CN101237036B - Making method for positive material LiFePO4 of poly-aniline coated lithium ion battery - Google Patents
Making method for positive material LiFePO4 of poly-aniline coated lithium ion battery Download PDFInfo
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- CN101237036B CN101237036B CN2008100305146A CN200810030514A CN101237036B CN 101237036 B CN101237036 B CN 101237036B CN 2008100305146 A CN2008100305146 A CN 2008100305146A CN 200810030514 A CN200810030514 A CN 200810030514A CN 101237036 B CN101237036 B CN 101237036B
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- ion battery
- lifepo
- lithium ion
- poly
- aniline
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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 discloses a method for preparing polyaniline coating Li-ion battery anode material LiFePO4. The method is coating polyaniline on the in-situ surface of the powder of Li-ion battery anodematerial LiFePO4. The method has the following favorable effects: the discharging voltage platform of the polyaniline coating anode material LiFePO4obtained is stable, the battery has higher specificcapacity up to one hundred and forty point three mAh/g, the granularity is distributed evenly, the grains are in good appearance and high in discharging capacity and long in cycling life, etc.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries.
Background technology
Lithium ion battery is the new generation of green high-energy battery of performance brilliance, has become one of emphasis of hi-tech development.It with its high voltage, high power capacity, low consumption, memory-less effect, nuisanceless, volume is little, internal resistance is little, self discharge is few, cycle-index is many etc., and distinguishing feature is shown one's talent in numerous batteries.The application of lithium ion battery constantly enlarges, and it is used and has been penetrated into numerous civilian and military fields such as comprising phone, notebook computer, video camera, digital camera at present.In addition, also competitively developing automobile, the high capacity lithium ion battery that aspects such as space flight and energy storage are required both at home and abroad.Positive electrode is the important component part of lithium ion battery.At present, the positive electrode that is applied to lithium ion battery mainly is the embedding lithium transition-metal oxide, mainly uses stratiform LiCoO
2, this material is used widely in compact battery, but except the restraining factors of cobalt resource, overcharges insecurity and determined it not to be applied in high capacity cell.People expect spinelle LiMn
2O
4Can be with its inexpensive and relative LiCoO
2The advantage of safety plays a role in high capacity cell, but the solution that does not always find at its capacity shortcoming low and the high temperature cyclic performance difference, so still can not in actual battery, promote.LiNiO
2Cost is lower, and capacity is higher, but the preparation difficulty, there are comparatively serious safety problem in the consistency of material property and poor reproducibility.Therefore, seek the desirable positive electrode active materials of lithium ion battery from resource, environmental protection and security performance aspect, be still the research focus of quite a while World chemical power supply circle from now on.The lithium iron phosphate positive material of quadrature olivine structural becomes new research focus both at home and abroad gradually.LiFePO
4Concentrated LiCoO
2, LiNiO
2, LiMn
2O
4The advantage separately that waits material: do not contain noble element, raw material cheapness, aboundresources; Operating voltage moderate (3.4V); Platform identity is good, and voltage pole is (can match in excellence or beauty with stabilized voltage power supply) steadily; Theoretical capacity big (170mAh/g); Stability Analysis of Structures, security performance is splendid; High-temperature behavior and good cycle; Volume-diminished during charging, the bulk effect when cooperating with carbon negative pole material is good; Good with most of electrolyte system compatibilities, storge quality is good; Nontoxic, be real green material.LiFePO
4Positive electrode room temperature electronic conductivity is low, and its electrode behavior is subjected to diffusion control how to improve LiFePO under room temperature and high current density condition
4Actual capacity be that the researcher is making great efforts a difficult problem of capturing always.Research work in recent years mainly launches around following 3 aspects: the size of (1) improvement synthetic method control product particle and pattern (2) are at LiFePO
4Particle surface coated with conductive material improves conductive capability (3) ion doping of composite material to improve LiFePO
4Electronic conductivity.Polyaniline is a kind of conducting polymer, and the polyaniline conductivity behind the protonic acid doping can reach 1-10S/cm, and polyaniline has reversible redox property, can be used as the electrode material of secondary cell.At LiFePO
4The surface coats polyaniline can improve its conductance, and polyaniline also participates in electrode reaction simultaneously, and the coating of polyaniline not only can improve LiFePO
4Initial discharge capacity, the improvement of its cycle performance is had effect more significantly.Up to now, adopt in-situ polymerization to coat polyaniline and do not see bibliographical information as yet at the LiFePO4 particle surface.
Summary of the invention
The purpose of this invention is to provide a kind of discharge capacity height, the anode material for lithium-ion batteries that has extended cycle life.
The objective of the invention is to realize in the following way: a kind of poly-aniline coated lithium ion battery positive electrode LiFePO
4The preparation method:
At anode material for lithium-ion batteries LiFePO
4The surface in situ of powder coats polyaniline.
Get Fe (NO
3)
39H
2O, Li (CH
3COO) 2H
2O is dissolved in the distilled water, adds excessive HOCH
2COOH adds stoichiometric proportion (Fe (NO again
3)
39H
2O, Li (CH
3COO) 2H
2O, NH
4H
2PO
4The amount of substance ratio be 1: 1: 1) NH
4H
2PO
4, get gel with ammoniacal liquor adjust pH to 8.5～9.2,60～80 ℃ of insulation 10～24h, heating gained gel, inert gas shielding, in 300～500 ℃ of following predecomposition 3～12h, compressing tablet is ground in the cooling back.Calcine 12～24h down at 600～800 ℃ and obtain LiFePO
4
With LiFePO
4Powder joins in the Bronsted acid and stirs, and adds aniline monomer and stirs, dropping oxidizing agent drips of solution, reaction temperature-5～25 ℃; continue to stir, inert gas shielding was reacted after 2～24 hours, stopped to stir; filter, wash to filtrate colourlessly, drying obtains the LiFePO that polyaniline coats
4
Described Bronsted acid is a kind of in hydrochloric acid, sulfuric acid, perchloric acid, phosphoric acid, nitric acid, p-methyl benzenesulfonic acid or the DBSA.
Bronsted acid concentration is 0.1～2mol/L.
The concentration ratio of Bronsted acid concentration and aniline monomer is 1: 1～10: 1.
Described oxidant is a kind of in ammonium persulfate, potassium bichromate, potassium hyperchlorate or the ferric trichloride.
The mol ratio of described oxidant and aniline monomer is 0.25: 1～2: 1.
Described oxidant is a solution with the hydrochloric acid solution of distilled water or 0.1～10mol/L in use, is made into the solution that concentration is 0.1mol/L～10mol/L, drips in aniline monomer solution.
Inert gas is nitrogen, argon gas.
The present invention has following beneficial effect, the LiFePO that resultant polyaniline coats
4The anode material discharging voltage platform is stable, has higher specific capacity, reaches 140.3mAh/g, and has even particle size distribution, and granule-morphology is good, the discharge capacity height, and characteristics such as have extended cycle life.
Description of drawings
Fig. 1 is the LiFePO that polyaniline of the present invention coats
4With pure LiFePO
4The discharge curve of contrast during with the 0.1C rate charge-discharge;
Fig. 2 is the LiFePO that polyaniline of the present invention coats
4With pure LiFePO
4The cycle performance figure of contrast during with the 1C rate charge-discharge;
Fig. 3 is the LiFePO that polyaniline of the present invention coats
4Sem photograph;
Embodiment
The present invention will be further described below in conjunction with embodiment:
Accurately take by weighing Li by stoichiometric proportion
2CO
3, FeC
2O
42H
2O, (NH
4)
2HPO
4, placing ball grinder, the ratio of sizes of balls is 1: 4, ball milling 10 hours is even to batch mixing.Then reactant is placed quartz boat, put into tube furnace and under argon shield, heat up.Earlier be warming up to 300 ℃ with 5 ℃/min, naturally cool to room temperature behind the constant temperature 8h, taking-up places tube furnace to rise to 700 ℃ with 10 ℃/min after grinding once more, and natural cooling behind the insulation 20h obtains LiFePO
4Take by weighing 4 gram LiFePO
4Powder joins among the HCl of 0.1mol/L and stirred 30 minutes, adds the 1mL aniline monomer and stirs 30 minutes, and 1.28 gram ammonium persulfates are dissolved among the HCl of 0.1mol/L and dropwise join in the mixed solution, react under the room temperature, continue to stir nitrogen protection.React after 12 hours, stop to stir, filter, wash to filtrate colourless.60 ℃ of dryings of vacuum obtain the LiFePO that polyaniline coats then
4With the lithium sheet is negative pole, records the LiFePO that this polyaniline coats
4First discharge specific capacity at room temperature is 138.5mAh/g.
Accurately take by weighing Fe (NO by stoichiometric proportion
3)
39H
2O, Li (CH
3COO) 2H
2O is dissolved in the distilled water, adds excessive HOCH
2COOH is with Fe
3+Be reduced into Fe
2+, add the NH of stoichiometric proportion again
4H
2PO
4, to 8.5-9.2,60 ℃ of insulation 24h get gel with the ammoniacal liquor adjust pH, heating gained gel, and argon shield, in 300 ℃ of following predecomposition 3h, compressing tablet is ground in the cooling back.Calcine 20h down at 600 ℃, obtain LiFePO
4Sample.Take by weighing 4 gram LiFePO
4Powder joins among the HCl of 0.1mol/L and stirred 30 minutes, adds the 1mL aniline monomer and stirs 30 minutes, and 1.28 gram ammonium persulfates are dissolved among the HCl of 0.1mol/L and dropwise join in the monomer solution, react under the room temperature, continue to stir nitrogen protection.React after 12 hours, stop to stir, filter, wash to filtrate colourless.60 ℃ of dryings of vacuum obtain the LiFePO4 that polyaniline coats then.With the lithium sheet is negative pole, and recording the LiFePO4 first discharge specific capacity at room temperature that this polyaniline coats is 140.3mAh/g, and capacity still is 118.7mAh/g after the 1C circulation 50 times.
Prepare LiFePO by embodiment 1 identical condition
4Take by weighing 4.5 gram LiFePO
4Powder joins among the HCl of 2mol/L and stirred 30 minutes, adds the 0.5mL aniline monomer and stirs 30 minutes, and 0.64 gram ammonium persulfate is dissolved among the HCl of 2mol/L and dropwise joins in the monomer solution, reacts under the room temperature, continues to stir nitrogen protection.React after 6 hours, stop to stir, filter, wash to filtrate colourless.60 ℃ of dryings of vacuum obtain the LiFePO4 that polyaniline coats then.With the lithium sheet is negative pole, and recording the LiFePO4 first discharge specific capacity at room temperature that this polyaniline coats is 133mAh/g, and capacity still is 110mAh/g after the 1C circulation 50 times.
Prepare LiFePO by embodiment 1 identical condition
4Take by weighing 4 gram LiFePO
4Powder joins in the neopelex solution and stirred 30 minutes, adds the 1mL aniline monomer and stirs 30 minutes, and 2.92 gram ferric trichlorides are dissolved in the 40mL distilled water and dropwise join then in the monomer solution, react under the room temperature, continue to stir nitrogen protection.React after 6 hours, stop to stir, filter, wash to filtrate colourless.60 ℃ of dryings of vacuum obtain the LiFePO4 that polyaniline coats then.With the lithium sheet is negative pole, and the LiFePO4 first discharge specific capacity at room temperature that records this polyaniline coating is 138mAh/g.
Claims (8)
1. poly-aniline coated lithium ion battery positive electrode LiFePO
4The preparation method, it is characterized in that: at anode material for lithium-ion batteries LiFePO
4The surface in situ of powder coats polyaniline; Get Fe (NO
3)
39H
2O, Li (CH
3COO) 2H
2O is dissolved in the distilled water, adds excessive HOCH
2COOH presses Fe (NO
3)
39H
2O, Li (CH
3COO) 2H
2O, NH
4H
2PO
4The amount of substance ratio be that 1: 1: 1 ratio adds NH
4H
2PO
4, get gel with ammoniacal liquor adjust pH to 8.5～9.2,60～80 ℃ of insulation 10～24h, heat the gained gel, inert gas shielding, in 300～500 ℃ of following predecomposition 3～12h, compressing tablet is ground in the cooling back, calcines 12～24h down at 600～800 ℃ and obtains LiFePO
4With LiFePO
4Powder joins in the Bronsted acid and stirs, and adds aniline monomer and stirs, dropping oxidizing agent drips of solution, reaction temperature-5～25 ℃; continue to stir, inert gas shielding was reacted after 2～24 hours, stopped to stir; filter, wash to filtrate colourlessly, drying obtains the LiFePO that polyaniline coats
4
2. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: described Bronsted acid is a kind of in hydrochloric acid, sulfuric acid, perchloric acid, phosphoric acid, nitric acid, p-methyl benzenesulfonic acid or the DBSA.
3. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: Bronsted acid concentration is 0.1～2mol/L.
4. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: the concentration ratio of Bronsted acid concentration and aniline monomer is 1: 1～10: 1.
5. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: described oxidant is a kind of in ammonium persulfate, potassium bichromate, potassium hyperchlorate or the ferric trichloride.
6. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: the mol ratio of described oxidant and aniline monomer is 0.25: 1～2: 1.
7. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: described oxidant is a solution with the hydrochloric acid solution of distilled water or 0.1～10mol/L in use, is made into the solution that concentration is 0.1mol/L～10mol/L, drips in aniline monomer solution.
8. a kind of poly-aniline coated lithium ion battery positive electrode LiFePO according to claim 1
4The preparation method, it is characterized in that: inert gas is nitrogen, argon gas.
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| CN102569767B (en) * | 2012-01-19 | 2015-02-18 | 中国科学院过程工程研究所 | Polymer composite lithium titanate electrode material and preparation method thereof |
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| US11870062B2 (en) * | 2017-11-20 | 2024-01-09 | Lg Energy Solution, Ltd. | Metal oxide coated with conductive polymer, electrode for electrochemical device comprising the same, and method of producing the metal oxide |
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