CN112886063B - Application of functionalized carbon dots in lithium battery electrolyte - Google Patents
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- 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 invention provides an application of functional carbon dots in lithium battery electrolyte, which comprises the step of mixing the functional carbon dots serving as additives with lithium salt electrolyte and electrolyte solvent to prepare the electrolyte; the functionalized carbon dots are N, S, P, F, B, Cl element doped carbon dots or carbon dots co-doped with more than two of the elements, and the mass concentration of the functionalized carbon dots in the electrolyte is 0.1-5.0 mg/mL. According to the invention, the multifunctional carbon dots doped with at least one element of N, S, P, F, B, Cl elements are applied to the lithium battery electrolyte as an additive, and when the battery is charged, the functionalized carbon dots are firstly anchored on the surface of a negative electrode and deposited on the surface of a current collector, so that the surface structure of the current collector is uniform, an electric field at an electrode-electrolyte interface is further uniform, the deposition behavior of lithium ions on the surface of the negative electrode is normalized, the effect of inhibiting the growth of irregular lithium dendrites is achieved, and the safety and the stability of the lithium battery are improved.
Description
Technical Field
The invention relates to the field of application of functionalized carbon dots, in particular to application of functionalized carbon dots in lithium battery electrolyte.
Background
As a novel zero-dimensional carbon material, the carbon dot shows a huge application prospect in the fields of energy storage, fluorescence anti-counterfeiting, biological imaging and the like by virtue of excellent physicochemical properties of the carbon dot. The existing carbon dot preparation methods can be divided into a bottom-up method and a top-down method. The bottom-up method is to strip or etch a large-size carbon target by chemical and physical means to form carbon dots, and the specific means is as follows: laser ablation, arc discharge, acid reflow, and the like. The principle from bottom to top means that the carbon dots are formed by forming a carbon skeleton structure by a micromolecule precursor under the conditions of high temperature, high pressure and the like, and the specific means comprises the following steps: hydrothermal method, template method, microwave method, and the like. However, the preparation method generally has the defects of high energy consumption, low yield and the like, so that the price of the existing carbon dots is high, and the large-scale application cannot be realized.
On the other hand, due to the wide application of portable electronic devices and smart grids, the demand of society for rechargeable batteries with high specific energy is increasing. Lithium batteries (e.g., lithium ion batteries and lithium metal batteries) are widely used due to their advantages of no memory effect, long cycle life, high volumetric specific energy, and the like. However, lithium dendrites inevitably grow on the negative electrode of the lithium battery during charging due to high reactivity of lithium metal and excessive charging current. The excessively long lithium dendrites pierce the separator, causing a short circuit of the battery, and further causing a serious safety accident. Therefore, the inhibition of the growth of the dendrites has important significance on the stability and safety of the lithium battery.
Therefore, the development of an economical and cheap lithium battery electrolyte with excellent performance is urgently needed in the society at present.
Disclosure of Invention
Based on the above technical problems in the prior art, the present invention provides an application of functionalized carbon dots in an electrolyte of a lithium battery, including a step of mixing the functionalized carbon dots as an additive with a lithium salt electrolyte and an electrolyte solvent to prepare an electrolyte, wherein the prepared electrolyte can effectively inhibit the growth of lithium dendrites and improve the safety and stability of the lithium battery.
In order to achieve the above purpose, the specific scheme of the invention is as follows:
the application of the functional carbon dots in the lithium battery electrolyte comprises the step of mixing the functional carbon dots serving as an additive with a lithium salt electrolyte and an electrolyte solvent to prepare the electrolyte; the functionalized carbon dots are N, S, P, F, B, Cl element doped carbon dots or carbon dots co-doped with more than two of the elements, and the mass concentration of the functionalized carbon dots in the electrolyte is 0.1-5.0 mg/mL.
In some embodiments, the functionalized carbon sites are N, S co-doped carbon sites.
In some embodiments, the functionalized carbon dots are prepared by a method comprising: preparing a uniform mixed solution of aldehyde, an acid catalyst and a functional modifier, and heating to 60-300 ℃ for hydrothermal reaction; after the reaction is finished, cooling to room temperature, and obtaining the nitrogen-sulfur functionalized carbon dots after ultrasonic dispersion, filtration, washing and drying; wherein the functional modifier is at least one of a nitrogen source, a sulfur source, a boron source, a phosphorus source, a chlorine source and a fluorine source.
In some embodiments, the ratio of the aldehyde to the functional modifier is 1 mL: (0.01-3.0) g; the ratio of the aldehyde to the acid catalyst is 1 mL: (0.5 to 30.0) g.
In some embodiments, the aldehyde is at least one of an aldehyde having a carbon number of less than or equal to 15, a dialdehyde, and a polyaldehyde; the acid catalyst includes at least one of a monobasic acid, a dibasic acid, and a tribasic acid.
In some embodiments, the aldehyde is at least one of acetaldehyde, propionaldehyde, butyraldehyde, isobutyraldehyde, valeraldehyde, isovaleraldehyde, caproaldehyde, isohexanal, heptanal, caprylic aldehyde, nonanal, decanal, undecanal, lauraldehyde, tridecanal, myristyl aldehyde, pentadecanal;
in some embodiments, the acid catalyst is at least one of hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, hydrofluoric acid, hydrobromic acid, hydroiodic acid, perchloric acid, perbromic acid, oxalic acid, boric acid, phytic acid, phthalic acid, citric acid, tartaric acid, lauric acid, salicylic acid, ascorbic acid, oleic acid, formic acid, acetic acid;
in some embodiments, the functional modifier is at least one of urea, sulfoxide chloride, thiourea, ammonium sulfate, ammonium fluoride, ammonium bifluoride, ammonium iodide, ammonium bromide, triethylamine, guanidium oleamide, sodium hypophosphite, sodium monohydrogen phosphate, sodium dihydrogen phosphate, boric acid, phenylboronic acid, sodium borohydride, sodium tetraborate decahydrate, sodium dodecyl sulfonate, potassium tetraborate, sodium fluoride, sodium chloride, sodium bromide, sodium iodide, hexadecylamine, and octadecylamine.
In some embodiments, the electrolyte solvent includes at least one of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, vinylene carbonate, fluoroethylene carbonate, difluoroethylene carbonate, methyl formate, ethyl formate, propyl formate, butyl formate, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl propionate, ethyl propionate, propyl propionate, methyl difluoroacetate, ethyl difluoroacetate, ethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, acetonitrile, malononitrile, glutaronitrile, tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, sulfolane, dimethyl sulfoxide.
In some embodiments, the lithium salt electrolyte comprises at least one of lithium bis (trifluoromethanesulfonyl) imide, lithium bis fluorosulfonylimide, lithium bis (trifluoromethanesulfonylimide), lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium hexafluoroarsenate, lithium bis (oxalato) borate, lithium trifluoromethanesulfonate.
Compared with the prior art, the invention has the following beneficial effects:
the application of the functionalized carbon dots in the lithium battery electrolyte is characterized in that the functionalized carbon dots are added into the electrolyte as an additive and mixed with a lithium salt electrolyte and an electrolyte solute to prepare the electrolyte, the electrolyte is applied to the lithium battery, and in the charging process of the battery, based on a plurality of lithium-philic functional groups contained on the surface of the functionalized carbon dots, the functionalized carbon dots are firstly anchored on the surface of a negative electrode and deposited on the surface of a current collector to uniform the surface structure of the current collector, so that the electric field at the interface of the electrode and the electrolyte is uniform, the deposition behavior of lithium ions on the surface of the negative electrode is normalized, the growth of irregular lithium dendrites is inhibited, and the safety and the stability of the lithium battery are improved.
The invention applies the functionalized carbon dots to the lithium battery electrolyte, and the lithium battery comprising the lithium battery electrolyte not only shows excellent electrochemical performance, but also has good cycle stability.
Drawings
FIG. 1 is a schematic diagram of the mechanism of the functionalized carbon dot formation process of example 1;
FIG. 2 is a digital picture of the functionalized carbon dot powder of example 1;
FIG. 3 is a TEM image of the functionalized carbon dot powder of example 1;
FIG. 4 is an infrared spectrum of the functionalized carbon dot powder of example 1;
FIG. 5 is a schematic illustration of comparative example 1, example 1 electrolyte additive deposition on a lithium negative electrode;
FIG. 6 is a scanning electron micrograph of the deposition morphology of lithium metal on a copper foil after a first cycle of comparative example 1;
FIG. 7 is a scanning electron micrograph of the deposition morphology of lithium metal of example 1 after a first cycle on the copper foil;
FIG. 8 shows the results of the Li/Cu half-cells of comparative example 1 and example 1 at 1.0mA cm-2Coulombic efficiency curves at current density;
FIG. 9 shows the results of the comparative example 1 and the Li/Li symmetrical battery of example 1 at 1.0mA cm-2Time-voltage curve at current density.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1 preparation of nitrogen and sulfur co-doped functionalized carbon dots
4.0g of thiourea and 40mL of acetaldehyde (35 wt%) were weighed into a beaker, sonicated for 1h to completely dissolve the thiourea, and 200. mu.L of concentrated sulfuric acid was added as a catalyst. The mixture was transferred to a 100mL hydrothermal reaction kettle and heated at 180 ℃ for 6 h. After the reaction was completed, the reaction mixture was naturally cooled to room temperature, and the resulting brown viscous substance was transferred to 2L of deionized water, and continuously sonicated until the product was uniformly dispersed. The filter cake (i.e., carbon dots) was collected by filtration through a microporous membrane (pore size 0.22 μm), and the carbon dots were washed with deionized water several times to remove impurities. And drying the mixture in an oven at 60 ℃ for 12 hours, and collecting nitrogen and sulfur co-doped functionalized carbon dot powder.
In this example, the process of forming the functionalized carbon dots is shown in fig. 1, and the appearance of the functionalized carbon dots is shown in fig. 2, as shown in fig. 2, the method of the present invention has high yield, and the prepared carbon dot powder has uniform texture.
The prepared functionalized carbon dots are subjected to TEM test by a transmission electron microscope, and the test result is shown in FIG. 3, as shown in FIG. 3, the microstructure of the functionalized carbon dots prepared in the embodiment is spherical, the average particle size is about 2.5nm, and the functionalized carbon dots are uniformly dispersed and have no obvious agglomeration.
The infrared spectrum detection is carried out on the prepared functionalized carbon dots, the test result is shown in figure 4, and the surface of the prepared functionalized carbon dots contains hydroxyl, amino, carbonyl and sulfenyl groups as shown in figure 4.
EXAMPLE 2 preparation of electrolyte
S1, mixing an organic solvent 1, 3-Dioxolane (DOL)/ethylene glycol dimethyl ether (DME) according to a volume ratio of 1:1 in an inert atmosphere to prepare an electrolyte solvent;
s2, dissolving the functionalized carbon dot powder prepared in example 1 and lithium salt lithium bistrifluoromethylsulfonyl imide (LiTFSI) in the solvent prepared in the step S1 under inert atmosphere, and adding 2 wt% LiNO3Stirring uniformly to prepare electrolyte; wherein the concentration of the LiTFSI is 1.0mol/L, and the concentration of the functionalized carbon dots is 0.3 mg/mL.
And (3) electrochemical performance testing:
(1) and (3) respectively dropwise adding 40 mu L of the prepared electrolyte on two sides of the PE diaphragm by taking a metal lithium sheet as a negative electrode and a copper foil as a positive electrode, and assembling the Li/Cu half cell. At a current density of 1mA cm-2The discharge capacity was 1mA cm-2The coulombic efficiency of the Li/Cu half-cell in the electrolyte is tested under the charge-discharge mechanism. The current density is 0.5mA cm-2The deposition capacity was 5.0mA cm-2Depositing the Li/Cu half-cell after the first circle under the condition of (1), disassembling, and observing the deposition shape of the metal lithium on the copper foil by using a scanning electron microscopeAnd (5) appearance.
(2) And (3) respectively dripping 40 mu L of the prepared electrolyte on two sides of the PE diaphragm by taking a metal lithium sheet as a negative electrode and a metal lithium sheet as a positive electrode, and assembling the Li/Li symmetrical battery. At a current density of 1.0mA cm-2The discharge capacity was 1.0mA cm-2The long cycle stability of lithium metal in the electrolyte was tested under the charge-discharge mechanism of (1).
Comparative example 1 preparation of electrolyte
S1, mixing organic solvents DOL and DME according to the volume ratio of 1:1 under an inert atmosphere;
s2, dissolving lithium salt LiTFSI in the solvent under inert atmosphere to enable the concentration of the lithium salt LiTFSI to be 1.0mol/L, and adding 2 wt% LiNO3And stirring uniformly to prepare a blank electrolyte.
And (3) electrochemical performance testing:
(1) a metal lithium sheet is taken as a negative electrode, a copper foil is taken as a positive electrode, 40 mu L of the blank electrolyte is respectively dripped on two sides of a PE diaphragm, and a Li/Cu half cell is assembled with a current density of 1mAcm-2And discharge capacity of 1mAcm-2The coulombic efficiency of the Li/Cu half-cell in the blank electrolyte is tested under the charge-discharge mechanism. The current density is 0.5mAcm-2The deposition capacity was 5.0mAcm-2The Li/Cu half-cell after the first cycle of deposition is disassembled, and the deposition morphology of the metal lithium on the copper foil is observed by utilizing a scanning electron microscope after the disassembly.
(2) And (3) respectively dripping 40 mu L of the blank electrolyte on two sides of the PE diaphragm by taking a metal lithium sheet as a negative electrode and a metal lithium sheet as a positive electrode, and assembling the Li/Li symmetrical battery. At a current density of 1.0mAcm-2The discharge capacity was 1.0mAcm-2The long cycle stability of lithium metal in the blank electrolyte was tested under the charge-discharge mechanism of (1).
The test results of example 2 and comparative example 1 are shown in fig. 5-9.
It can be seen from fig. 5 that, since the surface of the current collector is not uniform, the electric field distribution at the electrode-electrolyte interface is not uniform, and lithium ions are unevenly deposited in the deposition stage, so that irregular dendrites grow out, but based on numerous lithium-philic functional groups contained on the surface of the functionalized carbon dots, the functionalized carbon dots can be anchored on the surface of the negative electrode in the charging process of the lithium battery, and the electric field at the electrode-electrolyte interface is uniform, so that the deposition behavior of the lithium ions on the surface of the negative electrode is normalized, and the growth of the irregular lithium dendrites is inhibited.
As can be seen from FIG. 6, at a current density of 0.5mA cm-2The deposition capacity was 5.0mAh cm-2In comparative example 1, lithium ions are not uniformly deposited on the surface of the copper foil, and obvious dendritic crystal growth occurs.
As can be seen from FIG. 7, at a current density of 0.5mA cm-2The deposition capacity was 5.0mAh cm-2In example 1, lithium ions are uniformly and densely deposited on the surface of the copper foil without obvious dendritic growth.
As can be seen from FIG. 8, at a current density of 1.0mAcm-2The discharge capacity was 1.0mAcm-2The average coulomb efficiency of the first 120 cycles of the Li/Cu half-cell under the charging and discharging mechanism is 98.08 percent. Better cycling stability was shown compared to comparative example 1.
As can be seen from FIG. 9, at a current density of 1.0mAcm-2The discharge capacity was 1.0mAcm-2Under the charge and discharge mechanism, the Li/Li symmetrical battery stably circulates for 600 circles without soft short circuit. Better cycling stability was shown compared to comparative example 1.
It should be noted that, in addition to the nitrogen and sulfur co-doped carbon dots in the examples, other carbon dots doped with one of the N, S, P, F, B, Cl elements or co-doped with two or more of the N, S, P, F, B, Cl elements, functionalized carbon dots having lithium-philic functional groups, have the same effects, which are not listed here.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. The lithium battery electrolyte is characterized by comprising a doped carbon dot, a lithium salt electrolyte and an electrolyte solvent, wherein the doped carbon dot is an N, S co-doped carbon dot, and the mass concentration of the doped carbon dot in the electrolyte is 0.3 mg/mL.
2. The lithium battery electrolyte as claimed in claim 1, wherein the doped carbon dots are prepared by a method comprising: preparing a uniformly mixed solution of aldehyde, an acid catalyst and a functional modifier, and heating to 60-300 ℃ for hydrothermal reaction; after the reaction is finished, cooling to room temperature, and obtaining nitrogen-sulfur doped carbon dots after ultrasonic dispersion, filtration, washing and drying; wherein the functional modifier is a nitrogen source and a sulfur source.
3. The lithium battery electrolyte of claim 2 wherein the aldehyde and the functional modifier are present in a ratio of 1 mL: (0.01-3.0) g; the ratio of the aldehyde to the acid catalyst is 1 mL: (0.5 to 30.0) g.
4. The lithium battery electrolyte as claimed in claim 2, wherein the aldehyde is at least one of an aldehyde having 15 or less carbon atoms, a dialdehyde, and a polyaldehyde; the acid catalyst includes at least one of a monobasic acid, a dibasic acid, and a tribasic acid.
5. The lithium battery electrolyte as claimed in claim 2, wherein the aldehyde is at least one of acetaldehyde, propionaldehyde, butyraldehyde, isobutyraldehyde, valeraldehyde, isovaleraldehyde, caproaldehyde, isohexanal, heptaldehyde, caprylic aldehyde, nonanal, capric aldehyde, undecyl aldehyde, lauric aldehyde, tridecylaldehyde, myristyl aldehyde, and pentadecylaldehyde; and/or the acid catalyst is at least one of hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, hydrofluoric acid, hydrobromic acid, hydroiodic acid, perchloric acid, perbromic acid, oxalic acid, boric acid, phytic acid, phthalic acid, citric acid, tartaric acid, lauric acid, salicylic acid, ascorbic acid, oleic acid, formic acid, acetic acid; and/or the functional modifier is at least one of urea, thionyl chloride, thiourea, ammonium sulfate, ammonium fluoride, ammonium bifluoride, ammonium iodide, ammonium bromide, triethylamine, guanidine oleylamine hydrochloride, sodium hypophosphite, sodium monohydrogen phosphate, sodium dihydrogen phosphate, boric acid, phenylboronic acid, sodium borohydride, sodium tetraborate decahydrate, sodium dodecyl sulfonate, potassium tetraborate, sodium fluoride, sodium chloride, sodium bromide, sodium iodide, hexadecylamine and octadecylamine.
6. The lithium battery electrolyte of claim 1, wherein the electrolyte solvent comprises at least one of ethylene carbonate, propylene carbonate, dimethyl carbonate, diethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, vinylene carbonate, fluoroethylene carbonate, difluoroethylene carbonate, methyl formate, ethyl formate, propyl formate, butyl formate, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl propionate, ethyl propionate, propyl propionate, methyl difluoroacetate, ethyl difluoroacetate, ethylene glycol dimethyl ether, triethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, acetonitrile, malononitrile, glutaronitrile, tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, sulfolane, dimethyl sulfoxide.
7. The lithium battery electrolyte of claim 1 wherein the lithium salt electrolyte comprises at least one of lithium bis (trifluoromethanesulfonyl) imide, lithium bis (fluorosulfonyl) imide, lithium bis (trifluoromethanesulfonyl) imide, lithium hexafluorophosphate, lithium perchlorate, lithium tetrafluoroborate, lithium hexafluoroarsenate, lithium bis (oxalato) borate, lithium trifluoromethanesulfonate.
8. A lithium ion battery comprising the lithium battery electrolyte of any one of claims 1-7.
9. A lithium metal battery comprising the lithium battery electrolyte of any one of claims 1 to 7.
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| CN114430062B (en) * | 2022-01-24 | 2023-10-10 | 中南大学 | Composite electrolyte based on lithiated carbon point modification and preparation method and application thereof |
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