CN110504488A - A kind of electrolyte and preparation method thereof that graphene quantum dot is modified - Google Patents
A kind of electrolyte and preparation method thereof that graphene quantum dot is modified Download PDFInfo
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- CN110504488A CN110504488A CN201910732788.8A CN201910732788A CN110504488A CN 110504488 A CN110504488 A CN 110504488A CN 201910732788 A CN201910732788 A CN 201910732788A CN 110504488 A CN110504488 A CN 110504488A
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- 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
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- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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Abstract
The present invention provides a kind of electrolyte and preparation method thereof that graphene quantum dot is modified, belongs to lithium metal battery electrolyte field.The present invention in business electrolyte by adding graphene quantum dot and polymer, wherein graphene quantum dot can continue to provide forming core site, polymer disperses graphene quantum dot uniformly in the electrolytic solution, preparation process is easy, and it can be obviously improved circulation and high rate performance of the lithium metal battery under high current and high capacity operating condition, the lithium metal battery in modified by graphene quantum dot electrolyte reaches 4mA/cm in current density2Reach 4mAh/cm with circulation volume2When, still there is not short circuit phenomenon caused by Li dendrite, maintain preferable charge-discharge performance, there is potential application in lithium metal battery field, realizes the purpose of the cathode of lithium protection under high current and high capacity.
Description
Technical field
The invention belongs to lithium metal battery electrolyte fields, and in particular to a kind of modified electrolyte of graphene quantum dot and
Preparation method.
Background technique
With the fast development in the fields such as portable electronic device and electric car, society is to high-energy density energy-storage battery
Demand present explosive growth.Metal lithium electrode has the theoretical capacity for being equivalent to ten times of carbon-based lithium ion electrode
(3860mAh/g), thus obtained lithium metal battery, such as lithium-sulfur cell (Li-S) and lithium-oxygen battery (Li-O2), it is considered to be most
Potential high-energy density energy storage device.However, metal lithium electrode can generate a large amount of dendrite in charge and discharge process, not only
Cycle performance is influenced, diaphragm can be also punctured, make internal short-circuit of battery, cause to be brought rapidly up, brings fire even hidden peril of explosion.Cause
This, studies Li dendrite formation mechenism, then inhibits lithium dendrite growth, develops the lithium of high-energy density, high power and high security
Metal battery is extremely urgent.
In recent years, the strategy for inhibiting Li dendrite mainly includes the design of cathode carrier, the building of artificial SEI film, solid-state electricity
It solves the use of liquid and introduces additive in the electrolytic solution.Wherein, suitable lithium metal carrier can alleviate circulation electrochemistry and follow
The variation of negative electrode volume during ring, however, since carrier does not have electro-chemical activity, so its introducing causes electrode entirety energy
The reduction of metric density；Artificial constructed SEI film provides possibility for the careful design of electrochemical interface, but its manufacturing process is multiple
It is miscellaneous, be not suitable for the application of scale；Solid-state electrolytic solution has very high modulus of shearing, can prevent Li dendrite from penetrating electrolyte,
And the use of flammable liquid electrolyte is avoided, however its conductivity at room temperature is lower and interface contact resistance is higher
Problem is not resolved also.Therefore, it is necessary to a kind of new resolution policies.
The nucleation and growth course of lithium can be modulated by introducing additive in the electrolytic solution, be represented a kind of easy and great latent
The scheme of power.But existing technical solution, such as Kim et al. (Kim, etal.Controlled Lithium Dendrite
Growth by a Synergistic Effect of Multilayered Graphene Coating and an
Electrolyte Additive.Chem.Ma ter.2015,27 (8), 2780-2787.), Zhang.R et al. (Zhang.R,
etal.Conductive Nanostructured Sca ffolds Render Low Local Current Density to
Inhibit Lithium Dendrite Growth.Adv.Mater.2016,28 (11), 2155-62.) and Zheng.G et al.
(Zheng.G,etal.Interconnected hollow carbon nano spheres for stable lithium
Metal anodes.Nat.Nanotech.2014,9 (8), 618-623.), all it is only limitted to low current (≤2mA/cm2) and low appearance
Measure (≤2mAh/cm2) under Li dendrite inhibit research.And with the load and multiplying power of lithium metal battery (such as Li-S battery) anode
It is constantly promoted, lithium an- ode will be faced in bigger current density (>=3mA/cm2) and displacement volume (>=3mAh/cm2) under work
Make, relying solely on existing modulation strategy can no longer meet the demand that high-performance lithium metal battery protects cathode of lithium.In addition,
Common electrolysis additive (Ding.F, etal.Dendrite-free lithium de position via self-
Healing electrostatic shield mechanism.J.Am.Chem.Soc.2013,135 (11), 4450-6.) no
Forming core be can control to inhibit the formation of Li dendrite in root；And it is existing control lithium deposition forming core scheme (Liu.Y,
etal.Pre-planted nucleation seeds for rechargeable metallic lithium
Anodes.J.Mater.Chem.A 2017,5 (35), 18862-18869.) complex process, it is unfavorable for scale and commercialization.
Therefore, new cathode Preservation tactics are developed, the lithium an- ode without dendrite under high current and high capacity working environment, tool are obtained
There is highly important industrial application to be worth.
Summary of the invention
For the problems of background technique, the purpose of the present invention is to provide a kind of modified electricity of graphene quantum dot
Liquid and preparation method thereof is solved, the electrolyte in business electrolyte by adding graphene quantum dot and polymer, wherein graphite
Alkene quantum dot can continue to provide forming core site, and polymer disperses graphene quantum dot uniformly in the electrolytic solution, realizes
The purpose of cathode of lithium protection under high current and high capacity.
To achieve the above object, technical scheme is as follows:
A kind of modified electrolyte of graphene quantum dot, including lithium salts, organic solvent, additive, graphene quantum dot and
Polymer, wherein the concentration of the lithium salts is 0.5~1mol/L, and the content of additive is 1.5~2wt%, graphene quantum dot
Content in the electrolyte is 0.5~2mg/mL, and content of the polymer in the electrolyte is 25~100mg/mL.
Further, the lithium salts is LiTFSI, LiPF6、LiBF4、LiBOB、LiBC2O4F2、LiClO4、LiCF3SO3、
LiN(FSO2)2、LiN(CF3SO2)2One or more of, the additive is LiNO3, the organic solvent is 1,3- dioxy
Penta ring (DOL) and glycol dimethyl ether (1,2-dimethoxyethane) mixed solution.
Further, the volume ratio of two kinds of substances is 1:1 in the organic solvent.
Further, the polymer is that can make the evenly dispersed polymer in the electrolytic solution of graphene quantum dot, specifically
For polyethylene oxide (PEO).
A kind of preparation method for the electrolyte that graphene quantum dot is modified, comprising the following steps:
Step 1: lithium salts, organic solvent and additive being mixed, mixed solution A is obtained, wherein the concentration of lithium salts is 0.5
~1mol/L；
Step 2: add graphene quantum dot into mixed solution A, stirring 12~for 24 hours, obtain dispersion liquid B, wherein graphite
Content of the alkene quantum dot in dispersion liquid B is 0.5~2mg/mL；
Step 3: adding polymer into dispersion liquid B, stir 24~48h, the electrolyte of the modification can be obtained.
The present invention also provides application of the modified electrolyte of above-mentioned graphene quantum dot in lithium metal battery.
The principle of the present invention are as follows: graphene quantum dot represents a kind of size less than 30nm, has monoatomic layer or few layer
The novel zero dimension carbon material of graphene-structured has very strong quantum limitation effect and edge effect, in combination with graphene
With the excellent properties of both quantum dots.Graphene quantum dot have high-specific surface area, monoatomic layer thickness, small-size effect and easily
In surface is modified the advantages that, with great potential in terms of metal lithium electrode protection: (1) utilizing the Gao Bibiao of graphene quantum dot
Area and small size property can obtain smaller lithium forming core crystal grain, form dense uniform as heterogeneous forming core site
Deposition；(2) due to the monoatomic layer thickness property of graphene quantum dot, under the premise of not influencing lithium ion diffusion, graphene
Quantum dot can participate in constructing stable SEI film, avoid conventional decorative layer bring contact resistance and increase and electronics, ion biography
The problems such as conductance reduces.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
1. the present invention uses graphene quantum dot to be modified as additive to electrolyte, lithium ion transport is not being influenced
Under the premise of, as the homogeneous nucleation and growth deposition of forming core site guidance lithium, inhibit in metal lithium electrode charge and discharge cycles
Dendritic growth eliminates short-circuit hidden danger, in current density 3mA/cm2With capacity 3mAh/cm2Guarantee lithium metal battery under operating condition
Stabilization circulation time be more than 500 hours, overpotential is maintained at 15mV.
2. the modified electrolyte of graphene quantum dot disclosed by the invention has the characteristics that preparation process simplicity, and can show
The circulation and high rate performance for promoting lithium metal battery under high current and high capacity operating condition are write, in modified by graphene quantum dot
Lithium metal battery in electrolyte reaches 4mA/cm in current density2Reach 4mAh/cm with circulation volume2When, still do not occur
Short circuit phenomenon caused by Li dendrite maintains preferable charge-discharge performance, has potential application in lithium metal battery field.
Detailed description of the invention
Fig. 1 is lithium Symmetrical cells prepared by the embodiment of the present invention 1 in current density 3mA/cm2With capacity 3mAh/cm2Work
Long circulating performance map under the conditions of work.
Fig. 2 is the deposition morphology figure of lithium Symmetrical cells prepared by the embodiment of the present invention 1.
Fig. 3 is lithium Symmetrical cells prepared by the embodiment of the present invention 2 in current density 3mA/cm2With capacity 3mAh/cm2Work
Long circulating performance map under the conditions of work.
Fig. 4 is lithium Symmetrical cells prepared by the embodiment of the present invention 3 in current density 3mA/cm2With capacity 4mAh/cm2Work
Long circulating performance map under the conditions of work.
Fig. 5 is lithium Symmetrical cells prepared by the embodiment of the present invention 4 in current density 4mA/cm2With capacity 4mAh/cm2Work
Long circulating performance map under the conditions of work.
Fig. 6 is lithium Symmetrical cells prepared by comparative example in current density 3mA/cm2With capacity 3mAh/cm2Under operating condition
Long circulating performance map.
Fig. 7 is the deposition morphology figure of lithium Symmetrical cells prepared by comparative example.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below with reference to embodiment and attached drawing, to this hair
It is bright to be described in further detail.
A kind of modified electrolyte of graphene quantum dot, including lithium salts, organic solvent, additive, graphene quantum dot and
Polymer, wherein the concentration of the lithium salts is 0.5~1mol/L, and content of the graphene quantum dot in the electrolyte is 0.5
~2mg/mL, content of the polymer in the electrolyte are 25~100mg/mL.
The lithium salts is LiTFSI, LiPF6、LiBF4、LiBOB、LiBC2O4F2、LiClO4、LiCF3SO3、LiN(FSO2)2、
LiN(CF3SO2)2One or more of, additive is the LiNO of 2.0wt%3, the organic solvent is 1,3-dioxolane
(DOL) and glycol dimethyl ether (1,2-dimethoxyethane), the polymer are polyethylene oxide (PEO).
Embodiment 1
A kind of preparation method for the electrolyte that graphene quantum dot is modified, comprising the following steps:
Step 1: 1, the 2- dimethoxy-ethane of the DOL of 50ml and 50ml being mixed, organic solvent is obtained, then organic
The LiTFSI salt of 0.1mol is added in solvent, obtains mixed solution A；
Step 2: 50mg graphene quantum dot is added in the mixed solution A that step 1 obtains, stirring for 24 hours, obtains dispersion liquid
B；
Step 3: 5g polyethylene oxide is added into dispersion liquid B, for 24 hours, the electrolyte of the modification can be obtained in stirring.
The assembling and test of battery: using this field conventional sectional technique assemble lithium Symmetrical cells, comprising anode, cathode,
Diaphragm and the electrolyte of above-mentioned modification, wherein positive and cathode is all lithium metal piece.
Battery testing is constant current charge-discharge, and electric current is set as 3mA/cm2, single cycle capacity is set as 3mAh/cm2's
Long circulating performance map is as shown in Figure 1, deposition morphology figure is as shown in Figure 2.
Embodiment 2
The modified electrolyte of graphene quantum dot is prepared according to the step of embodiment 1, only by the graphene amount in step 2
Son point additional amount is adjusted to 100mg.
The lithium metal Symmetrical cells constant current charge-discharge curve that the present embodiment obtains is as shown in Figure 3.
Embodiment 3
The modified electrolyte of graphene quantum dot is prepared according to the step of embodiment 1, only by the graphene amount in step 2
Son point additional amount is adjusted to 150mg.
The lithium metal Symmetrical cells that the present embodiment obtains carry out constant current charge-discharge test, and electric current is set as 3mA/cm2, single
Secondary circulation volume is set as 4mAh/cm2, constant current charge-discharge curve is as shown in Figure 4.
Embodiment 4
The modified electrolyte of graphene quantum dot is prepared according to the step of embodiment 1, only by the graphene amount in step 2
Son point additional amount is adjusted to 200mg.
The lithium metal Symmetrical cells that the present embodiment obtains carry out constant current charge-discharge test, and electric current is set as 4mA/cm2, single
Secondary circulation volume is set as 4mAh/cm2, constant current charge-discharge curve is as shown in Figure 5.
Comparative example
By DOL and 1,1:1 prepares organic solvent to 2- dimethoxy-ethane by volume, and LiTFSI is added in organic solvent
Salt, the concentration for preparing LiTFSI salt is the electrolyte of 1mol/L.
Constant current charge-discharge test is carried out using electrolyte preparation lithium metal Symmetrical cells, electric current is set as 3mA/cm2,
Single cycle capacity is set as 3mAh/cm2, long circulating performance map is as shown in fig. 6, deposition morphology figure is as shown in Figure 7.
Fig. 1 is lithium Symmetrical cells prepared by the embodiment of the present invention 1 in current density 3mA/cm2With capacity 3mAh/cm2Work
Long circulating performance map under the conditions of work, it can be seen from the figure that lithium Symmetrical cells stable circulation, does not occur short circuit or polarization is existing
As overpotential is stablized in 15mV after the circulation greater than 500 hours；Fig. 2 is lithium Symmetrical cells prepared by the embodiment of the present invention 1
Deposition morphology scanning electron microscope image, it can be seen from the figure that, there is not Li dendrite in lithium depositing homogeneous；Fig. 3 is this
Lithium Symmetrical cells are in current density 3mA/cm prepared by inventive embodiments 22With capacity 3mAh/cm2Long circulating under operating condition
It can scheme, lithium Symmetrical cells stable circulation does not occur short circuit or polarization phenomena, and overpotential is stablized after 200 hours circulations
18mV；Fig. 4 is lithium Symmetrical cells prepared by the embodiment of the present invention 3 in current density 3mA/cm2With capacity 4mAh/cm2Operating condition
Under long circulating performance map, lithium Symmetrical cells stable circulation, do not occur short circuit or polarization phenomena, the mistake after 130 hours circulations
Current potential is stablized in 19mV；Fig. 5 is lithium Symmetrical cells prepared by the embodiment of the present invention 4 in current density 4mA/cm2With capacity 4mAh/
cm2Long circulating performance map under operating condition, as seen from the figure, lithium Symmetrical cells stable circulation, does not occur short circuit or polarization is existing
As overpotential is stablized in 23mV after 110 hours circulations；Fig. 6 is lithium Symmetrical cells prepared by comparative example in current density 3mA/
cm2With capacity 3mAh/cm2Long circulating performance map under operating condition, as seen from the figure, there is soft short circuit after 35 hours in battery
Phenomenon is circulated throughout potential drop as low as 8mV；Fig. 7 is lithium Symmetrical cells deposition morphology scanning electron microscope prepared by comparative example
Image, it can be seen from the figure that dendrite protrusion obviously occurs in lithium deposition.
The above description is merely a specific embodiment, any feature disclosed in this specification, except non-specifically
Narration, can be replaced by other alternative features that are equivalent or have similar purpose；Disclosed all features or all sides
Method or in the process the step of, other than mutually exclusive feature and/or step, can be combined in any way.
Claims (7)
1. a kind of modified electrolyte of graphene quantum dot, including lithium salts, organic solvent and additive, which is characterized in that described
Electrolyte further includes graphene quantum dot and polymer, wherein the concentration of the lithium salts is 0.5~1mol/L, and additive contains
Amount is 1.5~2wt%, and the content of graphene quantum dot is 0.5~2mg/mL, and the content of polymer is 25~100mg/mL.
2. the modified electrolyte of graphene quantum dot as described in claim 1, which is characterized in that the lithium salts be LiTFSI,
LiPF6、LiBF4、LiBOB、LiBC2O4F2、LiClO4、LiCF3SO3、LiN(FSO2)2、LiN(CF3SO2)2One of or it is several
Kind, the additive is LiNO3, the organic solvent is 1,3-dioxolane and glycol dimethyl ether mixed solution.
3. the modified electrolyte of graphene quantum dot as claimed in claim 2, which is characterized in that 1,3- bis- in the organic solvent
The volume ratio of butyl oxide link and glycol dimethyl ether is 1:1.
4. the modified electrolyte of graphene quantum dot as described in claim 1, which is characterized in that the polymer is that can make graphite
The evenly dispersed polymer in the electrolytic solution of alkene quantum dot.
5. the modified electrolyte of graphene quantum dot as claimed in claim 4, which is characterized in that described to make graphene quantum dot
Evenly dispersed polymer in the electrolytic solution is polyethylene oxide.
6. the preparation method of the modified electrolyte of graphene quantum dot as described in any one of Claims 1 to 5, which is characterized in that
The following steps are included:
Step 1: by lithium salts, organic solvent and additive mix, obtain mixed solution A, wherein the concentration of lithium salts be 0.5~
1mol/L；
Step 2: adding graphene quantum dot into mixed solution A, stir, obtain dispersion liquid B, wherein graphene quantum dot exists
Content in dispersion liquid B is 0.5~2mg/mL；
Step 3: adding polymer into dispersion liquid B, stir, the electrolyte of the modification can be obtained.
7. application of the modified electrolyte of any one of Claims 1 to 5 graphene quantum dot in lithium metal battery.
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| CN113422055A (en) * | 2021-05-27 | 2021-09-21 | 复旦大学 | Lithium-philic graphene quantum dot/lithium composite material and preparation method and application thereof |
| CN113998692A (en) * | 2021-10-12 | 2022-02-01 | 中南大学 | Graphene quantum dot, preparation method thereof, electrolyte containing graphene quantum dot and application of electrolyte in zinc ion battery |
| CN116264323A (en) * | 2021-12-15 | 2023-06-16 | 张家港市国泰华荣化工新材料有限公司 | Sodium ion battery electrolyte and sodium ion battery |
| WO2024058519A1 (en) * | 2022-09-14 | 2024-03-21 | 주식회사 그래피니드테크놀로지 | Electrolyte additive, and electrolyte for lithium metal battery or lithium-ion battery, comprising same |
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| CN116264323A (en) * | 2021-12-15 | 2023-06-16 | 张家港市国泰华荣化工新材料有限公司 | Sodium ion battery electrolyte and sodium ion battery |
| CN116264323B (en) * | 2021-12-15 | 2024-03-01 | 张家港市国泰华荣化工新材料有限公司 | Sodium ion battery electrolyte and sodium ion battery |
| WO2024058519A1 (en) * | 2022-09-14 | 2024-03-21 | 주식회사 그래피니드테크놀로지 | Electrolyte additive, and electrolyte for lithium metal battery or lithium-ion battery, comprising same |
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