CN107845836A - A kind of lithium ion cell positive mends lithium additive and its preparation method and application - Google Patents
A kind of lithium ion cell positive mends lithium additive and its preparation method and application Download PDFInfo
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- CN107845836A CN107845836A CN201710868151.2A CN201710868151A CN107845836A CN 107845836 A CN107845836 A CN 107845836A CN 201710868151 A CN201710868151 A CN 201710868151A CN 107845836 A CN107845836 A CN 107845836A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- 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
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- 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
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Abstract
This application discloses a kind of lithium ion cell positive to mend lithium additive and its preparation method and application.The lithium ion cell positive of the application mends lithium additive, for the rich lithium OXYFLUORIDE MATERIALS shown in chemical formula one, chemical formula one：Li2VO2F.The lithium ion cell positive of the application mends lithium additive Li2VO2F, 2 lithium ions can be discharged in theory, capacity is up to 462mAh/g, also, has preferable electric conductivity, can be very good to carry out benefit lithium to positive pole.The benefit lithium additive of the application is safe and environment-friendly, non-toxic, is laid a good foundation to prepare the lithium ion battery of high power capacity.
Description
Technical field
The application is related to field of lithium ion battery material, more particularly to a kind of lithium ion cell positive mend lithium additive and
Its preparation method and application.
Background technology
Lithium ion battery has the excellent chemical property such as high voltage, high-energy-density, is widely used in 3C, electronic vapour
Car and energy storage field.In recent years, the development of electric automobile even more further expands the demand of lithium ion battery, also to its energy
Density proposes higher requirement.
In order to improve the energy density of lithium ion battery, the silicium cathode material of height ratio capacity be increasingly becoming battery enterprise and
The selection of material supplier, turn into one of most potential lithium ion battery negative material of future generation.However, silicium cathode is larger
Volumetric expansion and relatively low coulombic efficiency first limit its practical application.At present, industrially all use in graphite system
Mix the modes of a small amount of silicon materials and improve the purpose of capacity to reach.But the incorporation of silicon materials still greatly reduces negative pole material
The coulombic efficiency first of material.So, because the coulombic efficiency of positive electrode is far above negative pole, positive electrode is necessarily caused
Capacity can not be brought into play completely, cause the waste of positive electrode and the reduction of battery capacity.This is primarily due to negative material
Surface can form solid electrolyte membrane, i.e. SEI films during initial charge, and this can consume lithium ion, and in the battery, lithium from
Sub- almost all is provided by positive electrode.Negative material efficiency is low will to cause battery not have in ensuing discharge process
Enough lithium ions, which return, to be embedded in positive electrode.
Therefore, there has been proposed the concept of " benefit lithium ", by negative pole, positive pole or barrier film " benefit lithium ", to supplement battery
The lithium ion that SEI films are consumed is formed during initial charge.
It is a kind of relatively common benefit lithium mode to carry out negative pole to mend lithium using lithium metal, typically that lithium powder or lithium band is directly multiple
Close on cathode pole piece surface, advantage is high as the lithium metal specific capacity for mending lithium material, and dosage is few.However, negative pole mends lithium technique
Cumbersome, equipment cost is higher, and production environment is harsh, and uniformity is difficult control, causes battery consistency poor, it is difficult to actual production
Using.Most of all, lithium is violent as the reaction of a kind of active metal and moisture in air, brought for actual production huge
Potential safety hazard.
Positive pole mends lithium as a kind of safe benefit lithium mode, new without extra exploitation without changing existing production technology
Equipment, it can reach uniform on the premise of cost is not improved and mend lithium effect.Positive pole mends lithium will typically mend lithium addition in homogenate
Agent is added in positive electrode slurry, or will mend lithium additive and be coated in positive electrode surface, and its key point is to select properly
Positive pole mend lithium additive.It is required that it has higher de- lithium capacity and reversible capacity low in the range of battery charging and discharging.Meaning
Taste positive pole and mends lithium additive equivalent to a kind of sacrificial lithium salts, and substantial amounts of lithium ion is deviate from charging and is used to supplement negative pole shape
The lithium ion consumed into SEI films so that the lithium ion of positive electrode abjection is not wasted in be formed on SEI films, so as to improve
Positive material utilization ratio.Reach the purpose of lifting battery energy density, the de- lithium capacity for mending lithium additive have to be larger than positive pole
The de- lithium capacity of material.
The content of the invention
The purpose of the application be to provide a kind of new formula lithium ion cell positive mend lithium additive and preparation method thereof and
Using.
The application employs following technical scheme：
The one side of the application discloses a kind of lithium ion cell positive and mends lithium additive, and the lithium ion cell positive mends lithium
Additive is the rich lithium OXYFLUORIDE MATERIALS shown in chemical formula one,
Chemical formula one：Li2VO2F。
It should be noted that the lithium ion cell positive of the application mends lithium additive, good conductivity, the de- lithium capacity of theory
462mAh/g, charging platform is low, about 2.5V, can be good at being used for lithium ion anode material, benefit lithium is carried out to it.
The another side of the application discloses the preparation method of the lithium ion cell positive benefit lithium additive of the application, including will
Li2O, LiF and V2O3Ball milling in an inert atmosphere after mixing, obtained product i.e. chemical formula Li2VO2Rich lithium fluorine oxidation shown in F
Thing material.
Preferably, Li2O, LiF and V2O3Mol ratio be Li2O:LiF:V2O3=(1~1.2):2:1.
Preferably, inert atmosphere is argon gas and/or nitrogen.
Preferably, the condition of ball milling is 300rpm-600rpm, ball milling 12h-60h.
It is furthermore preferred that the condition of ball milling is 400rpm-500rpm, ball milling 36h-48h.
The lithium ion cell positive that the another side of the application discloses the application mends lithium additive in positive electrode, lithium ion
Application in battery or lithium source material.
It is appreciated that the lithium ion cell positive of the application, which mends lithium additive, is inherently directed to lithium ion cell positive material
Material is mended lithium and designed, and therefore, can be used for positive electrode, lithium ion battery, plays and mends lithium effect, and then improves battery and hold
Amount.As lithium source material, mainly it is considered that for the not yet such as V of the positive electrode without lithium of business application at present2O5、FeF3
Etc., when it forms full battery with graphite or silicon etc. without cathode of lithium, the benefit lithium additive of the application can be used as lithium source, be
System provides active lithium-ion.
The application's simultaneously discloses a kind of rich lithium OXYFLUORIDE MATERIALS Li again2VO2Benefits of the F as lithium ion cell positive
The application of lithium additive.
The application's simultaneously discloses a kind of positive electrode of lithium ion battery again, contains the application's in the positive electrode
Lithium ion cell positive mends lithium additive.
Preferably, in positive electrode, the dosage that lithium ion cell positive mends lithium additive is positive electrode gross weight
0.1%-10%.
It is furthermore preferred that the positive active material of positive electrode includes but is not limited to LiCoO2、LiMnO2、LiFePO4, NCM and
At least one of NCA.
Wherein, NCM is nickel-cobalt-manganternary ternary anode material, and NCA is nickel cobalt aluminium tertiary cathode material.
It should be noted that the lithium ion cell positive of the application, which mends lithium additive, can be used for various lithium ion batteries just
Pole material, play a part of mending lithium；LiCoO2、LiMnO2、LiFePO4, NCM and NCA it is simply more conventional use of several at present
Active material, the lithium ion cell positive of the application mend lithium additive and are not limited in mending these positive electrode active materials
Lithium.
A kind of lithium ion cell positive containing the application that simultaneously discloses again of the application mends lithium additive or using this
The lithium ion battery of the positive electrode of application.
Preferably, the negative pole of lithium ion battery is in graphite, silicon, tin alloy, silica composite or Si-C composite material
One or more.
It is furthermore preferred that the negative pole of lithium ion battery is silicon, silica composite or Si-C composite material.
It should be noted that the lithium ion battery of the application, specifically limited, lithium ion battery is had no to cell negative electrode material
Applicable negative material such as graphite, silicon, tin alloy, silica composite and Si-C composite material etc. are used equally for the present invention.But
It is wherein silicon, silica composite and Si-C composite material etc. are first imitates low negative material, contains lithium-ion electric with the application
Pond positive pole mends the positive electrode matching of lithium additive, and the lifting effect to battery capacity becomes apparent.
The beneficial effect of the application is：
The lithium ion cell positive of the application mends lithium additive Li2VO2F, 2 lithium ions, capacity can be discharged in theory
Up to 462mAh/g, and there is preferable electric conductivity, it can be very good to carry out benefit lithium to positive pole.The benefit lithium additive of the application
It is safe and environment-friendly, non-toxic, laid a good foundation to prepare the lithium ion battery of high power capacity.
Brief description of the drawings
Fig. 1 is the actual gram volume of positive electrode and efficiency for charge-discharge test chart in the embodiment of the present application, wherein, " ■ " is to fill
The test curve of electricity, "●" are the test curve of electric discharge, and " ▲ " is efficiency curve；
Fig. 2 is the actual gram volume of positive electrode and efficiency for charge-discharge test chart in the application comparative example, wherein, " ■ " is to fill
The test curve of electricity, "●" are the test curve of electric discharge, and " ▲ " is efficiency curve.
Embodiment
Present inventor has found that the key that positive pole mends lithium is to select in the research process that lithium additive is mended to positive pole
Suitable benefit lithium additive is selected, these benefit lithium additives have to comply with claimed below：(1) in the range of battery charging and discharging have compared with
The de- lithium capacity of high charging and the embedding lithium capacity of very low electric discharge；(2) presence stable in the air；(3) there is good conduction
Property；(4) positive electrode performance is not influenceed.
Studied based on more than and understanding, a kind of creative new lithium ion cell positive that have developed of the application mend lithium addition
Agent, i.e., rich lithium OXYFLUORIDE MATERIALS Li2VO2F。Li2VO2F is the intercalation compound of unordered cube of lava structure, lithium deintercalation performance
It is good, 2 lithium ions can be discharged in theory, and capacity is up to 462mAh/g, and electric conductivity is good, can be stable in the air
In the presence of, and the influence to positive electrode is small；It is that more satisfactory positive pole mends lithium additive material.
The intercalation compound Li of unordered cube of lava structure2VO2F can discharge 2 lithium ions, its reaction side in theory
Formula is as follows：
Theoretical capacity is up to 462mAh/g, also, studies and find, at a temperature of 40 DEG C, 4.1-1.3V charging/discharging voltage
In the range of, when charge-discharge magnification is C/60, Li2VO2Up to 420mAh/g 1.8 electronics about occur for the actual charge/discharge capacities of F
Transfer, and cell volume varies less, only about ≈ 3%, Li2VO2F electrical conductivity is about 2.2 × 10-7S/cm, compare LiFePO4
High two orders of magnitude；It can be seen that Li2VO2F is that a kind of positive pole well mends lithium additive.
The application is described in further detail below by specific embodiment.Following examples only are entered to advance to the application
One step illustrates, should not be construed as the limitation to the application.
Embodiment
It is the rich lithium OXYFLUORIDE MATERIALS shown in chemical formula one that the lithium ion cell positive of this example, which mends lithium additive,
Chemical formula one：Li2VO2F
Li2VO2F preparation method is as follows：
Take 32.868g Li2O powder, 51.88g LiF powder and 149.88g V2O3Powder is raw material, in argon gas atmosphere
In with 450 revs/min of speed ball milling 48h, obtain Li2VO2The lithium ion cell positive of F powder, i.e. this example mends lithium additive.
The lithium ion cell positive of this example is mended into lithium additive positive plate of lithium battery is made, specifically included, this example is made
Li2VO2F lithium ion cell positives mend lithium additive, with positive electrode LiCoO2, super conductive black (abbreviation SP), gather inclined fluorine
Ethene (abbreviation PVDF), N-methyl pyrrolidones (abbreviation NMP) are coated on aluminium foil after being homogenized together is fabricated to positive plate.Its
In, LiCoO2、Li2VO2F, SP, PVDF, NMP, weight ratio be sequentially 100:5.69:1.3:0.81:12.72.Known positive pole material
Expect LiCoO2First charge-discharge efficiency be 94%, the actual discharge specific capacity measured in half-cell is 170mAh/g.
Negative plate first charge-discharge efficiency 83.5%, is measured in half-cell using doping 10wt%SiO graphite cathode
Actual discharge specific capacity 483mAh/g.Negative pole presses active material:SP:CMC:SBR:H2O=100:1:1.3:2.9:85 quality
Negative plate is made than being coated in after homogenate on copper foil.Both positive and negative polarity NP ratios are arranged to 1.05.
Above-mentioned positive plate and negative plate assembling are helped into battery.
Comparative example
By positive electrode LiCoO2, super conductive black (SP), Kynoar (PVDF), N-methyl pyrrolidones
(NMP) sequentially by weight 100:1.3:0.81:12.72 ratio is coated on aluminium foil after being homogenized together and positive plate is made.
Negative pole is using doping 10wt%SiO graphite cathode, first charge-discharge efficiency 83%, actual discharge specific capacity
483mAh/g.Negative pole presses active material:SP:CMC:SBR:H2O=100:1:1.3:2.9:It is coated in after 85 mass ratio homogenate
Negative plate is made on copper foil.Both positive and negative polarity NP ratios are arranged to 1.05.
By embodiment identical method, this example positive plate and negative plate are assembled into the full battery of same model.
The capacity and cycle performance of embodiment and the lithium ion battery of comparative example are entered respectively using constant current charge-discharge method
Row test.Discharge current size is 0.2C, and charging/discharging voltage scope is 4.4-2.5V.The actual gram volume of positive electrode of embodiment
With actual efficiency for charge-discharge as shown in figure 1, the actual gram volume of the positive electrode of comparative example and actual efficiency for charge-discharge such as Fig. 2 institutes
Show.
It can see from Fig. 1 and Fig. 2 test result, additive of the present invention with the addition of in embodiment, in positive electrode
The actual charging and discharging capacity of anode material for lithium-ion batteries close to the material half-cell test capacity, about 170mAh/g, such as
Shown in Fig. 1, hence it is evident that higher than the anode material for lithium-ion batteries gram volume that additive of the present invention is not added in comparative example, by Fig. 2
It can be seen that the capacity of comparative example is only about 150mAh/g.Because the lithium ion cell positive benefit lithium additive of the application can
Deviate from a large amount of lithium ions, the lithium ion for forming SEI films for supplementing silicon based anode material and being consumed so that positive material utilization ratio
Improve, given play to higher gram volume, and then improve the capacity of battery on the whole.
Above content is to combine the further description that specific embodiment is made to the application, it is impossible to assert this Shen
Specific implementation please is confined to these explanations.For the application person of an ordinary skill in the technical field, do not taking off
On the premise of conceiving from the application, some simple deduction or replace can also be made.
Claims (10)
1. a kind of lithium ion cell positive mends lithium additive, it is characterised in that：The lithium ion cell positive mends lithium additive
Rich lithium OXYFLUORIDE MATERIALS shown in chemical formula one,
Chemical formula one：Li2VO2F。
2. lithium ion cell positive according to claim 1 mends the preparation method of lithium additive, it is characterised in that：Including inciting somebody to action
Li2O, LiF and V2O3Ball milling in an inert atmosphere after mixing, obtained product i.e. chemical formula Li2VO2Rich lithium fluorine oxidation shown in F
Thing material.
3. preparation method according to claim 2, it is characterised in that：The Li2O, LiF and V2O3Mol ratio be Li2O:
LiF:V2O3=(1~1.2):2:1.
4. the preparation method according to Claims 2 or 3, it is characterised in that：The inert atmosphere is argon gas and/or nitrogen.
5. the preparation method according to Claims 2 or 3, it is characterised in that：The condition of the ball milling is 300rpm-
600rpm, ball milling 12h-60h；
Preferably, the condition of the ball milling is 400rpm-500rpm, ball milling 36h-48h.
A kind of 6. rich lithium OXYFLUORIDE MATERIALS Li2VO2Applications of the F as the benefit lithium additive of lithium ion cell positive.
A kind of 7. positive electrode of lithium ion battery, it is characterised in that：Contain the lithium described in claim 1 in the positive electrode
Ion battery positive pole mends lithium additive.
8. positive electrode according to claim 7, it is characterised in that：The lithium ion cell positive mends the use of lithium additive
Measure as the 0.1%-10% of positive electrode gross weight；
Preferably, the positive active material of the positive electrode includes but is not limited to LiCoO2、LiMnO2、LiFePO4, NCM and
At least one of NCA.
9. a kind of lithium ion cell positive containing described in claim 1 mends lithium additive or using described in claim 7 or 8
The lithium ion battery of positive electrode.
10. lithium ion battery according to claim 9, it is characterised in that：The negative pole of the lithium ion battery be graphite,
One or more in silicon, tin alloy, silica composite or Si-C composite material；
Preferably, the negative pole of the lithium ion battery is silicon, silica composite or Si-C composite material.
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| CN109004195A (en) * | 2018-07-24 | 2018-12-14 | 安普瑞斯（无锡）有限公司 | A kind of benefit lithium additive and preparation method thereof |
| CN109638341A (en) * | 2018-11-23 | 2019-04-16 | 浙江衡远新能源科技有限公司 | A kind of lithium ion full battery and preparation method thereof |
| CN109888274A (en) * | 2018-12-24 | 2019-06-14 | 中国电子科技集团公司第十八研究所 | Pre-lithiated lithium ion battery positive electrode material and preparation method thereof |
| CN110176641A (en) * | 2019-06-03 | 2019-08-27 | 哈尔滨工业大学 | A kind of nanometer of LiF/Fe/ graphite anode mends the preparation method and applications of lithium slurry |
| CN110294494A (en) * | 2019-07-25 | 2019-10-01 | 哈尔滨工业大学 | Lithium vanadate anode mends lithium additive and its application |
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| CN111403801A (en) * | 2020-03-23 | 2020-07-10 | 孚能科技(赣州)股份有限公司 | Lithium ion battery and preparation method thereof |
| CN112542589A (en) * | 2019-09-20 | 2021-03-23 | 华中科技大学 | Preparation method, product and application of positive electrode prelithiation material |
| CN112951620A (en) * | 2019-12-10 | 2021-06-11 | 中国科学院大连化学物理研究所 | Positive electrode lithium supplement additive, preparation method and application thereof |
| CN113611834A (en) * | 2021-07-30 | 2021-11-05 | 蜂巢能源科技有限公司 | Three-layer core-shell structured positive electrode material, preparation method and battery |
| CN114270568A (en) * | 2021-03-16 | 2022-04-01 | 宁德新能源科技有限公司 | Lithium supplement additive, electrochemical device comprising same, and electronic device |
| WO2023151459A1 (en) * | 2022-02-10 | 2023-08-17 | 深圳市德方创域新能源科技有限公司 | Lithium-supplementing additive, and preparation method therefor and application thereof |
| WO2023160307A1 (en) * | 2022-02-25 | 2023-08-31 | 深圳市德方创域新能源科技有限公司 | Positive electrode lithium replenishment additive, preparation method therefor and use thereof |
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| CN109004195A (en) * | 2018-07-24 | 2018-12-14 | 安普瑞斯（无锡）有限公司 | A kind of benefit lithium additive and preparation method thereof |
| CN109638341A (en) * | 2018-11-23 | 2019-04-16 | 浙江衡远新能源科技有限公司 | A kind of lithium ion full battery and preparation method thereof |
| CN109888274A (en) * | 2018-12-24 | 2019-06-14 | 中国电子科技集团公司第十八研究所 | Pre-lithiated lithium ion battery positive electrode material and preparation method thereof |
| CN111370657A (en) * | 2018-12-26 | 2020-07-03 | 宁德时代新能源科技股份有限公司 | Positive electrode lithium supplement material and preparation method and application thereof |
| CN111370657B (en) * | 2018-12-26 | 2021-05-07 | 宁德时代新能源科技股份有限公司 | Positive electrode lithium supplement material and preparation method and application thereof |
| CN110176641A (en) * | 2019-06-03 | 2019-08-27 | 哈尔滨工业大学 | A kind of nanometer of LiF/Fe/ graphite anode mends the preparation method and applications of lithium slurry |
| CN110294494A (en) * | 2019-07-25 | 2019-10-01 | 哈尔滨工业大学 | Lithium vanadate anode mends lithium additive and its application |
| CN110294494B (en) * | 2019-07-25 | 2022-04-01 | 哈尔滨工业大学 | Lithium vanadate anode lithium supplement additive and application thereof |
| CN112542589B (en) * | 2019-09-20 | 2021-10-08 | 华中科技大学 | Preparation method, product and application of positive electrode prelithiation material |
| CN112542589A (en) * | 2019-09-20 | 2021-03-23 | 华中科技大学 | Preparation method, product and application of positive electrode prelithiation material |
| CN112951620A (en) * | 2019-12-10 | 2021-06-11 | 中国科学院大连化学物理研究所 | Positive electrode lithium supplement additive, preparation method and application thereof |
| CN112951620B (en) * | 2019-12-10 | 2022-04-15 | 中国科学院大连化学物理研究所 | Positive electrode lithium supplement additive, preparation method and application thereof |
| CN111403801A (en) * | 2020-03-23 | 2020-07-10 | 孚能科技(赣州)股份有限公司 | Lithium ion battery and preparation method thereof |
| CN111403801B (en) * | 2020-03-23 | 2023-08-29 | 孚能科技(赣州)股份有限公司 | Lithium ion battery and preparation method thereof |
| CN114270568A (en) * | 2021-03-16 | 2022-04-01 | 宁德新能源科技有限公司 | Lithium supplement additive, electrochemical device comprising same, and electronic device |
| CN113611834A (en) * | 2021-07-30 | 2021-11-05 | 蜂巢能源科技有限公司 | Three-layer core-shell structured positive electrode material, preparation method and battery |
| CN113611834B (en) * | 2021-07-30 | 2023-01-24 | 蜂巢能源科技有限公司 | Three-layer core-shell structured positive electrode material, preparation method and battery |
| WO2023151459A1 (en) * | 2022-02-10 | 2023-08-17 | 深圳市德方创域新能源科技有限公司 | Lithium-supplementing additive, and preparation method therefor and application thereof |
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