CN101714629A - Tri-platform blended cathode material for lithium ion batteries and preparation method thereof - Google Patents
Tri-platform blended cathode material for lithium ion batteries and preparation method thereof Download PDFInfo
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- CN101714629A CN101714629A CN200910186470A CN200910186470A CN101714629A CN 101714629 A CN101714629 A CN 101714629A CN 200910186470 A CN200910186470 A CN 200910186470A CN 200910186470 A CN200910186470 A CN 200910186470A CN 101714629 A CN101714629 A CN 101714629A
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Abstract
The invention discloses a tri-platform blended cathode material for lithium ion batteries, which is characterized by comprising a multi-phase mixture formed by three types of cathode materials, and the three types of the cathode materials are respectively within 3.0-3.7 V, 3.9-4.4 V and 4.5-5.1 V corresponding to a discharging voltage platform of metal lithium in an organic solvent. The combination of the three types of cathode materials based on a single-discharging platform material enables an electrode to have the property of a tri-discharging platform, can display a charge state, particularly the charge state of a dynamical lithium ion battery, reduces control circuits used in finished batteries, and lowers the battery cost.
Description
Technical field
The invention belongs to lithium ion motor positive electrode research preparing technical field, be specifically related to design of a kind of tri-platform blended cathode material for lithium ion batteries and preparation method thereof.
Background technology
Anode material for lithium-ion batteries is a kind of compound with host structure, can allow lithium ion reversibly to deviate from and embed in bigger compositing range.Comparatively common positive electrode is the oxide of some transition metal, as LiCoO
2, LiNiO
2And LiMn
2O
4Deng.LiCoO
2Commercialization, but its selling at exorbitant prices, toxicity is bigger; LiNiO
2Synthetic relatively difficulty; LiMn
2O
4Then there is the shortcoming that theoretical capacity is low, cycle performance is relatively poor.Therefore, battery circle is at the positive electrode of development of new constantly.
Contain polyanion, as SO
4 2-, PO
4 3-Or AsO
4 3-Compound be subjected at present widely paying close attention to, the gesture that replaces above-mentioned several oxide materials is arranged greatly.Especially the LiFePO4 of olivine structural, because of it has advantageous advantage, as it is abundant, cheap, nontoxic etc. to originate, and becomes the focus in the anode material for lithium-ion batteries research.LiFePO
4Theoretical capacity higher relatively (170mAh/g), good thermal stability, less moisture absorption and good charge-discharge performance are arranged under full-charge state.This material after the modification might make lithium battery break through the present memory capacity and the electric energy limit, and then promote that volume is smaller and more exquisite, lighter, and the appearance of products such as mobile phone that service time is more permanent and notebook computer becomes the watershed of battery industry.
Use at present with LiCoO
2Be main anode material for lithium-ion batteries, be characterized in that discharge platform is steady, the production technology maturation, good cycle, reliability is high.And the lithium ion battery of developing material of future generation comprises LiFePO
4, LiMnPO
4, LiCoPO
4, spinel structure LiMn2O4, rich lithium LiMnO
2-Li
2MnO
3-LiCoO
2Stratiform solid solution series etc., the characteristics of these materials are that discharge voltage plateau is steady especially.Discharge voltage plateau has guaranteed that battery capacity in use can fully be utilized stably, yet causes the capacity of battery to be difficult to judge.
The capacity of commercialization lithium ion battery judges that the normal way that adopts is supporting electronic control circuit at present, is remembered and judged the state-of-charge of battery by control circuit.For example in the lithium ion battery of microcomputer, extensively adopt this technology.If electrokinetic cell, for example equipment such as electric motor car reduces the battery production cost, and the electronic control circuit of simplifying the finished product battery extremely is necessary, because the cost of control circuit accounts for 15～20% of battery total cost, simplified control circuit just can make more client accept.The way of at present the easiest judgement state-of-charge is exactly the voltage of battery.For the customer, can be when a certain charging state battery display voltage acute variation, and battery can guarantee that still electric motor car moves a segment distance (for example 2 kilometers) and reaches charging station after this, is crucial, also is easily.In addition, charging process also is like this.For example, for LiCoO
2, because its charging voltage changes slowly, therefore, the termination voltage that is set in 4.2V usually causes and can not be full of.
In the prior art, the anode material for lithium-ion batteries that uses comprises LiCoO at present
2, spinel lithium manganates etc. generally all use single composition, use even multi-component mixes, and it is also little that the discharge voltage plateau of these compositions differs; And because the anode material discharging voltage that adopts is smooth, when obviously jumping downwards appearred in discharge voltage, battery had not had electric weight; During charging, owing to be subjected to LiCoO
2Restriction (promptly not being that lithiums all in the positive pole can participate in charging) with spinel lithium manganate charging mechanism, can only take to think the way charging of control charging cut-ff voltage, such advantage is to have ensured cycle life, can not quick charge but shortcoming is a battery, otherwise be difficult to be charged to rated capacity.
Summary of the invention
The object of the invention is to provide a kind of tri-platform blended cathode material for lithium ion batteries, solved in the prior art that capacity of lithium ion battery is difficult to judge and be difficult to be full of during charging, discharge does not have electric weight substantially when sudden change occurring and can not satisfy electric motor car user's problems such as demand.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of tri-platform blended cathode material for lithium ion batteries, it is characterized in that described blended anode material comprises the multiphase mixture that three kinds of positive electrode components form, and three kinds of positive electrode components with respect to the discharge voltage plateau of the lithium metal in the organic solvent respectively in 3.0-3.7V, 3.9-4.4V and 4.5-5.1V scope.
Preferably, described discharge voltage plateau is one or more the LiFePO that is selected from the positive electrode component of 3.0-3.7V
4, LiMiO
2Positive electrode; LiMiO wherein
2Representative is based on LiMnO
2, Li
2MnO
3, LiMlO
2Rich lithium lamellar compound, Ml is selected from Co, Ni, Al transition metal and combination thereof.
Preferably, described discharge voltage plateau is one or more the LiMnPO that is selected from the positive electrode component of 3.9-4.4V
4, LiCoO
2, LiNiO
2, LiMO
2, spinel structure Li
1+ αMn
2+ δO
4+ βPositive electrode, wherein M is selected from two or more Co, Ni, Al, Mg element;-0.5＜α, β, δ＜0.5.
Preferably, described discharge voltage plateau is one or more the LiCoPO that is selected from the positive electrode component of 4.5-5.1V
4, LiMn
nMl
2-nO
4+kPositive electrode; Wherein, Ml is selected from Co, Ni, Al transition metal and combination thereof, 0.8＜n＜1.5 ,-0.5＜k＜0.5.
Preferably, described three kinds of positive electrode components are calculated by its relative molar content in blending constituent, discharge voltage plateau at the positive electrode component ratio of 3.0-3.7V and 4.5-5.1V less than 50%; Discharge voltage plateau at the component ratio of 3.9-4.4V greater than 50%.
Preferably, described multiphase mixture is the multiple compound simple and mechanical mixture or the multicomponent mixture of (comprising single-phase compound or multi-phase composites), or synthetic solid solution mixtures or synthetic dephasign mixture of a step of a step.
Preferably, described blended anode material is a tri-platform blended cathode material, comprises LiFePO
4, LiMnPO
4, LiCoPO
4Three kinds of positive electrode components.
Another object of the present invention is to provide a kind of method for preparing tri-platform blended cathode material for lithium ion batteries, it is characterized in that described method comprises respectively the step of carrying out the synthetic step preparation of high temperature after the various positive electrode component mechanical mixture with the step of the synthetic preparation of the various positive electrode component high temperature of tri-platform blended cathode material back mechanical mixture or tri-platform blended cathode material.
When the present invention prepares tri-platform blended cathode material for lithium ion batteries, can adopt to comprise the high temperature solid-state synthetic method the synthetic blended anode material of chemical liquid phase method synthetic and physics; The solid phase synthesis product mainly is by transition metal oxide that contains Ni, Co, Mn or oxide precursor (comprising carbonate, hydroxide etc.), after mixing with lithium-containing compound, and the product that obtains of direct sintering at high temperature.Chemical liquid phase synthetic method key step comprises the preparation of presoma, mixes lithium and three steps of sintering.Generally, earlier co-precipitation goes out the co-precipitation presoma of hydroxide or carbonate from the soluble metal salting liquid, and after presoma and lithium salts were mixed, at high temperature sintering prepared nickle cobalt lithium manganate.The key of this method is the preparation of presoma, in coprecipitation process, better controlled pH value, temperature, flox condition, concentration and other to influence the factor of product crystal structure, purity and physical property.
The present invention reaches a certain numerical value voltage and undergos mutation in order to satisfy in charging process state-of-charge, and after sudden change, still can allow to charge into the concrete specification requirement of the electric weight of some, design by composition anode material for lithium-ion batteries, adopt the design of three platform positive electrodes in the technical solution of the present invention, mainly comprise C1, C2, three kinds of positive electrodes of C3, C1 represents discharge voltage plateau at the positive electrode between the 3.7-3.0V (voltage refers to for the lithium metal in the organic solvent), or the discharge voltage plateau of this material has part between 3.7-3.0V; C2 represents the positive electrode of discharge voltage plateau between 3.9-4.4V; C3 represents the positive electrode of discharge voltage plateau in the 4.5-5.1V scope, and the design of such composition has a great deal of practical meanings for the fail safe of battery.
On behalf of three classes, C1, C2 have the material of different discharge voltage plateaus with C3, and wherein, C1 can be LiFePO
4, LiMiO
2The mixture of one or more in the material can be simple mechanical mixture, also can be synthetic heterogeneous composition compound of a step, wherein LiMiO
2Representative is based on LiMnO
2, Li
2MnO
3, LiMlO
2The rich lithium lamellar compound of (Ml can be Co, Ni, Al, one or more of transition metals such as Cr); C2 can be LiMnPO
4, LiCoO
2, LiNiO
2, LiMO
2(M is Co, Ni, Al, the two kinds or more of elements among the Mg), the Li of spinel structure
1+ αMn
2+ δO
4+ βIn the material one or more can be the simple and mechanical mixtures of each compound, also can be directly synthetic multi-phase composites. wherein-0.5＜α, δ, β＜0.5, i.e. Li
1+ αMn
2+ δO
4+ βRepresent the composition of various spinel structures, as stoichiometric proportion spinelle LiMn2O4, the rich lithium-spinel of oxygen enrichment, oxygen debt rich lithium-spinel etc.; C3 can be LiCoPO
4, LiMn
nM
2-nO
4+kIn one or several, wherein, M can be Co, Ni, one or several of transition metals such as Al, 0.8＜n＜1.5 ,-0.5＜k＜0.5.If suppose x, y, the numerical value of z represent C1, C2, three kinds of compositions of C3 relative molar content separately in blending constituent, y＞0.5 then, and corresponding component C2 is the main component of positive electrode, x+z＜0.5, and x＞0, z＞0; Also can be according to the client to the requirement of battery performance and change components contents.Can be a kind of single-phase compound in the component, can be the simple and mechanical mixture of multiple compound, also can be a kind of synthetic compound with heterogeneous composition of a step.For the C1 component, can be synthetic respectively earlier LiFePO
4And LiMnO
2, Li2MnO
3, LiMlO
2, and then two kinds of materials are mixed and made into by mechanical mixture method (for example ball milling); Also can be directly to synthesize in a step to have hLiFePO
4, jLiMnO
2, kLi
2MnO
3, mLiMlO
2(h wherein, j, k, m are the corresponding molar contents of forming in total the composition, 0＜h, and j, k, m＜1, composite material h+j+k+m=1), this material can be single-phase compositions, also can be heterogeneous compositions.For the C2 component, can be synthetic respectively LiNiO2 and the mechanical mixture of LiCoO2, also can be according to LiNi
xCo
1-xO
2Direct He Cheng composite material.
Wherein discharge platform is meant in the median of two knee voltages of discharge curve or the scope of knee voltage.As first flex point is 3.8V, and second flex point is 3.6V, and so, its discharge platform is 3.7V, and the discharge platform that perhaps is expressed as this battery is 3.6V～3.8V, represents with value range.Positive electrode can be divided into three classes according to discharge voltage plateau in the technical solution of the present invention, and a class voltage platform is at 3.0-3.7V, and a class also has a class at 4.5-5.2V at 3.9-4.4V.Wherein main discharge platform is a platform 2, and capacity corresponding accounts for more than 50% of total capacity, the main energy sources that it provides lithium ion battery work to use.
LiMiO wherein
2Representative is based on LiMnO
2, Li
2MnO
3, LiMlO
2The rich lithium lamellar compound of (Ml can be Co, Ni, Al, one or more of transition metals such as Cr); LiMn
nM
2-nO
4+kIn, M can be Co, Ni, one or several of transition metals such as Al, 0.8＜n＜1.5 ,-0.5＜k＜0.5.Platform 1 mainly is LiMn in this composition
nM
2-nO
4+k, platform 2 main corresponding LiMnPO
4, 3 on platform and LiMiO
2Correspondence, as shown in Figure 1.LiMn
nM
2-nO
4+kThe synthetic high temperature process that can adopt synthetic.
The composition sample of blended anode material of the present invention can be synthetic respectively, and then mechanical mixture (being called multicomponent); Also can be synthetic dephasign mixture of a step, or solid solution (being called one pack system).No matter electrode material of the present invention is multicomponent or single-component mixture, all is multiphase mixture.Can be the separately synthetic mechanical mixture then of each phase compound together, also can be directly synthetic solid solution or dephasign compound with heterogeneous composition.
With respect to scheme of the prior art, advantage of the present invention is:
1. technical solution of the present invention forms discharge voltage plateau respectively in 3.0-3.7V, 3.9-4.4V and 4.5-5.1V scope by comprising three kinds of positive electrode components at least; During discharge, the charged attitude that the hop variation of voltage can clearly show battery changes, remind the electric motor car client that battery needs charging, and, discharge platform 3.0-3.7V after the voltage hop can also provide a small amount of electric weight, is used to guarantee that similar devices such as electric motor car still can move a segment distance and arrive charging station; Voltage platform 3.0-3.7V capacity corresponding can be according to the distribution of charging station, client's needs and design the C3 components contents.
2. adopt the design of three discharge platforms in the optimal technical scheme of the present invention, when guaranteeing charging, voltage platform 3.9-4.4V is to the simple charged state of indicating battery of the voltage hop of voltage platform 3.0-3.7V, platform 3.0-3.7V capacity corresponding can play the protection battery and avoid overcharging, and increases battery security; Simultaneously can simplify the electronic circuit that is used for controlling the battery charge attitude. at the finished product battery, control circuit occupies the 15-20% of total cost.Therefore, three design of Platform can obviously reduce battery cost.
3. in the optimal technical scheme of the present invention, three platforms are preferably designed for LiFePO
4, LiMnPO
4, LiCoPO
4Form, can also make full use of LiFePO
4And LiMnPO
4The charged capacity of phase not only can have jumbo characteristics and pure LiFePO
4Compare, also have the advantage of high specific energy.And the crystalline texture of three kinds of compositions is identical, can synthesize the olivine solid solution product of single-phase composition a step, has the simple more advantage of material preparation equipment.
In sum, the present invention is based on the combination of single discharge platform material, make electrode have the characteristic of three discharge platforms; By comprising that at least three kinds of positive electrode components form discharge voltage plateau and design at the positive electrode of 3.0-3.7V, 3.9-4.4V and 4.5-5.1V scope respectively, the multi-platform blended anode material that makes the present invention obtain can show state-of-charge, power lithium-ion battery state-of-charge particularly, reduce the control circuit that uses in the finished product battery, reduce the battery cost.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described:
Fig. 1 obtains the discharge curve schematic diagram of blended anode material for the embodiment of the invention 1;
Fig. 2 is the discharge curve schematic diagram of component C1 in the embodiment of the invention 3;
Fig. 3 is the discharge curve schematic diagram of component C2 in the embodiment of the invention 3;
Fig. 4 is the discharge curve schematic diagram of component C3 in the embodiment of the invention 3;
The discharge curve schematic diagram of the mixing three platform electrode materials that Fig. 5 obtains for the embodiment of the invention 3.
Embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are used to the present invention is described and are not limited to limit the scope of the invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment 1 Li (Fe, Mn, Co) PO
4Tri-platform blended cathode material and preparation thereof
Form design:
The preparation method:
Respectively with FeC
2O
42H
2O (AR), (NH
4)
2HPO
4(AR), Li
2CO
3(AR) take by weighing by stoichiometric proportion.Ground 10 minutes putting into crucible after the raw material mixing, add people's acetone then and mix, through ball mill ball milling 8h.After treating acetone evaporated, mixed raw materials put in the program control electric furnace of people carry out pre-burning in 400 ℃ of following constant temperature 4h and handle.Take out once more then and grind, at 650 ℃ of following sintering 18h.Pre-burning and sintering process are all carried out under inert atmosphere.
LiMnPO
4And LiCoPO
4Preparation carry out according to as above step; The LiFePO for preparing
4, LiMnPO
4And LiCoPO
4Carry out mechanical mixture and obtain required Li (Fe, Mn, Co) PO
4Tri-platform blended cathode material
The positive electrode that present embodiment obtains has constant current discharge curvilinear characteristic as shown in Figure 1 through discharging and recharging experiment confirm.Among Fig. 1, its discharge platform 1 correspondence was that C3 forms during positive electrode was formed, and corresponding capacity is a capacity 1; Discharge platform 2 corresponding positive electrode main body composition C2, corresponding capacity is a capacity 2; Equally, the discharge platform 3 corresponding C1 that form, corresponding capacity is a capacity 3.In above-mentioned composition, the ratio that the capacity that the main body composition has occupies in total capacity is more than 50%.
Embodiment 2 Li (Fe, Mn, Co) PO
4Tri-platform blended cathode material and preparation thereof
Form design:
With MnC
2O
42H
2O (AR), CoC
2O
42H
2O (AR), FeC
2O
42H
2O (AR), (NH
4)
2HPO
4(AR), Li
2CO
3(AR) take by weighing by stoichiometric proportion.Grind in the crucible, add then after acetone mixes, pre-burning is 4 hours under argon gas atmosphere, temperature 400 degree; Take out sample then, grind once more, and then in 800 calcinings.The above-mentioned sample that obtains is LiFePO
4, LiMnPO
4And LiCoPO
4Solid solution, during directly as electrode material, also have electrode discharge curvilinear characteristic as shown in Figure 1, the main body composition is LiMnPO
4, the corresponding platform 2 of its discharge platform.
Embodiment 3 LiMiO
2+ LiMnPO
4+ LiMn
nM
2-nO
4+kTri-platform blended cathode material and preparation thereof
LiMn wherein
nM
2-nO
4+kPreparation be to carry out as follows:
Li
2CO
3, MnO
2Grind with the CoO powder, add an amount of ascorbic acid then and continue to grind 10 minutes, spend sintering 12 hours 800 then; LiMnPO
4Synthetic as described in the embodiment 1; LiMiO
2Preparation adopt classical high temperature synthetic method, Li[Li
xNi
yMn
zCo
lCr
mAl
p] O
2The composition of (wherein 0≤x, y, l, m, p≤0.3,0.3≤z≤0.7), according to the metal acetate salt of corresponding stoichiometric proportion weighing correspondence, and Li
2CO
3, ground then 10 minutes, add ethylene glycol again and ground 10 minutes, at first 400 degree were calcined 4 hours then, 850 degree calcinings 12 hours, got final product again.More than obtain blended anode material after the mechanical lapping after the material mixing of Huo Deing.
Through test, the component separately that records and its discharge curve of blended anode material are shown in Fig. 2～5; As can be seen from Figure 2, the discharge curve of component C1, its discharge platform are platform 3, and simultaneously, it all has contribution to capacity 1 and capacity 2; Among Fig. 3, component C2 has single platform discharge curve, has roughly identified the position of platform of component C1 and C3 at Fig. 3; Among Fig. 4, component C3 has following discharge curve feature: have two platform features, and 1 contribution of 1 pair of capacity of platform, 2 pairs of capacity of platform 2 are contributed, and have identified the 3rd position of platform of component C1 in the drawings.As can be seen from Figure 5, this three platforms positive electrode is similar to three platforms among the embodiment 1, but slightly tilts, platform 1 corresponding capacity 1 wherein, and corresponding C3 forms, discharge platform 2 corresponding positive electrode main body composition C2, corresponding capacity is a capacity 2; Equally, the discharge platform 3 corresponding C1 that form, corresponding capacity is a capacity 3.Forming C1 this moment all has the capacity contribution to platform 1 and platform 2, but mainly still utilizes the characteristic of its platform 3, and it belongs to additional contribution to the contribution of capacity 1 and capacity 2.For forming C3, mainly utilize the characteristic of its platform 1, simultaneously to the also contribution to some extent of capacity of platform 2, be in the design needs of three platforms, mainly utilize the characteristic of its platform 1, its capacity contribution to platform 2 belongs to extra utilization.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (8)
1. tri-platform blended cathode material for lithium ion batteries, it is characterized in that described blended anode material comprises the multiphase mixture that three kinds of positive electrode components form, and three kinds of positive electrode components with respect to the discharge voltage plateau of the lithium metal in the organic solvent respectively in 3.0-3.7V, 3.9-4.4V and 4.5-5.1V scope.
2. tri-platform blended cathode material for lithium ion batteries according to claim 1 is characterized in that described discharge voltage plateau is one or more the LiFePO that is selected from the positive electrode component of 3.0-3.7V
4, LiMiO
2Positive electrode; LiMiO wherein
2Representative is based on LiMnO
2, Li
2MnO
3, LiMlO
2Rich lithium lamellar compound, Ml is selected from Co, Ni, Al transition metal and combination thereof.
3. tri-platform blended cathode material for lithium ion batteries according to claim 1 is characterized in that described discharge voltage plateau is one or more the LiMnPO that is selected from the positive electrode component of 3.9-4.4V
4, LiCoO
2, LiNiO
2, LiMO
2, spinel structure Li
1+ αMn
2+ δO
4+ βPositive electrode, wherein M is selected from two or more Co, Ni, Al, Mg element; α, β, δ be all greater than-0.5, and all less than 0.5.
4. tri-platform blended cathode material for lithium ion batteries according to claim 1 is characterized in that described discharge voltage plateau is one or more the LiCoPO that is selected from the positive electrode component of 4.5-5.1V
4, LiMn
nMl
2-nO
4+kPositive electrode; Wherein, Ml is selected from Co, Ni, Al transition metal and combination thereof; 0.8＜n＜1.5 ,-0.5＜k＜0.5.
5. tri-platform blended cathode material for lithium ion batteries according to claim 1, it is characterized in that described three kinds of positive electrode components calculate by its relative molar content in blending constituent, discharge voltage plateau at the positive electrode component ratio of 3.0-3.7V and 4.5-5.1V less than 50%; Discharge voltage plateau at the component ratio of 3.9-4.4V greater than 50%.
6. tri-platform blended cathode material for lithium ion batteries according to claim 1 is characterized in that described multiphase mixture is the multi-component simple and mechanical mixture or the synthetic solid solution mixtures or the synthetic dephasign mixture of a step of a step of multiple compound.
7. tri-platform blended cathode material for lithium ion batteries according to claim 1 is characterized in that described blended anode material is a tri-platform blended cathode material, comprises LiFePO
4, LiMnPO
4, LiCoPO
4Three kinds of positive electrode components.
8. method for preparing the described tri-platform blended cathode material for lithium ion batteries of claim 1 is characterized in that described method comprises respectively the step of carrying out the synthetic step preparation of high temperature after the various positive electrode component mechanical mixture with the step of the synthetic preparation of the various positive electrode component high temperature of tri-platform blended cathode material back mechanical mixture or tri-platform blended cathode material.
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