CN107994214A - A kind of high-performance iron phosphate lithium composite material and preparation method thereof - Google Patents
A kind of high-performance iron phosphate lithium composite material and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
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Abstract
The invention belongs to field of lithium ion battery material preparation, specifically a kind of high-performance iron phosphate lithium composite material and preparation method thereof, specifically bombarded first by high velocity beam and nano metal or nano metal compound material are implanted into the top layer of LiFePO4, it is soaked in afterwards in catalyst solution, then graphene is grown to improve the electric conductivity of material and its high rate performance on its surface by chemical vapor deposition method.Graphene growth is significantly improved the compacted density and its electric conductivity of its material by its material prepared by chemical bond in LiFePO4 surface, and its doping metals are accurately controlled in the uniformity and its depth and quantity of material surface using particle injection method, the specific capacity of its material is improved, and is applied to high-energy-density density lithium ion battery.
Description
Technical field
The invention belongs to field of lithium ion battery material, be specifically related to a kind of high-performance iron phosphate lithium composite material and its
Preparation method.
Background technology
Lithium ion battery anode material lithium iron phosphate (LiFePO4) theoretical capacity is 170mAh/g, reversible charge specific capacity
It is higher, while there is the advantages such as raw material sources are extensive, pollution is low, security is good, has extended cycle life again, it is ideal at present
Power type and accumulation energy type anode material for lithium-ion batteries.But the ionic conductance of LiFePO4 and electron conductivity are relatively low,
It is only suitable for carrying out discharge and recharge under low current density, specific capacity reduces during high power charging-discharging, which has limited the application of the material,
Its specific capacity is relatively low at the same time, limits its popularization in high-energy-density density lithium ion field of batteries.Although both at home and abroad to ferric phosphate
Lithium has carried out substantial amounts of study on the modification to improve the electric conductivity of LiFePO4, main to include preparing nanoscale LiFePO4, carbon bag
Cover, the mode such as metal ion mixing, and carbon coating is the most frequently used simple method, i.e., mainly by being coated on LiFePO4 surface
The carbon source organic matters such as glucose sugar, sucrose improve its electric conductivity, such as patent（200610035986.1）Disclose a kind of high pressing
Be combined to the method for lithium iron phosphate positive material, this method its mainly by lithium salts, molysite, phosphate by lithium, iron, phosphorus chemistry based on
For amount than being uniformly mixed for 1: 1: 1 ratio, 6~24h of ball milling obtains presoma, and in its coated with carbon material, inventive method
Technique is simple, and raw material sources enrich, and can shorten the reaction time using high-pressure atmosphere, reduces reaction temperature, and products therefrom is actual to be held
Amount is high, and cycle performance is excellent, but the relatively low gram volume for influencing its material of the conductivity of its coated with carbon material play and its
High rate performance.Patent（CN1958441A）Disclose a kind of preparation method of LiFePO 4 powder, its mainly by by lithium salts,
Molysite, microcosmic salt, the organic matter precursor of a small amount of carbon and doped metal ion are according to matching and carry out high-performance ball milling mixing simultaneously
High performance LiFePO 4 material is prepared, but the implant uniformity of metal ion is poor and its there is ladder between LiFePO4
Degree difference causes its performance not give full play to, and the combination force difference between surface coated carbon material and metal, and uniformity is poor, influences
The comprehensive performance of its material plays.
The content of the invention
For current LiFePO 4 material gram volume and its conductivity it is relatively low there are the problem of, the present invention provides a kind of high
The chemical property such as performance composite ferric lithium phosphate material, the conductivity of the composite material, specific capacity is high.
Present invention also offers a kind of preparation method of above-mentioned composite material, this method is sunk by particle injection method and gas phase
Area method improves the gram volume and conduction of its material in its LiFePO 4 material surface doping metallic element and its coated graphite alkene
Rate, and controllable preparation has been carried out to material.
To achieve the above object, the present invention uses following technical scheme:
A kind of high-performance iron phosphate lithium composite material, the composite ferric lithium phosphate material by LiFePO4 and its nano metal or
The complex of nano metal compound composition, and formed in complex surfaces coated graphite alkene；Wherein described nano metal or
The quality of nano metal compound accounts for the 0.5%~5% of LiFePO4 quality；The quality of the graphene accounts for LiFePO4 quality
0.5%~5%.
Further, nano metal or nano metal the compound particle diameter is 100nm~500nm；The nanogold
Belong to for nano-titanium simple substance, nanometer Mg simple substance, nanostructured manganese simple substance, nano V simple substance, nanometer niobium simple substance, nanometer chromium simple substance or Nano-Zinc
Simple substance；The nano metal compound for nano-titanium fluoride, nanometer Mg fluoride, nanostructured manganese fluoride, nano V fluoride,
Nanometer niobium fluoride, nanometer chromium fluoride, Nano-Zinc fluoride.
The preparation method of above-mentioned composite material, it is characterised in that using following steps：
1）It is prepared by ferric lithium phosphate precursor：
Nano metal or nano metal compound are implanted in the top layer of LiFePO4 bulk material by particle injection method and obtained
To persursor material A, compound concentration is the catalyst solution of 5%-20%, and the catalyst solution is mixed with citric acid to be mixed
Persursor material A, is then added in mixed solution B by solution B, is 20 DEG C~100 DEG C immersion 1h~24h in temperature, afterwards
Material C is obtained by being dried in vacuo, crushing；The molar ratio of wherein described catalyst and citric acid is 1:1~10；Materials A is with mixing
The mass ratio for closing solution B is 5~20：200；
2）The preparation of LiFePO4/grapheme material：
Material C is inserted in the middle part of tube type resistance furnace, is heated up under argon gas or nitrogen protection；Kept the temperature after being warming up to 600~1200 DEG C,
Stop logical argon gas or nitrogen, change logical 1~350min of hydrogen, then kept the temperature at 600~1200 DEG C, stop logical hydrogen, change logical carbon source
1~300min of gas；Finally it is cooled to room temperature under the protection of argon gas or nitrogen, that is, obtains the LiFePO4 composite wood
Material.
Further, step（1）The particle injection method parameter is, the high-velocity particles be infused in selected from argon gas,
Carried out under any one atmosphere of oxygen, nitrogen, ammonia or two kinds of atmosphere；Gas flow is 5~60sccm, air pressure 2 × 10-4~
5×10-4Pa, implantation temperature is at 100~500 DEG C.
Preferably, the atmosphere is oxygen or ammonia.
Preferably, step（1）The catalyst is Nanoscale Iron, nanometer cobalt or nano nickel, its particle diameter for 50nm~
500nm。
Preferably, the carbon-source gas are one kind in acetylene, methane and its natural gas.
Particle injection method is a kind of new modified technology to grow up in recent years, i.e., is bombarded by high velocity beam by institute
Element is needed to be injected into material matrix, it has the advantages that the uniformity is high, strong with reference to power, while can be wanted according to technical parameter
Ask, injection different size, the nano-particle of different depth, it, which adulterates particle and material precursor and has, combines that power is strong, stability
High characteristic, and combine vapour deposition process and combine the strong graphene composite material of power in its surface cladding, it can further improve
The conductivity of its material.
Beneficial effect：
1）Mixed with nano metal thing is injected into inside LiFePO4 and its top layer by the present invention, have the uniformity it is high, with reference to power it is strong,
Process control, while metal ion is to be combined by Physical with LiFePO4, side reaction, which will not occur, makes its chemical stability
Height, and the present invention can adjust the species, injection depth and its number of particles of nano metal, process control, relatively using chemistry
Method doped metal ion has obvious advantage.
2）The present invention adsorbs catalyst solution makes its catalyst solution be immersed in material on ferric lithium phosphate precursor surface
Internal and surface, by the inducing action for the catalyst iron of connection, cobalt or nickel, makes the carbon atom in carbon-source gas in phosphoric acid
The connection of chemical bond is formed on contact point between iron lithium, so that LiFePO4 and grapheme material be by chemical key connection,
Combination power and its electric conductivity between graphene coated layer and LiFePO4 can be improved, graphene is sunk by vapour deposition process
Product has the advantages that the uniformity is high, cladding thickness is small and its mechanical strength is big on LiFePO4 surface and its inside, can be obvious
The conductivity and its gram volume for improving its material play, and significantly improve the electrochemistry such as the specific capacity of its composite ferric lithium phosphate material
Performance.
Brief description of the drawings
Fig. 1 is the SEM figures for the composite ferric lithium phosphate material that embodiment 1 is prepared.
Embodiment
The present invention is further illustrated with comparative example in conjunction with the embodiments, it should explanation, the description below be only for
Explain the present invention, its content is not defined.
The preparation of ferric lithium phosphate precursor uses following methods in the embodiment of the present invention：
Using lithium dihydrogen phosphate LiH2PO4, di-iron trioxide Fe2O3, magnesium hydroxide Mg (OH)2For raw material, by atomic ratio Li: Fe:
Mg: P=1: 0.99: 0.01: 1, by 31179g LiH2PO4、23715gFe2O3、174.9gMg(OH)2, 3420g nano zircites
Ball is added in ball mill；Deionized water 70kg, wet-milling 12h are added afterwards；Above-mentioned slurry is spray-dried afterwards, does spraying
Dry machine inlet temperature is 200~350 DEG C, and outlet temperature is not less than 120 DEG C, obtains spherical LiFePO 4 material body.
Embodiment 1
First by particle injection method, carried out under oxygen atmosphere, gas flow 30sccm, air pressure 3 × 10-4Under Pa, adjustment
Implantation temperature be 300 DEG C, by quality for 5g, a diameter of 200nm nano-titanium be injected into 100g LiFePO4 bodies, carry out afterwards
Crush, classification is obtained in ferric lithium phosphate precursor A；
The Raney nickel that 5.8g particle diameters are 100nm is weighed at the same time with 96g citric acids to be added in the deionized water of 914ml and make
Concentration be 10% mixed solution（Abbreviation B solution）.
10g persursor materials A is added in 200ml solution Bs afterwards, and is 60 DEG C of immersion 12h in temperature, is passed through afterwards
Vacuum drying, crushing obtain material C；
Material C is inserted in the middle part of tube type resistance furnace afterwards, is heated up under argon gas protection；120min is kept the temperature after being warming up to 800 DEG C, is changed
Logical hydrogen 120min, then keeps the temperature 2h at 900 DEG C, is passed through methane gas 60min；Finally room is cooled under the protection of argon gas
Temperature obtains composite ferric lithium phosphate material.
Embodiment 2
First by particle injection method, carried out under ammonia atmosphere, gas flow 5sccm, air pressure 2 × 10-4Under Pa, adjustment
Implantation temperature be 100 DEG C, by quality for 5g, a diameter of 100nm nano V be injected into 100g LiFePO4 bodies, it is laggard
Row crushes, classification is obtained in ferric lithium phosphate precursor A；
The Co catalysts that 5.9g particle diameters are 10nm are weighed after at the same time with 19.2g citric acids to be added in the deionized water of 100ml
The concentration made is 20% mixed solution（Abbreviation B solution）.
5g persursor materials A is added in 200ml solution Bs afterwards, and is 20 DEG C of immersion 24h in temperature, is passed through afterwards
Vacuum drying, crushing obtain material C；
Material C is inserted in the middle part of tube type resistance furnace afterwards, is heated up under argon gas protection；2h is kept the temperature after being warming up to 600 DEG C, changes logical hydrogen
Gas 60min, then keeps the temperature 2h at 1000 DEG C, is passed through acetylene gas 10min；Finally it is cooled to room temperature under the protection of argon gas
To composite ferric lithium phosphate material.
Embodiment 3
First by particle injection method, carried out under oxygen atmosphere, gas flow 60sccm, air pressure 5 × 10-4Under Pa, adjustment
Implantation temperature be 500 DEG C, by quality for 5g, a diameter of 500nm nanometer chromium be injected into 100g LiFePO4 bodies, it is laggard
Row crushes, classification is obtained in ferric lithium phosphate precursor A；
The Co catalysts that 5.5g particle diameters are 200nm are weighed at the same time with 192g citric acids to be added in the deionized water of 3752ml and prepare
Go out the mixed solution that concentration is 5%（Abbreviation B solution）.
20g persursor materials A is added in 200ml solution Bs afterwards, and is 100 DEG C of immersion 1h in temperature, is passed through afterwards
Vacuum drying, crushing obtain material C；
Material C is inserted in the middle part of tube type resistance furnace afterwards, is heated up under nitrogen protection；2h is kept the temperature after being warming up to 800 DEG C, changes logical hydrogen
Gas 60min, then keeps the temperature 1h at 1200 DEG C, is passed through natural gas gas 10min；Finally it is cooled to room temperature under the protection of nitrogen
Obtain composite ferric lithium phosphate material.
Comparative example：
Spherical LiFePO 4 material body is put into the middle part of tube furnace, is heated up under argon gas protection；Kept the temperature after being warming up to 800 DEG C
2h, changes logical hydrogen 120min, then keeps the temperature 2h at 900 DEG C, be passed through methane gas 60min；It is finally cold under the protection of argon gas
But to room temperature.
The measure of various physical property, evaluation are carried out as follows in above example：
1）SEM is tested
Fig. 1 be embodiment 1 prepare obtain the SEM of composite ferric lithium phosphate material, in Fig. 1 as can be seen that material presentation ball
Shape, size distribution is uniform, and particle diameter exists（1~10）Between μm.
2）Button cell is tested：
Respectively by embodiment 1~3 and comparative example gained lithium-ion battery lithium iron phosphate material be assembled into button cell A1, A2,
A3 and B1；Its preparation method is：Binding agent, conductive agent and solvent are added in LiFePO 4 material, is stirred slurrying, is coated
It is obtained by drying, rolling on aluminium foil.Binding agent used is PVDF binding agents, and conductive agent SP, positive electrode is embodiment 1
~3 and the positive electrode prepared of comparative example, solvent NMP, its ratio be：Positive electrode：SP：PVDF：NMP=93g:3.5g:
3.5g:200ml；Electrolyte is LiPF6/EC+DEC（1:1), metal lithium sheet is to electrode, and membrane uses polyethylene (PE), poly- third
Alkene (PP) or poly- second propylene (PEP) composite membrane, simulated battery are assemblied in the glove box for be flushed with hydrogen gas and carry out, and chemical property is in force
Carried out on the new prestige 5v/10mA type cell testers of the blue electricity of the Chinese, charging/discharging voltage scope is 2.5V to 4.2V, and charge-discharge velocity is
0.1C。
It is as shown in Figure 1 to detain electrical test results.
1 embodiment of table buckles electrical test results contrast with comparative example
As it can be seen from table 1 using electric battery is detained made from 1~3 gained positive electrode of embodiment, its discharge capacity and efficiency are all
Apparently higher than comparative example.Test result indicates that positive electrode of the invention can make battery have good discharge capacity and efficiency.
Reason is：The doped metallic elements in LiFePO4, the gram volume for improving its material play, while the graphene of surface growth
Have the characteristics that conductivity is high, imbibition ability is strong, improve the transmission rate of lithium ion in its charge and discharge process, and improve it first
Efficiency.At the same time in material doped with high specific density metal-doped element improve its material tap density and material in graphite
Alkene is to be connected to by chemical bond in kernel LiFePO4 body, with reference to power by force so as to improve its tap density.
（2）Soft-package battery is tested
Respectively with embodiment 1, embodiment 2, the LiFePO 4 material that embodiment 3 and comparative example are prepared as positive electrode, and
Anode pole piece is prepared, using Delanium as negative material, using LiPF6/EC+DEC（Volume ratio 1: 1）For electrolyte,
2400 films of Celgard are membrane, prepare 5Ah soft-package battery C1, C2, C3 and D1, and test the cycle performance of its soft-package battery
And high rate performance；
Multiplying power test parameter：Rate of charge is 0.5C, discharge-rate 0.5C, 1.0C, 2.0C, 4.0C, 8.0C, temperature be 23 ±
3 DEG C, voltage is 2.5 ~ 4.2V；
Cycle performance test parameter：Multiplying power is 1.0C/1.0C, under conditions of voltage is 2.5 ~ 4.2V.
The high rate performance and cycle performance form that table 2 is tested for embodiment and comparative example.
Table 2, embodiment are compared with the chemical property of comparative example
As can be seen from Table 2, the cycle performance for the material that embodiment is prepared is substantially better than comparative example, the reason for this is that graphene
LiFePO4 surface and its inside are firmly incorporated into by chemical bond, has and combines power is strong, conductivity is high, imbibition ability is high etc.
Characteristic, make its material and its battery improved in charge and discharge process its electronics transmission rate and its heat dissipation performance so as to improving it
The cycle performance of soft-package battery.Simultaneously because metallic element is entrained in LiFePO4 by particle injection method, uniformity height,
The consistency height of doping particle causes its stability high, so as to further improve the cycle performance of its material.
At the same time from table 2 it can be seen that the high rate performance for the soft-package battery that embodiment is prepared is also superior to comparative example, its reason
For under big multiplying power, the characteristic that surface coated graphene has electronic conductivity high improves the high rate charge-discharge energy of its material
Power.
Claims (7)
1. a kind of high-performance iron phosphate lithium composite material, it is characterised in that the composite ferric lithium phosphate material is by LiFePO4
And its nano metal or nano metal compound composition complex, and formed in complex surfaces coated graphite alkene；It is wherein described
Nano metal or the quality of nano metal compound account for the 0.5%~5% of LiFePO4 quality；The quality of the graphene accounts for phosphorus
The 0.5%~5% of sour iron lithium quality.
2. composite material according to claim 1, it is characterised in that nano metal or nano metal the compound particle diameter
For 100nm~500nm；The nano metal is nano-titanium simple substance, nanometer Mg simple substance, nanostructured manganese simple substance, nano V simple substance, is received
Rice niobium simple substance, nanometer chromium simple substance or Nano-Zinc simple substance；The nano metal compound is nano-titanium fluoride, nanometer Mg is fluorinated
Thing, nanostructured manganese fluoride, nano V fluoride, nanometer niobium fluoride, nanometer chromium fluoride, Nano-Zinc fluoride.
3. the preparation method of the composite material described in a kind of claim 1, it is characterised in that using following steps：
1）It is prepared by ferric lithium phosphate precursor：
Nano metal or nano metal compound are implanted in the top layer of LiFePO4 bulk material by particle injection method and obtained
To persursor material A, compound concentration is the catalyst solution of 5%-20%, and the catalyst solution is mixed with citric acid to be mixed
Persursor material A, is then added in mixed solution B by solution B, is 20 DEG C~100 DEG C immersion 1h~24h in temperature, afterwards
Material C is obtained by being dried in vacuo, crushing；The molar ratio of wherein described catalyst and citric acid is 1:1~10；Materials A is with mixing
The mass ratio for closing solution B is 5~20：200；
2）The preparation of LiFePO4/grapheme material：
Material C is inserted in the middle part of tube type resistance furnace, is heated up under argon gas or nitrogen protection；Kept the temperature after being warming up to 600~1200 DEG C,
Stop logical argon gas or nitrogen, change logical 1~350min of hydrogen, then kept the temperature at 600~1200 DEG C, stop logical hydrogen, change logical carbon
1~300min of source gas body；Finally it is cooled to room temperature under the protection of argon gas or nitrogen, that is, obtains the LiFePO4 composite wood
Material.
4. the preparation method of composite material according to claim 3, it is characterised in that step（1）The particle injection
Method parameter is that the high-velocity particles is infused in selected from any one atmosphere of argon gas, oxygen, nitrogen, ammonia or two kinds of atmosphere
Lower progress；Gas flow is 5~60sccm, air pressure 2 × 10-4~5 × 10-4Pa, implantation temperature is at 100~500 DEG C.
5. the preparation method of composite material according to claim 4, it is characterised in that the atmosphere is oxygen or ammonia
Gas.
6. the preparation method of composite material according to claim 3, it is characterised in that step（1）The catalyst is
Nanoscale Iron, nanometer cobalt or nano nickel, its particle diameter are 50nm~500nm.
7. preparation method according to claim 3, it is characterised in that the carbon-source gas are acetylene, methane or natural gas.
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| CN111653736A (en) * | 2020-04-17 | 2020-09-11 | 中国航发北京航空材料研究院 | Preparation method of double-coating-layer positive electrode composite material |
| CN114122357A (en) * | 2021-11-10 | 2022-03-01 | 云南中晟新材料有限责任公司 | Lithium salt-coated graphene-doped silicon-carbon composite material and preparation method thereof |
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| CN106129374A (en) * | 2016-08-26 | 2016-11-16 | 深圳博磊达新能源科技有限公司 | A kind of transition metal oxide/binary carbon net anode composite material and aluminium ion battery |
| CN106876708A (en) * | 2017-04-12 | 2017-06-20 | 中国科学院金属研究所 | A kind of method that metal sulfide is applied to cathode plate for lithium secondary battery |
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| CN111653736A (en) * | 2020-04-17 | 2020-09-11 | 中国航发北京航空材料研究院 | Preparation method of double-coating-layer positive electrode composite material |
| CN111653736B (en) * | 2020-04-17 | 2022-08-09 | 中国航发北京航空材料研究院 | Preparation method of double-coating-layer positive electrode composite material |
| CN114122357A (en) * | 2021-11-10 | 2022-03-01 | 云南中晟新材料有限责任公司 | Lithium salt-coated graphene-doped silicon-carbon composite material and preparation method thereof |
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