CN101106188A - Making method for LiFePO4-carbon composite cathode material of lithium ion battery - Google Patents

Making method for LiFePO4-carbon composite cathode material of lithium ion battery Download PDF

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CN101106188A
CN101106188A CNA2006101481201A CN200610148120A CN101106188A CN 101106188 A CN101106188 A CN 101106188A CN A2006101481201 A CNA2006101481201 A CN A2006101481201A CN 200610148120 A CN200610148120 A CN 200610148120A CN 101106188 A CN101106188 A CN 101106188A
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ion battery
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lithium ion
cathode material
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CN100527482C (en
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刘辉
解晶莹
王可
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Shanghai Institute of Microsystem and Information Technology of CAS
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Abstract

The invention relates to a method for preparing a ferrous lithium phosphate-carbon compound positive material, which is characterized in that the Fe3+ compounds serve as the raw material, and the preparation is implemented based on the ethers organic solvent system, by using the sol-gel method, and combining the carbothermal reduction method. Ferrous lithium phosphate in the prepared compound material is in an olivine type with the particle size of 400-800nm, and the positive compound material has a stable charging and discharging voltage platform at 3.4V with the reversible charging-discharging capacity under the current of 2C reaching to 134.5mAh/g. The compound material has stable structure, good cycle performance, and is the environment-friendly material.

Description

The lithium ion battery preparation method of LiFePO 4-carbon composite cathode material
Technical field
The present invention relates to the preparation method of lithium ion battery, particularly a kind of preparation method of LiFePO 4-carbon composite cathode material with anode composite material.Belong to the lithium ion battery material field.
Background technology
Lithium ion battery is the novel green high-power rechargeable battery that occurs early 1990s, has become the emphasis that competitively research and develop countries in the world at present.Positive electrode is as an important component part of lithium ion battery, and research mainly concentrates on the lithium-containing transition metal oxide aspect of Co, Ni and Mn.LiCoO 2Be the positive electrode of unique large-scale commercial, the research comparative maturity, high comprehensive performance, but cost an arm and a leg, capacity is lower, and toxicity is bigger, has certain safety issue, and the new material that needs to seek high-performance and low-cost replaces it.LiNiO 2Cost is lower, and capacity is higher, but preparation difficulty, the consistency of material property and and poor reproducibility, have comparatively serious safety problem.Spinel-type LiMn 2O 4Cost is low, and fail safe is good, but high temperature cyclic performance is poor, and certain dissolubility is arranged in electrolyte.The research of two yuan or multi-element composite positive pole material mainly concentrates on LiNi 1-xCo xO 2And LiNi xCo yMn 1-x-yO 2The lamellar compound aspect, they are than LiCoO 2Positive electrode has advantages such as the cost of raw material is lower, specific capacity is higher, energy density is bigger, and fail safe is better, but large current discharging capability and tap density are than LiCoO 2On the low side, preparation cost increases, and has strengthened the difficulty that secondary resource reclaims to a certain extent.Therefore, the novel anode material of further researching and developing high energy, safety, environmental protection becomes the research focus of lithium ion battery circle.
LiFePO 4 (LiFePO 4) material is considered to the anodal substitution material of the most potential kalium ion battery of future generation, have abundant raw material, cost is low, specific capacity is higher, thermal stability and cyclical stability is good, nontoxic, environmental friendliness etc. is outstanding advantages, from people such as Padhi in 1997 first with the LiFePO of quadrature olivine structural 4As anode material for lithium-ion batteries, the research of this material is become gradually the research focus of various countries' researcher.But the conductivity of this material is very poor, can only discharge and recharge under minimum multiplying power under the room temperature, has influenced its high rate performance; In addition, preparation technology is usually with Fe 2+As source of iron, price is than Fe 3+Salt is high and need multistep to grind and heat treatment step, and preparation technology is complicated, and product purity is not easy control, thereby cost is increased, and these have all hindered its application in practical lithium-ion.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of LiFePO 4-carbon composite cathode material is with Fe 3+Compound is a raw material, based on the ether organic solvent system, by sol-gel process, prepares the LiFePO 4-carbon composite material in conjunction with carbothermic method.
1. lithium ion battery comprises as follows with the preparation method of LiFePO 4-carbon composite cathode material:
1) with Fe 3+Compound is dissolved in the ether organic solvent, be mixed with 1～2mol/L solution, mix excessive carbon source (consumption of carbon source makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then and contain in the ethereal solution, form homodisperse colloidal sol, and stir 3～8 hours one-tenth of evaporation gel down at 60～80 ℃, last vacuumize is to xerogel;
2) xerogel, lithium salts and phosphate are mixed in proportion and ground and mixed even, Li: Fe wherein: the P mol ratio is 1: 1: 1;
3) mixture being put into tube type resistance furnace, is under 5～50 liters/minute the inert gas protection, in 250 ℃～500 ℃ preliminary treatment 0.5～5 hour, to get rid of residual moisture and CO in the presoma at flow velocity 2, NH 3Deng gas;
4) mixture that preliminary treatment is obtained grinds evenly, and under the same inert atmosphere, heat treatment is 4～24 hours under 550 ℃～800 ℃ temperature, is cooled to room temperature and promptly obtains the lithium ferrous phosphate composite material that carbon coats.
Organic solvent used in the present invention is gylcol ether, diethylene glycol (DEG) ethers, propylene glycol ethers etc.
The used molysite of the present invention can be selected from ferric nitrate, ironic citrate, ferric acetate etc.; Lithium salts can be selected from lithium hydroxide, lithium carbonate, lithium oxalate or lithium acetate etc., and phosphate can be ammonium hydrogen phosphate, ammonium dihydrogen phosphate or ammonium phosphate.
Carbon source used in the present invention is sucrose, glucose, maltose, fructose or lactose etc.
Gas used in the present invention is the mist (volumn concentration of hydrogen is 2～10% in the mist) of argon gas, nitrogen or argon gas and hydrogen.
The present invention is based on the ether organic solvent system, pass through Fe 3+The sol-gel process of compound has prepared LiFePO 4-carbon composite cathode material in conjunction with carbothermic method.This anode composite material has the charging/discharging voltage platform about 3.4V stably, and electric conductivity and heavy-current discharge performance are good, and the reversible specific capacity that discharges and recharges reaches 134.5mAh/g under the 2C electric current; This composite structure is stable, and cyclical stability is good; Not containing Co, Ni etc. has the element of bigger pollution to environment, thereby is environmentally friendly material; The raw material that is adopted is Fe 3+Compound, cheap, wide material sources.
Description of drawings
Fig. 1 is the X ray diffracting spectrum by the prepared LiFePO 4-carbon composite cathode material of embodiment 1, adopts Rigaku-D/MAX 2200 type X ray polycrystalline diffractometer (Cu target k αRay, wavelength X=0.1540562nm).
Fig. 2 is FE-SEM (the Field emission scan electron microscope) photo according to the prepared LiFePO 4-carbon composite cathode material of embodiment 1, adopts S-4700 type field emission scanning electron microscope, and multiplication factor is 20000 times.
Fig. 3 is that voltage range is 2.5-4.2V according to the prepared discharge curve of simulation lithium ion battery under different charge-discharge magnifications of embodiment 1, and electrolyte is 1mol/L LiPF 6/ EC-DMC (1: 1), charge-discharge magnification is respectively 0.2C, 0.5C, 2C, and the measurement temperature is a room temperature.
Fig. 4 is that voltage range is 2.5-4.2V according to the prepared cycle performance curve of simulation lithium ion battery under different charge-discharge magnifications of embodiment 1, and electrolyte is 1mol/L LiPF 6/ EC-DMC (1: 1), charge-discharge magnification is respectively 0.2C, 0.5C, 2C, and the measurement temperature is a room temperature.
Embodiment
Embodiment 1
1) takes by weighing 0.5molFe (NO 3) 39H 2O is dissolved in the EGME organic solvent, be mixed with 1.5mol/L solution, mix organic carbon source sucrose (consumption of sucrose makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then in the EGME solution, form homodisperse colloidal sol, and stir 8 hours one-tenth of evaporation gel down at 70 ℃, last vacuumize is to xerogel;
2) it is even to take by weighing 0.5mol lithium hydroxide and 0.5mol ammonium dihydrogen phosphate and xerogel ground and mixed, and mixture is put into tube type resistance furnace, is under 5～50 liters/minute the argon shield, in 300 ℃ of preliminary treatment 5 hours at flow velocity;
3) mixture that preliminary treatment is obtained grinds evenly, and under the argon gas atmosphere, heat treatment is 10 hours under 725 ℃ of temperature, is cooled to room temperature and promptly obtains the LiFePO 4 composite positive pole that carbon coats.
The quality percentage composition that records residual carbon in the gained composite material is about 3%, and its XRD spectra is seen Fig. 1, and the reference standard card is olivine-type LiFePO 4(belonging to the Pnma space group), the diffraction maximum of residual carbon does not occur, and illustrates that it mainly exists with the form of amorphous carbon.Fig. 2 is the FE-SEM surface topography analysis chart under 20000 times of the multiplication factors, as we can see from the figure the gained material be particle diameter between between the 400nm to 800nm, have the part aggregation phenomenon between the particle.
Composite material with embodiment 1 gained is made electrode according to following method.
Take by weighing the composite material of embodiment 1 gained respectively with 80: 10: 10 mass ratioes: conductive carbon (SuperP): polytetrafluoroethylene (PTFE) grinds mixing and paint electrode on aluminium foil, 120 ℃ of vacuumizes obtained positive plate in 24 hours, with the pure metal lithium sheet is negative pole, to be dissolved in the 1.0mol/L LiPF in ethylene fat+dimethyl carbonate (volume ratio is 1: 1) mixed solvent 6Be electrolyte, the polypropylene microporous membrane is a diaphragm material, forms the simulation lithium ion battery.From Fig. 3, can see on the discharge curve of 0.2C multiplying power when the 2.5V-4.2V cut-ff voltage, the battery of surveying has 3.36V discharge voltage plateau stably, the reversible specific capacity that can calculate composite material among this embodiment is 155.7mAh/g, and reversible specific capacity can reach 134.5mAh/g under the 2C multiplying power.Fig. 4 is the respective battery cycle performance under 0.2C, 0.5C and 2C multiplying power respectively.Wherein, specific capacity is with LiFePO 4Mass Calculation, but not LiFePO 4The quality of+carbon composite.
Embodiment 2
1) taking by weighing the 0.5mol ironic citrate is dissolved in the EGME organic solvent, be mixed with 1.5mol/L solution, mix sucrose (consumption of sucrose makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then in the EGME solution, form homodisperse colloidal sol, and stir 8 hours one-tenth of evaporation gel down at 60 ℃, last vacuumize is to xerogel;
2) it is even to take by weighing 0.5mol lithium hydroxide and 0.5mol ammonium dihydrogen phosphate and xerogel ground and mixed, and mixture is put into tube type resistance furnace, is under 5～50 liters/minute the argon shield, in 300 ℃ of preliminary treatment 5 hours at flow velocity;
3) mixture that preliminary treatment is obtained grinds evenly, and under the argon gas atmosphere, heat treatment is 10 hours under 725 ℃ of temperature, is cooled to room temperature and promptly obtains the LiFePO 4 composite positive pole that carbon coats.All the other are with embodiment 1.
Embodiment 3
1) takes by weighing 0.5molFe (NO 3) 39H 2O is dissolved in the propylene glycol monomethyl ether organic solvent, be mixed with 1.5mol/L solution, mix organic carbon source sucrose (consumption of sucrose makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then in the propylene glycol monomethyl ether solution, form homodisperse colloidal sol, and stir 8 hours one-tenth of evaporation gel down at 80 ℃, last vacuumize is to xerogel;
2) it is even to take by weighing 0.5mol lithium hydroxide and 0.5mol ammonium dihydrogen phosphate and xerogel ground and mixed, and mixture is put into tube type resistance furnace, is under 5～50 liters/minute the argon shield, in 300 ℃ of preliminary treatment 5 hours at flow velocity;
3) mixture that preliminary treatment is obtained grinds evenly, and under the argon gas atmosphere, heat treatment is 10 hours under 725 ℃ of temperature, is cooled to room temperature and promptly obtains the LiFePO 4 composite positive pole that carbon coats.All the other are with embodiment 1.
Embodiment .4
1) takes by weighing 0.5molFe (NO 3) 39H 2O is dissolved in the EGME organic solvent, be mixed with 1.5mol/L solution, mix organic carbon source glucose (consumption of sucrose makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then in the EGME solution, form homodisperse colloidal sol, and stir 8 hours one-tenth of evaporation gel down at 70 ℃, last vacuumize is to xerogel;
2) it is even to take by weighing 0.5mol lithium hydroxide and 0.5mol ammonium dihydrogen phosphate and xerogel ground and mixed, and mixture is put into tube type resistance furnace, is under 5～50 liters/minute the argon shield, in 350 ℃ of preliminary treatment 5 hours at flow velocity;
3) mixture that preliminary treatment is obtained grinds evenly, and under the same argon gas atmosphere, heat treatment is 10 hours under 725 ℃ of temperature, is cooled to room temperature and promptly obtains the LiFePO 4 composite positive pole that carbon coats.All the other are with embodiment 1.
Embodiment 5
1) takes by weighing 0.5molFe (NO 3) 39H 2O is dissolved in the EGME organic solvent, be mixed with 1.5mol/L solution, mix organic carbon source sucrose (consumption of sucrose makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then in the EGME solution, form homodisperse colloidal sol, and stir 8 hours one-tenth of evaporation gel down at 70 ℃, last vacuumize is to xerogel;
2) it is even to take by weighing 0.5mol lithium hydroxide and 0.5mol ammonium hydrogen phosphate and xerogel ground and mixed, and mixture is put into tube type resistance furnace, is under 5～50 liters/minute the argon shield, in 300 ℃ of preliminary treatment 5 hours at flow velocity;
3) mixture that preliminary treatment is obtained grinds evenly, and under the same argon gas atmosphere, heat treatment is 10 hours under 725 ℃ of temperature, is cooled to room temperature and promptly obtains the LiFePO 4 composite positive pole that carbon coats.All the other are with embodiment 1.
Embodiment 6
1) takes by weighing 0.5molFe (NO 3) 39H 2O is dissolved in the EGME organic solvent, be mixed with 1.5mol/L solution, mix a certain amount of sucrose (consumption of sucrose makes that carbon content is 1～10% in the product), add distilled water and make it dissolving, join then in the EGME solution, form homodisperse colloidal sol, and stir 8 hours one-tenth of evaporation gel down at 70 ℃, last vacuumize is to xerogel;
2) it is even to take by weighing 0.25mol lithium carbonate and 0.5mol ammonium dihydrogen phosphate and xerogel ground and mixed, and mixture is put into tube type resistance furnace, is under 5～50 liters/minute the argon shield, in 350 ℃ of preliminary treatment 5 hours at flow velocity;
3) mixture that preliminary treatment is obtained grinds evenly, and under the same argon gas atmosphere, heat treatment is 10 hours under 750 ℃ of temperature, is cooled to room temperature and promptly obtains the LiFePO 4 composite positive pole that carbon coats.All the other are with embodiment 1.

Claims (9)

1. lithium ion battery is characterized in that with Fe with the preparation method of LiFePO 4-carbon composite cathode material 3+Compound is a raw material, based on the ether organic solvent system, by sol-gel process, prepares in conjunction with carbothermic method.
2. by the preparation method of the described lithium ion battery of claim 1, it is characterized in that preparation process is with LiFePO 4-carbon composite cathode material:
(1) with Fe 3+Compound is dissolved in the ether organic solvent, be mixed with 1～2mol/L solution, mix excessive carbon source, the consumption of carbon source makes that the quality percentage composition of carbon is 1～10% in the end product, add distilled water and make it dissolving, join then that containing dissolves each other in the ethereal solution forms homodisperse colloidal sol, and stir down at 60～80 ℃ and to flash to gel, last vacuumize is to xerogel;
(2) xerogel, lithium salts and phosphate are mixed in proportion and ground and mixed even, Li: Fe wherein: the P mol ratio is 1: 1: 1;
(3) mixture being put into tube type resistance furnace, is under 5～50 liters/minute the inert atmosphere protection, in 250 ℃～500 ℃ preliminary treatment at flow velocity;
(4) mixture that preliminary treatment is obtained grinds evenly, and under identical inert atmosphere, heat treatment under 550 ℃～800 ℃ temperature is cooled to room temperature and promptly obtains the lithium ferrous phosphate composite material that carbon coats;
Wherein, 1. employed ether organic solvent is gylcol ether, diethylene glycol (DEG) ethers or propylene glycol ethers;
2. described Fe 3+Compound is selected from ferric nitrate, ironic citrate or ferric acetate;
3. described lithium salts is lithium hydroxide, lithium carbonate, lithium oxalate or lithium acetate;
4. described phosphate is ammonium hydrogen phosphate, ammonium dihydrogen phosphate or ammonium phosphate;
5. described carbon source is sucrose, glucose, maltose, fructose or lactose.
3. lithium ion battery according to claim 2 is characterized in that with the preparation method of LiFePO 4-carbon composite cathode material the time that the 1. middle stirring of step flashes to gel is 3-8 hour.
4. lithium ion battery according to claim 2 is characterized in that with the preparation method of LiFePO 4-carbon composite cathode material the 3. middle pretreatment time of step is 0.5-5 hour.
5. lithium ion battery according to claim 2 is characterized in that with the preparation method of LiFePO 4-carbon composite cathode material the 4. middle heat treatment time of step is 4-24 hour.
6. lithium ion battery according to claim 1 is characterized in that with the preparation method of LiFePO 4-carbon composite cathode material employed gas is the mist of argon gas, nitrogen or argon gas and hydrogen.
7. by the preparation method of the described lithium ion battery of claim 6 with LiFePO 4-carbon composite cathode material, the volumn concentration that it is characterized in that hydrogen in the described mist is 2-10%.
8. by the preparation method of any described lithium ion battery of claim 1-6 with LiFePO 4-carbon composite cathode material, it is characterized in that LiFePO 4 is an olivine-type in the prepared composite material, particle diameter is 400-800nm.
9. by the preparation method of the described lithium ion battery of claim 8 with LiFePO 4-carbon composite cathode material, it is characterized in that described anode composite material has 3.4V charging/discharging voltage platform stably, charging and discharging capacity reversible under the 2C electric current reaches 134.5mAh/g.
CNB2006101481201A 2006-12-27 2006-12-27 Making method for LiFePO4-carbon composite cathode material of lithium ion battery Expired - Fee Related CN100527482C (en)

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Cited By (5)

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CN103403932A (en) * 2011-03-04 2013-11-20 住友大阪水泥股份有限公司 Electrode active substance and method for producing same
CN107226475A (en) * 2017-06-08 2017-10-03 西安交通大学 A kind of kalium ion battery positive electrode and preparation method thereof and kalium ion battery
CN107732218A (en) * 2017-11-22 2018-02-23 广西师范大学 The preparation method of alundum (Al2O3) and the common coated lithium ferrous phosphate composite material of carbon
CN108075108A (en) * 2017-12-26 2018-05-25 北京康力优蓝机器人科技有限公司 A kind of preparation method of iron phosphate lithium positive pole piece for smart home battery
CN113363463A (en) * 2021-06-02 2021-09-07 湖北亿纬动力有限公司 Sludge/biomass co-pyrolysis coke-coated lithium iron phosphate cathode material and preparation method and application thereof

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CN1291508C (en) * 2004-12-29 2006-12-20 浙江大学 Method for preparing carbon coated lithium ferrous phosphate composite material including metal conductive agent
CN1285541C (en) * 2005-04-14 2006-11-22 上海交通大学 Process for preparing quantum para electric EuTiO3 film by sol-gel

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103403932A (en) * 2011-03-04 2013-11-20 住友大阪水泥股份有限公司 Electrode active substance and method for producing same
CN107226475A (en) * 2017-06-08 2017-10-03 西安交通大学 A kind of kalium ion battery positive electrode and preparation method thereof and kalium ion battery
CN107226475B (en) * 2017-06-08 2020-03-31 西安交通大学 Potassium ion battery positive electrode material, preparation method thereof and potassium ion battery
CN107732218A (en) * 2017-11-22 2018-02-23 广西师范大学 The preparation method of alundum (Al2O3) and the common coated lithium ferrous phosphate composite material of carbon
CN108075108A (en) * 2017-12-26 2018-05-25 北京康力优蓝机器人科技有限公司 A kind of preparation method of iron phosphate lithium positive pole piece for smart home battery
CN113363463A (en) * 2021-06-02 2021-09-07 湖北亿纬动力有限公司 Sludge/biomass co-pyrolysis coke-coated lithium iron phosphate cathode material and preparation method and application thereof

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