CN101562248A - Graphite composite lithium ion battery anode material lithium iron phosphate and preparation method thereof - Google Patents
Graphite composite lithium ion battery anode material lithium iron phosphate and preparation method thereof Download PDFInfo
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- CN101562248A CN101562248A CNA2009100524133A CN200910052413A CN101562248A CN 101562248 A CN101562248 A CN 101562248A CN A2009100524133 A CNA2009100524133 A CN A2009100524133A CN 200910052413 A CN200910052413 A CN 200910052413A CN 101562248 A CN101562248 A CN 101562248A
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Abstract
The invention relates to a graphene composite lithium ion battery anode material lithium iron phosphate and a preparation method thereof. The composite material of lithium iron phosphate and graphene is connected by interface of chemical bonding. The invention also provides the method for preparing the graphene composite lithium ion battery anode material lithium iron phosphate in an in-situ symbiosis reaction mode, and the obtained anode material has high tap density and good magnifying performance, and is suitable to be used as a anode material of a lithium ion power battery.
Description
Technical field
The present invention relates to compound lithium ion battery anode material lithium iron phosphate of a kind of Graphene and preparation method thereof, the composite material of this LiFePO4 and Graphene is connected by the interface of chemical bonding, the method for preparing lithium ion battery anode material lithium iron phosphate with original position symbiosis reactive mode is provided simultaneously, the tap density height of gained positive electrode, good rate capability are suitable as in lithium ion power battery cathode material.
Background technology
Graphene is a kind of carbonaceous new material by the two-dimentional hexagonal lattice structure of the tightly packed one-tenth of monolayer carbon atom, is the elementary cell that makes up other dimension carbonaceous materials (as zero dimension fullerene, one dimension carbon nano-tube, three-dimensional graphite).Graphene has excellent electricity, calorifics and mechanical property, is expected in the acquisition extensive use of fields such as high-performance nanometer electronic device, composite material, field emmision material, gas sensor and energy storage.Graphene is the highest material of intensity on the present the known world.Graphene film not only possesses high rigidity and high tensile, and its electrology characteristic also is best in the current material, and electron mobility reaches 200,000cm
2/ Vs is far above 2 of crystal Si, 000cm
2/ Vs.The number of plies difference of high-quality Graphene, marked change can take place in the electronic structure of Graphene, therefore realizes that graphene layer numerical control system is very crucial.
The LiFePO4 intrinsic pure phase of using as anode material for lithium-ion batteries is an insulator, by nanometer copmbined-carbon coating technology.The LiFePO that reduces
4Particle diameter shortens the evolving path of lithium ion in lattice, but volume energy density reduces significantly; Can improve the electronic conductivity of material by adding the conductive agent interpolation as conductive carbon black or carbon coating technology, but also can reduce the tap density of former LiFePO 4 material greatly; Can conductivity by element doping, but feasibility and working mechanism are unclear at present, also can reduce theoretical capacity along with doping increases.The positive electrode that lithium battery is used need be electronics and lithium ion mixed conductor, and the electronic conductivity of LiFePO4 is lower, and therefore need and conductive agent are compound to improve electron transport ability in the electrochemical process.General used method is for adding conductive carbon powder or carbon containing conductive agent presoma ([J] J.F.NiProgress in Chemistry 16 (4) 554-5602004, [J] Y.Q.Hu et al Journal of the ElectrochemicalSociety 151 (8) A1279-A1285 2004, [J] S.T.Myung et al Electrochimica Acata 49 (24) 4213-42222004, [J] J.Shim et al Journal of Power Sources 119 955-958 2003, A.S.Anderssonet al Journal of Power Sources 97-8:503-507 2001, US6528033, US2004/0151649, CN1410349A).These conductive carbon powders can be natural graphite powder, graphous graphite powder, carbon black, carbon containing conductive agent presoma is the mixture of sucrose, glucose, polyacrylic acid, ethylene glycol, polyvinyl alcohol, starch or gelatin, the compound electron conduction ability that can improve material greatly of LiFePO4/carbon.Yet the simple substance carbon that carbon coats and surface texture more complicated, the interface resistance of oxide are bigger, and capacity can descend significantly when rate charge-discharge; The tap density of lithium iron phosphate positive material descends significantly behind the carbon technique by adding in addition, usually is lower than 1.0g/cm
3The positive electrode that lithium-ion-power cell is used must have high stored energy capacitance, high-tap density, high power charging-discharging.In order to improve the high rate performance of battery, the compound positive electrode of carbon need be filled more carbon, thereby can reduce the tap density of material greatly, causes the lithium-ion-power cell volume excessive.
Summary of the invention
The present invention provides compound lithium ion battery anode material lithium iron phosphate of a kind of Graphene and preparation method thereof just in order to overcome above-mentioned deficiency, and this composite material is made up of LiFePO4 and Graphene, is connected by chemical bond between the two.Because the electron conduction of Graphene is free on the hexagoinal lattice plane, electron mobility is very big, compound with LiFePO4 is desirable electronic conductor, the method for preparing lithium ion battery anode material lithium iron phosphate with original position symbiosis reactive mode is provided simultaneously, only need the participation of a small amount of Graphene compound, the gained positive electrode can improve tap density height, good rate capability, is suitable as in lithium ion power battery cathode material.
The lithium ion battery anode material lithium iron phosphate that a kind of Graphene is compound has improved electronic conductivity, tap density, the high rate performance of lithium iron phosphate positive material greatly.Concrete enforcement can be taked following a kind of method wherein:
Implementation method one: nano-grade lithium iron phosphate pure phase powder and fully mixed 2-50 hour by the 0.1-2.5% Graphene or the graphene oxide of LiFePO4 weight ratio; in the 300-850 ℃ of stove that nitrogen, argon gas or hydrogen argon hybrid protection atmosphere are arranged insulation reaction 0.1-5 hour; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.
Implementation method two: with iron content, lithium and phosphate radical is 1.0 in molar ratio: 0.85-1.00: 0.95-1.05 and the raw material of pressing LiFePO4 weight ratio 0.5-5% Graphene or graphene oxide; fully mixed 2-50 hour; in the 600-850 ℃ of stove that nitrogen, argon gas or hydrogen argon hybrid protection atmosphere are arranged insulation reaction 1-10 hour; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.
The Graphene that the present invention adopts is that the two-dimentional lonsdaleite material between 1 to 10 is formed by the individual layer or the number of plies.
The lithium source that the present invention adopts is a kind of or combination of lithia, lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate, lithium phosphate, lithium dihydrogen phosphate.
The source of iron that the present invention adopts is a kind of or combination of iron, ferrous oxide, tri-iron tetroxide, di-iron trioxide, ferrous sulfate, iron ammonium sulfate, ferric phosphate, ferrous phosphate, ferrous ammonium phosphate, ferrous citrate.
The phosphorus source that the present invention adopts is a kind of or combination of phosphorus pentoxide, phosphoric acid, ammonium di-hydrogen phosphate, lithium dihydrogen phosphate, DAP, ferrous ammonium phosphate, phosphoric acid hydrogen ammonia salt.
The Graphene raw material that the present invention adopts can make Graphene or graphene oxide, and graphene oxide is carbon atom part grafting hydrogen-oxygen or the carboxylic group on the Graphene.
The even mixed method of iron content, lithium, phosphate radical and the Graphene that the present invention adopts or the raw material of graphene oxide is that solid phase or solid-liquid machinery fully mix, and liquid phase substance can be the abrasive fluid phase medium of using always (as ethanol), looks actual conditions and mixes 2-50 hour.
The prepared lithium ion battery anode material lithium iron phosphate of the present invention is characterised in that the lithium iron phosphate positive material finished particle is by receiving brilliant LiFePO
4With the offspring that the Graphene original position is compounded to form, Graphene is distributed in granule interior or surface, is built into the electron conduction network material.Because of the agent of Graphene electron conduction is the material with carbon element of six side's coplanes of individual layer, only need a spot of addition, this electric conducting material and LiFePO4 form very dense conductive network, thereby can improve electronic conductivity better, reduce material internal resistance, improve battery high power forthright, the more important thing is that low electricity that prepared positive electrode overcomes the graphite layers direction leads and improved the comprehensive conductivity and and the tap density of material greatly.
The distinguishing feature of method that the present invention prepares the lithium ion battery anode material lithium iron phosphate composite material is: have strong chemical b ` between LiFePO4 and the Graphene, thereby can improve electronic conductivity better, reduce the internal resistance of positive electrode, thereby the high power that has improved battery is forthright, the more important thing is that prepared positive electrode overcomes that loose graphite powder exists and the tap density that improved material greatly.The positive electrode of the present invention preparation, the interface interaction of LiFePO4 and graphene conductive agent is strong, and these advantages cause the lithium ion and the electronic conductivity height of material, the tap density height, and be suitable for big multiplying power and charge and discharge.The composite material and preparation method thereof uniqueness that the present invention adopts, synthesis technique is simple, is easy to large-scale production, and the product material chemical property is good.
Description of drawings
Fig. 1 presses the X-ray diffracting spectrum of 1 Graphene composite positive pole of embodiment.
Fig. 2 presses the stereoscan photograph of 1 Graphene composite positive pole of embodiment.
Fig. 3 charges and discharge curve first by the 1C/1C multiplying power of embodiment 1 prepared lithium ion battery.
Embodiment
Embodiment 1
Fully mixed 5 hours with nano-grade lithium iron phosphate pure phase powder with by 1% Graphene of LiFePO4 weight ratio, insulation reaction is 1.5 hours in 550 ℃ of stoves of nitrogen protection atmosphere are arranged, and is cooled to room temperature then, obtains the compound lithium iron phosphate positive material of Graphene.The Graphene composite lithium iron phosphate conductance from pure phase 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.8g/cm
3Fig. 1 is the x-ray diffraction pattern, and the raw material LiFePO4 of analyzing gained is the LiFePO4 of pure olivine-type rhombic system phase structure, and Fig. 2 is the transmission electron microscope photo of composite material.
Active material iron phosphate powder, conductive agent acetylene black and binding agent Kynoar mixed to be applied to by mass ratio at 8.5: 0.5: 1 make positive plate on the aluminium foil.In the argon gas atmosphere dry glove box, be to electrode with metal lithium sheet, the UB3025 film is a barrier film, ethylene carbonate (EC)+dimethyl carbonate (DMC)+1MLiPF
6Be electrolyte, be assembled into the button cell test performance.
Under 20 ± 2 ℃, battery is carried out the constant current charge-discharge test in 2.5V～4.2V voltage range.Fig. 3 is with 0.2C multiplying power (34mAg
-1) the first charge-discharge curve, gained LiFePO 4 material discharge voltage is about 3.4V as can be known, reversible specific capacity is 95% of theoretical specific capacity up to 160mAh/g.High-rate charge-discharge capability excellence, 1C, 2C, 5C and 20C charge ratio capacity reach 153,143,115 and 100mAh/g (the 1C/1C gram volume is seen Fig. 3); Cycle performance of battery is also very superior.
Embodiment 2
Is being the abundant ball milling of liquid phase medium 2 hours with nano-grade lithium iron phosphate pure phase powder with by 0.1% Graphene of LiFePO4 weight ratio for 2 times of ethanol of all raw material weight ratios; insulation reaction is 5 hours in 300 ℃ of stoves of argon shield atmosphere are arranged; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.The conductance of compound front and back is from 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.9g/cm
3Products therefrom during with 1C and 20C multiplying power discharging specific capacity be about 145 and 96mAhg respectively
-1
Embodiment 3
Fully mixed 30 hours with nano-grade lithium iron phosphate pure phase powder with by 2.5% graphene oxide of LiFePO4 weight ratio; insulation reaction is 2 hours in 850 ℃ of stoves that hydrogen argon hybrid protection atmosphere is arranged; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.The conductance of compound front and back is from 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.75g/cm
3Products therefrom during with 1C and 20C multiplying power discharging specific capacity be about 152 and 103mAhg respectively
-1
Embodiment 4
The compound method preparing phosphate iron lithium of a kind of anode material for lithium-ion batteries Graphene; with lithium dihydrogen phosphate, ferrous oxalate as raw material; the mol ratio of control phosphorus, iron and lithium is 1.0: 1.0: 1.0 and the raw material of pressing LiFePO4 weight ratio 2.5% Graphene; evenly mixed 20 hours; insulation reaction is 10 hours in 600 ℃ of stoves of nitrogen hybrid protection atmosphere are arranged; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.The conductance of compound front and back is from 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.85g/cm
3Products therefrom during with 1C and 20C multiplying power discharging specific capacity be about 154 and 101mAhg respectively
-1
Embodiment 5
The compound method preparing phosphate iron lithium of a kind of anode material for lithium-ion batteries Graphene; with iron hydroxide, lithium carbonate, ammonium di-hydrogen phosphate and graphene oxide as raw material; the mol ratio of control phosphorus, iron and lithium is 1.0: 0.85: 0.95 and the raw material of pressing LiFePO4 weight ratio 5% graphene oxide; evenly mixed 20 hours; insulation reaction is 1 hour in 850 ℃ of stoves that hydrogen argon hybrid protection atmosphere is arranged; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.The conductance of the LiFePO4 of compound front and back is from 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.86g/cm
3Products therefrom during with 1C and 20C multiplying power discharging specific capacity be about 155 and 105mAhg respectively
-1
Embodiment 6
The compound method preparing phosphate iron lithium of a kind of anode material for lithium-ion batteries Graphene; with ferrous oxide, lithium carbonate, ammonium di-hydrogen phosphate and Graphene as raw material; the mol ratio of control phosphorus, iron and lithium is 1: 1: 1 and the raw material of pressing LiFePO4 weight ratio 0.5% Graphene; evenly mixed 50 hours; insulation reaction is 2 hours in 700 ℃ of stoves that hydrogen argon hybrid protection atmosphere is arranged; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.The conductance of the LiFePO4 of compound front and back is from 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.9g/cm
3Products therefrom during with 1C and 20C multiplying power discharging specific capacity be about 150 and 90mAhg respectively
-1
Embodiment 7
The compound method preparing phosphate iron lithium of a kind of anode material for lithium-ion batteries Graphene; with ferric phosphate, lithium carbonate and Graphene as raw material; the mol ratio of control phosphorus, iron and lithium is 1: 1: 1 and the raw material of pressing LiFePO4 weight ratio 5% graphene oxide; in the medium of ethanol, evenly mixed 2 hours; insulation reaction is 2 hours in 750 ℃ of stoves of nitrogen hybrid protection atmosphere are arranged; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.The conductance of the LiFePO4 of compound front and back is from 10
-9S/cm brings up to 10
-4The S/cm order of magnitude, tap density are 1.9g/cm
3Products therefrom during with 1C and 20C multiplying power discharging specific capacity be about 152 and 106mAhg respectively
-1
Claims (10)
1. lithium ion battery anode material lithium iron phosphate that Graphene is compound, the composite material that it is characterized in that LiFePO4 and Graphene is connected by the interface of chemical bonding.
2. the compound lithium ion battery anode material lithium iron phosphate of a kind of Graphene according to claim 1 is characterized in that Graphene is individual layer or is made up of the two-dimentional lonsdaleite material of the number of plies between 1 to 10.
3. the interface of chemical bonding according to claim 1 connects, and the interface that it is characterized in that chemical bonding is at LiFePO
4Reaction in-situ in generate.
4. the preparation method of the lithium ion battery anode material lithium iron phosphate that a kind of Graphene according to claim 1 is compound; it is characterized in that nano-grade lithium iron phosphate pure phase powder and fully mixed 2-50 hour by the 0.1-2.5% Graphene or the graphene oxide of LiFePO4 weight ratio; in the 300-850 ℃ of stove that nitrogen, argon gas or hydrogen argon hybrid protection atmosphere are arranged insulation reaction 0.1-5 hour; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.
5. the preparation method of the lithium ion battery anode material lithium iron phosphate that a kind of Graphene according to claim 1 is compound; it is characterized in that with iron content, lithium and phosphate radical be 1.0 in molar ratio: 0.85-1.00: 0.95-1.05 and the raw material of pressing LiFePO4 weight ratio 0.5-5% Graphene or graphene oxide; evenly mix; in the 600-850 ℃ of stove that nitrogen, argon gas or hydrogen argon hybrid protection atmosphere are arranged insulation reaction 1-10 hour; be cooled to room temperature then, obtain the compound lithium iron phosphate positive material of Graphene.
6. according to claim 1 and 5 described preparation methods, the even mixing that it is characterized in that the raw material of iron content, lithium, phosphate radical and Graphene or graphene oxide is that solid phase or solid-liquid machinery fully mix.
7. according to the preparation method of claim 1 and 5 described a kind of lithium ion battery anode material lithium iron phosphates, it is characterized in that the lithium source is a kind of or combination of lithia, lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate, lithium phosphate, lithium dihydrogen phosphate.
8. according to the preparation method of claim 1 and 5 described a kind of lithium ion battery anode material lithium iron phosphates, it is characterized in that source of iron is a kind of or combination of iron, ferrous oxide, tri-iron tetroxide, di-iron trioxide, ferrous sulfate, iron ammonium sulfate, ferric phosphate, ferrous phosphate, ferrous ammonium phosphate, ferrous citrate.
9. according to the preparation method of claim 1 and 5 described a kind of lithium ion battery anode material lithium iron phosphates, it is characterized in that the phosphorus source is a kind of or combination of phosphorus pentoxide, phosphoric acid, ammonium di-hydrogen phosphate, lithium dihydrogen phosphate, DAP, ferrous ammonium phosphate, phosphoric acid hydrogen ammonia salt.
10. according to claim 1 and 5 described graphene oxides, it is characterized in that carbon atom part grafting hydrogen-oxygen or carboxylic group on the Graphene.
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