CN103259013A - Method for improving performance of anode material LiFePO4 for lithium ion cell - Google Patents

Method for improving performance of anode material LiFePO4 for lithium ion cell Download PDF

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CN103259013A
CN103259013A CN2013101389633A CN201310138963A CN103259013A CN 103259013 A CN103259013 A CN 103259013A CN 2013101389633 A CN2013101389633 A CN 2013101389633A CN 201310138963 A CN201310138963 A CN 201310138963A CN 103259013 A CN103259013 A CN 103259013A
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lifepo
electrode
lithium ion
modification
anode material
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邵宗平
吴关
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Nanjing Tech University
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Nanjing Tech University
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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 belongs to the field of a lithium ion cell and provides a method for improving the performance of an anode material LiFePO4 for a lithium ion cell. The method comprises the specific steps of: 1. utilizing a polyhydric alcohol reduction method to prepare a pure-phase LiFePO4 material; 2. uniformly mixing the pure-phase LiFePO4 material and appropriate amount of a carbon precursor in de-ionized water; carrying out drying heat treatment in an air atmosphere at a certain temperature; and 3. carrying out high-temperature heat treatment on powder obtained by the step 2 under an inert atmosphere for a period of time to obtain the nano-grade lithium ion anode material LiFePO4 with uniform flake-shaped appearance, increasing of electron conductivity and improvement of ion diffusion rate. According to the method, the process is simple, and expensive experimental apparatuses are not needed. Intrinsic electronic conductivity and lithium ion diffusion rate of the anode material are improved obviously, so that the electrochemical performance of the anode material is obviously improved.

Description

A kind of raising anode material for lithium-ion batteries LiFePO 4The method of performance
Technical field
The present invention relates to a kind of raising anode material for lithium-ion batteries LiFePO 4The method of performance belongs to the lithium ion battery field.
Background technology
At present, lithium ion battery by widespread usage, and may be played the part of very important role at electric automobile and hybrid-electric car market in consumer electronics product market in the near future.Yet, before large-scale the application, still exist some technical problems to need to be resolved hurrily, the application of lithium ion battery and development depend mainly on its security performance, energy density, durability and cost price, what is particularly worth mentioning is that, select a kind of suitable positive electrode that the performance quality of entire lithium ion battery system is significant.In recent years, LiFePO4 (LiFePO 4) because it has the potentiality that become anode material for lithium-ion batteries of future generation by the careful research of many scientific research groups.With traditional anode material for lithium-ion batteries as LiCoO 2, LiNiO 2And LiMn 2O 4Deng comparing LiFePO 4Have many advantages, for example it has the higher theoretical capacity that reaches 170mAh/g; The suitable charge and discharge platform that is positioned at 3.4-3.5V is arranged; In addition, LiFePO4 also has durability strong, and cost of material is cheap, environmentally friendly and excellent advantages such as high-temperature stability.Yet, since special immanent structure, the LiFePO of monoblock 4Usually present low and slow two shortcomings of lithium ion diffusion rate of electronic conductivity, this has caused capacity to cross result low and the high rate performance difference usually.Generally speaking, there are three kinds of methods commonly used to improve LiFePO 4Electronic conductivity and ions diffusion speed, that is: with conductive carbon material material and LiFePO 4Coat or compound; At LiFePO 4The external metal ion of the high price of mixing in the particle; Reduce LiFePO by optimizing synthetic method or condition 4The particle diameter of particle.Use conductive carbon material and LiFePO 4Compoundly can effectively improve LiFePO usually 4Performance and the Costco Wholesale of material are cheap, therefore have good feasibility, and have been proved to be to improve LiFePO 4One of effective means of electrode kinetics characteristic.Yet, therefore most traditional carbon source and carbon coating technology still can't satisfy the demand of high-performance positive electrode, resemble such novel conductive carbonaceous additive such as Graphene, carbon nano-tube and novel complex method also constantly is used for attempting raising LiFePO with technology 4The performance of electrode.Recently, many scientific researches team attempts with different carbon sources such as amorphous carbon, carbon nano-tube, Graphene etc. LiFePO 4Modify and obtained good effect jointly.For example, utilize the common LiFePO that modifies of amorphous carbon and Graphene 4Material just has been proved to be its performance and has been better than separately by the LiFePO of Graphene or amorphous carbon modification 4Electrode.But these methods relate to the high processing cost mostly, and complicated processing step has improved the production cost of battery greatly.Therefore it is simple to develop a kind of processing step, and cost method of modifying relatively low and that can significantly improve the positive electrode chemical property has very important meaning.
Summary of the invention
The objective of the invention is for solving present LiFePO 4The intrinsic electronic conductivity that positive electrode is extremely low and the problem of lithium ion diffusion rate, and a kind of raising anode material for lithium-ion batteries LiFePO is provided 4The method of performance, this method are passed through different material with carbon elements to LiFePO 4Positive electrode is modified, thereby significantly improves its cycle performance and high rate performance, need not to use the auxiliary equipment of complexity and high price in preparation process, and technology simply is easy to repeat preparation.
Technical scheme of the present invention is: a kind of raising anode material for lithium-ion batteries LiFePO 4The method of performance, its concrete steps are as follows:
A, utilize polyol reduction method, raw material is mixed in polyalcohol and boiling reflux prepares the LiFePO of pure phase 4Material; B, with the pure phase LiFePO for preparing 4Mix in deionized water with different material with carbon element presomas and in air atmosphere, carry out dry heat handle powder; C, with powder high-temperature heat treatment under inert atmosphere of step B gained, the lithium ion anode LiFePO after obtaining namely that different material with carbon elements are common and modifying 4Material.
The LiFePO of pure phase among the preferred steps A 4Material adopts conventional polyol reduction method preparation, i.e. the stoichiometric proportion of product according to target is with raw material Fe (CH 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) mixes in polyalcohol and boiling reflux prepares the LiFePO of pure phase 4Material; Preferred described polyalcohol is a kind of in diethylene glycol (DEG), triethylene glycol or the tetraethylene glycol; The time of the boiling reflux described in the preferred steps A is 12-32h.
Different material with carbon element presomas described in the preferred steps B are one or more in glucose, carbon nano-tube or the graphene oxide (with disclosed Hummer method preparation now).
Baking temperature described in the preferred steps B is 50-120 ° of C, and be 12-24h drying time.Inert gas described in the preferred steps C is a kind of in argon gas, helium or the xenon.Heat treatment temperature described in the preferred steps C is 600-800 ° of C; Heat treatment time is 1-3h.
Different material with carbon element quality described in the preferred steps C account for the lithium ion anode LiFePO after the modification 4The 3-8% of quality of materials.
The present invention adopts traditional electrochemistry cyclic voltammetric method of testing and AC impedance spectrometry to the test of the chemical property of anode electrode.Electrochemistry cyclic voltammetric (CV) test condition: work electrode is diameter 14mm(S=1.54cm 2) unmodified processing or the positive pole of modification after handling, be the lithium sheet to electrode; Electrolyte is to be solvent with the ethylene carbonate of volume ratio 1:1 (EC) and dimethyl carbonate (DMC), and concentration is 1molL -1LiPF 6Solution; Sweep limits: 2.0V～4.0V sweeps speed: 0.1-1mV/s.Electrochemical impedance (EIS) test condition: work electrode is diameter 14mm(S=1.54cm 2) unmodified processing or the positive pole of modification after handling, be the lithium sheet to electrode; Electrolyte is to be solvent with the ethylene carbonate of volume ratio 1:1 (EC) and dimethyl carbonate (DMC), and concentration is 1mol L -1LiPF 6Solution; Measuring frequency scope: 5mHz-100kHz adds AC signal amplitude: 10mV.
The present invention also carries out the half-cell charge-discharge test to anode electrode.Its test condition is: work electrode is diameter 14mm(S=1.54cm 2) unmodified processing or the positive pole of modification after handling, be the lithium sheet to electrode; Electrolyte is to be solvent with the ethylene carbonate of volume ratio 1:1 (EC) and dimethyl carbonate (DMC), and concentration is 1mol L -1LiPF 6Solution; Charging/discharging voltage scope: 2.5-4.0V; Charging and discharging currents multiplying power: 0.1-20C.
Beneficial effect:
The resultant LiFePO that is modified by different material with carbon elements of the present invention 4Positive electrode has uniform sheet pattern, compare with not modified positive electrode have higher electronic conductivity, more outstanding lithium ion diffusion rate, in lithium ion battery, show better cycle ability and high rate performance.
Description of drawings
Fig. 1 is the LiFePO before embodiment 1 modification is handled 4The resulting LiFePO in back is handled in positive electrode (a) and modification 4The microscopic appearance comparison diagram of positive electrode (b);
Fig. 2 is LiFePO before embodiment 1 modification is handled 4The charging curve (1) of electrode under the 0.1C multiplying power handled the resulting LiFePO in back with discharge curve (1 ') and modification 4The charging curve (2) of electrode under the 0.1C multiplying power and discharge curve (2 ') comparison diagram;
Fig. 3 is LiFePO before embodiment 1 modification is handled 4Electrode (1) is handled the resulting LiFePO in back with modification 4The electrochemistry cyclic voltammetric characteristic comparison diagram of electrode (2);
Fig. 4 is LiFePO before embodiment 1 modification is handled 4Electrode (1) is handled the resulting LiFePO in back with modification 4The electrochemical impedance characteristic comparison diagram of electrode (2);
Fig. 5 is that the resulting LiFePO in back is handled in embodiment 2 modifications 4The discharge curve of electrode under each multiplying power of 0.1-20C;
Fig. 6 is LiFePO before embodiment 2 modifications are handled 4Electrode (1) is handled the resulting LiFePO in back with modification 4The electrochemistry cyclic voltammetric characteristic comparison diagram of electrode (2).
Embodiment
Embodiment 1
This experiment realizes by following steps: one, be the Fe (CH of 1:1:1 by stoichiometric proportion 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) in triethylene glycol (Triethylene glycol, be called for short TEG) mixes and boiling reflux 16h prepares the LiFePO of pure phase 4Material; Two, with deionized water with pure phase LiFePO 4Mix (the Graphene mass fraction is 2% in the final gained electrode material, and the carbon nano-tube mass fraction is 3%, and namely total carbon content is 5%) with graphene oxide and carbon nano-tube, dry 24h under 60 ° of C in air; Three, with powder 700 ° of C high-temperature heat treatment 2h in argon gas of step 2 gained.
Fig. 1 is the LiFePO before modification is handled 4The resulting LiFePO in back is handled in positive electrode (a) and modification 4The microscopic appearance comparison diagram of positive electrode (b), as can be seen from the figure, (a) in the pure phase LiFePO of doped graphene and carbon nano-tube not 4Material presents the sheet pattern, and its average grain diameter agglomeration do not occur about 500nm, by LiFePO after the common modification of passing through Graphene and carbon nano-tube in (b) as can be known 4The not too big change of the sheet pattern of particle and particle diameter can be seen graphene film being distributed in the sample and LiFePO at random simultaneously 4The closely contact of the surface of particle, and carbon nano-tube also is present in the sample equably and adhere to or penetrate sheet LiFePO 4Particle, the carbon nano-tube in the material and graphene film all interlaced with each other and will be independently LiFePO 4Particle couples together, thereby has formed the conductive network of an inside and external mix, and this high-effective conductive network not only can accelerate electrical conductivity also for the diffusion process of lithium ion provides more passage, finally cause more outstanding chemical property.
Fig. 2 is LiFePO before embodiment 1 modification is handled 4The charging curve (1) of electrode under the 0.1C multiplying power handled the resulting LiFePO in back with discharge curve (1 ') and modification 4The charging curve (2) of electrode under the 0.1C multiplying power and discharge curve (2 ') comparison diagram, as can be seen from the figure, the specific discharge capacity of electrode is that the electrode discharge specific capacity after 134mAh/g and modification are handled is 166mAh/g before the modification, and LiFePO after the modification of passing through the hybrid conductive network that Graphene and carbon nano-tube form be described 4The specific capacity of electrode has obtained significantly promoting.
Fig. 3 is LiFePO before modification is handled 4Electrode (1) is handled the resulting LiFePO in back with modification 4The electrochemistry cyclic voltammetric characteristic comparison diagram of electrode (2) has among the figure can observe, a pair of redox peak correspondence all appears in two curves in the electrode lithium ion embed/take off the two phase reaction of embedding.Wherein, the oxidation peak of electrode and reduction peak appear at 3.69 and the 3.22V place respectively before the modification, and the peak-to-peak voltage difference of redox is 0.47V; The oxidation peak of modification rear electrode and reduction peak appear at 3.53 and the 3.36V place respectively, and the peak-to-peak voltage difference of redox is 0.17V.Illustrate that the hybrid conductive network of Graphene and carbon nano-tube composition has increased the invertibity of electrode reaction, has reduced polarity of electrode and has also finally showed by the electrode material after the modification more outstanding specific capacity and high rate performance.
Fig. 4 is LiFePO before modification is handled 4Electrode (1) is handled the resulting LiFePO in back with modification 4The electrochemical impedance characteristic comparison diagram of electrode (2).By among the figure as can be known, the impedance spectrum of two electrodes represents the semicircle of electrode and the impedance of electrolyte interface charge-conduction by high-frequency region and oblique line that low frequency part represents the Warburg impedance is formed.By among the figure as can be known, the conduction resistance of modification rear electrode only is～720ohm, and before the modification conduction resistance of electrode up to～1690ohm, explanation is after the modification of the hybrid conductive network that process is made up of Graphene and carbon nano-tube, the charge-conduction impedance of electrode has significantly been reduced, and namely the electronic conductivity of electrode has had significantly raising.
Embodiment 2
This experiment realizes by following steps: one, be the Fe (CH of 1:1:1 by stoichiometric proportion 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) in triethylene glycol (Triethylene glycol, be called for short TEG) mixes and boiling reflux 32h prepares the LiFePO of pure phase 4Material; Two, with deionized water with pure phase LiFePO 4Mix (the Graphene mass fraction is 1% in the final gained electrode material, and amorphous carbon quality mark is 2%, and namely total carbon content is 3%) with graphene oxide and glucose, dry 16h under 80 ° of C in air; Three, with powder 600 ° of C high-temperature heat treatment 3h in argon gas of step 2 gained.
LiFePO after modification is handled 4Electrode, electronic conductivity and ions diffusion speed significantly improve, and charge transport capability significantly increases, and cycle performance and high rate performance obviously improve.Fig. 5 is that the resulting LiFePO in back is handled in modification 4The discharge curve of electrode under each multiplying power of 0.1-20C, by among the figure as can be known, the anode electrode after modification under each multiplying power all has smooth discharge platform and suitable discharge potential, 0.1,0.5,1,5, its specific discharge capacity is respectively 152,136 under 10, the 20C multiplying power, 125,91,82,59mAh/g.Illustrate through LiFePO after the common modification of amorphous carbon and Graphene 4Electrode is the equal outstanding chemical property of tool under each multiplying power.
Fig. 6 is LiFePO before modification is handled 4Electrode (1) is handled the resulting LiFePO in back with modification 4The electrochemistry cyclic voltammetric characteristic comparison diagram of electrode (2), the peak point current of modification rear electrode than modification before the peak point current height of electrode, and the peak-to-peak voltage difference of modification rear electrode redox is 0.19V, and before the modification anodizing to reduce peak-to-peak voltage difference be 0.50V.This explanation LiFePO after mixed amorphous carbon and Graphene 4Polarization of electrode has reduced, and lithium ion embeds/take off embedding reaction invertibity to have strengthened.
Embodiment 3
This experiment realizes by following steps: one, be the Fe (CH of 1:1:1 by stoichiometric proportion 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) mixes in tetraethylene glycol and boiling reflux 12h prepares the LiFePO of pure phase 4Material; Two, with deionized water with pure phase LiFePO 4Mix (final gained electrode material in total carbon content be 4%) with glucose, dry 24h under 50 ° of C in air; Three, with powder 800 ° of C high-temperature heat treatment 1h in nitrogen of step 2 gained.The result shows, and compares the LiFePO after modification is handled before modification is handled 4Electrode electronic conductivity and lithium ion diffusion rate obviously improve, and specific discharge capacity also is largely increased.
Embodiment 4
This experiment realizes by following steps: one, be the Fe (CH of 1:1:1 by stoichiometric proportion 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) mixes in diethylene glycol (DEG) and boiling reflux 24h prepares the LiFePO of pure phase 4Material; Two, with deionized water with pure phase LiFePO 4Mix (final gained electrode material in total carbon content be 8%) with carbon nano-tube, dry 18h under 120 ° of C in air; Three, with powder 750 ° of C high-temperature heat treatment 1.5h in argon gas of step 2 gained.Electrochemistry cyclic voltammetric characteristic test result shows, compare with untreated electrode, the peak-to-peak voltage difference of redox of the electrode after modification is handled has been reduced to 0.23V by original 0.50V, the two phase reaction invertibity that discharges and recharges that the modification rear electrode then is described has improved, and charge transfer resistance also reduces (having reduced to about 950 Ω by 1690 Ω before handling) to some extent simultaneously.
Embodiment 5
This experiment realizes by following steps: one, be the Fe (CH of 1:1:1 by stoichiometric proportion 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) in triethylene glycol (Triethylene glycol, be called for short TEG) mixes and boiling reflux 20h prepares the LiFePO of pure phase 4Material; Two, with deionized water with pure phase LiFePO 4Mix (final gained electrode material in total carbon content be 6%) with graphene oxide, dry 16h under 100 ° of C in air; Three, with powder 650 ° of C high-temperature heat treatment 2.5h in argon gas of step 2 gained.The result shows, the electrode after modification is handled and the LiFePO before the processing 4Electrode is compared, and charge transport capability improves a lot, and specific discharge capacity has improved approximately 35% under the 0.1C multiplying power, improves about 32% in 1C multiplying power setting point specific capacity.
Embodiment 6
This experiment realizes by following steps: one, be the Fe (CH of 1:1:1 by stoichiometric proportion 3COO) 24H 2It is pure that O(analyzes), LiCH 3COO2H 2O(analyzes pure) and NH 4H 2PO 4(analyzing pure) mixes in tetraethylene glycol and boiling reflux 28h prepares the LiFePO of pure phase 4Material; Two, with deionized water with pure phase LiFePO 4Mix (the carbon nano-tube mass fraction is 2% in the final gained electrode material, and amorphous carbon quality mark is 5%, and namely total carbon content is 7%) with carbon nano-tube and glucose, dry 22h under 90 ° of C in air; Three, with powder 750 ° of C high-temperature heat treatment 2.5h in xenon of step 2 gained.The charge-discharge test result shows, the electrode after modification is handled and the LiFePO before the processing 4Electrode compares that specific discharge capacity has improved 28% under the 1C multiplying power; Electrochemistry cyclic voltammetric characteristic test result shows, the electrode after modification is handled and the LiFePO before the processing 4Electrode is compared the peak-to-peak voltage difference of redox and is reduced, and illustrates that the invertibity of electrode reaction has improved.

Claims (8)

1. one kind is improved anode material for lithium-ion batteries LiFePO 4The method of performance, its concrete steps are as follows:
A, utilize polyol reduction method, raw material is mixed in polyalcohol and boiling reflux prepares the LiFePO of pure phase 4Material; B, with the pure phase LiFePO for preparing 4Mix in deionized water with different material with carbon element presomas and in air atmosphere, carry out dry heat handle powder; C, with powder high-temperature heat treatment under inert atmosphere of step B gained, the lithium ion anode LiFePO after obtaining namely that different material with carbon elements are common and modifying 4Material.
2. method according to claim 1 is characterized in that the polyalcohol described in the steps A is a kind of in diethylene glycol (DEG), triethylene glycol or the tetraethylene glycol.
3. method according to claim 1, the time that it is characterized in that the boiling reflux described in the steps A is 12-32h.
4. method according to claim 1 is characterized in that the different material with carbon element presomas described in the step B are one or more in glucose, carbon nano-tube or the graphene oxide.
5. method according to claim 1 is characterized in that the baking temperature described in the step B is 50-120 ° of C, and be 12-24h drying time.
6. method according to claim 1 is characterized in that the inert gas described in the step C is a kind of in argon gas, helium or the xenon.
7. method according to claim 1 is characterized in that the heat treatment temperature described in the step C is 600-800 ° of C; Heat treatment time is 1-3h.
8. method according to claim 1 is characterized in that the different material with carbon element quality described in the step C account for lithium ion anode LiFePO 4The 3-8% of quality of materials.
CN2013101389633A 2013-04-19 2013-04-19 Method for improving performance of anode material LiFePO4 for lithium ion cell Pending CN103259013A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104716320A (en) * 2015-03-10 2015-06-17 中国科学院过程工程研究所 Composite-coated lithium iron phosphate, preparation method of composite-coated lithium iron phosphate, and lithium ion battery
CN108807904A (en) * 2018-06-12 2018-11-13 四会市恒星智能科技有限公司 A kind of preparation method of lithium battery modified phosphate iron lithium anode material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曹雁冰ET AL: "多元醇还原法合成锂离子电池正极材料LiFePO4", 《无机化学学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104716320A (en) * 2015-03-10 2015-06-17 中国科学院过程工程研究所 Composite-coated lithium iron phosphate, preparation method of composite-coated lithium iron phosphate, and lithium ion battery
US10243211B2 (en) 2015-03-10 2019-03-26 Institute Of Process Engineering, Chinese Academy Of Sciences Composite-coated lithium iron phosphate and preparation method therefor, and lithium ion battery
CN108807904A (en) * 2018-06-12 2018-11-13 四会市恒星智能科技有限公司 A kind of preparation method of lithium battery modified phosphate iron lithium anode material
CN108807904B (en) * 2018-06-12 2021-02-05 信丰永冠塑电科技有限公司 Preparation method of modified lithium iron phosphate cathode material for lithium battery

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Application publication date: 20130821