CN105870452A - Anode material, lithium ion battery with anode material and preparation method - Google Patents

Anode material, lithium ion battery with anode material and preparation method Download PDF

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Publication number
CN105870452A
CN105870452A CN201610334569.0A CN201610334569A CN105870452A CN 105870452 A CN105870452 A CN 105870452A CN 201610334569 A CN201610334569 A CN 201610334569A CN 105870452 A CN105870452 A CN 105870452A
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lithium
positive electrode
positive
lithium ion
anode material
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卢永强
王涛
肖海河
张艳丽
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Ningde Amperex Technology Ltd
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Ningde Amperex Technology Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • H01M10/058—Construction or manufacture
    • H01M10/0587—Construction or manufacture of accumulators having only wound construction elements, i.e. wound positive electrodes, wound negative electrodes and wound separators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention belongs to the technical field of lithium ion batteries, and in particular relates to an anode material, a lithium ion battery with the anode material and a preparation method. The anode material provided by the invention comprises an anode active substance, a conductive agent and an adhesive, wherein the anode material is added with a lithium-rich compound; the lithium-rich compound is selected from at least one of LiTiO2, Li6VO4, LixMF3 or LixR2.5P4; M is selected from Ti, Mn, Fe or V; R is selected from Ti, Mn or V; x is greater than 0 and less than 9. By adopting the anode material provided by the invention, the gram volume volatilization of the anode can be effectively improved, and the energy density of a battery can be increased. The lithium-rich compound of the anode material has a relatively low de-intercalation potential and a relatively high lithium-removal capacity in an organic electrolyte, extra lithium ions for compensating irreversible lithium ion loss can be provided for a cathode in a cell formation process, and the lithium ions do not participate in electrochemical reaction at the working position of an anode piece.

Description

A kind of positive electrode, the lithium ion battery containing this positive electrode and preparation method
Technical field
The invention belongs to technical field of lithium ion, particularly relate to a kind of positive electrode, lithium containing this positive electrode Ion battery and preparation method.
Background technology
Along with popularizing of high power consumption intelligent portable equipment, the raising of lithium ion battery energy density becomes current research work Emphasis, owing to commercial graphite cathode material theoretical specific capacity is only 372mAhg-1, affect the raising of lithium ion energy density, lithium Power plant business and research institution begin one's study the negative materials such as silica-based, the tinbase of height ratio capacity or oxide-base, and this kind of material gram holds Amount is far above graphite material, but owing to this kind of material is limited to self electrochemical reaction mechanism, irreversible capacity is higher, coulomb Efficiency the lowest (about 70%), affects positive electrode gram volume and plays.
For solving negative pole coulombic efficiency this problem relatively low, the mode of current researcher's many employings negative pole preliminary filling lithium makes up not The loss of reversible capacity, as used Vacuum Deposition lithium or adding lithium powder, the mode of lithium paper tinsel, can be effectively improved coulombic efficiency, improve Battery energy density and electrical property.Or lithium metal, negative material and on-aqueous liquid are mixed to form slurry by employing, slurry is coated On collector, then it is dried slurries, or uses the method for vacuum evaporation to become layer of metal lithium layer in negative plate surface evaporation. But owing to lithium metal is excessively active, requiring the highest to preliminary filling lithium operating environment, and the gram volume of lithium metal is too high, lithium metal is micro- The uneven of amount can result in lithium content skewness in pole piece, complex process, it is difficult to batch production.
For the defect of prior art, special proposition the application.
Summary of the invention
The primary goal of the invention of the application is to propose a kind of positive electrode.
Second goal of the invention of the application is to propose a kind of lithium ion battery containing this positive electrode.
3rd goal of the invention of the application is to propose the preparation method of this lithium ion battery.
In order to complete the purpose of the application, the technical scheme of employing is:
The application relates to a kind of positive electrode, containing positive active material, conductive agent and binding agent in described positive electrode, Being added with rich lithium compound in described positive electrode, described rich lithium compound is selected from LiTiO2、Li6VO4、LixMF3Or LixR2.5P4 In at least one, wherein M be selected from Ti, Mn, Fe or V；R is selected from Ti, Mn or V；0<x<8.
Preferably, described rich lithium compound is selected from Li3TiF3、Li3MnF3、Li3FeF3、Li3VF3、Li7Ti2.5P4、 Li7.5V2.5P4In at least one.
Preferably, described rich lithium compound mass percentage content in described positive electrode is 0.1～10%, preferably It is 1～5%.
Preferably, the removal lithium embedded current potential of described rich lithium compound is 1.0V～3.5V, de-lithium capacity be 150mAh～ 1500mAh。
Preferably, described positive active material, described conductive agent, described binding agent and the mass ratio of described rich lithium compound For: 90～98:1～2:1～2:0.1～10；It is preferably 91～97:1～2:1～2:1～5.
Preferably, described positive active material is in cobalt acid lithium, lithium nickelate, nickle cobalt lithium manganate, LiMn2O4, LiFePO4 At least one.
Preferably, described conductive agent is led selected from carbon black class conductive agent, superconduction carbon black, CNT, carbon fiber and graphite-like At least one in electricity agent；Described binding agent is oiliness or aqueous binders；Described oiliness binding agent selected from polyvinylidene fluoride, At least one in polytetrafluoroethylene (PTFE), Viton, polyurethane；Described aqueous binders is selected from butadiene-styrene rubber, polyacrylic acid, gathers At least one in PAA, polyvinyl alcohol, alginic acid, sodium alginate.
The application further relates to a kind of lithium ion battery, and including positive plate, negative plate, electrolyte, described positive plate just includes Pole collector and positive pole diaphragm, described positive pole diaphragm is the positive electrode of the application.
Preferably, described negative plate is carbon material negative pole or/and material negative pole.
The application further relates to the preparation method of this lithium ion battery, and the preparation method of anode pole piece is: by positive electrode active material Matter, binding agent, conductive agent carbon black, rich lithium compound in mass ratio 90～98:1～2:1～2:0.1～10 are scattered in organic solvent In, it is then coated with on plus plate current-collecting body, after drying, rolling, cutting, soldering polar ear, obtains described anode pole piece, You Jirong Agent is selected from NMP.
What the positive electrode of the application and lithium ion battery at least can reach has the beneficial effect that
The application can be effectively improved positive pole gram volume and play, and improves battery energy density.
The rich lithium compound of the application has the relatively low removal lithium embedded current potential (oxygen on the basis of lithium metal in organic electrolyte Change reduction potential) and higher de-lithium capacity, removal lithium embedded current potential is less than 3.5V, and de-lithium capacity is 150mAh～1500mAh, preferably 200～1000mAh.
The rich lithium compound of the application provides extra lithium ion in the battery core chemical conversion stage to negative pole, is used for compensating irreversible Lithium ion loss, electrochemical reaction can be not involved at anode pole piece operating potential.
Detailed description of the invention
Below in conjunction with specific embodiment, the application is expanded on further.Should be understood that these embodiments are merely to illustrate the application Rather than restriction scope of the present application.
The application adds the rich lithiumation with higher de-lithium amount by the way of positive pole anticathode mends lithium in positive electrode Compound, provides extra lithium to negative pole, to make up the irreversible consumption of negative pole during initial charge.
The application relates to a kind of positive electrode, and containing positive active material, conductive agent and binding agent in positive electrode, this is just Being added with rich lithium compound in the material of pole, rich lithium compound is selected from LiTiO2、Li6VO4、LixMF3Or LixR2.5P4In at least one Kind, wherein M is selected from Ti, Mn, Fe or V；R is selected from Ti, Mn or V；0<x<8.
The rich lithium compound of the application is selected from Li3TiF3、Li3MnF3、Li3FeF3、Li3VF3、Li7Ti2.5P4、Li7.5V2.5P4 In at least one.
The rich lithium compound of the application removal lithium embedded current potential in organic solvent is 1.0V～3.5V, and de-lithium capacity is 150mAh～1500mAh.The rich lithium compound of the application has relatively low removal lithium embedded current potential and higher taking off in organic electrolyte Lithium capacity, only provides extra lithium ion to be used for compensating the loss of irreversible lithium ion, just in the battery core chemical conversion stage to negative pole Pole pole piece operating potential can be not involved in electrochemical reaction.
The rich lithium compound of the application mass percentage content in positive electrode is 0.1～10%, preferably 1～ 5%.Rich lithium compound is needed in positive pole, adding proportion can be according to being added the lithium amount and negative pole that richness lithium compound can provide For make up irreversible loss lithium amount calculate.The excessive easy processing characteristics that affects of adding proportion, and significant pair may be caused Chemical reaction, causes degradation of cell performance, and the compensating action of the too small then lithium ion of adding proportion is inconspicuous.
The application further relates to a kind of lithium ion battery, and including positive plate, negative plate, electrolyte, positive plate includes positive pole collection Fluid and positive pole diaphragm, positive pole diaphragm is the positive electrode of the application.
The anode plate for lithium ionic cell of the application is carbon material negative pole or/and material negative pole, it is preferred that for material with carbon element Negative pole is or/and material negative pole.
The application further relates to the preparation method of this lithium ion battery, and wherein, the preparation method of anode pole piece is: lived by positive pole Property material, binding agent, conductive agent carbon black, rich lithium compound in mass ratio 90～98:1～2:1～2:0.1～1 be scattered in organic In solvent, it is then coated with on plus plate current-collecting body, obtains described anode pole piece after drying, rolling, cutting, soldering polar ear, have Machine solvent is selected from NMP.
Owing to the rich lithium compound of the application should have preferable stability in dry air, can meet and with NMP be The anode sizing agent of solvent uses.
Embodiment 1～10
(1) anode pole piece: positive active material cobalt acid lithium, binding agent polyvinylidene fluoride, conductive agent carbon black, rich lithiumation are closed The ratio of thing four kinds of components (97.0-x): 1.5:1.5:x in mass ratio is scattered in organic solvent NMP, is then evenly applied to In current collector aluminum foil, after drying, rolling is to required compacted density, soldering polar ear after point bar cut-parts, just obtains used by lithium ion battery Pole pole piece.Kind and the content of concrete rich lithium compound are as shown in table 1.
(2) cathode pole piece: cathode pole piece is by Delanium, binding agent polyvinylidene fluoride, conductive agent carbon black in mass ratio 95.0:3.0:2.0 is scattered in organic solvent NMP, is then evenly applied on copper foil of affluxion body, and after drying, rolling is to required pressure Real density, soldering polar ear after point bar cut-parts, obtain cathode pole piece used by lithium ion battery.
(3) battery assembles: by anode pole piece, high-molecular porous barrier film, cathode pole piece through being wound into core, add routine Through the prepared lithium ion battery that can carry out discharge and recharge of chemical conversion after lithium-ion battery electrolytes.
Table 1
The battery prepared carries out the detection of battery performance.
Detection method is: by the constant current charge of 0.1C (160mA) to 4.35V, then with 4.35V constant-voltage charge to electricity Flow down and drop to 0.05C (80mA), be then discharged to 3.0V with the constant current of 0.2C (160mA), obtain the charge and discharge first of battery Capacitance.Repeat charge and discharge process 500 times, obtain the residual capacity after 500 circulations, residual capacity and discharge capacity first Ratio is circulation volume conservation rate.
Testing result is as shown in table 2, table 3.
Table 2:
Embodiment Charging capacity mAh Discharge capacity mAh Positive pole gram volume mAh/g
Embodiment 1 1665 1540 159
Embodiment 2 1672 1548 160
Embodiment 3 1680 1557 161
Embodiment 4 1704 1586 164
Embodiment 5 1723 1604 166
Embodiment 6 1720 1595 165
Embodiment 7 1724 1606 166
Embodiment 8 1717 1595 165
Embodiment 9 1712 1605 166
Embodiment 10 1709 1612 167
Comparative example 1 1663 1538 159
Comparative example 2 1650 1528 158
Comparative example 3 1660 1539 159
Comparative example 4 1654 1526 158
Comparative example 5 1663 1535 159
Comparative example 6 1665 1538 159
Comparative example 7 1727 1602 166
Note: gram volume calculation is to calculate by the summation of positive active material and rich lithium compound.
Table 3:
Comparative example 1 is traditional lithium-ion battery, and capacity plays, and coulomb and cycle life are in normal level first, contrast Example 2～5 is for add other conventional cathode material in cobalt acid lithium, and result as it is expected that there is not substantially help to battery core capacity.
Compared with comparative example, embodiment 1～10 significantly improves capacity of lithium ion battery by the rich lithium compound of interpolation and sends out Waving, be by lithium capacity de-during improving initial charge, the mode of the lithium ion loss making up negative pole improves lithium ion battery Capacity.Rich lithium compound initial charge gram volume is the highest, and addition is the biggest, and battery capacity is the highest, but too much rich lithium compound (comparative example 7) can cause the reduction of cycle performance.
Embodiment 11～15
(1) anode pole piece: positive active material cobalt acid lithium, binding agent polyvinylidene fluoride, conductive agent carbon black, rich lithiumation are closed The ratio of thing four kinds of components (97.0-x): 1.5:1.5:x in mass ratio is scattered in organic solvent NMP, is then evenly applied to In current collector aluminum foil, after drying, rolling is to required compacted density, soldering polar ear after point bar cut-parts, just obtains used by lithium ion battery Pole pole piece.Kind and the content of concrete rich lithium compound are as shown in table 4.
(2) cathode pole piece: cathode pole piece is by Delanium, nano silicon oxide SiOxNegative pole, binding agent polyvinylidene fluoride, Conductive agent carbon black 84.0:10.0:4.0:2.0 in mass ratio is scattered in organic solvent NMP, is then evenly applied to collector copper On paper tinsel, after drying, rolling is to required compacted density, and soldering polar ear after point bar cut-parts obtains cathode pole piece used by lithium ion battery.
(3) battery assembles: by anode pole piece, high-molecular porous barrier film, cathode pole piece through being wound into core, add routine Through the prepared lithium ion battery that can carry out discharge and recharge of chemical conversion after lithium-ion battery electrolytes.As described in Example 1 to preparation The lithium ion battery obtained is carried out shown in performance detection, experimental result chart 5 and table 6.
Table 4:
Table 5:
Embodiment Charging capacity mAh Discharge capacity mAh Positive pole gram volume mAh/g
Embodiment 11 1908 1560 161
Embodiment 12 1726 1472 152
Embodiment 13 1861 1562 161
Embodiment 14 1770 1495 155
Embodiment 15 1806 1538 159
Comparative example 6 1668 1364 141
Note: gram volume calculation is to calculate by the summation of positive active material and rich lithium compound.
Table 6:
Note: gram volume calculation is to calculate by the summation of positive active material and rich lithium compound.
Comparative example is the most inefficient, and capacity is low, is the nano silicon oxide SiOx negative pole added due to negative pole, irreversible lithium Losses of ions causes more greatly.
Embodiment 11～15 is by adding high power capacity richness lithium compound, and lithium ion abjection amount when improve charging, compensation is negative The lithium ion loss of pole, hence it is evident that improve battery capacity.Silicium cathode gram volume is far above graphite, but the most inefficient, needs Lithium ion outside supplementary quota improves the gram volume of positive electrode, embodiment 11～15 by add high power capacity richness lithium compound, Lithium ion abjection amount when improve charging, compensates the lithium ion loss of negative pole, hence it is evident that improve battery capacity.Added by negative pole Silicon materials, positive pole adds rich lithium compound mode, can obtain the capacity higher than ordinary graphite negative battery.
Rich lithium compound initial charge gram volume is the highest, and addition is the biggest, and battery capacity is the highest, but too much rich lithiumation is closed Thing can cause the reduction of cycle performance.
Although the application is open as above with preferred embodiment, but is not for limiting claim, any this area skill Art personnel, on the premise of conceiving without departing from the application, can make some possible variations and amendment, therefore the application Protection domain should be defined in the range of standard with the application claim.

Claims (10)

1. a positive electrode, containing positive active material, conductive agent and binding agent in described positive electrode, it is characterised in that Being added with rich lithium compound in described positive electrode, described rich lithium compound is selected from LiTiO2、Li6VO4、LixMF3Or LixR2.5P4 In at least one, wherein M be selected from Ti, Mn, Fe or V；R is selected from Ti, Mn or V；0<x<8.
Positive electrode the most according to claim 1, it is characterised in that described rich lithium compound is selected from Li3TiF3、Li3MnF3、 Li3FeF3、Li3VF3、Li7Ti2.5P4、Li7.5V2.5P4In at least one.
Positive electrode the most according to claim 1, it is characterised in that described rich lithium compound is in described positive electrode Mass percentage content is 0.1～10%, preferably 1～5%.
Positive electrode the most according to claim 1, it is characterised in that the removal lithium embedded current potential of described rich lithium compound is 1.0V ～3.5V, de-lithium capacity is 150mAh～1500mAh.
Positive electrode the most according to claim 1, it is characterised in that described positive active material, described conductive agent, described Binding agent with the mass ratio of described rich lithium compound is: 90～98:1～2:1～2:0.1～10；It is preferably 91～97:1～2:1 ～2:1～5.
Positive electrode the most according to claim 1, it is characterised in that described positive active material is selected from cobalt acid lithium, nickel acid At least one in lithium, nickle cobalt lithium manganate, LiMn2O4, LiFePO4.
Positive electrode the most according to claim 1, it is characterised in that described conductive agent is selected from carbon black class conductive agent, superconduction At least one in carbon black, CNT, carbon fiber and graphite-like conductive agent；Described binding agent is oiliness or aqueous binders； At least one in polyvinylidene fluoride, polytetrafluoroethylene (PTFE), Viton, polyurethane of described oiliness binding agent；Described water Property binding agent in butadiene-styrene rubber, polyacrylic acid, Sodium Polyacrylate, polyvinyl alcohol, alginic acid, the sodium alginate at least one Kind.
8. a lithium ion battery, including positive plate, negative plate, electrolyte, described positive plate includes plus plate current-collecting body and positive pole Diaphragm, it is characterised in that described positive pole diaphragm is the positive electrode described in claim 1～7 any claim.
Lithium ion battery the most according to claim 8, it is characterised in that described negative plate is that carbon material negative pole is or/and contain Silicon materials negative pole.
10. the preparation method of a lithium ion battery as described in claim 8 or 9, it is characterised in that the preparation side of anode pole piece Method is: by positive active material, binding agent, conductive agent carbon black, rich lithium compound in mass ratio 90～98:1～2:1～2:0.1 ～10 be scattered in organic solvent, it be then coated with on plus plate current-collecting body, after drying, rolling, cutting, soldering polar ear, obtain institute State anode pole piece.
CN201610334569.0A 2016-05-19 2016-05-19 Anode material, lithium ion battery with anode material and preparation method Pending CN105870452A (en)

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