CN102299334A - Carbon coated LiFePO4 porous anode and preparation method thereof - Google Patents

Carbon coated LiFePO4 porous anode and preparation method thereof Download PDF

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Publication number
CN102299334A
CN102299334A CN2011101986902A CN201110198690A CN102299334A CN 102299334 A CN102299334 A CN 102299334A CN 2011101986902 A CN2011101986902 A CN 2011101986902A CN 201110198690 A CN201110198690 A CN 201110198690A CN 102299334 A CN102299334 A CN 102299334A
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lifepo
gelatin
preparation
positive pole
carbon
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黄雅钦
刘冉冉
王维坤
张�浩
李中博
余仲宝
苑克国
王安邦
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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 relates to a carbon coated LiFePO4 porous anode and a preparation method thereof. By carrying out high-heat treatment on a traditional LiFePO4 anode to let gelatin be subject to in situ carbonization, the carbon coated LiFePO4 porous anode is obtained, LiFePO4 and acetylene black are distributed uniformly, the pole slice has a porous structure, the gelatin-based carbon is uniformly distributed in LiFePO4, acetylene black and current collectors, and the structure is stable. Using the carbon coated LiFePO4 porous anode in the lithium ion battery anode is good for infiltration of the electrolyte, improves the conductive performance of the pole slice, and thus improving the electrochemical performance of the lithium ion battery, especially the discharge rate. The preparation method is simple and the cost is low.

Description

A kind of carbon coats LiFePO＜sub〉4＜/sub〉the porous positive pole and preparation method thereof
Technical field:
The present invention relates to a kind of carbon and coat LiFePO 4Porous positive pole and preparation method thereof belongs to technical field of lithium ion.
Background technology:
Lithium ion battery has that specific energy is big, operating voltage is high, memory-less effect and advantage such as environmentally friendly, not only in compact electric apparatus such as mobile phone, camera, notebook, obtained using widely, and the application in Large Electric equipment such as electric motor car, satellite, fighter plane also enjoys favor.In lithium ion battery, because the specific capacity and the cycle performance of carbon negative pole material all can reach higher level (300mAh/g), but the specific capacity of positive electrode lower (130mAh/g), and the irreversible capacity loss that needs the added burden negative pole again, so the research of positive electrode is the key issue of Study on Li-ion batteries using with improving always.LiFePO 4Owing to have high security, good cycle, environmental friendliness etc. are one of at present main anode material for lithium ion battery, but itself conductivity is lower by (10 -9Scm -2), the lithium ion diffusion coefficient is little by (10 -14～10 -16Cm 2s -1) and to cause the high rate performance difference be to limit the one of the main reasons of its industrial applications, particularly limited its application in Large Electric equipment.
In recent years, in order to improve the high rate performance of LiFePO4, the scientific research personnel had made very big effort, and such as by reducing grain size, carbon coats or preparation LiFePO 4/ C composite material etc.CN101913588A, CN101393982, CN101777648A, CN101428781, US7344659 etc. are by reducing LiFePO 4The powder granule particle diameter, synthesis nano LiFePO 4, make LiFePO 4High rate performance improve greatly.When scantling reduced, specific area generally can increase.The current density of electrode is reduced, reduce the polarization of electrode effect; Can be the lithium ion migration simultaneously more passage is provided, shorten migration path, reduce diffusion impedance.But in actual applications, can not compensate the negative effect that it brings when reducing particle diameter, descend, tap density reduction and production cost increase etc. such as cycle performance.CN101800311A, CN101339991, CN101567441, US11993925, US11267107, US12105895 etc. coat LiFePO by add the synthetic carbon of different carbon sources in synthetic 4, not only can improve conductivity, and at LiFePO 4Can control grain growth in the building-up process, make particle diameter less, thereby improve its high rate performance.But the method that coats by conductive doped dose and carbon not only improve multiplying power degree on limited, can cause LiFePO simultaneously 4Tap density reduce, processing cost increases greatly.
Summary of the invention:
The objective of the invention is to propose a kind of carbon and coat LiFePO 4Porous positive pole and preparation method thereof is by to traditional LiFePO 4Positive pole carries out high-temperature heat treatment makes the carbonization of gelatin original position obtain carbon coating LiFePO 4The porous positive pole, LiFePO 4And acetylene black is evenly distributed, and pole piece is loose structure, and gelatin-based carbon is uniformly distributed in LiFePO 4And between acetylene black and collector, Stability Analysis of Structures.Be used for the infiltration that lithium ion cell positive helps electrolyte, improve the electric conductivity of pole piece, and then improve chemical property, the especially high rate performance of lithium ion battery.
A kind of carbon provided by the invention coats LiFePO 4The preparation method of porous positive pole is by to the gelatin being traditional LiFePO of binding agent 4Positive pole (comprises collector, LiFePO 4Particle, conductive agent and gelatin binding agent) carry out high-temperature heat treatment and make the method for gelatin original position carbonization obtain carbon to coat LiFePO 4The porous positive pole.Concrete steps and condition are:
To with the gelatin LiFePO of binding agent 4Anode pole piece is warming up to 200～350 ℃ gradually under nitrogen protection, carry out pre-carbonization 1.5～3h; Be warming up to 400～600 ℃ more gradually, and keep 1～3h, carry out carbonization; Under nitrogen protection, naturally cool to room temperature then, obtain carbon and coat LiFePO 4The porous positive pole.
In the said method of the present invention, described pre-carbonization optimum temperature is 300 ℃.
In the said method of the present invention, heating rate is 2～10 ℃/min gradually.
The present invention is above-mentioned to be the LiFePO of binding agent with the gelatin 4The preparation method of anode pole piece is a prior art, with LiFePO 4, acetylene black and gelatin solution (mass concentration 1～20%) press LiFePO 4, acetylene black and gelatin be with 70～85: 0～9: 6～20 mass ratioes mix, and wherein acetylene black is optional ingredient, after wet-milling, mixed dope is coated on the collector aluminium foil, obtains in 60～120 ℃ of vacuumize 2～24h.
The invention has the advantages that selected binding agent is a gelatin; it is a kind of big molecule of water-soluble biological of natural environmental-protective; cheap; wide material sources; have good caking property and dispersiveness, active material and acetylene black are evenly distributed, under nitrogen protection, pole piece is carried out high-temperature heat treatment; the gelatin of insulation is converted into the gelatin-based carbon with certain conductivity, is uniformly distributed in LiFePO 4And between acetylene black and collector, help the transportation of electronics, reduce the pole piece impedance.Because the decomposition and the contraction of gelatin form loose structure, increase the contact area of electrolyte and active material simultaneously, help the infiltration of electrolyte, thereby help the transportation of lithium ion.The present invention is by the control of gelatin binding agent and optimize LiFePO 4And the distribution of acetylene black, the carbonization by the gelatin binding agent reaches pore-creating and the effect that improves conductivity, has not change tap density, and technology is simple, low cost and other advantages.
Effect of the present invention: adopt the carbon of the present invention's preparation to coat LiFePO 4The porous positive pole is used for lithium ion battery, has improved electronics, the ionic conduction performance of pole piece, and test result shows that chemical property improves greatly, especially high rate performance.Preparation method of the present invention is simple simultaneously, and cost is lower, is fit to industrial production, is LiFePO 4New way has been opened up in the raising of anodal high rate performance.
Description of drawings:
Fig. 1 is the sem photograph of Comparative Examples 1 gained pole piece
Fig. 2 is the sem photograph of embodiment 1 gained pole piece
Fig. 3 is the discharge curve of embodiment 1 gained pole piece under 0.5C and 5C multiplying power
Fig. 4 is the bending photo of embodiment 2 gained pole pieces
Embodiment:
Below by embodiment the present invention is further detailed, but protection scope of the present invention is not limited to cited embodiment.
Comparative Examples 1:
With LiFePO 4With acetylene black under 120 ℃ of vacuum dry 6 hours in advance, gelatin was dissolved in 60 ℃ of deionized waters and is made into the 2wt.% gelatin solution, with LiFePO 4, acetylene black and gelatin press mass ratio and mix at 85: 9: 6, behind the wet-milling 1h, mixed dope coated on the aluminium foil, 60 ℃ of vacuumize 12h obtain pole piece.Its SEM schemes as shown in Figure 1, because gelatin has good caking property and dispersiveness, LiFePO 4Be evenly distributed with acetylene black.
It is that the disk of 12mm is as positive pole that pole piece is cut into diameter; adopting the 1mol/L lithium hexafluoro phosphate to be dissolved in ethylene carbonate/diethyl carbonate (volume ratio 1: 1) is electrolyte; in the glove box under the argon shield, the lithium sheet is done negative pole and is assembled into the CR2025 button cell and carries out electrochemical property test.Test result shows that specific discharge capacity is 130mAh/g under the 0.5C.Specific discharge capacity is 90mAh/g under the 5C.
Comparative Examples 2:
With LiFePO 4With acetylene black under 120 ℃ of vacuum dry 6 hours in advance, gelatin was dissolved in 60 ℃ of deionized waters and is made into the 3wt.% gelatin solution, with LiFePO 4, acetylene black and gelatin press mass ratio and mix at 85: 5: 10, behind the wet-milling 1h, mixed dope coated on the aluminium foil, 80 ℃ of vacuumize 16h obtain pole piece.Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 109.5mAh/g under the 0.5C, and specific discharge capacity is 78.4mAh/g under the 5C.
Comparative Examples 3:
With LiFePO 4With acetylene black under 120 ℃ of vacuum dry 6 hours in advance, gelatin was dissolved in 60 ℃ of deionized waters and is made into the 4wt.% gelatin solution, with LiFePO 4, acetylene black and gelatin press mass ratio and mix at 78: 2: 20, behind the wet-milling 1h, mixed dope coated on the aluminium foil, 120 ℃ of vacuumize 8h obtain pole piece.Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 96.6mAh/g under the 0.5C, and specific discharge capacity is 29.3mAh/g under the 5C.
Comparative Examples 4:
With LiFePO 4Under 120 ℃ of vacuum dry 6 hours in advance, gelatin was dissolved in 60 ℃ of deionized waters and is made into the 10wt.% gelatin solution, with LiFePO 4Press mass ratio with gelatin and mix at 80: 20, behind the wet-milling 1h, mixed dope is coated on the aluminium foil, 60 ℃ of vacuumize 24h obtain pole piece.Be assembled into battery with Comparative Examples 1 described method, test result shows that specific discharge capacity is 94.7mAh/g under the 0.5C.Specific discharge capacity is 24.8mAh/g under the 5C.
Embodiment 1:
The pole piece of Comparative Examples 1 preparation is placed in the tube furnace under the nitrogen protection heating rate with 3 ℃/min is warming up to 300 ℃ and keep 1.5h, carry out pre-carbonization; Heating rate with 5 ℃/min is warming up to 600 ℃ then, and keeps 1h, carries out carbonization and obtains pole piece.Its SEM schemes as shown in Figure 2, after the carbonization, and LiFePO 4Still evenly distribute with acetylene black, high temperature because the decomposition and the contraction of gelatin have formed hole not of uniform size on pole piece, these holes will help the infiltration of electrolyte, increases the contact area of electrolyte and active material down, thereby helps the transportation of lithium ion.
Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 145mAh/g under the 0.5C, and specific discharge capacity is 108mAh/g under the 5C.0.5C with its discharge platform under the 5C as shown in Figure 3, discharge platform is steady, discharge platform voltage still can reach 3.3V under 5C.Thereby loose structure helps the transportation that the infiltration of electrolyte helps lithium ion, guarantees under the pole piece globality that the gelatin as binding agent is converted into gelatin-based carbon in carbonisation, has reduced LiFePO greatly 4, the transportation of electronics between acetylene black and collector impedance, thereby high rate performance is improved greatly.
Embodiment 2:
The pole piece of Comparative Examples 1 preparation is placed in the tube furnace under the nitrogen protection heating rate with 3 ℃/min is warming up to 330 ℃ and keep 2h, carry out pre-carbonization; Heating rate with 6 ℃/min is warming up to 500 ℃ then, and keeps 2h, carries out carbonization and obtains pole piece.Its macroscopic view bends picture as shown in Figure 4, and under the bending of tweezers, pole piece can keep good intensity and toughness, breakage occurs and falls the slag phenomenon, has guaranteed the stability of pole piece, has avoided the loss of active material.
Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 142mAh/g under the 0.5C.Specific discharge capacity is 102mAh/g under the 5C.
Embodiment 3:
The pole piece of Comparative Examples 1 preparation is placed in the tube furnace under the nitrogen protection heating rate with 3 ℃/min is warming up to 350 ℃ and keep 2h, carry out pre-carbonization; Heating rate with 5 ℃/min is warming up to 400 ℃ then, and keeps 3h, carries out carbonization and obtains pole piece.
Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 146mAh/g under the 0.5C.Specific discharge capacity is 99mAh/g under the 5C.
Embodiment 4:
The pole piece of Comparative Examples 2 preparation is placed in the tube furnace under the nitrogen protection heating rate with 3 ℃/min is warming up to 300 ℃ and keep 1.5h, carry out pre-carbonization; Heating rate with 4 ℃/min is warming up to 600 ℃ then, and keeps 1.5h, carries out carbonization and obtains pole piece.
Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 143.3mAh/g under the 0.5C.Specific discharge capacity is 107.8mAh/g under the 5C.
Embodiment 5:
The pole piece of Comparative Examples 3 preparation is placed in the tube furnace under the nitrogen protection heating rate with 3 ℃/min is warming up to 330 ℃ and keep 1.5h, carry out pre-carbonization; Heating rate with 3 ℃/min is warming up to 600 ℃ then, and keeps 1h, carries out carbonization and obtains pole piece.
Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 151.2mAh/g under the 0.5C.Specific discharge capacity is 115.6mAh/g under the 5C.
Embodiment 6:
The pole piece of Comparative Examples 4 preparation is placed in the tube furnace under the nitrogen protection heating rate with 3 ℃/min is warming up to 330 ℃ and keep 1.5h, carry out pre-carbonization; Heating rate with 8 ℃/min is warming up to 600 ℃ then, and keeps 1h, carries out carbonization and obtains pole piece.
Be assembled into battery with Comparative Examples 1 described method, Electrochemical results shows that specific discharge capacity is 149.1mAh/g under the 0.5C.Specific discharge capacity is 110.6mAh/g under the 5C.

Claims (4)

1. a carbon coats LiFePO 4Porous positive pole and preparation method thereof is by to the gelatin being traditional LiFePO of binding agent 4Positive pole carries out high-temperature heat treatment makes the method for gelatin original position carbonization obtain carbon coating LiFePO 4The porous positive pole; Concrete steps and condition are:
To with the gelatin LiFePO of binding agent 4Anode pole piece is warming up to 200～350 ℃ gradually under nitrogen protection, carry out pre-carbonization 1.5～3h; Be warming up to 400～600 ℃ more gradually, and keep 1～3h, carry out carbonization; Under nitrogen protection, naturally cool to room temperature then, obtain carbon and coat LiFePO 4The porous positive pole.
2. carbon according to claim 1 coats LiFePO 4The preparation method of porous positive pole is characterized in that: described pre-carburizing temperature is 300 ℃.
3. carbon according to claim 1 coats LiFePO 4The preparation method of porous positive pole is characterized in that: heating rate is 2～10 ℃/min gradually.
4. coat LiFePO according to claim 1 or 2 or 3 described carbon 4The preparation method of porous positive pole is characterized in that: be the LiFePO of binding agent with the gelatin 4Anode pole piece adopts following method preparation: with LiFePO 4, acetylene black and mass concentration 1～20% gelatin solution press LiFePO 4, acetylene black, gelatin 70～85: 0～9: 6～20 mass ratioes mix, and wherein acetylene black is optional ingredient, after wet-milling, mixed dope is coated on the collector aluminium foil, obtains in 60～120 ℃ of vacuumize 2～24h.
CN2011101986902A 2011-07-15 2011-07-15 Carbon coated LiFePO4 porous anode and preparation method thereof Pending CN102299334A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN102517602A (en) * 2011-12-29 2012-06-27 北京化工大学 Gelatin hole forming method for gas diffusion electrodes
CN103346325A (en) * 2013-06-28 2013-10-09 中国科学院宁波材料技术与工程研究所 Lithium ion battery cathode material and preparation method thereof as well as lithium ion battery
CN103956482A (en) * 2014-03-28 2014-07-30 北京理工大学 Preparation method of foamed ferroferric oxide/carbon composite negative electrode material of lithium ion battery
CN108155368A (en) * 2017-12-29 2018-06-12 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods
CN109546103A (en) * 2018-10-25 2019-03-29 北京化工大学 A kind of electrode material and its preparation method and application of binder as carbon precursor
CN110165143A (en) * 2019-05-24 2019-08-23 东莞市安德丰电池有限公司 A kind of lithium battery electrode plate and the preparation method and application thereof
CN113113575A (en) * 2020-01-13 2021-07-13 万华化学集团股份有限公司 Ternary positive electrode material for lithium ion secondary battery and preparation method thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102517602A (en) * 2011-12-29 2012-06-27 北京化工大学 Gelatin hole forming method for gas diffusion electrodes
CN102517602B (en) * 2011-12-29 2014-10-29 北京化工大学 Gelatin hole forming method for gas diffusion electrodes
CN103346325A (en) * 2013-06-28 2013-10-09 中国科学院宁波材料技术与工程研究所 Lithium ion battery cathode material and preparation method thereof as well as lithium ion battery
CN103346325B (en) * 2013-06-28 2015-12-23 中国科学院宁波材料技术与工程研究所 A kind of lithium ion battery negative material, its preparation method and lithium ion battery
CN103956482A (en) * 2014-03-28 2014-07-30 北京理工大学 Preparation method of foamed ferroferric oxide/carbon composite negative electrode material of lithium ion battery
CN103956482B (en) * 2014-03-28 2016-02-17 北京理工大学 A kind of method preparing lithium ion battery foam-like ferroferric oxide/carbon composite negative electrode material
CN108155368A (en) * 2017-12-29 2018-06-12 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods
CN109546103A (en) * 2018-10-25 2019-03-29 北京化工大学 A kind of electrode material and its preparation method and application of binder as carbon precursor
CN110165143A (en) * 2019-05-24 2019-08-23 东莞市安德丰电池有限公司 A kind of lithium battery electrode plate and the preparation method and application thereof
CN113113575A (en) * 2020-01-13 2021-07-13 万华化学集团股份有限公司 Ternary positive electrode material for lithium ion secondary battery and preparation method thereof
CN113113575B (en) * 2020-01-13 2022-07-12 万华化学集团股份有限公司 Ternary positive electrode material for lithium ion secondary battery and preparation method thereof

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Application publication date: 20111228