CN103746094A - C-LiFePO4/PTPAn composite material, its application and lithium battery produced by composite material thereof - Google Patents
C-LiFePO4/PTPAn composite material, its application and lithium battery produced by composite material thereof Download PDFInfo
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- CN103746094A CN103746094A CN201310689063.8A CN201310689063A CN103746094A CN 103746094 A CN103746094 A CN 103746094A CN 201310689063 A CN201310689063 A CN 201310689063A CN 103746094 A CN103746094 A CN 103746094A
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- lifepo
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- triphenylamine
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- 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 provides a C-LiFePO4/PTPAn composite material, its application and a lithium battery produced by the composite material thereof. The C-LiFePO4/PTPAn composite material is characterized by taking a carbon-coated LiFePO4 material and PTPAn as raw materials and prepared by a solution blending method. The C-LiFePO4/PTPAn composite material which is taken as a lithium ion batteries cathode material has good charge and discharge performances, cycle stability and high magnification performance.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of C-LiFePO
4/ PTPAn composite material and as the application of anode material of lithium battery and the lithium ion battery making thus.
Background technology
Along with further developing of human society, the energy problem that the whole world faces, resource problem, environmental problem are also on the rise.Because current energy resource structure is built in petrochemical industry substantially, so expect on the basis of (oil, coal, natural gas), this has not only caused the exhaustion of resource also to pollute environment.And electric energy because it is clean, safety and conveniently will play the part of more and more important role in future.Therefore the lithium ion battery that, has good mobility and a convenient accumulate supply power mode in future plays a part very important by take electric energy in basic society.
Traditional anode material for lithium-ion batteries mainly adopts transition metal oxide, as oxide of cobalt-lithium oxide, nickel oxide lithium, manganese oxide lithium and vanadium etc., these materials mainly be take noble metal as main, often have the defects such as mineral resources are limited, price is high, contaminated environment, preparation cost height.Therefore,, for the sustainable development of human society, it is particularly crucial that research and development novel high-performance electrochemical power source and material just become.LiFePO
4although positive electrode is compared with other materials, have very large advantage, himself still exists many defects, as the electronic conductivity of material and ion diffusion rate low, cause high-rate charge-discharge capability poor, therefore need to carry out study on the modification to it.At present, address the above problem and mainly contain two kinds of approach: improve LiFePO
4that the research of electronic conductivity mainly concentrates on is metal-doped, metal ion mixing, carbon is coated and the coated several respects in organic conducting polymer surface; Improving ion diffusion rate is mainly to control synthesis condition, may obtain that complete in crystal formation, structure are single, the LiFePO of grain refine
4.
Conducting polymer is because himself good conductivity and electro-chemical activity have caused people's extensive concern.In recent years, along with the progress of conductive polymer molecules design and fabrication technology, conducting polymer is applied to as positive electrode the very big interest that lithium ion battery field has caused people.The existing similar poly-high electronic conductivity skeleton to benzene (PPP) of poly-triphenylamine (PTPAn), the high-energy-density that possesses again polyaniline (PAn) unit, the porous framework structure of poly-triphenylamine makes poly-triphenylamine have ultrafast electron transfer rate constant and remarkable ion transportation ability, so poly-triphenylamine shows stable cycle performance as positive electrode; The free oxidation reduction center of while poly-triphenylamine inside is stable and is subject to the frame protection of polymer inside; even if make poly-triphenylamine still embody superior charge-discharge performance under high power charging-discharging condition; but due to its theoretical capacity (109mAh/g) on the low side, limited it separately as the application of anode material of lithium battery.
As positive electrode, inorganic nano LiFePO
4the electronics that positive electrode is inside and outside and Li
+diffusion and transmission rate low be the subject matter that affects lithium battery performance.And organic conducting polymer poly-triphenylamine has and LiFePO at 3.5V place as positive electrode
4similar stable charging/discharging voltage platform, its loose structure is more conducive to Li
+diffusion, as lithium ion battery material, show superior stable circulation performance and high-rate charge-discharge capability.Consider LiFePO
4with the pluses and minuses of poly-triphenylamine, the present invention adopt a small amount of poly-triphenylamine by solution blended process to C-LiFePO
4modifying surface, wishes to utilize the distinctive porous framework of poly-triphenylamine by C-LiFePO
4material construction becomes electronics network structure, makes up LiFePO
4as the defect of positive electrode, improve the lithium ion migration rate of material, thereby improve LiFePO
4chemical property as positive electrode.
Summary of the invention
First object of the present invention is to provide a kind of C-LiFePO
4/ PTPAn composite material, this composite material has good charge-discharge performance, cyclical stability and high rate capability.
Second object of the present invention is to provide described C-LiFePO
4/ PTPAn composite material is as the application of anode material for lithium-ion batteries.
The 3rd object of the present invention is to provide by described C-LiFePO
4the lithium ion battery that/PTPAn composite material makes as positive electrode.
For achieving the above object, the present invention has adopted following technical scheme:
The invention provides a kind of C-LiFePO
4/ PTPAn composite material, described C-LiFePO
4/ PTPAn composite material is with the coated LiFePO of carbon
4material and poly-triphenylamine are raw material, by solution blended process, make.
In the present invention, the LiFePO that carbon is coated
4material is to take sucrose as carbon source, makes LiFePO
4mix with a certain amount of sucrose, at N
2in heat-treat and obtain, heat-treat condition is as follows: first with the preferred 5 ℃/min of 2-10 ℃/min() speed by room temperature, rise to 250-400 ℃ (preferably 350 ℃), the preferred 1h of insulation 0.5～2h(), again with the preferred 5 ℃/min of 2-10 ℃/min() speed be warming up to 500-700(preferably 650) ℃, sintering 2～10 hours (preferably 5 hours).Preferably, sucrose quality is LiFePO
42～10% of quality, more preferably 8%.
In the present invention, poly-triphenylamine makes according to conventional chemical oxidization method, and wherein oxidant is iron chloride.
Further, described C-LiFePO
4mass content≤20% of poly-triphenylamine in/PTPAn composite material, is preferably 3～20%, and more preferably 5～15%, more preferably 10%.
Further, described solution blended process is specially: make the coated LiFePO of carbon
4material and poly-triphenylamine fully disperse in solvent, and then solvent evaporated, is drying to obtain C-LiFePO
4/ PTPAn composite material; Described solvent is selected from halogenated hydrocarbon solvent or phenols reagent.
Further, described solvent is preferably chloroform or cresols.
The present invention also provides described C-LiFePO
4/ PTPAn composite material is as the application of anode material of lithium battery, and concrete application process adopts routine operation.
Compared with prior art, the present invention has following technique effect:
(1) compare C-LiFePO of the present invention with other inorganic positive electrodes
4/ PTPAn composite material specific discharge capacity can reach 140～155mAh/g; After 50 circulations, specific discharge capacity remains on more than 90%; Under high magnification, charge-discharge performance is superior, and under 10C multiplying power, specific discharge capacity can reach 90～115mAh/g.
(2) lithium battery that prepared by the present invention and other inorganic material of existing use are as positive electrode (pure LiFePO
4, LiMnPO
4) lithium battery compare, there is higher charging and discharging capacity, superior cyclical stability and the very outstanding advantages such as fast charging and discharging performance.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is described in detail.
Fig. 1 is (a) C-LiFePO
4, (b) C-LiFePO
4/ 3%PTPAn, (c) C-LiFePO
4/ 10%PTPAn, (d) C-LiFePO
4the stereoscan photograph of/20%PTPAn; (e) C-LiFePO
4/ 10%PTPAn transmission electron microscope photo; (f) C-LiFePO
4/ 10%PTPAn high power transmission electron microscope photo.
Fig. 2 is respectively with PTPAn, LiFePO
4, C-LiFePO
4, C-LiFePO
4/ PTPAn composite material be the positive electrode of active material in 0.1C charge-discharge magnification situation, LiPF
6in EC/DMC (V/V, 1:1) electrolyte, the first charge-discharge curve in 2.5-4.2V voltage range.
Fig. 3 is respectively with C-LiFePO
4, C-LiFePO
4/ PTPAn composite material be the positive electrode of active material in 0.1C charge-discharge magnification situation, LiPF
6in EC/DMC (V/V, 1:1) electrolyte, the cycle performance figure in 2.5-4.2V voltage range.
Fig. 4 is respectively with C-LiFePO
4, C-LiFePO
4/ PTPAn composite material be the positive electrode of active material in the situation that of 0.1C, 0.2C, 0.5C, 1C, 2C, 5C, 10C charge-discharge magnification, LiPF
6in EC/DMC (V/V, 1:1) electrolyte, first charge-discharge curve in 2.5-4.2V voltage range.
Fig. 5 is respectively with C-LiFePO
4, C-LiFePO
4/ PTPAn composite material be the positive electrode of active material in the situation that of 0.1C, 0.2C, 0.5C, 1C, 2C, 5C, 10C charge-discharge magnification, LiPF
6in EC/DMC (V/V, 1:1) electrolyte, the cycle performance figure in 2.5-4.2V voltage range.
Embodiment
Further illustrate by the following examples the present invention.
Embodiment
First by the LiOHH of 0.045mol
2o joins in 120mL ethylene glycol, at the uniform velocity stirs, then by the H of 0.015mol
3pO
4feSO with 0.015mol
47H
2o is mixed with mixed solution (H
2o30mL) dropwise join in above-mentioned solution, after having fed intake, system is heated to 120 ℃ of reaction 20h.After reaction finishes, be cooled to room temperature, by centrifugal, deionized water, wash, precipitation is dried to constant weight, obtain LiFePO
4precursor, by itself and a certain amount of sucrose, (sucrose quality is LiFePO
4quality 8%) mix, in tube furnace in mobile high-purity N
2program temperature control sintering, heat-treat condition is as follows: first the speed with 5 ℃/min is warming up to 350 ℃ by room temperature, insulation 1h, then be warming up to 650 ℃ with the speed of 5 ℃/min, insulation 5h, is then cooled to room temperature, finally obtains C-LiFePO
4, its stereoscan photograph is shown in Fig. 1.
In reaction vessel, add 0.5g triphenylamine (TPA) monomer, 1.9282g iron chloride and 20mL chloroform, at N
2under protection, under normal temperature and pressure, carry out polymerization reaction, after reaction 24h, add a large amount of methyl alcohol to make product precipitation, then filter, filter cake 60 ℃ of vacuumizes in baking oven are spent the night, obtain canescence PTPAn pressed powder.
By solution blended process, prepare inorganic-organic nanocomposite C-LiFePO
4/ PTPAn: the PTPAn with loose structure of preparation is dissolved in chloroform, more in proportion by C-LiFePO
4nano material is put into wherein, ultrasonic dispersion, and ultrasonic dispersion frequency 53KHz, power 100%, time 15min, finally, by solvent chloroform evaporate to dryness, vacuumize obtains C-LiFePO
4/ x%PTPAn composite material, wherein x% represents the mass percent of PTPAn in composite material.C-LiFePO has specifically been prepared in experiment
4/ 3%PTPAn, C-LiFePO
4/ 10%PTPAn, C-LiFePO
4tri-kinds of composite materials of/20%PTPAn.
Wherein, C-LiFePO
4the scanning electron microscope (SEM) photograph of/3%PTPAn, C-LiFePO
4the scanning electron microscope (SEM) photograph of/10%PTPAn, transmission electron microscope picture, high power transmission electron microscope picture and C-LiFePO
4the scanning electron microscope (SEM) photograph of/20%PTPAn is all shown in Fig. 1.
Electrical performance testing:
PTPAn, LiFePO to make respectively
4, C-LiFePO
4, C-LiFePO
4/ 3%PTPAn composite material, C-LiFePO
4/ 10%PTPAn composite material, C-LiFePO
4/ 20%PTPAn composite material, as positive electrode, is prepared as follows lithium ion battery:
A) take the positive electrode powder of 1 part of adhesive powder, 2 parts of acetylene blacks, 7 parts of preparations, mix;
B) mixture in a) is dispersed in 1-METHYLPYRROLIDONE solvent, grinds, be uniformly dispersed;
C) by b) in slurry be evenly applied on aluminium foil, be placed in 60 ℃ of vacuumize 24h of baking oven, obtain positive plate;
D) take c) in the positive plate of preparation be positive pole, metal lithium sheet is negative pole, 1mol/L LiPF
6eC/DMC (V/V, 1:1) is electrolyte, and PP film is barrier film, in being full of the glove box of argon gas, assembles button cell.
PTPAn, LiFePO
4, C-LiFePO
4, C-LiFePO
4/ 3%PTPAn composite material, C-LiFePO
4/ 10%PTPAn composite material, C-LiFePO
4the electric property of/20%PTPAn composite material as Figure 2-Figure 5, from Fig. 2-Fig. 5, the C-LiFePO that the present invention makes
4/ PTPAn composite material has higher charging and discharging capacity, superior cyclical stability and very outstanding fast charging and discharging performance.
Claims (10)
1. a C-LiFePO
4/ PTPAn composite material, described C-LiFePO
4/ PTPAn composite material is with the coated LiFePO of carbon
4material and poly-triphenylamine are raw material, by solution blended process, make.
2. C-LiFePO as claimed in claim 1
4/ PTPAn composite material, is characterized in that: described C-LiFePO
4mass content≤20% of poly-triphenylamine in/PTPAn composite material.
3. C-LiFePO as claimed in claim 1
4/ PTPAn composite material, is characterized in that: described C-LiFePO
4in/PTPAn composite material, the mass content of poly-triphenylamine is 3～20%.
4. C-LiFePO as claimed in claim 1
4/ PTPAn composite material, is characterized in that: described C-LiFePO
4in/PTPAn composite material, the mass content of poly-triphenylamine is 5～15%.
5. C-LiFePO as claimed in claim 1
4/ PTPAn composite material, is characterized in that: described C-LiFePO
4in/PTPAn composite material, the mass content of poly-triphenylamine is 10%.
6. the C-LiFePO as described in one of claim 1～5
4/ PTPAn composite material, is characterized in that: the LiFePO that carbon is coated
4material is to take sucrose as carbon source, makes LiFePO
4mix with sucrose, at N
2in heat-treat and obtain, heat-treat condition is: first the speed with 2-10 ℃/min rises to 250-400 ℃ by room temperature, insulation 0.5～2h, then be warming up to 500-700 ℃ with the speed of 2-10 ℃/min, sintering 2～10 hours; Sucrose quality is LiFePO
42～10% of quality.
7. the C-LiFePO as described in one of claim 1～5
4/ PTPAn composite material, is characterized in that: described solution blended process is specially: make the coated LiFePO of carbon
4material and poly-triphenylamine fully disperse in solvent, and then solvent evaporated, is drying to obtain C-LiFePO
4/ PTPAn composite material; Described solvent is selected from halogenated hydrocarbon solvent or phenols reagent.
8. C-LiFePO as claimed in claim 7
4/ PTPAn composite material, is characterized in that: described solvent is chloroform or cresols.
9. C-LiFePO as claimed in claim 1
4/ PTPAn composite material is as the application of anode material of lithium battery.
10. with C-LiFePO claimed in claim 1
4the lithium battery that/PTPAn composite material makes as positive electrode.
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| CN108461752A (en) * | 2018-03-12 | 2018-08-28 | 华南师范大学 | A kind of side chain carries triphen amine polymer and the preparation and application of conjugated carbonyl compound |
| WO2020090344A1 (en) * | 2018-11-02 | 2020-05-07 | 日産化学株式会社 | Active material composite formation composition, active material composite, and production method for active material composite |
| CN113860280A (en) * | 2021-09-24 | 2021-12-31 | 惠州亿纬锂能股份有限公司 | Lithium manganese iron phosphate cathode material and preparation method and application thereof |
| CN114094057A (en) * | 2021-11-16 | 2022-02-25 | 惠州亿纬锂能股份有限公司 | Ternary positive electrode plate of composite polytriphenylamine and preparation method and application thereof |
| US11639403B2 (en) | 2018-11-09 | 2023-05-02 | Samsung Electronics Co., Ltd. | Polymer, composite positive active material including the same, and lithium secondary battery including electrode including the positive active material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105591085A (en) * | 2016-03-16 | 2016-05-18 | 江苏乐能电池股份有限公司 | Method for preparing high-power and long-service-life lithium iron phosphate anode material |
| CN108461752A (en) * | 2018-03-12 | 2018-08-28 | 华南师范大学 | A kind of side chain carries triphen amine polymer and the preparation and application of conjugated carbonyl compound |
| WO2020090344A1 (en) * | 2018-11-02 | 2020-05-07 | 日産化学株式会社 | Active material composite formation composition, active material composite, and production method for active material composite |
| JPWO2020090344A1 (en) * | 2018-11-02 | 2021-09-24 | 日産化学株式会社 | Composition for forming an active material complex, an active material complex, and a method for producing an active material complex. |
| JP7359156B2 (en) | 2018-11-02 | 2023-10-11 | 日産化学株式会社 | Composition for forming active material composite, active material composite, and method for producing active material composite |
| US11639403B2 (en) | 2018-11-09 | 2023-05-02 | Samsung Electronics Co., Ltd. | Polymer, composite positive active material including the same, and lithium secondary battery including electrode including the positive active material |
| CN113860280A (en) * | 2021-09-24 | 2021-12-31 | 惠州亿纬锂能股份有限公司 | Lithium manganese iron phosphate cathode material and preparation method and application thereof |
| CN114094057A (en) * | 2021-11-16 | 2022-02-25 | 惠州亿纬锂能股份有限公司 | Ternary positive electrode plate of composite polytriphenylamine and preparation method and application thereof |
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