CN110176641A - A kind of nanometer of LiF/Fe/ graphite anode mends the preparation method and applications of lithium slurry - Google Patents
A kind of nanometer of LiF/Fe/ graphite anode mends the preparation method and applications of lithium slurry Download PDFInfo
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- CN110176641A CN110176641A CN201910477185.8A CN201910477185A CN110176641A CN 110176641 A CN110176641 A CN 110176641A CN 201910477185 A CN201910477185 A CN 201910477185A CN 110176641 A CN110176641 A CN 110176641A
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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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- 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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- 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
Abstract
The invention discloses the preparation method and applications that a kind of nanometer of LiF/Fe/ graphite anode mends lithium slurry, and described method includes following steps: Step 1: LiF, Fe powder, graphite are mixed evenly；Step 2: being transferred in high-energy ball milling tank after dehydrated alcohol being added in uniformly mixed LiF, Fe powder, graphite powder, high-energy ball milling, obtains nanometer LiF/Fe/ graphite anode and mends lithium slurry under inert gas protection.Nanometer LiF/Fe/ graphite anode obtained by the above method, which mends lithium slurry, can be applied to lithium ion cell positive benefit lithium.LiF is reacted with Fe after lithium ion battery initial charge to 4.5 V generates FeF3And discharge Li+, FeF when discharging into 3.0 V3LiF and Fe, extra Li are not returned to+It is formed and Li caused by the dead lithium of following cycle for compensating SEI film+Consumption.The present invention prepares that cost of material is low, and manufacture craft is simple, preparation process clean and environmental protection.
Description
Technical field
The invention belongs to technical field of energy material, it is related to a kind of LiF/Fe anode and mends the preparation method of lithium slurry and its answer
With more particularly to a kind of nanometer of LiF/Fe/ graphite anode mend the preparation method and applications of lithium slurry.
Background technique
It is currently the lithium ion battery of cathode during first charge-discharge using graphite or silicon-carbon, the work of about 10 % in anode
Property lithium can be consumed, and form irreversible stable SEI film on the surface of cathode, lead to irreversible capacity loss, and then reduce
The energy density of lithium ion battery.Researcher wishes this part irreversible capacity loss can be made to disappear by the method for mending lithium
It removes.It is usually all to supplement part metals lithium powder in negative terminal surface, but because safety is bad without large-scale application.Anode mends lithium
Because it has many advantages, such as relatively stable, cheap, high benefit lithium capacity and safety, receive significant attention.
Following condition need to be met by mending lithium material as anode :(a) electrolyte compatibility.It mends lithium material and its decomposes and produce
Object be in traditional electrolyte it is stable, the penalty of lithium ion battery will not be caused.(b) current potential is suitable for.Mend lithium material
De- lithium current potential should be less than the charge cutoff current potential of conventional lithium ion battery, and intercalation potential equally should be less than conventional lithium ion battery
Because the reasons such as structure change active lithium can not be again reversible etc. after electric discharge stopping potential or de- lithium.(c) high benefit lithium capacity.It mends
Lithium material should have benefit lithium capacity as high as possible, mend lithium capacity and energy per volume should be higher than that existing conventional lithium ion
Battery.The charge cutoff current potential of conventional lithium ion battery is generally greater than 4.2 V (vs.Li/Li at present+), discharge stopping potential one
As be higher than in 2.5 V(vs.Li/Li+), such as LiFePO4(4.1-2.8 V), LiCoO2(4.2-3.2 V), LiMn2O4(4.3-3
) and LiNi V0.5Mn1.5O4(4.9-3.5 V) etc..
LiF/Fe is FeF3When the product reacted with Li, completely conversion, 712 mAh/g are up to corresponding to theoretical specific capacity.
FeF3Generally as the anode of high-energy density, however because reacting the problems such as poorly reversible, cycle performance restricts its application,
It cannot achieve business application in a short time.However FeF3Specific capacity with higher, and mend lithium material current potential as anode and just fit
For traditional lithium ion battery.
Summary of the invention
The present invention is directed to the existing lithium ion battery lower problem of coulombic efficiency for the first time, provides a kind of nanometer of LiF/Fe/
Graphite anode mends the preparation method and applications of lithium slurry, and the anode containing height ratio capacity LiF/Fe and high conductivity graphite mends lithium
Slurry can be obtained by high-energy ball milling, simple and easy.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of nanometer of LiF/Fe/ graphite anode mends the preparation method of lithium slurry, includes the following steps:
Step 1: LiF, Fe powder, graphite are mixed evenly according to the mass ratio of 7:5:1 ~ 5；
In this step, LiF, Fe powder, graphite are procurement of commodities, without special processing；The mixing of LiF, Fe powder, graphite
Mass ratio can be 7:5:1,7:5:2,7:5:3 etc..
Step 2: being shifted being added in uniformly mixed LiF, Fe powder, graphite powder after appropriate dehydrated alcohol forms slurry
Into high-energy ball milling tank, high-energy ball milling, obtains nanometer LiF/Fe/ graphite anode and mends lithium slurry under inert gas protection, in which:
Material, ball material and solvent ratios 5 ~ 2:1:0.5 ~ 2；
In this step, the inert gas is one of argon gas, nitrogen, hydrogen-argon-mixed；The revolving speed of the high-energy ball milling is
500 ~ 3000 rpm/min, time are 2 ~ 12 hours.
The nanometer LiF/Fe/ graphite anode that the above method is prepared, which mends lithium slurry, can be applied to lithium ion cell positive benefit
Lithium, application method are as follows:
Nanometer LiF/Fe/ graphite anode benefit lithium slurry is added drop-wise to LiFPO4、LiCoO2、LiNi0.8Co0.1Mn0.1O2Equal positive plates
Surface by spreader or is coated in positive plate surface manually and covers one layer of nanometer LiF/Fe/ graphite anode benefit lithium slurry (coating
With a thickness of 2 ~ 15 μm), the pole piece after 100 DEG C of dryings is assembled as lithium ion cell positive for lithium ion battery, wherein
It is 2 ~ 15 % that LiF/Fe/ graphite anode, which mends accounting of the lithium slurry in positive gross mass,.The lithium ion battery initial charge arrives
LiF is reacted with Fe after 4.5 V generates FeF3And discharge Li+, FeF when discharging into 3.0 V3LiF and Fe, extra Li are not returned to+
It is formed and Li caused by the dead lithium of following cycle for compensating SEI film+Consumption.
Compared with the prior art, the present invention has the advantage that
(1) LiF/Fe has height ratio capacity and suitable decomposition voltage, and a large amount of Li can be provided for anode+, supplement initial charge
When cathode formed SEI film consumption Li+(Fig. 1).
(2) FeF formed after initial charge3It will not be re-converted into LiF/Fe in discharge voltage section, and can mention
For certain capacity.
(3) the quality accounting that can control LiF/Fe in anode by different slurry mixed proportion and coating thickness, from
And control battery entirety specific capacity.
(4) prepare that cost of material is low, and manufacture craft is simple, preparation process clean and environmental protection.
Detailed description of the invention
Fig. 1 is that tertiary cathode is added to first charge-discharge curve after 5 wt% LiF/Fe/ graphite benefit lithium slurry.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
2 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling is mended into lithium slurry and LiFPO is added dropwise4Positive plate surface (mass fraction
About 5%), it is coated using spreader, with a thickness of 5 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 2
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
4 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling is mended into lithium slurry and LiFPO is added dropwise4Positive plate surface (mass fraction
About 5%), it is coated using spreader, with a thickness of 5 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 3
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
8 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling is mended into lithium slurry and LiFPO is added dropwise4Positive plate surface (mass fraction
About 5%), it is coated using spreader, with a thickness of 5 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 4
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
12 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling is mended into lithium slurry and LiFPO is added dropwise4Positive plate surface (mass fraction
About 5%), it is coated using spreader, with a thickness of 5 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 5
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
2 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling is mended into lithium slurry and LiFPO is added dropwise4Positive plate surface (mass fraction
About 10%), it is coated using spreader, with a thickness of 10 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 6
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
12 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling benefit lithium slurry is added drop-wise to LiFPO4Positive plate surface (quality point
About 10%) number, is coated using spreader, with a thickness of 10 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 7
(1) 7 g LiF, 5 g Fe powder, 1 g graphite is taken to be uniformly mixed；
(2) 20 ml dehydrated alcohols are added in uniformly mixed powder, slurry is transferred in high-energy ball milling tank after mixing evenly
12 h of high-energy ball milling；
(3) the nanometer LiF/Fe/ graphite anode obtained after ball milling is mended into lithium slurry and LiCoO is added dropwise2Positive plate surface (mass fraction
About 10%), it is coated using spreader, with a thickness of 10 μm, can be used as lithium ion cell positive use after 100 DEG C of dryings.
Embodiment 8
The preparation and performance test of electrode: it is anode that lithium slurry is mended in coating, uses lithium metal as cathode, uses Celgard
2400 model diaphragms, the LiPF of 1mol/L6Electrolyte is done in dissolution EC/DMC (volume ratio 1:1) solvent, in glove box
In be assembled into button cell.Using the pond Neware test macro carry out constant current charge-discharge test, charging/discharging voltage range be 3 ~
4.5 V。
Claims (9)
1. the preparation method that a kind of nanometer of LiF/Fe/ graphite anode mends lithium slurry, it is characterised in that the method includes walking as follows
It is rapid:
Step 1: LiF, Fe powder, graphite are mixed evenly according to the mass ratio of 7:5:1 ~ 5；
Step 2: be transferred in high-energy ball milling tank after dehydrated alcohol being added in uniformly mixed LiF, Fe powder, graphite powder,
High-energy ball milling under inert gas shielding obtains nanometer LiF/Fe/ graphite anode and mends lithium slurry, in which: material, ball material and solvent ratio
Example 5 ~ 2:1:0.5 ~ 2.
2. the preparation method that according to claim 1 nanometer of LiF/Fe/ graphite anode mends lithium slurry, it is characterised in that described
LiF, Fe powder, graphite mixing mass ratio be 7:5:1,7:5:2 or 7:5:3.
3. the preparation method that according to claim 1 nanometer of LiF/Fe/ graphite anode mends lithium slurry, it is characterised in that described
Inert gas is one of argon gas, nitrogen, hydrogen-argon-mixed.
4. the preparation method that according to claim 1 nanometer of LiF/Fe/ graphite anode mends lithium slurry, it is characterised in that described
The revolving speed of high-energy ball milling is 500-3000 rpm/min, and the time is 2 ~ 12 hours.
Exist 5. the nanometer LiF/Fe/ graphite anode that claim 1-4 any claim the method is prepared mends lithium slurry
Lithium ion cell positive mends the application in lithium.
6. according to claim 5 nanometer of LiF/Fe/ graphite anode is mended lithium slurry and is mended in lithium in lithium ion cell positive
Using, it is characterised in that the nanometer LiF/Fe/ graphite anode mends lithium slurry and mends the user in lithium in lithium ion cell positive
Method is as follows:
Nanometer LiF/Fe/ graphite anode benefit lithium slurry is added drop-wise to positive plate surface, covers one layer of nanometer on positive plate surface
LiF/Fe/ graphite anode mends lithium slurry, and the pole piece after drying is assembled as lithium ion cell positive for lithium ion battery.
7. according to claim 5 nanometer of LiF/Fe/ graphite anode is mended lithium slurry and is mended in lithium in lithium ion cell positive
Using, it is characterised in that the positive plate is LiFPO4、LiCoO2Or LiNi0.8Co0.1Mn0.1O2。
8. according to claim 5 nanometer of LiF/Fe/ graphite anode is mended lithium slurry and is mended in lithium in lithium ion cell positive
Using, it is characterised in that the coating thickness that the nanometer LiF/Fe/ graphite anode mends lithium slurry is 2 ~ 15 μm.
9. according to claim 5 nanometer of LiF/Fe/ graphite anode is mended lithium slurry and is mended in lithium in lithium ion cell positive
Using, it is characterised in that it is 2 ~ 15 % that the nanometer LiF/Fe/ graphite anode, which mends accounting of the lithium slurry in positive gross mass,.
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Cited By (6)
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| CN111834622A (en) * | 2020-07-22 | 2020-10-27 | 华中科技大学 | Multilayer positive plate with lithium/sodium supplementing function, battery and preparation method |
| CN112271279A (en) * | 2020-10-22 | 2021-01-26 | 欣旺达电动汽车电池有限公司 | Composite cathode material, preparation method and application thereof, and lithium ion battery |
| CN112271281A (en) * | 2020-10-22 | 2021-01-26 | 欣旺达电动汽车电池有限公司 | Composite cathode material, preparation method and application thereof, and lithium ion battery |
| CN112290022A (en) * | 2020-10-20 | 2021-01-29 | 合肥国轩高科动力能源有限公司 | Lithium ion battery anode lithium supplement additive and preparation method and application 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 |
| CN112670476A (en) * | 2020-12-22 | 2021-04-16 | 江苏双登富朗特新能源有限公司 | Preparation method of lithium ion storage battery anode material LiF/Fe compound |
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Application publication date: 20190827 |