CN102347473A - Anode composite material particle of lithium ion battery and preparation method thereof - Google Patents
Anode composite material particle of lithium ion battery and preparation method thereof Download PDFInfo
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- CN102347473A CN102347473A CN2010102425224A CN201010242522A CN102347473A CN 102347473 A CN102347473 A CN 102347473A CN 2010102425224 A CN2010102425224 A CN 2010102425224A CN 201010242522 A CN201010242522 A CN 201010242522A CN 102347473 A CN102347473 A CN 102347473A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to an anode composite material particle of a lithium ion battery and a preparation method thereof. The composite material particle comprises anode active substance particles and an aluminium phosphate layer cladded thereon. The invention also relates to the preparation method of the anode composite material particle of a lithium ion battery. The method comprises steps of: providing an aluminium nitrate solution; adding anode active substance particles to be cladded in the aluminium nitrate solution, controlling an addition of the anode active substance and forming a mixture; adding a phosphate solution into the mixture for reaction to form an aluminium phosphate layer on the anode active substance particle surfaces; and carrying out heat treatment on anode active substance particle with the aluminium phosphate layer to obtain the anode composite material particles.
Description
Technical field
The present invention relates to a kind of anode composite material of lithium ion battery particle and preparation method thereof, relate in particular to a kind of anode composite material of lithium ion battery particle and preparation method thereof with aluminum phosphate.
Background technology
Adopting other material to form to the particle surface of active substance of lithium ion battery anode and coat, is the common method of in the prior art positive active material being carried out modification.For example, coat one deck carbon at the particle surface of LiFePO4 and can effectively solve the lower problem of LiFePO4 conductivity, make the LiFePO4 that is coated with carbon-coating have conductivity preferably.In addition, prior art shows, coats the thermal stability that aluminum phosphate can improve lithium ion cell positive at cobalt acid lithium or other positive active material particle surface and (sees also document " Correlation between AlPO
4Nanoparticle coating thickness on LiCoO
2Cathode and thermal stablility " J.Cho, Electrochimica Acta 48 (2003) 2807-2811 and the patent No. are 7,326,498 United States Patent (USP)).
Method with aluminum phosphate clad anode active material in the prior art is to prepare the dispersion liquid that the aluminum phosphate Dispersion of Particles forms in water earlier; And in the dispersion liquid with this aluminum phosphate particle for preparing of positive active material particle adding; Effect through absorption makes the aluminum phosphate particle be adsorbed on the positive active material large particle surface; Again with the water evaporate to dryness in the dispersion liquid; And, form the positive active material that the surface has the aluminum phosphate particle 700 ℃ of following heat treatments.
Yet; Because aluminum phosphate is water insoluble; The aluminum phosphate particle possibly form reunion when in water, disperseing; And when adding a large amount of positive active materials in the aluminum phosphate dispersion liquid; The positive active material that adds adsorbs a large amount of aluminum phosphate particles earlier, and the positive active material particle that the back adds then possibly adsorb less than enough aluminum phosphate particles.See also Fig. 8, even can be good at coating, this product 20 of said method decision sees that from microcosmic to be aluminum phosphate be distributed in positive active material bulky grain 24 surfaces with the form of granule 22, is not the even aluminum phosphate material layer of one deck.Therefore; Even inadequately through said method at the aluminum phosphate coating layer that the positive active material surface forms; Can't guarantee that each positive active material surface all can coat one deck aluminum phosphate uniformly; Thereby make the lithium ion battery cycle performance of using this positive active material bad, make this method be difficult to heavy industrialization and use.
Summary of the invention
In view of this, necessaryly provide a kind of and can form the method for even aluminum phosphate coating layer, and have the positive active material of this aluminum phosphate coating layer on positive active material surface.
A kind of anode composite material of lithium ion battery particle, the phosphoric acid aluminium lamination that it comprises the positive active material particle and is coated on this positive active material particle surface.
A kind of preparation method of anode composite material of lithium ion battery particle, it comprises: aluminum nitrate solution is provided; Positive active material particle to be coated is added in this aluminum nitrate solution, control the addition of this positive active material, form a muddy mixture; Phosphate solution is added this muddy mixture react, form the phosphoric acid aluminium lamination at this positive active material particle surface; And this surface of heat treatment has the positive active material particle of phosphoric acid aluminium lamination, obtains the anode composite material particle.
Compared to prior art, the present invention has avoided causing aluminum phosphate to coat uneven phenomenon because the absorption that solid mixing produces is inhomogeneous, is fit to the heavy industrialization application.In addition, the present invention can generate the even and continuous phosphoric acid aluminium lamination of a layer thickness at the positive active material particle surface, but not with the aluminum phosphate particle packing at the positive active material particle surface, therefore have better chemical property.
Description of drawings
Fig. 1 is the structural representation of embodiment of the invention aluminum phosphate clad anode active material.
Fig. 2 coats the stereoscan photograph of cobalt acid lithium for embodiment of the invention aluminum phosphate.
Fig. 3 coats the transmission electron microscope photo of cobalt acid lithium for embodiment of the invention aluminum phosphate.
Fig. 4 is the stereoscan photograph that the aluminum phosphate of contrast experiment's high power amplification coats cobalt acid lithium.
Fig. 5 is the stereoscan photograph that the aluminum phosphate of contrast experiment's low power amplification coats cobalt acid lithium.
Fig. 6 is the cycle performance test curve of the positive active material of embodiment of the invention aluminum phosphate coating.
Fig. 7 is the cycle performance test curve of the positive active material that coats of contrast experiment's aluminum phosphate.
Fig. 8 is the structural representation of the aluminum phosphate clad anode active material of prior art.
The main element symbol description
Anode composite material particle 10
Positive active material particle 12
Phosphoric acid aluminium lamination 14
Granule 22
Embodiment
To combine accompanying drawing and specific embodiment that anode composite material particle provided by the invention and preparation method thereof is done further to describe in detail below.
See also Fig. 1, the embodiment of the invention provides a kind of anode composite material particle 10, the phosphoric acid aluminium lamination 14 that it comprises positive active material particle 12 and is coated on this positive active material particle surface.The mass percent of this phosphoric acid aluminium lamination 14 in this anode composite material particle 10 is 0.1% to 3%.The thickness of this phosphoric acid aluminium lamination 14 is preferably 5 nanometer to 20 nanometers.This phosphoric acid aluminium lamination 14 is created on this positive active material particle 12 surfaces for original position.This phosphoric acid aluminium lamination 14 is the even and continuous aluminum phosphate material layer of thickness.Further, 12 of this phosphoric acid aluminium lamination 14 and this positive active material particles possibly form interfacial diffusion at the interface, cobalt atom is diffused in this phosphoric acid aluminium lamination 14.
The material of this positive active material particle 12 can be by chemical formula Li
xCo
1-yM
yO
2, Li
xMn
1-yM
yO
2Or Li
xFe
1-yM
yPO
4Expression, 0.1≤x≤1.1,0≤y≤0.9 wherein, M is selected from least a among Mn, Cr, Co, Ni, V, Ti, Al, Ga and the Mg.Preferably, the material of this positive active material particle 12 is the cobalt acid lithium (Li of stratiform
xCoO
2), the LiMn2O4 (Li of stratiform
xMnO
2) or olivine-type LiFePO4 (Li
xFePO
4).
It is a kind of with aluminum phosphate coated lithium ion battery positive active material that the embodiment of the invention provides, and forms the method for said anode composite material particle 10, and it may further comprise the steps:
Step 1 provides aluminum nitrate solution;
Step 2 adds positive active material particle to be coated in this aluminum nitrate solution, forms a mixture;
Step 3 adds this mixture with phosphate solution and reacts, and makes this positive active material particle surface form the phosphoric acid aluminium lamination; And
Step 4, this surface of heat treatment has the positive active material particle of phosphoric acid aluminium lamination, obtains the anode composite material particle.
This aluminum nitrate solution comprises liquid phase solvent and is dissolved in the aluminum nitrate of this solvent.Being appreciated that this solvent is chosen as can make aluminum nitrate dissociate to form Al
3+Solvent get final product.Therefore this solvent is not limited to water, can also be volatile organic solvent, and preferably, this solvent is one or several mixing in ethanol, acetone, dichloroethanes and the chloroform.With respect to adopting water, as solvent, can avoid the reaction of positive active material particle and water to make the reduction of positive active material performance with organic solvent such as ethanol as solvent.
In above-mentioned steps two, this positive active material particle is insoluble to this aluminum nitrate solution, and both mix for solid-liquid, and purpose is evenly to adhere to one deck Al on the surface of this positive active material particle
3+Because Al
3+Exist with ionic species, can be attached to the positive active material particle surface uniformly, this positive active material particle is formed the coating of atom level.Further, the addition of this positive active material of may command, the ratio of this positive active material particle and aluminum nitrate solution is controlled to be made as and to make this aluminum nitrate solution can cover this positive active material particle surface to get final product, make the mixture that obtains be muddy.The purpose that forms the muddy mixture mainly is just enough to form one deck aluminum phosphate coating layer at the positive active material particle surface for the addition of controlling aluminum nitrate solution.Particularly, the volume ratio of the volume of this aluminum nitrate solution and this positive active material particle is about 1: 10 to 1: 40.This positive active material particle grain size is preferably less than 20 microns.The addition of this aluminum nitrate solution can account for the mass percent of anode composite material particle through the aluminum phosphate coating layer that needs form and confirm that preferably, the mass percent of this aluminum phosphate coating layer in this anode composite material particle is 0.1% to 3%.
In above-mentioned steps three, this phosphate solution comprises water as solvent, and the soluble phosphate that is dissolved in this solvent, like phosphoric acid ammonia salt.This phosphoric acid ammonia salt comprises ammonium dihydrogen phosphate (NH
4H
2PO
4), diammonium hydrogen phosphate ((NH
4)
2HPO
4) and triammonium phosphate ((NH
4)
3PO
4) in one or more mixing.Contain phosphate anion in this phosphate solution.This phosphate anion can be positive phosphorus acid ion (PO
4 3-), dihydrogen phosphate ions (H
2PO
4 -) and phosphoric acid one hydrogen radical ion (HPO
4 2-) in one or more mixing.When this phosphate solution is added to said muddy mixture, this phosphate anion and the Al that is attached to the positive active material particle surface
3+Reaction, thus layer of even aluminum phosphate deposition formed in positive active material particle surface original position.Preferably, this phosphate solution can dropwise add this muddy mixture, and stirs, thereby makes this phosphate anion and this Al
3+Can react uniformly at this positive active material particle surface.With aluminum nitrate solution similarly, the addition of this phosphate solution can account for the mass percent of anode composite material particle through the aluminum phosphate coating layer that needs form and confirm.
In above-mentioned steps four, this heat treated purpose is that this aluminum phosphate is better being combined with positive active material at the interface, forms composite material, and removes the ammonium nitrate of residual solvent and reaction generation.Through this heat treatment, possibly form interfacial diffusion at the interface at aluminum phosphate and positive active material, cobalt atom is diffused in this phosphoric acid aluminium lamination.This heat treatment temperature can be 400 ℃ to 800 ℃.This heat treatment period is preferably 0.5 to 2 hour.
Because this method joins the positive active material particle in the aluminum nitrate solution earlier; In this aluminum nitrate solution, add the phosphate solution that can generate aluminum phosphate again with the aluminium ion reaction, thereby at the continuous phosphoric acid aluminium lamination of positive active material particle surface original position generation one deck.Because the aluminum nitrate solution of liquid phase mixes with the positive active material particle of solid phase; Can make aluminium ion be coated on this positive active material particle surface uniformly earlier; Therefore, the aluminum phosphate deposition that is generated by aluminium ion behind the reaction in-situ also can more evenly be coated on this positive pole active particle surface.With earlier synthetic aluminum phosphate particle; The mode that makes the aluminum phosphate particle be adsorbed onto the positive active material particle surface through suction-operated is compared again; This method has been avoided causing aluminum phosphate to coat uneven phenomenon because the absorption that solid mixing produces is inhomogeneous, is fit to the heavy industrialization application.In addition, this method can generate the even and continuous phosphoric acid aluminium lamination of a layer thickness at the positive active material particle surface, but not with the aluminum phosphate particle packing at the positive active material particle surface.This phosphoric acid aluminium lamination can pass through ion in the electron transfer between isolated electrolyte and the active material; Thereby avoid electrolyte under high voltage, to decompose in the embedding of accomplishing lithium ion with when deviating from, therefore make this positive active material can under high voltage, have better battery performance and capacity maintenance performance.
Embodiment
Present embodiment specifically adopts said method to prepare said anode composite material particle through aluminum phosphate clad anode active material particle, and this anode composite material particle is applied to carry out in the lithium ion battery performance test.This positive active material particle can be cobalt acid lithium or doping cobalt acid lithium particle, and present embodiment is a cobalt acid lithium particle.This aluminum phosphate-cobalt acid lithium composite material particle comprises cobalt acid lithium particle and is coated on the phosphoric acid aluminium lamination of this cobalt acid lithium particle surface.
In the preparation of this aluminum phosphate-cobalt acid lithium composite material particle, this aluminum nitrate solution is the solution that aluminum nitrate forms in ethanol.The volume of this aluminum nitrate solution is 30 milliliters, and molar concentration is 0.16 mol.The addition of this cobalt acid lithium particle is 100g.This phosphate solution is (NH
4)
2HPO
4The aqueous solution.Be respectively 400 ℃, 500 ℃ and 600 ℃ in heat treatment temperature, the mass percent that the phosphoric acid aluminium lamination accounts for gross mass is to prepare 3 kinds of aluminum phosphates-cobalt acid lithium composite material particulate samples under 1% the condition.In addition, be 600 ℃ in heat treatment temperature, the mass percent that the phosphoric acid aluminium lamination accounts for gross mass is to prepare a kind of aluminum phosphate-cobalt acid lithium composite material particulate samples under 1.5% the condition.See also Fig. 2 and Fig. 3; In the sample that obtains; The phosphoric acid aluminium lamination is coated on this cobalt acid lithium particle surface uniformly, through the high magnification transmission electron microscope observing, can see clearly that this aluminum phosphate is that form with the uniform material layer of thickness covers this cobalt acid lithium particle surface.Respectively with these 4 kinds of samples as positive electrode active materials; Mix with a certain proportion of conductive agent and binding agent and to be coated on the anode collection surface and to process positive pole; With metal lithium sheet as negative pole; Positive pole and negative pole are assembled into lithium ion battery at interval and with the electrolyte infiltration through barrier film, carry out the charge-discharge performance test.
The contrast experiment
For the anode composite material particle with embodiment of the invention preparation compares, with another comparative sample of method preparation of prior art, concrete steps are:
With (NH
4)
2HPO
4The aqueous solution mixes with aluminum nitrate aqueous solution, in water, generates the aluminum phosphate particle, forms dispersion liquid;
Cobalt acid lithium particle is dropped in this dispersion liquid, make the aluminum phosphate particle be adsorbed on cobalt acid lithium particle surface through the effect of adsorbing; And
600 ℃ of these surface adsorption of following heat treatment the cobalt acid lithium particle of aluminum phosphate particle is arranged, obtain said comparative sample.See also Fig. 4 and Fig. 5, in the comparative sample through art methods preparation, aluminum phosphate is that the form of particle accumulates in this cobalt acid lithium particle surface, and the aluminum phosphate particle reunites, and makes coating inhomogeneous.
As positive electrode active materials, the charge-discharge performance test is carried out in assembled battery under the condition identical with present embodiment with this comparative sample.The cobalt acid lithium particle that also will not coat any material in addition is assembled into lithium ion battery as positive electrode active materials under the condition identical with present embodiment, carry out the charge-discharge performance test.Above-mentioned present embodiment and contrast experiment's difference only is positive electrode active materials, and other battery condition and test condition are all identical.
Be coated with the positive active material particle of aluminum phosphate; Because the aluminum phosphate that plays the coating effect has improved the surface texture of positive active material particle; Provide to take off to lithium ion and owed platform; Play the effect on barrier layer simultaneously; Suppress the reaction of tetravalence cobalt ions and electrolyte effectively; Stablize cobalt acid lithium structure, improved the electrochemistry cycle performance.See also Fig. 6, above-mentioned 4 kinds of samples are carried out the constant current charge-discharge loop test under the 0.5C electric current, the cut-ff voltage of this charging is 4.5V, and the cut-ff voltage of discharge is 2.7V.From figure, can find; Adopt the sample of the inventive method preparation; Because aluminum phosphate can coat cobalt acid alumina particles uniformly; Charging still can have higher capacity and stable capability retention under high voltage; Capability retention after 50 circulations is all more than 90%, and specific capacity is 160mAh/g to 175mAh/g.And along with the raising of heat treatment temperature, the capacity of battery increases to some extent.The change of this aluminum phosphate percentage composition is little to the influence of battery capacity.See also Fig. 7; The circulation volume of the cobalt acid lithium particulate samples of this comparative sample and not coating then sharply descends; Capability retention after 50 circulations is all less than 85%; This mainly is because cobalt acid lithium particle coats inhomogeneous or do not coat; Make when under high pressure charging the capacity reduction that cobalt acid lithium and electrolyte react and makes battery.
In addition, those skilled in the art also can do other variations in spirit of the present invention, and certainly, these all should be included within the present invention's scope required for protection according to the variation that the present invention's spirit is done.
Claims (16)
1. anode composite material of lithium ion battery particle, it comprises the positive active material particle, it is characterized in that, further comprises the phosphoric acid aluminium lamination that is coated on this positive active material particle surface.
2. anode composite material of lithium ion battery particle as claimed in claim 1 is characterized in that, the mass percent of this phosphoric acid aluminium lamination in this anode composite material particle is 0.1% to 3%.
3. anode composite material of lithium ion battery particle as claimed in claim 1 is characterized in that, the mass percent of this phosphoric acid aluminium lamination in this anode composite material particle is 1% to 1.5%.
4. anode composite material of lithium ion battery particle as claimed in claim 1 is characterized in that, the thickness of this phosphoric acid aluminium lamination is 5 nanometer to 20 nanometers.
5. anode composite material of lithium ion battery particle as claimed in claim 1 is characterized in that, this phosphoric acid aluminium lamination is that original position is created on this positive active material particle surface.
6. anode composite material of lithium ion battery particle as claimed in claim 1 is characterized in that, this aluminum phosphate layer thickness is even and continuous.
7. anode composite material of lithium ion battery particle as claimed in claim 1 is characterized in that the material of this positive active material particle is by chemical formula Li
xMn
1-yM
yO
2, or Li
xFe
1-yM
yPO
4Expression, 0.1≤x≤1.1,0≤y≤0.9 wherein, M is at least a among Mn, Cr, Co, V, Ti, Al, Ga and the Mg.
8. anode composite material of lithium ion battery particle as claimed in claim 7 is characterized in that, the material of this positive active material particle is stratiform cobalt acid lithium, layered lithium manganate or olivine-type LiFePO4.
9. the preparation method of an anode composite material of lithium ion battery particle, it comprises:
Aluminum nitrate solution is provided;
Positive active material particle to be coated is added in this aluminum nitrate solution, form mixture;
Phosphate solution is added this mixture react, form the phosphoric acid aluminium lamination at this positive active material particle surface; And
This surface of heat treatment has the positive active material particle of phosphoric acid aluminium lamination.
10. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 9; It is characterized in that; Add in the step of this aluminum nitrate solution at said positive active material particle that will be to be coated, further control the addition of this positive active material, make mixture be muddy.
11. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 9 is characterized in that, this aluminum nitrate solution comprises solvent and is dissolved in the aluminum nitrate of this solvent.
12. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 11 is characterized in that, this solvent is an ethanol.
13. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 9 is characterized in that, this phosphate solution comprises water and is dissolved in the phosphoric acid ammonia salt of water.
14. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 13 is characterized in that, this phosphoric acid ammonia salt comprises one or more the mixing in ammonium dihydrogen phosphate, diammonium hydrogen phosphate and the triammonium phosphate.
15. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 9 is characterized in that, this heat treatment temperature is 400 ℃ to 800 ℃.
16. the preparation method of anode composite material of lithium ion battery particle as claimed in claim 9 is characterized in that, the volume ratio of the volume of this aluminum nitrate solution and this positive active material particle is 1: 10 to 1: 40.
Priority Applications (9)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010242522.4A CN102347473B (en) | 2010-08-02 | 2010-08-02 | Anode composite material particle of lithium ion battery and preparation method thereof |
| US13/092,135 US8568620B2 (en) | 2010-08-02 | 2011-04-21 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| US13/106,994 US9219276B2 (en) | 2010-08-02 | 2011-05-13 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| US13/106,996 US9054379B2 (en) | 2010-08-02 | 2011-05-13 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| US13/107,006 US20120028120A1 (en) | 2010-08-02 | 2011-05-13 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| US13/106,999 US8349494B2 (en) | 2010-08-02 | 2011-05-13 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| US13/107,003 US9203087B2 (en) | 2010-08-02 | 2011-05-13 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| US13/108,101 US8277979B2 (en) | 2010-08-02 | 2011-05-16 | Electrode composite material, method for making the same, and lithium ion battery using the same |
| JP2011146851A JP5491459B2 (en) | 2010-08-02 | 2011-06-30 | ELECTRODE COMPOSITE MATERIAL, ITS MANUFACTURING METHOD, AND LITHIUM ION BATTERY USING THE SAME |
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Also Published As
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| CN102347473B (en) | 2014-03-26 |
| JP2012033481A (en) | 2012-02-16 |
| JP5491459B2 (en) | 2014-05-14 |
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