CN102005564A - Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid - Google Patents
Method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid Download PDFInfo
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- CN102005564A CN102005564A CN2010105000512A CN201010500051A CN102005564A CN 102005564 A CN102005564 A CN 102005564A CN 2010105000512 A CN2010105000512 A CN 2010105000512A CN 201010500051 A CN201010500051 A CN 201010500051A CN 102005564 A CN102005564 A CN 102005564A
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Abstract
The invention relates to a method for preparing nanocrystalline lithium iron phosphate powder by adopting iron hydroxide colloid, which comprises the steps of: with Fe(OH)3 colloid as a raw material, adding a lithium source, a phosphorus source and an organic carbon source in the colloid, powerfully and uniformly stirring and drying in vacuum at low temperature to form a uniform nano precursor containing lithium, iron, phosphorus and carbon; and placing in a crucible and raising the temperature to 500-800 DEG C in a muffle furnace protected by inert atmosphere, preserving the temperature for 2-24h, cracking the organic carbon source into carbon under the inert atmosphere, reducing ferric iron into ferrous iron by the carbon to form carbon wrapped lithium iron phosphate, naturally cooling to room temperature, and then grinding or crushing to obtain the nanocrystalline lithium iron phosphate powder. The colloid Fe(OH)3 is used as an iron source, the prepared lithium iron phosphate is of nano level, has excellent electrochemical property and low-temperature discharge property, is simple in process, and is suitable for industrialized production.
Description
Technical field:
The present invention relates to a kind of method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder, belong to the preparation method of a kind of lithium-ion-power cell with positive electrode.
Background technology:
Safe, pollution-free, advantages such as raw material sources extensive, good cycling stability that the olivine-type LiFePO4 has are considered to be used for the power battery anode material that pure electric automobile, hybrid-electric car, electric bicycle, electric tool, energy-accumulating power station etc. require big capacity, high-power field the best.
But pure phase LiFePO4 poorly conductive, ionic conductance are low, and it is rapid to make it when heavy-current discharge capacity attenuation; Lithium ion diffusion rate and temperature have very directly relation, and particularly during low temperature (20 ℃ ,-40 ℃), the lithium ion diffusion rate is lower, causes the discharge capacity of LiFePO4 and voltage platform very low.By reducing material primary particle size to nanoscale, shorten the lithium ion the evolving path, can significantly shorten diffusion time, thus the specific capacity of material when improving multiplying power discharging, low temperature discharge.
The extensive source of iron that adopts of synthesizing iron lithium phosphate mainly is ferrous oxalate, iron oxide, ferric phosphate etc. at present; after mixing with lithium salts, microcosmic salt, carbon source, high-temperature roasting under inert atmosphere protection is by carbon thermal reduction; ferric iron is a ferrous iron by carbon reduction, the LiFePO4 that synthetic carbon coats.Coat by metal ion mixing, carbon and to have improved the material electronics conductivity, thereby improve the specific discharge capacity, cyclical stability etc. of material.But adopt these raw materials and synthetic method, the LiFePO 4 material primary particle of preparation is bigger, and the secondary agglomeration body is bigger, obviously is unfavorable for material multiplying power discharging, low temperature discharge etc.
Patent of invention 200710013369.6 discloses the method for preparing equal dispersion ferric phosphate lithium nano crystal by hydrothermal synthetis, the LiFePO4 particle diameter of preparation is all dispersions lithium iron phosphate nano crystalline substance of 0.2-0.5 μ m, but the hydrothermal synthesis method that adopts is only limited to the preparation of a small amount of powder, if will enlarge preparation amount, its large high-temperature autoclave to manufacture and design difficulty bigger, difficultly realize industrialization.
Number of patent application is 200810029616.6 to disclose a kind of method that adopts the Prepared by Sol Gel Method nano lithium iron phosphate material, but need a large amount of auxiliary agents and complexing agent, as polyvinyl alcohol or octadecyl trimethylammonium bromide, citric acid, malic acid or tartaric acid etc., cause problems such as the dry contraction of presoma is big, the industrialization difficulty is big, synthesis cycle is long.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art and a kind of nano level primary particle that has is provided, the rapid diffusion that helps lithium ion, improve low temperature discharge, heavy-current discharge characteristic and the cyclical stability of material, energy consumption is low, and the employing ferric hydroxide colloid that technology simply is suitable for suitability for industrialized production prepares the method for nanocrystalline LiFePO 4 powder.
Purpose of the present invention can reach by following measure: a kind of method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder is characterized in that: adopt Fe (OH)
3Colloid is a source of iron, adds lithium source, phosphorus source and organic carbon source in colloid, according to product Li
xFe
yPO
4(x=0.8～1.2; y=0.8～1.2) molecular formula is carried out the raw material proportioning; the end product carbon content is 1～10%; brute force stirs and under 50～100 ℃ then; vacuum degree remains on 0.02～0.09MPa; dry 5～24h; form nanoscale presoma uniform, that contain lithium iron phosphorus carbon; put into crucible and be warmed up to 500-800 ℃ at the Muffle furnace of inert atmosphere protection; be incubated 2-24 hour; form the LiFePO4 that carbon coats, naturally cool to room temperature after pulverizing or grinding obtain nanocrystalline LiFePO 4 powder.
In order further to realize purpose of the present invention, described Fe (OH)
3The preparation raw material of colloid is FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3In one or more.
In order further to realize purpose of the present invention, described lithium source is one or more in lithium carbonate, lithium hydroxide, lithium dihydrogen phosphate, lithium nitrate, the lithium chloride.
In order further to realize purpose of the present invention, described phosphorus source is one or more in phosphoric acid, MAP, Diammonium phosphate (DAP), the lithium dihydrogen phosphate.
In order further to realize purpose of the present invention, described organic carbon source is one or more in sucrose, glucose, fructose, citric acid, tartaric acid, the starch.
The present invention can produce following good effect compared with the prior art: the present invention adopts colloid Fe (OH) first
3For source of iron prepares nanocrystalline LiFePO4.Method provided by the invention, raw material is the micelle of Nano grade, realizes that with lithium source, phosphorus source molecular level evenly mixes, and forms nanocrystalline carbon-coated LiFePO 4 for lithium ion batteries by Low Temperature Heat Treatment, the material of preparation has nanostructure, higher specific capacity and low temperature, multiplying power property.This method has been avoided the problems such as high energy consumption of a large amount of complexing agents of sol-gal process, high temperature solid-state method, and technology simply is suitable for suitability for industrialized production.Colloid Fe (OH)
3The size of particle is the nanoscale of 1～100nm (by the diameter of colloidal solid), and it has determined colloidal particle to have huge specific area and very strong absorption affinity, and this makes ion or the SS of micelle surface in can adsorbent solution.At Fe (OH)
3Add in the colloid and contain Li
+And PO
4 3-Ion solution or lithium salts, phosphate nano grade particles can be adsorbed in colloidal grain surface, under positive and negative charge or stirring action, and colloid generation coagulation, Li
+And PO
4 3-The colloid of ion or lithium salts, phosphate nano grade particles and coagulation wraps up mutually or is mingled with, and adds organic carbon source simultaneously as reducing agent and carbon encapsulated material, obtains precursor powder through dried.Presoma has nano-scale, and crystal grain is superfine, and the evolving path of atom is shorter, and through lower heat treatment temperature, ferric iron is ferrous by carbon reduction, can form the nanocrystalline ferric phosphate lithium cell material of the carbon coating of complete crystallization.The LiFePO4 conductivity of carbon coated is very not low, is 10
-10～10
-9S/cm coats through original position carbon reduction of the present invention and carbon, forms one deck carbon between particle and coats film, has improved electrical conductivity speed between particle, and conductivity reaches 10
-3～10
-2S/cm.By the carbon-coated LiFePO 4 for lithium ion batteries that preparation method provided by the invention synthesizes, have nano level primary particle, help the rapid diffusion of lithium ion, improve low temperature discharge, the heavy-current discharge characteristic of material, and cyclical stability.
Description of drawings:
Fig. 1 is a process chart of the present invention;
Fig. 2 is the XRD figure spectrum of the LiFePO 4 material of embodiment 1 preparation;
Fig. 3 is the charging and discharging curve of the LiFePO 4 material of embodiment 1 preparation, and wherein charge-discharge magnification is 0.2C, and voltage range is 2.5～4.1V, and probe temperature is respectively 25 degree and 0 degree (mixture of ice and water);
Fig. 4 is that the specific discharge capacity of LiFePO 4 material 0.2C charge and discharge cycles under 25 degree of embodiment 1 preparation and middle threshold voltage are with the cycle-index situation of change.
Embodiment:
Embodiment 1:
With 85.61gFeCl
36H
2O is dissolved in the 93.26mL deionized water, forms FeCl
3Saturated solution, and dropwise splash into the fresh bronzing Fe (OH) of preparation in the boiling water
3Colloid obtains colloid by the Tyndall phenomenon checking.In above-mentioned colloid, add and contain 32.94gLiH
2PO
4The aqueous solution, add 19.60g starch simultaneously as organic carbon source, mix fast, remain on 0.09MPa 50 ℃ of following vacuum degrees then, dry 24h obtains precursor powder.Presoma is put into the Muffle furnace of nitrogen protection, is warmed up to 500 ℃ with the speed of 1 ℃/min, and insulation 24h naturally cools to room temperature then, through grinding or pulverizing, obtains LiFePO after the taking-up
4/ C dusty material.
The XRD of the product that present embodiment obtains as can be seen, has synthesized the LiFePO 4 material of pure phase olivine-type structure as shown in Figure 2.The electrochemical property test of material is tested by the following method, is positive active material with iron phosphate powder of the present invention, and the lithium sheet is a negative pole, is assembled into the R2025 button cell and tests.Positive pole consists of 80% active material, 10% conductive carbon, 10%PVDF; Electrolyte is the LiPF of 1mol/L
6(EC+DMC), in glove box, be assembled into button cell.The battery testing charging system is: with the 0.2C constant current charge to 4.1V, then with the 4.1V constant voltage charge to electric current less than 0.005mA, static 2min, constant-current discharge are to 2.5V, system is carried out loop test according to this.The test environment temperature is respectively 25 ℃ and 0 ℃.
Fig. 3 is the charging and discharging curve of the LiFePO 4 material of embodiment 1 preparation, and wherein charge-discharge magnification is 0.2C, and voltage range is 2.5～4.1V.25 degree 0.2C specific discharge capacity down are 142.5mAh/g, and 0 degree 0.2C specific discharge capacity down is 105.8mAh/g, and 0 degree specific discharge capacity reaches 74.2% of 25 degree, and the material of the present invention's preparation has the good low-temperature discharge performance.Fig. 4 be the specific discharge capacity of 0.2C charge and discharge cycles of LiFePO 4 material of embodiment 1 preparation and middle threshold voltage with the cycle-index situation of change, 100 capacity of circulation are unattenuated down for 25 degree, middle threshold voltage is unattenuated, illustrative material has extraordinary cycle performance.
Embodiment 2:
With 85.61gFeCl
36H
2O is dissolved in the 93.26mL deionized water, forms FeCl
3Saturated solution dropwise splashes in the deionized water then, adds a small amount of 10%NH simultaneously
3H
2O forms fresh bronzing Fe (OH)
3Colloid obtains colloid by the Tyndall phenomenon checking.In above-mentioned colloid, add 12.89gLi
2CO
3Solid nano level powder and contain 36.43gNH
4H
2PO
4The aqueous solution, add 21.40g glucose simultaneously as organic carbon source, stir fast, then and remain on 0.02MPa 100 ℃ of following vacuum degrees, dry 5h obtains precursor powder.Presoma is put into Muffle furnace, is warmed up to 800 ℃ with the speed of 0.5 ℃/min, and insulation 2h naturally cools to room temperature then, through grinding or pulverizing, obtains LiFePO after the taking-up
4/ C dusty material.
Test above-mentioned positive electrode electrical property, 25 degree 0.2C specific discharge capacity down are 139.2mAh/g, and 0 degree 0.2C specific discharge capacity down is 101.0mAh/g, and 25 degree, 100 capacity of circulation down are unattenuated.
Embodiment 3:
With 128.03gFe (NO
3)
39H
2O is dissolved in the 114.31mL deionized water, forms saturated solution, dropwise splashes into then in the deionized water, adds a small amount of 10%NH simultaneously
3H
2O forms fresh bronzing Fe (OH)
3Colloid obtains colloid by the Tyndall phenomenon checking.In above-mentioned colloid, add solution and the 36.55mLH that contains 7.60gLiOH
3PO
4(85%w.t.) solution adds 19.60g starch simultaneously as organic carbon source, stirs fast, remains on 0.08MPa 70 ℃ of following vacuum degrees then, obtains precursor powder under the dry 15h.Presoma is put into Muffle furnace, is warmed up to 650 ℃ with the speed of 1.5 ℃/min, and insulation 10h naturally cools to room temperature then, through grinding or pulverizing, obtains LiFePO after the taking-up
4/ C dusty material.
Test above-mentioned positive electrode electrical property, 25 degree 0.2C specific discharge capacity down are 144.0mAh/g, and 0 degree 0.2C specific discharge capacity down is 109.3mAh/g, and 25 degree, 100 capacity of circulation down are unattenuated.
Embodiment 4:
With 128.03gFe (NO
3)
39H
2O is dissolved in the 114.31mL deionized water, forms saturated solution, dropwise splashes into then in the deionized water, adds a small amount of 10%NH simultaneously
3H
2O forms fresh bronzing Fe (OH)
3Colloid obtains colloid by the Tyndall phenomenon checking.In above-mentioned colloid, add and contain 10.95gLiNO
3Mixed solution and 36.55mLH with 6.74gLiCl
3PO
4(85%w.t.) solution adds 15g fructose and 6.4g sucrose simultaneously as organic carbon source, stirs fast, remains on 0.08MPa 70 ℃ of following vacuum degrees then, obtains precursor powder under the dry 15h.Presoma is put into Muffle furnace, is warmed up to 750 ℃ with the speed of 1.5 ℃/min, and insulation 10h naturally cools to room temperature then, through grinding or pulverizing, obtains LiFePO after the taking-up
4/ C dusty material.
Test above-mentioned positive electrode electrical property, 25 degree 0.2C specific discharge capacity down are 140.0mAh/g, and 0 degree 0.2C specific discharge capacity down is 98.3mAh/g, and 25 degree, 100 capacity of circulation down are unattenuated.
Embodiment 5:
With 196.03gFe
2(SO
4)
39H
2O is dissolved in the 44.60mL ionized water and forms saturated solution, dropwise splashes into then in the deionized water, adds a small amount of 10%NH simultaneously
3H
2O forms fresh bronzing Fe (OH)
3Colloid obtains colloid by the Tyndall phenomenon checking.In above-mentioned colloid, add and contain 12.89gLi
2CO
3Solid nano level powder and contain 36.43gNH
4H
2PO
4The aqueous solution, add the 21.40g citric acid simultaneously as organic carbon source, stir fast and form pasty state, remain on 0.08MPa 70 ℃ of following vacuum degrees then, obtain precursor powder under the dry 15h.Presoma is put into Muffle furnace, is warmed up to 650 ℃ with the speed of 1.5 ℃/min, and insulation 15h naturally cools to room temperature then, through grinding or pulverizing, obtains LiFePO after the taking-up
4/ C dusty material.
Test above-mentioned positive electrode electrical property, 25 degree 0.2C specific discharge capacity down are 138.8mAh/g, and 0 degree 0.2C specific discharge capacity down is 97.5mAh/g, and 25 degree, 100 capacity of circulation down are unattenuated.
Claims (5)
1. a method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder is characterized in that: adopt Fe (OH)
3Colloid is a source of iron, adds lithium source, phosphorus source and organic carbon source in colloid, according to product Li
xFe
yPO
4(x=0.8～1.2; y=0.8～1.2) molecular formula is carried out the raw material proportioning; the end product carbon content is 1～10%; brute force stirs and under 50～100 ℃ then; vacuum degree remains on 0.02～0.09MPa; dry 5～24h; form nanoscale presoma uniform, that contain lithium iron phosphorus carbon; put into crucible and be warmed up to 500-800 ℃ at the Muffle furnace of inert atmosphere protection; be incubated 2-24 hour; form the LiFePO4 that carbon coats, naturally cool to room temperature after pulverizing or grinding obtain nanocrystalline LiFePO 4 powder.
2. according to the described a kind of method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder of claim 1, it is characterized in that described Fe (OH)
3The preparation raw material of colloid is FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3In one or more.
3. according to the described a kind of method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder of claim 1, it is characterized in that described lithium source is one or more in lithium carbonate, lithium hydroxide, lithium dihydrogen phosphate, lithium nitrate, the lithium chloride.
4. according to the described a kind of method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder of claim 1, it is characterized in that described phosphorus source is one or more in phosphoric acid, MAP, Diammonium phosphate (DAP), the lithium dihydrogen phosphate.
5. according to the described a kind of method that adopts ferric hydroxide colloid to prepare nanocrystalline LiFePO 4 powder of claim 1, it is characterized in that described organic carbon source is one or more in sucrose, glucose, fructose, citric acid, tartaric acid, the starch.
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|---|---|---|---|---|
| CN102593461A (en) * | 2012-03-01 | 2012-07-18 | 合肥国轩高科动力能源有限公司 | Preparation method of positive material carbon-coated LiFePO4 of lithium ion secondary cell |
| CN102867954A (en) * | 2012-09-13 | 2013-01-09 | 清华大学 | Method for synthesizing lithium iron phosphate anode material by adopting emulsion liquid phase |
| CN102881903A (en) * | 2012-10-23 | 2013-01-16 | 兰州理工大学 | Preparation method of porous lithium iron phosphate powder |
| CN102909390A (en) * | 2012-09-21 | 2013-02-06 | 南京师范大学 | Method for preparing nano zero-valent iron particles by utilizing liquid-phase reduction method |
| CN110723754A (en) * | 2019-09-19 | 2020-01-24 | 桂林理工大学 | Using Fe (OH)3Preparation of alpha-Fe from colloid and sucrose2O3Method for preparing electrode material |
| CN111533103A (en) * | 2020-05-08 | 2020-08-14 | 蒋达金 | High-compaction ferric phosphate and preparation method of high-compaction lithium ferric phosphate |
| CN112117433A (en) * | 2020-09-01 | 2020-12-22 | 深圳市德方纳米科技股份有限公司 | Preparation method of lithium ferrite |
| CN115676895A (en) * | 2022-11-09 | 2023-02-03 | 山东海科创新研究院有限公司 | Lithium-rich lithium iron oxide and synthesis method thereof |
| CN115849321A (en) * | 2022-12-27 | 2023-03-28 | 博创宏远新材料有限公司 | FePO for lithium ion battery anode material 4 Preparation method of hollow microspheres |
| CN116177515A (en) * | 2022-12-27 | 2023-05-30 | 昆明精粹工程技术有限责任公司 | Method for preparing battery-grade lithium iron phosphate by using pyrite cinder |
| CN117712544A (en) * | 2024-02-06 | 2024-03-15 | 邢东(河北)锂电科技有限公司 | Resource utilization method of waste lithium iron phosphate battery |
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| CN102593461B (en) * | 2012-03-01 | 2014-12-03 | 合肥国轩高科动力能源股份公司 | Preparation method of positive material carbon-coated LiFePO4 of lithium ion secondary cell |
| CN102593461A (en) * | 2012-03-01 | 2012-07-18 | 合肥国轩高科动力能源有限公司 | Preparation method of positive material carbon-coated LiFePO4 of lithium ion secondary cell |
| CN102867954A (en) * | 2012-09-13 | 2013-01-09 | 清华大学 | Method for synthesizing lithium iron phosphate anode material by adopting emulsion liquid phase |
| CN102867954B (en) * | 2012-09-13 | 2014-09-24 | 清华大学 | Method for synthesizing lithium iron phosphate anode material by adopting emulsion liquid phase |
| CN102909390A (en) * | 2012-09-21 | 2013-02-06 | 南京师范大学 | Method for preparing nano zero-valent iron particles by utilizing liquid-phase reduction method |
| CN102881903A (en) * | 2012-10-23 | 2013-01-16 | 兰州理工大学 | Preparation method of porous lithium iron phosphate powder |
| CN110723754B (en) * | 2019-09-19 | 2022-03-22 | 桂林理工大学 | Using Fe (OH)3Preparation of alpha-Fe from colloid and sucrose2O3Method for preparing electrode material |
| CN110723754A (en) * | 2019-09-19 | 2020-01-24 | 桂林理工大学 | Using Fe (OH)3Preparation of alpha-Fe from colloid and sucrose2O3Method for preparing electrode material |
| CN111533103A (en) * | 2020-05-08 | 2020-08-14 | 蒋达金 | High-compaction ferric phosphate and preparation method of high-compaction lithium ferric phosphate |
| CN112117433A (en) * | 2020-09-01 | 2020-12-22 | 深圳市德方纳米科技股份有限公司 | Preparation method of lithium ferrite |
| CN112117433B (en) * | 2020-09-01 | 2022-05-03 | 深圳市德方创域新能源科技有限公司 | Preparation method of lithium ferrite |
| CN115676895A (en) * | 2022-11-09 | 2023-02-03 | 山东海科创新研究院有限公司 | Lithium-rich lithium iron oxide and synthesis method thereof |
| CN115849321A (en) * | 2022-12-27 | 2023-03-28 | 博创宏远新材料有限公司 | FePO for lithium ion battery anode material 4 Preparation method of hollow microspheres |
| CN116177515A (en) * | 2022-12-27 | 2023-05-30 | 昆明精粹工程技术有限责任公司 | Method for preparing battery-grade lithium iron phosphate by using pyrite cinder |
| CN115849321B (en) * | 2022-12-27 | 2024-02-23 | 博创宏远新材料有限公司 | FePO for lithium ion battery anode material 4 Preparation method of hollow microsphere |
| CN117712544A (en) * | 2024-02-06 | 2024-03-15 | 邢东(河北)锂电科技有限公司 | Resource utilization method of waste lithium iron phosphate battery |
| CN117712544B (en) * | 2024-02-06 | 2024-04-12 | 邢东(河北)锂电科技有限公司 | Resource utilization method of waste lithium iron phosphate battery |
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