CN113224387B - Lithium-sulfur electrolyte added with Grignard reagent derivative, and preparation method and application thereof - Google Patents
Lithium-sulfur electrolyte added with Grignard reagent derivative, and preparation method and application thereof Download PDFInfo
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- 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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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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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
- H01M10/42—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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Abstract
The invention discloses a lithium-sulfur electrolyte added with a Grignard reagent derivative, and a preparation method and application thereof, and belongs to the technical field of lithium batteries. The electrolyte is obtained as follows: adding a Grignard reagent derivative into a lithium-sulfur electrolyte; the lithium-sulfur electrolyte is an organic solvent of lithium salt, the concentration of the lithium salt in the organic solvent is 0.5-2 mol/L, and the addition amount of the Grignard reagent derivative is 0.2-0.3% of the volume of the lithium-sulfur electrolyte; the lithium salt is one or more of lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, lithium tris (trifluoromethylsulfonyl) methide, lithium bisoxalato borate and the like. According to the invention, a trace amount of Grignard reagent derivatives are added into the lithium sulfur electrolyte, so that the conversion and catalysis of polysulfide of an intermediate product are promoted, and the dissolution of the intermediate product is reduced; meanwhile, a small amount of Grignard reagent derivatives can have a certain protection effect on the lithium cathode, inhibit the shuttle effect and improve the capacity and the cycling stability of the battery.
Description
Technical Field
The invention belongs to the field of lithium batteries, and particularly relates to a lithium sulfur electrolyte added with a Grignard reagent derivative, and a preparation method and application thereof.
Background
With the development of science and technology, people have higher and higher requirements on energy storage devices, and therefore, the development of secondary batteries with high energy density becomes a major topic of the current society. Compared with the traditional lithium ion battery, the sulfur anode material has the characteristics of high theoretical capacity, low cost and environmental friendliness, so that the lithium sulfur battery is considered as the next generation of energy storage device with a very wide prospect; however, the poor solubility of the discharge product and the severe shuttling effect during the cycling process, and the formation of lithium dendrite causes the poor electrochemical performance of the lithium-sulfur battery, which is greatly limited in practical application.
In order to prevent polysulfide from dissolving, improve the utilization rate of sulfur, inhibit shuttle effect and hinder the formation of lithium dendrites, researchers have conducted a great deal of work and research on positive electrode materials, electrolyte, diaphragms and lithium negative electrode materials, although the utilization rate of sulfur can be improved to a certain extent and the shuttle effect is inhibited, the adopted scheme is complex in process and not beneficial to large-scale industrial production; although the conventional lithium sulfur electrolyte greatly improves the electrochemical capacity of the battery, it does not well prevent the dissolution of intermediate products, inhibit the shuttle effect, and improve the stability of the battery, so it is necessary to develop a low-cost and high-efficiency lithium sulfur electrolyte. According to the invention, additive Grignard reagent derivatives are added into the common lithium sulfur electrolyte to promote the catalysis and conversion of polysulfide, improve the utilization rate of sulfur, and simultaneously have good protection effect on a lithium cathode, prevent the formation of lithium dendrites and improve the electrochemical performance of the battery.
Disclosure of Invention
The invention aims to provide a lithium sulfur electrolyte added with a Grignard reagent derivative, and a preparation method and application thereof.
The invention has simple process, less consumption, low cost and low equipment requirement, can efficiently and simply obtain the required lithium-sulfur electrolyte, and is suitable for large-scale industrial production.
According to the invention, trace Grignard reagent derivatives are added into the common lithium sulfur electrolyte to promote the catalysis and conversion of polysulfide of a discharge product, so that the reduction of sulfur utilization rate caused by polysulfide dissolution is prevented; meanwhile, a proper amount of the Grignard reagent derivative has a good protection effect on the lithium cathode, prevents the formation of lithium dendrites, inhibits a shuttle effect, and further improves the electrochemical capacity and stability of the lithium-sulfur battery.
Based on the purpose, the invention adopts the following technical scheme:
a lithium sulfur electrolyte with added Grignard reagent derivative is obtained by the following processes: adding a grignard reagent derivative into a lithium-sulfur electrolyte; the lithium-sulfur electrolyte is an organic solvent of lithium salt, the concentration of the lithium salt in the organic solvent is 0.5-2 mol/L, and the addition amount of the Grignard reagent derivative is 0.2-0.3% of the volume of the lithium-sulfur electrolyte; the lithium salt is one or more of lithium hexafluorophosphate, lithium tetrafluorophosphate, lithium nitrate, lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, tris (trifluoromethylsulfonyl) methyllithium or lithium bisoxalateborate, and the organic solvent is composed of ethylene glycol dimethyl ether and dioxolane in a volume ratio of 1: 1.
Preferably, the lithium salt is lithium bistrifluoromethanesulfonylimide, and the grignard reagent derivative is magnesium hexamethyldisilazide (HMDSMgCl), magnesium bis-hexamethyldisilazide ((HMDS)2Mg)。
The preparation method of the lithium sulfur electrolyte added with the Grignard reagent derivative comprises the following steps:
(1) in a glove box filled with argon, the water content in the glove box is less than 1ppm, the oxygen content value is less than 10ppm, and a proper amount of lithium-sulfur electrolyte is taken;
(2) and sealing the Grignard reagent derivative in a glove box, adding the Grignard reagent derivative into the lithium sulfur electrolyte, and uniformly mixing to prepare the lithium sulfur electrolyte containing 0.2-0.3% of the Grignard reagent derivative by volume fraction.
Preferably, the lithium sulfur electrolyte is a 1.0 mol/L solution of ethylene glycol dimethyl ether and dioxolane of LiTFSI, the volume ratio of the ethylene glycol dimethyl ether to the dioxolane is 1:1, and the Grignard reagent derivatives are hexamethyldisilazane magnesium chloride (HMDSMgCl), bis-hexamethyldisilazane magnesium ((HMDS)2Mg)。
The application of the lithium-sulfur electrolyte added with the Grignard reagent derivative in the lithium battery is characterized in that graphene and sulfur powder are mixed and ground according to the mass ratio of 4:6, wherein the graphene powder is purchased from Shandong Yuhuang New energy science and technology Limited company, the ground two materials are subjected to sulfur filling in a 160 ℃ oven for 720min to obtain a positive electrode material, the positive electrode material is uniformly mixed with acetylene black and PVDF according to the mass ratio of 7:2:1, N-methylpyrrolidone is added to be mixed into slurry, the slurry is coated on an aluminum foil, the slurry is dried in the 50 ℃ oven for 720min to obtain a positive electrode sheet, the lithium sheet is taken as a negative electrode, the lithium-sulfur electrolyte added with the Grignard reagent derivative is taken as an electrolyte, and the battery is assembled in a glove box.
Preferably, the loading amount of the high-conductivity graphene on the aluminum foil after sulfur loading is 1.01 mg/cm2The area of the lithium sheet is 2.01 cm2Lithium sulfurThe amount of the electrolyte added was 200. mu.L.
The invention has the beneficial effects that:
the invention provides a lithium sulfur electrolyte added with a trace amount of a Grignard reagent derivative, and preparation and application thereof. According to the preparation method, a small amount of Grignard reagent derivatives are added into the common lithium-sulfur electrolyte, so that the preparation method is simple to operate and low in cost, and large-scale industrial production can be realized; and trace Grignard reagent derivatives can promote the catalysis and conversion of polysulfide, have good protection effect on a lithium cathode, and have good application prospect in the aspect of lithium-sulfur electrolyte.
Drawings
In order to more simply and clearly explain the technical solution of the embodiment of the present invention, the pictures used in the embodiment are briefly described, and the following drawings are only examples of the present invention, do not limit the scope, and can obtain other information from the drawings.
FIG. 1 shows 8 mmol/L polysulfide Li2S4Solution, Grignard reagent derivatives HMDSMgCl and 8 mmol/L polysulfide Li2S4Adding 5 or 10 mu L of Grignard reagent derivative into the solution for ultraviolet-visible spectrum;
FIG. 2 is a charge and discharge curve of the lithium sulfur electrolyte prepared in example 1 and comparative example applied to a lithium sulfur battery;
FIG. 3 is a graph showing electrochemical cycle performance of lithium sulfur batteries to which the lithium sulfur electrolytes prepared in example 1 and comparative example were applied;
fig. 4 is a graph of electrochemical rate performance of the lithium sulfur electrolyte prepared in example 1 and comparative example applied to a lithium sulfur battery;
fig. 5 is an ex-situ SEM of a lithium negative electrode of the lithium sulfur battery prepared in example 1;
fig. 6 is an ex-situ SEM of a lithium sulfur battery lithium negative electrode prepared by a comparative example.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In order to make the features of the embodiments of the present invention more obvious, the technical solutions in the embodiments of the present invention are specifically described below. Instruments and reagents used in the experiment can be purchased from the market.
Example 1
A lithium sulfur electrolyte added with a Grignard reagent derivative comprises the following components: the lithium sulfur electrolyte is 1.0 mol/L LiTFSI in DOL/DME (volume ratio of 1: 1) with 0.1M LiNO3The amount of HMDSMgCl Grignard reagent derivative added was 0.25% by volume of the lithium-sulfur electrolyte.
The preparation method of the lithium sulfur electrolyte added with the Grignard reagent derivative comprises the following steps:
the method comprises the following steps: preparing a THF solution of HMDSMgCl; for details, reference is made to the Structure and compatibility of a magnesium electrolyte with a sulfate catalyst (DOI: 10.1038/ncomms 1435).
Step two: in a glove box filled with argon, the water content of the glove box is less than 1ppm, the oxygen content value is less than 10ppm, 1.0 mol/L LiTFSI in DOL of lithium-sulfur electrolyte is taken, DME =1:1 Vol% with 0.1M LiNO3 2mL；
Step three: and sealing the Grignard reagent derivative in a glove box, adding 5 mu L of HMDSMgCl into the lithium-sulfur electrolyte, and uniformly mixing to prepare the lithium-sulfur electrolyte containing 0.25% of Grignard reagent derivative by volume fraction.
Example 2
A preparation method of a lithium sulfur electrolyte added with a Grignard reagent derivative comprises the following steps:
the method comprises the following steps: in a glove box filled with argon, the water content of the glove box is less than 1ppm, the oxygen content value is less than 10ppm, 1.0 mol/L LiTFSI in DOL of lithium-sulfur electrolyte is taken, DME =1:1 Vol% with 0.1M LiNO3 2mL；
Step two: the Grignard reagent derivative was sealed in a glove box, and 5. mu.L of 97% pure (HMDS) was purchased2Mg is added into the lithium-sulfur electrolyte and mixedAnd (3) uniformly mixing to prepare the lithium-sulfur electrolyte containing 0.25 volume percent of Grignard reagent derivatives.
Comparative example
The comparative example is a common lithium sulfur electrolyte 1.0M/L LiTFSI in DOL DME =1:1 Vol% with 0.1M LiNO3The lithium-sulfur battery was produced without adding grignard reagent derivatives.
Examples of the experiments
80 mg of graphene (graphene powder YH-GP-03, D50=25 +/-3 mu m, conductivity is not less than 15000S/m, carbon content is not less than 95wt%, purchased from Shandong Yuhuang New energy science and technology Limited) and sulfur powder (Aladdin, purity is not less than 99.99%) are mixed and ground according to the mass ratio of 4:6, the mixture is baked in an oven at 160 ℃ for 720min to obtain a positive electrode material, the obtained positive electrode material is uniformly mixed with acetylene black and PVDF according to the mass ratio of 7:2:1, N-methyl pyrrolidone is added to be mixed to form slurry, the positive electrode material slurry is coated on an aluminum foil by a coating device, and the loading capacity of the high-conductivity graphene after sulfur loading is 1.01 mg/cm2And drying in a drying oven at 50 ℃ for 720min to obtain the positive plate. A lithium sheet having a diameter of 16 mm was used as a negative electrode, 200. mu.L of the lithium sulfur electrolyte containing methyl magnesium chloride in example 1 was added, and the cell was assembled in a glove box at a charge-discharge voltage of 2.8V (V vs. Li)+and/Li), the charge and discharge curve and the cycle stability of the lithium-sulfur battery are shown in fig. 2 and 3 when the charge and discharge current density is 0.5C, and the ex-situ SEM test is performed on the lithium sheet in the battery after 200 cycles of the cycle, and the electron microscope image of the lithium sheet is shown in fig. 5.
Comparative experiment example a lithium sulfur electrolyte containing no grignard reagent derivative additive was used, and the positive electrode sheet and the negative electrode sheet were the same as in experiment example 1, and the battery was assembled in a glove box, and the discharge voltage was 2.8V (vs. Li/Li +), and the charge and discharge current density was 0.5C, except that the lithium sulfur electrolyte used was a general lithium sulfur electrolyte without the grignard reagent derivative in the comparative example, the charge and discharge curve and the cycle stability of the lithium sulfur battery were as shown in fig. 2 and 3, and the ex-situ SEM test was also performed on the lithium sheet in the battery after 200 cycles of the cycle, as shown in fig. 6, which is an electron microscope image of the lithium sheet.
In order to more directly observe the catalytic effect of the grignard reagent derivative on polysulfide, the change of the peak in the uv-vis spectrum was observed by adding the grignard reagent derivative to the polysulfide solution.
FIG. 1 shows 5. mu.L of Grignard reagent derivative HMDSMgCl, 5. mu.L and 10. mu.L of Grignard reagent derivative HMDSMgCl added thereto, respectively, and no Grignard reagent derivative added thereto to 2 mL of Li having a concentration of 8 mmol/L2S4Uv-vis spectra measured in solution. Wherein Li2S4The preparation of (A) is as follows: 137.8 mg of Li are taken2The S powder and 673.26 mg of sulfur powder are added into 10 ml of DME, and the mixture is mixed and stirred for 24 hours to prepare 8 mmol/L Li2S4A solution; it can be observed that, when the grignard reagent derivative is added to the polysulfide solution, the original Li2 S4And Li2S6The peak of (a) disappears and Li appears2The peak of S shows that the addition of trace Grignard reagent derivative can catalyze the conversion of long-chain polysulfide into chain-breaking multi-retention Li2S。
Fig. 2 is a first-turn charge-discharge curve of the batteries of the experimental example and the comparative experimental example at a current density of 0.5C, and it can be seen that the experimental example has a smaller polarization voltage than the comparative experimental example, and the ratio of the second discharging platform to the first discharging platform is larger, which indicates that the shuttle effect can be well inhibited and polysulfide conversion can be promoted by adding the grignard reagent derivative.
Fig. 3 is a graph of the cycle performance of the batteries of the experimental example and the comparative experimental example at a current density of 0.5C, and it can be seen that the discharge specific capacity of the second cycle of the lithium-sulfur battery added with the grignard reagent derivative can reach 1179 mAh/g, and 76.7% of the initial specific capacity can be maintained after 100 cycles, while the discharge specific capacity of the second cycle of the lithium-sulfur battery not added with the grignard reagent derivative is 1057 mAh/g, and 39.5% of the initial specific capacity after 100 cycles, and the experimental example has good cycle stability and higher capacity compared with the comparative experimental example.
FIG. 4 is a graph of rate performance at different current densities, with experimental examples having better capacity at different rates; the experimental examples have higher capacity than the comparative experimental examples under different multiplying factors, and the experimental examples can reach the initial 0.5C capacity at the final 0.5C multiplying factor, which indicates that the experimental examples have better reversible performance.
Fig. 5 and fig. 6 are ex-situ SEM of the lithium sheet after battery cycling, and comparing the two figures, it can be clearly observed that the lithium sheet of the experimental example is flatter than the comparative experimental example, which shows that the addition of the grignard reagent derivative can well protect the lithium negative electrode, prevent the formation of lithium dendrite, and promote the catalytic conversion and have a good protection effect on the lithium negative electrode.
In summary, the invention provides a lithium sulfur electrolyte additive with catalytic conversion and lithium negative electrode protection and application thereof, the invention adopts the grignard reagent derivative as the lithium sulfur electrolyte additive, the operation is simple, the large-scale industrial production can be realized, and the trace grignard reagent derivative as the lithium sulfur electrolyte additive promotes the polysulfide conversion, has good protection effect on the lithium negative electrode and inhibits the shuttle effect, so that the lithium sulfur battery keeps good electrochemical performance, and has good application prospect in the lithium sulfur battery.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (6)
1. A lithium sulfur electrolyte to which a grignard reagent derivative is added, characterized by being obtained by the following process: adding a grignard reagent derivative into a lithium-sulfur electrolyte; the lithium-sulfur electrolyte is an organic solvent of lithium salt, the concentration of the lithium salt in the organic solvent is 0.5-2 mol/L, and the addition amount of the Grignard reagent derivative is 0.2-0.3% of the volume of the lithium-sulfur electrolyte; the lithium salt is one or more of lithium hexafluorophosphate, lithium tetrafluorophosphate, lithium nitrate, lithium trifluoromethanesulfonate, lithium bistrifluoromethanesulfonylimide, tris (trifluoromethylsulfonyl) methyllithium or lithium bisoxalateborate, the organic solvent consists of glycol dimethyl ether and dioxolane in a volume ratio of 1:1, and the Grignard reagent derivative is hexamethyldisilazane magnesium chloride (HMDSMgCl) or bis-hexamethyldisilazane magnesium ((HMDS)2Mg)。
2. The grignard reagent derivative-added lithium sulfur electrolyte according to claim 1, wherein the lithium salt is lithium bistrifluoromethanesulfonylimide.
3. The method of preparing a grignard reagent derivative-added lithium sulfur electrolyte according to claim 1 or 2, characterized by comprising the steps of:
(1) in a glove box filled with argon, the water content in the glove box is less than 1ppm, the oxygen content value is less than 10ppm, and a proper amount of lithium-sulfur electrolyte is taken;
(2) and sealing the Grignard reagent derivative in a glove box, adding the Grignard reagent derivative into the lithium sulfur electrolyte, and uniformly mixing to prepare the lithium sulfur electrolyte containing 0.2-0.3% of the Grignard reagent derivative by volume fraction.
4. The method for preparing a lithium sulfur electrolyte added with a grignard reagent derivative according to claim 3, wherein the lithium sulfur electrolyte is a 1.0 mol/L solution of ethylene glycol dimethyl ether and dioxolane of LiTFSI, and the volume ratio of the ethylene glycol dimethyl ether to the dioxolane is 1: 1.
5. The application of the lithium sulfur electrolyte added with the grignard reagent derivative in a lithium battery as claimed in claim 1 or 2 is characterized in that graphene and sulfur powder are mixed and ground according to the mass ratio of 4:6, sulfur filling is carried out, a positive electrode material is obtained, the positive electrode material, acetylene black and PVDF are uniformly mixed according to the mass ratio of 7:2:1, N-methyl pyrrolidone is added to be mixed into slurry, the slurry is coated on an aluminum foil, drying is carried out, a positive electrode sheet is prepared, a lithium sheet is taken as a negative electrode, the lithium sulfur electrolyte added with the grignard reagent derivative is taken as an electrolyte, and the battery is assembled in a glove box.
6. The use according to claim 5, wherein the loading of the positive electrode material on the aluminum foil is 1.01 mg/cm2The temperature during sulfur filling is 160 ℃, the time is 720min, and the area of the lithium sheet is 2.01 cm2The amount of the lithium-sulfur electrolyte added was 200. mu.L.
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