CN120413984B - Sodium lignin sulfonate-based polymer artificial SEI film and preparation method and application thereof - Google Patents
Sodium lignin sulfonate-based polymer artificial SEI film and preparation method and application thereofInfo
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Abstract
The invention relates to the technical field of lithium metal batteries, in particular to a sodium lignosulfonate-based polymer artificial SEI film and a preparation method and application thereof. The preparation method comprises the steps of mixing sodium lignin sulfonate with a first solvent to obtain a sodium lignin sulfonate solution, mixing silicon dioxide powder with a second solvent to obtain silicon dioxide dispersion liquid, mixing hexamethylene diisocyanate, the silicon dioxide dispersion liquid and the sodium lignin sulfonate solution, reacting under a protective atmosphere to obtain a sodium lignin sulfonate-based polymer, mixing the sodium lignin sulfonate-based polymer with a third solvent, adding polyvinylidene fluoride, mixing to obtain a precursor liquid, placing the precursor liquid on the surface of lithium metal, and drying to obtain the sodium lignin sulfonate-based polymer artificial SEI film. The artificial SEI film has good mechanical property and interface stability, and the ionic conductivity and migration number can be effectively improved.
Description
Technical Field
The invention relates to the technical field of lithium metal batteries, in particular to a sodium lignosulfonate-based polymer artificial SEI film and a preparation method and application thereof.
Background
Lithium Metal Batteries (LMB) have high energy density and theoretical specific capacity (3830, 3860 mA h g -1), but side reactions of their lithium metal negative electrodes with liquid electrolytes form natural Solid Electrolyte Interface (SEI) films. The membrane has the problems of uneven structure, poor cyclical stability, weak volume change adaptability, easiness in cracking and the like, and after cracking, the electrolyte reaction is aggravated, and local charge accumulation is initiated, so that lithium dendrites grow rapidly. Lithium dendrites not only shorten battery life, but may also penetrate the separator to raise short-circuit safety risks.
To solve the above problems, an artificial SEI film strategy has been proposed, which can improve battery stability and safety by inhibiting lithium dendrite growth. The ideal artificial SEI needs to have high ionic conductivity, strong mechanical properties, chemical stability and capability of isolating side reactions. Inorganic SEI layers (e.g., ceramics, carbon, halides) are of interest for mechanical properties and ionic conductivity, but the poor brittleness and interfacial stability result in mechanical delamination, limiting their application in lithium metal batteries. The polymer SEI layer has good flexibility and strong designability, and can adapt to interface fluctuation, but the mechanical strength is insufficient, and lithium dendrite is difficult to completely inhibit. In addition, anions are easy to gather at the electrode interface in the charge and discharge process, concentration polarization and dendrite growth are induced, and the electrochemical performance is reduced.
Therefore, the development of an artificial SEI film with excellent mechanical properties, ion conductivity and interface stability has important significance for promoting the large-scale application of lithium metal batteries.
Disclosure of Invention
In view of the above, the present invention provides an artificial SEI film of sodium lignin sulfonate based polymer, a preparation method and application thereof, which at least solves one problem existing in the prior art.
In a first aspect, the present invention provides a method for preparing an artificial SEI film of sodium lignin sulfonate based polymer, comprising the steps of:
mixing sodium lignin sulfonate with a first solvent to obtain a sodium lignin sulfonate solution;
Mixing silicon dioxide powder with a second solvent to obtain silicon dioxide dispersion liquid;
Mixing Hexamethylene Diisocyanate (HDI), the silicon dioxide dispersion liquid and the sodium lignin sulfonate solution, and reacting in a protective atmosphere to obtain a sodium lignin sulfonate-based polymer;
mixing the sodium lignin sulfonate-based polymer with a third solvent, adding polyvinylidene fluoride (PVDF), and mixing to obtain a precursor solution;
And placing the precursor solution on the surface of lithium metal, and drying to obtain the sodium lignin sulfonate-based polymer artificial SEI film.
In a second aspect, the invention provides a sodium lignosulfonate-based polymer artificial SEI film, which is obtained by the preparation method of the sodium lignosulfonate-based polymer artificial SEI film.
In a third aspect, the invention provides an application of the sodium lignosulfonate-based polymer artificial SEI film in a lithium metal battery.
In a fourth aspect, the present invention provides a lithium metal battery comprising the above sodium lignosulfonate-based polymer artificial SEI film.
By adopting the technical scheme, the embodiment of the invention has the following beneficial effects:
(1) Sodium lignin sulfonate and silicon dioxide are used as raw materials, HDI is used as a cross-linking agent, and isocyanate groups in the HDI structure are utilized to react with sodium lignin sulfonate and hydroxyl on the surface of dioxide to form a two-dimensional cross-linked network structure, so that the organic and inorganic hybrid polymer artificial SEI film with a stable cross-linked structure is prepared;
(2) Compared with a single structure of sodium lignin sulfonate, the sodium lignin sulfonate-based polymer can remarkably improve the mechanical property of an artificial SEI film, is favorable for inhibiting the growth of lithium dendrites in a lithium deposition process, can better adapt to the volume change of a lithium metal anode in a charging and discharging process, reduces SEI layer cracking caused by volume expansion, improves the safety of a polymer lithium metal battery, and can inhibit the growth of lithium dendrites due to electrostatic repulsion on the surface of a lithium metal negative electrode tip formed by a large number of negatively charged-SO 3 - groups (such as sulfonic groups) in the structure;
(3) In addition, the lithium ion can also take the-SO 3 - group as a jump anchor point of ion conduction by means of the interaction with the-SO 3 - group, and conduct fast near the uniformly distributed-SO 3 - group, thereby improving the conduction of lithium ions in an artificial SEI film;
(4) The unique structural design can solve the problem that the lithium dendrite growth is accelerated due to the concentration of the electric field in the lithium deposition process of the lithium metal negative electrode at present, and further inhibit the growth of the lithium dendrite in the battery.
Drawings
Fig. 1 is a physical image of SiO 2 @ SL prepared in example 1 of the present invention, wherein the inset is an SEI film scanning electron microscope image prepared on lithium metal.
FIG. 2 is a cross-sectional view of SiO 2 @ SL prepared in example 1 of the present invention.
FIG. 3 is a Fourier infrared spectrum of SiO 2 @ SL prepared in example 1 of the present invention.
Fig. 4 is a graph of the cyclic performance test of a SiO 2 @ SL modified lithium metal anode assembled symmetric battery prepared according to example 1 of the present invention.
FIG. 5 is a graph of the conductivity of SiO 2 @ SL prepared in example 1 and SiO 2 @ Lignin prepared in comparative example 1, and SiO 2/PVDF prepared in comparative example 2 according to the present invention.
Detailed Description
The conception and the technical effects of the present invention will be clearly and completely described below with reference to examples and drawings to fully illustrate the objects, aspects and effects of the present invention.
The artificial SEI film of the sodium lignin sulfonate-based polymer is prepared by utilizing the addition reaction of hydroxyl and isocyanate to polymerize silicon dioxide (SO 2), hexamethylene Diisocyanate (HDI) and sodium lignin sulfonate (NaSL), which unexpectedly improves the conductivity and migration number of the artificial SEI film and simultaneously endows the artificial SEI film with excellent mechanical properties and interface stability.
In a first aspect, the present invention provides a method for preparing an artificial SEI film of sodium lignin sulfonate based polymer, comprising the steps of:
mixing sodium lignin sulfonate with a first solvent to obtain a sodium lignin sulfonate solution;
Mixing silicon dioxide powder with a second solvent to obtain silicon dioxide dispersion liquid;
mixing hexamethylene diisocyanate, the silicon dioxide dispersion liquid and the sodium lignin sulfonate solution, and reacting in a protective atmosphere to obtain a sodium lignin sulfonate-based polymer;
mixing the sodium lignin sulfonate-based polymer with a third solvent, adding polyvinylidene fluoride (PVDF), and mixing to obtain a precursor solution;
And placing the precursor solution on the surface of lithium metal, and drying to obtain the sodium lignin sulfonate-based polymer artificial SEI film.
The sodium lignin sulfonate based polymer artificial SEI film has the characteristics of a film, and the thickness can be 0.1-120 micrometers. In the artificial SEI film of the sodium lignosulfonate polymer, sodium lignosulfonate, silicon dioxide and hexamethylene diisocyanate react to form a crosslinking compound, wherein the crosslinking compound has a two-dimensional crosslinking network structure, and the structural formula of the crosslinking compound can be expressed as follows:
Wherein the circle in the center of the formula represents SiO 2, n represents a positive integer, for example, n can be 30-50.
Sodium lignin sulfonate is a byproduct obtained in the industrial papermaking process, has the characteristics of low price and abundant raw materials, and takes the sodium lignin sulfonate as the raw material to prepare the high-performance artificial SEI film, thereby providing an effective way for the high-value utilization of the green sustainable chemicals. The structure of sodium lignin sulfonate is as follows:
The chemical structural formula of hexamethylene diisocyanate is as follows:
in some alternative embodiments, the first solvent is at least one of tetrahydrofuran, N-dimethylformamide, acetonitrile, methanol, and dimethylsulfoxide.
In some alternative embodiments, the second solvent is at least one of ethanol, acetonitrile, tetrahydrofuran, N-dimethylformamide, methanol, and dimethylsulfoxide.
In some alternative embodiments, the third solvent is at least one of N-methylpyrrolidone, tetrahydrofuran, N-dimethylformamide, methanol, and dimethylsulfoxide.
In some alternative embodiments, the sodium lignin sulfonate and the first solvent are mixed at 50-130 ℃ for 5-12 hours.
In some alternative embodiments, the mass ratio of sodium lignosulfonate to silica powder is 1/10-10/1, the mass ratio of silica powder to hexamethylene diisocyanate is 1/10-5/1, and the mass ratio of sodium lignosulfonate-based polymer to polyvinylidene fluoride is 1/10-5/1.
In some alternative embodiments, the protective atmosphere is an argon atmosphere.
In some alternative embodiments, the temperature of the reaction is 80-155 ℃ and the reaction time is 5-12 hours.
In some alternative embodiments, the sodium lignosulfonate-based polymer, the third solvent, and the polyvinylidene fluoride are mixed at ambient temperature for a period of 3 to 5 hours.
In some alternative embodiments, the sodium lignosulfonate-based polymer is present in the third solvent at a concentration of 0.1 percent wt to 30 percent wt percent by mass.
In a second aspect, the invention provides a sodium lignosulfonate-based polymer artificial SEI film, which is obtained by the preparation method of the sodium lignosulfonate-based polymer artificial SEI film. The sodium lignin sulfonate-based polymer artificial SEI film has greatly improved electrochemical performance, high safety and good electrochemical performance, and can provide a new method for preparing novel flame-retardant polymer electrolyte.
In a third aspect, the invention provides an application of the sodium lignosulfonate-based polymer artificial SEI film in a lithium metal battery.
In a fourth aspect, the present invention provides a lithium metal battery comprising the above sodium lignosulfonate-based polymer artificial SEI film.
Some typical examples are described below and compared with comparative examples.
Example 1
35.2 Mg sodium lignin sulfonate was dissolved in 70 mL of N, N-Dimethylformamide (DMF), dried argon was introduced and stirred in a 100℃oil bath for 8 hours to give sodium lignin sulfonate solution. The powder of 6mg SiO 2 was dispersed in 10mL DMF and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The SiO 2 dispersion and 19.8: 19.8 mg HDI were added to the sodium lignin sulfonate solution and reacted under argon atmosphere at 155 ℃ for 5 hours. After the reaction is finished, the reaction product is centrifugally separated and dried to obtain the sodium lignin sulfonate-based polymer. 10.2 mg of the sodium lignin sulfonate based polymer was dissolved in 3mL N-methylpyrrolidone (NMP) and dispersed by ultrasonic waves for 30 minutes. 15.4 mg polyvinylidene fluoride (PVDF) was added and stirred for 4 hours to give a homogeneous precursor solution. And (3) taking 25 mu L of the precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the sodium lignin sulfonate-based polymer artificial SEI film (called SO 2 @SL for short).
Fig. 1 is a physical diagram of an artificial SEI film of sodium lignin sulfonate-based polymer, wherein the inset is a SEI film scanning electron microscope image prepared on lithium metal, and the surface of the SEI film is compact and flat.
Fig. 2 is a cross-sectional view of a sodium lignosulfonate-based polymer artificial SEI film, which can be seen to have a thickness of 3 micrometers.
Fig. 3 is a fourier infrared spectrum of a sodium lignosulfonate-based polymer artificial SEI film.
Fig. 4 is a cycle performance test chart of a battery assembled by li|li symmetry mode for a sodium lignosulfonate-based polymer artificial SEI film modified lithium metal anode. It can be seen that the cycle life is longer than 1700 hours, the polarization voltage is stable, and internal short circuit caused by lithium dendrite does not occur in the cycle process.
Comparative example 1
35.2 Mg lignin was dissolved in 70 mL of N, N-Dimethylformamide (DMF), dried argon was introduced and stirred in a 100℃oil bath for 8 hours to give lignin solution. The powder of 6mg SiO 2 was dispersed in 10mL DMF and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. SiO 2 dispersion and 19.8 mg HDI were added to the lignin solution and reacted under argon atmosphere at 155℃for 5 hours. After the reaction is finished, the reaction product is centrifugally separated and dried to obtain the lignin-based polymer. 10.2 mg of the lignin-based polymer was dissolved in 3mL N-methylpyrrolidone (NMP) and dispersed by ultrasonic waves for 30 minutes. 15.4 mg PVDF was added and stirred for 4 hours to give a homogeneous precursor solution. And (3) taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form an artificial SEI film (called SiO 2 @Lignin for short).
Comparative example 2
The powder of 6mg SiO 2 was dispersed in 10mL DMF and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. 30.4 mg PVDF was added to the SiO 2 dispersion and stirred for 4 hours to give a homogeneous precursor solution. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form an artificial SEI film (SiO 2/PVDF).
FIG. 5 is a graph comparing conductivities of sodium lignosulfonate-based polymer artificial SEI films and comparative examples, wherein room temperature conductivities of SiO 2@SL、SiO2 @ Lignin and SiO 2/PVDF are 1.115×10 -3S cm-1、0.92×10-3S cm-1 and 0.303×10 -3S cm-1, respectively. The test results show that the-SO 3 - group can improve the ionic conductivity of the SEI film through the interaction with lithium ions.
Example 2
10.2 Mg sodium lignin sulfonate (NaSL) was dissolved in 100 mL THF, dried argon was introduced and stirred in a 50 ℃ oil bath for 5 hours to give a sodium lignin sulfonate solution. 102 mg SiO 2 of the powder was dispersed in 10 mL THF, and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 10.2: 10.2 mg HDI were added to a sodium lignin sulfonate solution and reacted under argon atmosphere at 80 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugally separated and dried to obtain the sodium lignin sulfonate-based polymer. 865.2 mg the sodium lignin sulfonate based polymer was dissolved in 3 mL THF and dispersed by ultrasonic wave for 30 minutes. 173 mg PVDF is added and stirred for 3 hours to obtain uniform precursor liquid. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the artificial SEI film. The artificial SEI film prepared in this example had a conductivity of 0.92×10 -3S cm-1.
Example 3
15.2 Mg sodium lignin sulfonate (NaSL) was dissolved in 70 mL acetonitrile, dried argon was introduced and stirred in a 60 ℃ oil bath for 6 hours to give a sodium lignin sulfonate solution. 30.4 mg SiO 2 of the powder was dispersed in 10 mL of acetonitrile and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 55.7: 55.7 mg HDI were added to a sodium lignin sulfonate solution and reacted under argon atmosphere at 90 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugated and dried to obtain the sodium lignin sulfonate-based polymer. 426.6 mg of the sodium lignin sulfonate based polymer was dissolved in 3 mL DMF and dispersed by ultrasonic waves for 30 minutes. 85.3 PVDF was added and stirred for 4 hours to give a homogeneous precursor solution. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the artificial SEI film.
Example 4
20.6 Mg sodium lignin sulfonate (NaSL) was dissolved in 70 mL DMSO, dried argon was introduced and stirred in a 70 ℃ oil bath for 7 hours to give a sodium lignin sulfonate solution. 61.8 mg SiO 2 of the powder was dispersed in 10 mL DMSO and dispersed by ultrasonic waves for 1 hour to give a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 61.8: 61.8 mg HDI were added to a sodium lignin sulfonate solution and reacted under argon atmosphere at 100 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugated and dried to obtain the sodium lignin sulfonate-based polymer. 15.5 mg of the sodium lignin sulfonate based polymer was dissolved in 3 mL NMP and dispersed by ultrasonic waves for 30 minutes. 21.7 mg PVDF was added and stirred for 4 hours to give a homogeneous precursor solution. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the artificial SEI film.
Example 5
25.4 Mg sodium lignin sulfonate (NaSL) was dissolved in 70 mL methanol, dried argon was introduced and stirred in an 80 ℃ oil bath for 8 hours to give a sodium lignin sulfonate solution. 50.8 mg SiO 2 of the powder was dispersed in 10mL of methanol and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 25.4: 25.4 mg HDI were added to a sodium lignin sulfonate solution and reacted under argon atmosphere at 110 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugated and dried to obtain the sodium lignin sulfonate-based polymer. 23.1 mg of the sodium lignin sulfonate based polymer was dissolved in 3mL DMSO and dispersed by ultrasonic waves for 30 minutes. 20.8 mg PVDF was added and stirred for 4 hours to obtain a uniform precursor solution. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the artificial SEI film.
Example 6
30.3 Mg sodium lignin sulfonate (NaSL) was dissolved in 70 mL DMF, dried argon was introduced and stirred in a 90 ℃ oil bath for 10 hours to give a sodium lignin sulfonate solution. 10.1 mg SiO 2 of the powder was dispersed in 10mL DMF and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 6.7: 6.7 mg HDI were added to a sodium lignin sulfonate solution and reacted under argon atmosphere at 120 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugated and dried to obtain the sodium lignin sulfonate-based polymer. 273.3 mg of the sodium lignin sulfonate based polymer was dissolved in 3.3 mL of methanol and dispersed by ultrasonic wave for 30 minutes. 79.1mg of PVDF was added and stirred for 4 hours to give a uniform precursor solution. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the artificial SEI film.
Example 7
45.5 Mg sodium lignin sulfonate (NaSL) was dissolved in 70 mL DMF, dried argon was introduced and stirred in a 110 ℃ oil bath for 8 hours to give a sodium lignin sulfonate solution. 5.4 mg SiO 2 of the powder was dispersed in 10 mL DMF and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 3 mg HDI were added to a sodium lignin sulfonate solution and reacted under an argon atmosphere at 135 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugated and dried to obtain the sodium lignin sulfonate-based polymer. 20.5 mg of the sodium lignin sulfonate based polymer was dissolved in 3mL NMP and dispersed by ultrasonic waves for 30 minutes. 10.1 mg PVDF was added and stirred for 4 hours to give a uniform precursor solution. And taking 25 mu L of precursor liquid by using a liquid transfer device, uniformly dripping the precursor liquid on the surface of lithium metal, and naturally drying at room temperature to form the artificial SEI film.
Example 8
18.2 Mg sodium lignin sulfonate (NaSL) was dissolved in 70 mL DMF, dried argon was introduced and stirred in an oil bath at 135 ℃ for 10 hours to give a sodium lignin sulfonate solution. 1.9 mg SiO 2 of the powder was dispersed in 10 mL DMF and dispersed by ultrasonic waves for 1 hour to obtain a uniform SiO 2 dispersion. The resulting SiO 2 dispersion and 1.2mg HDI were added to a sodium lignin sulfonate solution and reacted at 155 ℃ for 4 hours. After the reaction is finished, the reaction product is centrifugated and dried to obtain the sodium lignin sulfonate-based polymer. 5 mg of the sodium lignin sulfonate based polymer was dissolved in 3 mL NMP and dispersed by ultrasonic waves for 30 minutes. 15 mg PVDF is added and stirred for 5 hours to obtain uniform precursor liquid. 25 mu L of the precursor solution is taken by using a pipette and uniformly dripped on the surface of the lithium metal. Naturally drying at room temperature to form the artificial SEI film.
In conclusion, compared with the prior art, the sodium lignin sulfonate crosslinked network in the embodiment of the invention can improve the mechanical strength and chemical stability of the SEI film and inhibit the growth of lithium dendrites, a matrix with a crosslinked structure can also better adapt to the volume change of a lithium metal anode in the charge-discharge process, the SEI layer cracking caused by volume expansion is reduced, the safety of a polymer lithium metal battery is improved, a large number of negatively charged-SO 3 - groups in the structure form electrostatic repulsive force on the surface of the lithium metal negative electrode tip, the growth of lithium dendrites is inhibited, the uniform diffusion of lithium ions is realized through the interaction of-SO 3 - groups on lithium ions, and the ion conductivity and migration number of the polymer artificial SEI film are improved. In addition, the sodium lignin sulfonate polymer artificial SEI film provided by the embodiment of the invention has good mechanical property and interface stability, and the ionic conductivity and migration number can be effectively improved.
The present invention is not limited to the above embodiments, but is merely preferred embodiments of the present invention, and the present invention should be construed as being limited to the above embodiments as long as the technical effects of the present invention are achieved by the same means. Various modifications and variations are possible in the technical solution and/or in the embodiments within the scope of the invention.
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