CN102509793B - Method for preparing zinc and barium activated lithium iron phosphate cathode material - Google Patents
Method for preparing zinc and barium activated lithium iron phosphate cathode material Download PDFInfo
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- CN102509793B CN102509793B CN201110335932.8A CN201110335932A CN102509793B CN 102509793 B CN102509793 B CN 102509793B CN 201110335932 A CN201110335932 A CN 201110335932A CN 102509793 B CN102509793 B CN 102509793B
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Abstract
The invention relates to a method for preparing a zinc and barium activated lithium iron phosphate cathode material. Raw materials for preparing the zinc and barium activated lithium iron phosphate cathode material include lithium sources, ferrum sources, phosphate radical sources, zinc sources and barium sources, all the raw materials are mixed according to a proportion of 1 mol Li : 0.00002-0.00005 mol Zn : 0.0003 mol Ba : 1 mol Fe : 1 mol P, performed with ball milling at high speed with rotation speed at 200 r/min in absolute ethyl alcohol media, dried at 105-120 DEG C to obtain a precursor, and the precursor obtained through drying is placed in a high temperature furnace to be roasted for 24 hours at 500-750 DEG C high temperature in nitrogen atmosphere so as to obtain the zinc and barium activated lithium iron phosphate cathode material. Due to the fact that a small amount of doping replaces zinc and barium, control on shape and particle size of products is facilitated, stable lithium iron phosphate compound can be obtained, crystal lattice of the lithium iron phosphate compound is activated, lithium-ion diffusion coefficient is enlarged, and first discharge capacity of obtained materials reaches 160.52 mAh/g. A charge-discharge platform of the zinc and barium activated lithium iron phosphate cathode material is about 3.5 V relative to electric potential of lithium electrodes, first discharge capacity of the charge-discharge platform surpasses 168 mAh/g, and capacity of the charge-discharge platform is reduced to about 1.2% after 100 times of charge-discharge circulation. Compared with a lithium iron phosphate (LiFePO4) comparison embodiment without doping, the zinc and barium activated lithium iron phosphate cathode material is greatly improved in both specific capacity and cycle stability.
Description
Technical field
Zinc of the present invention, barium activation lithium iron phosphate positive material preparation method, belong to a kind of anode material of lithium battery preparation method, particularly a kind of lithium iron phosphate battery positive material preparation method.
Background technology
At present, the Present study of LiFePO4 doping vario-property: LiFePO4 LiFePO4 is because it is nontoxic, environmentally friendly, safe, raw material source is abundant, specific capacity is high, stable cycle performance, cheap, there is the steady discharge platform of the theoretical capacity 3.5V of 170mAh/g, LiFePO 4 material has high energy density, cheap price, excellent fail safe, is specially adapted to electrokinetic cell.But its resistivity is larger.Due to LiFePO4, under normal temperature, the dynamics of LiFePO4 is bad, high rate performance extreme difference, researchers both domestic and external have used and have improved high rate performance methods such as coated, doping, nanometer, and basic idea improves exactly conductivity and shortens ion, electric transmission path.Doping is the important material modification method of a class.2002, the reported first lithium position doping vario-properties such as Massachusetts science and engineering Chiang professor Yet-Ming can improve LiFePO4 electronic conductivity greatly.They carry out the doping of high volence metal ion (Mg2+, Al3+, Ti4+, Zr4+, Nb5+ and W6+) solid solution in lithium position, electronic conductivity has improved 8 orders of magnitude.Sample through above-mentioned doping has good chemical property, particularly high-rate performance, under the electric current of 21.5C (3225mA/g), discharges, and still can obtain the capacity of 60mAh/g.Doping carbon: carbon has good electric conductivity and lower mass density, adds a small amount of carbon of people, can improve on the one hand the electric conductivity of material, can reduce on the other hand the particle diameter yardstick of material.Xxx has studied different phase and has mixed the impact of people's carbon on material electrochemical performance.Shi Zhicong etc. " adopt solid phase reaction in conjunction with high speed ball-milling method, synthetic positive electrode LiFePO4, experiment shows: LiFePO4 has the discharge voltage plateau of 3.4V, discharge capacity reaches 147mAh/g charge and discharge cycles and only decays 9.5% afterwards 100 times first.LiFePO4/C composite material after carbon dope, granule-morphology rule, spherical for class, particle is little, and particle diameter distributes and all hooks.Carbon is scattered between crystal grain, has strengthened the electrical conductance between particle.LiFePO4 specific discharge capacity and cycle performance after carbon dope all significantly improve.Lithium position doping: LiFePO4 crushed grain is assorted is a kind of important method of improving chemical property.The doping of lithium position can improve the conductivity of LiFePO4.Tan Xianyan etc. " " adopt calcination method synthesizing lithium ionic cell positive pole material lithium iron phosphate, mix a small amount of Mg2+ and significantly improved the conductivity of material, have improved the chemical property of LiFePO4.After doping, LiFePO4 first discharge capacity reaches 135.52mAh/g; Unadulterated LiFePO4 first discharge capacity only has 116.25mAh/g.Conductivity after doping has obtained certain raising.This is because a small amount of metal ion of doping replaces Li+ position, forms p-type semiconductor, has increased the conductivity of material.The identical ^ of Liu adopts improved solid phase method to prepare LiFePO4 and the Li0 that particle is fine, particle diameter is evenly distributed, 98Mn, and o.o2LiFePO4 compound, doping is conducive to control pattern and the particle diameter of product on a small quantity, obtains stable LiFePO4 compound.Because Mn2+ octahedral coordination radius is less than Fe2+, can think that magnesium ion occupies replacement lithium ion.Result shows: in material, the relative lithium electrode current potential of the charge and discharge platform of lithium ion is 3.5V left and right, and initial discharge capacity exceedes 160mAh/g, and after 50 charge and discharge cycles, capacity only decays 5.5%, shows that the method has improved specific energy and cyclical stability.Iron position is disastrously assorted: although the doping of lithium position can improve the conductivity of material, because foreign atom can hinder the diffusion of lithium ion in one dimension passage, thereby be unfavorable for improving the high-rate charge-discharge capability of material.And the doping of iron position can improve the rate charge-discharge performance of LiFePO4, improve cycle performance.The ^ such as Liu Fangling adopt parcel carbon to improve its surface electronic conductivity, and doped metal ion is to improve its body electronic conductivity.Having chosen ionic radius approaches and 4 different metal ion species Ca3+ of valence state, Ti5+, Ta5+, the Fe position doping of MO6+, sample unit cell volume after doping all has minimizing, electronic conductivity has improved 4-6 the order of magnitude than the electronic conductivity of LiFePO4, and its impedance in electrolyte solution is greatly reduced, and chemical property also obviously improves.The ^ such as Hu Huanyu adopt the synthetic tiny uniform nanoscale positive electrode LiFePO4 of particle of high-temperature solid phase reaction method, have good capacity circulating performance, but its high rate capability are poor.Mix a small amount of manganese and can reduce the polarization of material, improve the high rate capability of material.This is mainly the unit cell volume that has increased LiFePO4 due to the doping of manganese, more be conducive to deviating from of lithium, the doping of manganese has caused sintering process to produce crystal structure defects in addition, has improved the electron conduction of material, thereby the high-rate charge-discharge capability of material is made moderate progress.Phosphate potential crushed grain is assorted: P site doped is feasible in theory, but seldom has the doping of carrying out separately phosphate potential.The ^ such as Zhang Yurong have studied olivine structural Li2+2xTi2-xCu2x (NbO) 2, and having obtained conductivity by Ti and Cu replacement P is that 1.26 × 10-6S/cm-adds, the positive electrode that initial discharge capacity is 805.8mAh/g.Such material has higher conductivity, but because Fe is all replaced by Ti and Cu, ' guiding discharge voltage is lower, and cycle performance is poor.Although phosphate potential is feasible in theory, study relatively less.
Through retrieval, record at present 1043 of relevant lithium battery applications for a patent for invention, 2181 of lithium ion battery applications for a patent for invention, wherein having a great deal of is relevant method of adulterating.
Be confirmed to be in theory lithium position, or iron position, or phosphate potential is adulterated and role, and relevant authoritative experts, still have different separately brilliant idea, also constantly studying, exploring.
Current more consistent viewpoint is, the advantage such as LiFePO4 has that fail safe is good, pollution-free, stable cycle performance, specific capacity are high and cheap, but also there is poorly conductive and the lower shortcoming of tap density.Poorly conductive is the biggest factor that affects LiFePO4 application, conductivity can be improved by doping, and high-rate charge-discharge capability also improves, and has suppressed to a certain extent the effect of capacity attenuation.Doping approach can improve, improve lithium ion anode material performance, has been a kind of feasible mode of generally acknowledging.
summary of the invention
The object of the invention is to: the structural limitations of the lithium iron phosphate positive material (LiFePO4) based on prior art, there is its poorly conductive and the low deficiency of lithium ion diffusion coefficient, now propose zinc, barium activation lithium iron phosphate positive material preparation method that the activation of a kind of zinc, barium improves its performance.
The present invention, in view of doping approach can improve, improve lithium ion anode material performance, has been a kind of feasible mode of generally acknowledging.According to the chemical property of barium/lithium, electric property, crystal structure characteristic is the feature of akin element:
Barium, is element the most active in alkaline-earth metal, because it is very active, and easily oxidized, should be kept in kerosene and atoleine.
5.212 electron-volts of ionization energy, the first ionization energy 502.9kJ/mol;
Crystal structure: structure cell is body centred cubic cell, each structure cell contains 2 metallic atoms;
Cell parameter: a=502.8pm; B=502.8pm; C=502.8pm; α=90 °; β=90 °; γ=90 °.
Lithium, metallic element, can react with a large amount of inorganic reagents and organic reagent.With all energy chemical combination such as oxygen, nitrogen, sulphur, due to easily oxidated and dimmed, and density ratio kerosene is little, therefore should deposit in atoleine.
5.392 electron-volts of ionization energy, the first ionization energy 520.2kJ/mol;
Crystal structure: structure cell is body centred cubic cell, each structure cell contains 2 metallic atoms;
Cell parameter: a=351pm; B=351pm; C=351pm; α=90 °; β=90 °; γ=90 °.
Think that barium should be to be easy to lithium position chanza most.The present invention be adulterate by barium test, in the situation with barium doping, can add again 1-2 other element, form 2 yuan or 3 yuan of doping, to obtain the good anode material of lithium battery of performance.
Zinc of the present invention, barium activation lithium iron phosphate positive material, is characterized in that: its chemical composition or chemical general formula can be expressed as: LiZnxBayFePO4, x=0.00002-0.00005, y=0.0003; Wherein the mol of Li, Zn, Ba, Fe, P ratio is: 1mol Li: 0.00002-0.00005mol Zn: 0.0003mol Ba: 1 mol Fe: 1mol P.
Zinc of the present invention, barium activation lithium iron phosphate positive material preparation method, it is characterized in that: its lithium source, source of iron, phosphoric acid root, zinc source, the raw material in barium source, according to 1mol Li: 0.00002-0.00005mol Zn: 0.0003mol Ba: 1mol Fe: after 1mol P ratio is mixed, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in high temperature furnace, in nitrogen atmosphere, through 500-750 DEG C of high-temperature calcination 16-24h, obtain zinc, barium activation lithium iron phosphate positive material.Its lithium source is one of lithium carbonate, lithium hydroxide, source of iron is ferrous oxalate, phosphoric acid root is one of ammonium dihydrogen phosphate or diammonium hydrogen phosphate, and zinc source is one of zinc carbonate, zinc oxide, and barium source is one of brium carbonate, barium hydroxide, barium chloride, barium nitrate, barium monoxide, barium sulphide.
The present invention's beneficial effect compared with prior art: zinc of the present invention, barium activation lithium iron phosphate positive material preparation method, perhaps, resulting materials replaces zinc, barium because doping is a small amount of, be conducive to control pattern and the particle diameter of product, obtain stable LiFePO4 compound, zinc, barium ions occupy replacement lithium ion, its lattice has obtained activation, has improved lithium ion diffusion coefficient; Although the doping of barium lithium position can improve the conductivity of material, due to doping ion, can hinder the diffusion of lithium ion in one dimension passage, thereby be unfavorable for improving the high-rate charge-discharge capability of material.Product unit cell volume after zinc doping all has minimizing, and electronic conductivity improves than the electronic conductivity of LiFePO4, and its impedance in electrolyte solution is greatly reduced, and chemical property also obviously improves; Its first discharge capacity reach 160.52mAh/g; The relative lithium electrode current potential of its charge and discharge platform is about 3.5V, and initial discharge capacity exceedes 168mAh/g, capacity 1.2% left and right of approximately decaying after 100 charge and discharge cycles; Specific capacity and cyclical stability and unadulterated LiFePO4 first discharge capacity only have compared with 116.25mAh/g, are greatly improved.
embodiment
Below in conjunction with embodiment, the invention will be further described, but embodiments of the present invention are not limited to this.
Below adopt calcination method synthetic method, to zinc of the present invention, barium activation lithium iron phosphate positive material preparation method, be illustrated.
Zinc of the present invention, barium activation lithium iron phosphate positive material preparation method, its lithium source can be used: the lithium salts such as lithium carbonate, lithium hydroxide or lithium dihydrogen phosphate, source of iron can be used: ferrous oxalate etc., phosphoric acid root can be used: ammonium dihydrogen phosphate or diammonium hydrogen phosphate etc., zinc source is zinc carbonate ZnCO3, zinc oxide ZnO etc., and barium source can be used: the barium salts such as brium carbonate, barium hydroxide, barium chloride, barium nitrate, barium monoxide, barium sulphide.
Select: lithium carbonate (Li2CO3) (99.73%), zinc carbonate (99.8%), brium carbonate (BaCO3) (99.8%), ferrous oxalate (FeC2O4.2H2O) (99.06%), diammonium hydrogen phosphate (NH4H2PO4) (98%) is raw material; According to 1mol Li: 0.00002-0.00005mol Zn: 0.0003mol Ba: 1mol Fe: after 1molP ratio is mixed, in ethanol medium, rotating speed 200-800r/min high speed ball milling 15-20h, with 105-120 DEG C of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in high temperature furnace, in nitrogen atmosphere, through 500-750 DEG C of high-temperature calcination 16-24h, obtain zinc of the present invention, barium activation lithium iron phosphate positive material.Embodiment 1
Li2CO3 (99.73%), ZnCO3 (99.8%), BaCO3 (99.8%), FeC2O4.2H2O (99.06%), NH4H2PO4 (98%) raw material, according to 1mol Li: 0.00002mol Zn: 0.0003mol Ba: 1mol Fe: after 1mol P ratio is mixed, in absolute ethyl alcohol (AR) medium, high speed ball milling 20h (rotating speed 200r/min.After 105-120 DEG C of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in high temperature furnace, in common purity nitrogen (> 99.5%) atmosphere, and through 500-750 DEG C, high-temperature calcination 24h.Obtain zinc of the present invention, barium activation lithium iron phosphate positive material.
Embodiment 2 (not mixing contrast)
By Li2CO3 (99.73%), FeC2O4.2H2O (99.06%), NH4H2PO4 (98%) raw material, according to 1mol Li: 1mol Fe: after 1mol P ratio is mixed, in absolute ethyl alcohol (AR) medium, high speed ball milling 20h (rotating speed 200r/min.After 105-120 DEG C of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in high temperature furnace, in common purity nitrogen (> 99.5%) atmosphere, and through 500-750 DEG C, high-temperature calcination 24h.Obtain lithium ion anode material.
Adopt the testing equipment of prior art and the method for testing of prior art, zinc, barium to above embodiment 1 activate lithium iron phosphate positive material, carry out test result be with the control Example 2 of not mixing:
The zinc of the embodiment of the present invention 1, barium activation lithium iron phosphate positive material, more than discharge capacity reaches 155.52mAh/g first; Unadulterated LiFePO4 first discharge capacity only has in 116.25mAh/g.
The barium activation lithium iron phosphate positive material of the embodiment of the present invention 1, the relative lithium electrode current potential of its charge and discharge platform is 3.5V left and right, initial discharge capacity exceedes 164mAh/g, capacity 3.0% left and right of approximately decaying after 100 charge and discharge cycles.
Barium activation lithium iron phosphate positive material preparation method of the present invention, assorted after doping, the raising of resulting materials specific capacity and cyclical stability, this is perhaps to replace zinc, barium because doping is a small amount of, be conducive to control pattern and the particle diameter of product, obtain stable LiFePO4 compound, barium ions occupies replacement lithium ion, its lattice has obtained activation, has improved lithium ion diffusion coefficient; Although the doping of barium lithium position can improve the conductivity of material, due to doping ion, can hinder the diffusion of lithium ion in one dimension passage, thereby be unfavorable for improving the high-rate charge-discharge capability of material.And the doping of iron position can improve the rate charge-discharge performance of LiFePO4, improve cycle performance.Product unit cell volume after zinc doping all has minimizing, and electronic conductivity improves than the electronic conductivity of LiFePO4, and its impedance in electrolyte solution is greatly reduced, and chemical property also obviously improves; Its first discharge capacity reach 155.52mAh/g; The relative lithium electrode current potential of its charge and discharge platform is about 3.5V, and initial discharge capacity exceedes 164mAh/g, capacity 3.0% left and right of approximately decaying after 100 charge and discharge cycles; Specific capacity and cyclical stability and unadulterated LiFePO4 first discharge capacity only have compared with 116.25mAh/g, are greatly improved.Be to replace zinc, barium because doping is a small amount of, be conducive to control pattern and the particle diameter of product, obtain stable LiFePO4 compound, its lattice has obtained activation, has improved the result of lithium ion diffusion coefficient.
Claims (1)
1. a zinc, barium activation lithium iron phosphate positive material preparation method, it is characterized in that: select: lithium carbonate, zinc carbonate, brium carbonate, ferrous oxalate, diammonium hydrogen phosphate is raw material, after mixing according to 1mol Li:0.00002-0.00005mol Zn:0.0003mol Ba:1mol Fe:1mol P ratio, in ethanol medium, rotating speed 200--800r/min high speed ball milling 15--20h, with 105-120 DEG C of oven dry, obtain presoma, the presoma that oven dry is obtained is placed in high temperature furnace, in nitrogen atmosphere, through 500-750 DEG C of high-temperature calcination 16-24h, obtain zinc, barium activation lithium iron phosphate positive material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006048991A (en) * | 2004-08-02 | 2006-02-16 | Sumitomo Osaka Cement Co Ltd | Positive electrode active material for lithium battery, its manufacturing method, and lithium battery |
| CN101393982A (en) * | 2008-10-28 | 2009-03-25 | 南京海泰纳米材料有限公司 | Method for producing carbon coated nano stage lithium iron phosphate by precipitation |
| CN101582498A (en) * | 2009-06-18 | 2009-11-18 | 东北师范大学 | Method for preparing nanometer ferrous phosphate lithium /carbon composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006048991A (en) * | 2004-08-02 | 2006-02-16 | Sumitomo Osaka Cement Co Ltd | Positive electrode active material for lithium battery, its manufacturing method, and lithium battery |
| CN101393982A (en) * | 2008-10-28 | 2009-03-25 | 南京海泰纳米材料有限公司 | Method for producing carbon coated nano stage lithium iron phosphate by precipitation |
| CN101582498A (en) * | 2009-06-18 | 2009-11-18 | 东北师范大学 | Method for preparing nanometer ferrous phosphate lithium /carbon composite material |
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