h postcooling, dry grinding 2～8h, go into stove once more and feed rare gas element, temperature rise rate with 2～10 ℃/min is warming up to 650～750 ℃, insulation 8～20h obtains lithium ferrous phosphate as anode material of lithium ion battery after the cooling.
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|---|---|---|---|---|
| CN102275889A (en) * | 2011-06-08 | 2011-12-14 | 上海应用技术学院 | Method for preparing lithium iron phosphate cathode material of lithium-ion battery |
| CN103531794A (en) * | 2013-10-28 | 2014-01-22 | 金瑞新材料科技股份有限公司 | Lithium ion battery positive material lithium ferrous phosphate and preparation method |
| TWI464109B (en) * | 2011-07-20 | 2014-12-11 | Advanced Lithium Electrochemistry Co Ltd | Preparation method of battery composite material and precursor thereof |
| CN104752724A (en) * | 2015-04-14 | 2015-07-01 | 张家港市山牧新材料技术开发有限公司 | Preparation method of LiFePO4 positive electrode material and lithium ion battery |
| CN105322162A (en) * | 2014-08-04 | 2016-02-10 | 湖北工程学院 | Preparation method for high-performance lithium iron phosphate composite positive electrode material |
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| CN109148836A (en) * | 2017-06-19 | 2019-01-04 | 中天新兴材料有限公司 | Carbon-coated LiFePO 4 for lithium ion batteries positive electrode and preparation method thereof |
| CN110350189A (en) * | 2019-05-23 | 2019-10-18 | 青海泰丰先行锂能科技有限公司 | A kind of preparation method of the high densification olivine cathode material of high capacity |
| CN110828823A (en) * | 2019-11-19 | 2020-02-21 | 湖北理工学院 | Preparation method of lithium manganese borate/carbon composite material |
| CN110957490A (en) * | 2019-07-30 | 2020-04-03 | 哈尔滨工业大学 | Preparation method of carbon-coated sodium iron phosphate electrode material with hollow structure |
| CN111082010A (en) * | 2019-12-17 | 2020-04-28 | 合肥国轩电池材料有限公司 | Positive electrode material and preparation method and application thereof |
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| CN115072694A (en) * | 2022-06-28 | 2022-09-20 | 衢州华友钴新材料有限公司 | Lithium iron phosphate anode material, preparation method thereof and lithium ion battery |
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| CN102275889A (en) * | 2011-06-08 | 2011-12-14 | 上海应用技术学院 | Method for preparing lithium iron phosphate cathode material of lithium-ion battery |
| TWI464109B (en) * | 2011-07-20 | 2014-12-11 | Advanced Lithium Electrochemistry Co Ltd | Preparation method of battery composite material and precursor thereof |
| US9321648B2 (en) | 2011-07-20 | 2016-04-26 | Advanced Lithium Electrochemistry Co., Ltd. | Preparation method of battery composite material and precursor thereof |
| CN103531794A (en) * | 2013-10-28 | 2014-01-22 | 金瑞新材料科技股份有限公司 | Lithium ion battery positive material lithium ferrous phosphate and preparation method |
| CN105322162A (en) * | 2014-08-04 | 2016-02-10 | 湖北工程学院 | Preparation method for high-performance lithium iron phosphate composite positive electrode material |
| CN105322162B (en) * | 2014-08-04 | 2018-04-10 | 湖北工程学院 | A kind of preparation method of high-performance iron phosphate lithium composite positive pole |
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| CN107204484A (en) * | 2017-05-25 | 2017-09-26 | 全球能源互联网研究院 | A kind of lithium-ion capacitor battery |
| CN107275600B (en) * | 2017-05-31 | 2019-11-15 | 浙江大学 | Molybdenum disulfide/carbon composite preparation method of hollow sphere |
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| CN109148836A (en) * | 2017-06-19 | 2019-01-04 | 中天新兴材料有限公司 | Carbon-coated LiFePO 4 for lithium ion batteries positive electrode and preparation method thereof |
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| CN110828823A (en) * | 2019-11-19 | 2020-02-21 | 湖北理工学院 | Preparation method of lithium manganese borate/carbon composite material |
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| CN114618485A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院理化技术研究所 | Carbon-based hollow supported microsphere catalyst and preparation method and application thereof |
| CN114618485B (en) * | 2020-12-11 | 2024-02-23 | 中国科学院理化技术研究所 | Carbon-based hollow supported microsphere catalyst and preparation method and application thereof |
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