CN114865074A - Composite solid electrolyte membrane and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a composite solid electrolyte membrane and a preparation method and application thereof, belonging to the technical field of electrochemical energy storage. The composite solid electrolyte membrane comprises an organic polymer main body, a lithium ion conductor and nano silicon nitride powder. The nano silicon nitride powder is amorphous nano silicon nitride powder, alpha crystal phase silicon nitride powder or beta crystal phase silicon nitride powder. The silicon nitride introduced by the invention can improve the interface chemistry of the lithium metal cathode, can effectively inhibit the growth condition of lithium dendrite under large current, and greatly improves the rate capability and cycle performance of the battery.
Description
Technical Field
The invention relates to the technical field of electrochemical energy storage, in particular to a composite solid electrolyte membrane and a preparation method and application thereof, and particularly relates to a composite electrolyte membrane for a lithium metal battery.
Background
Lithium ion batteries are the main sources of energy storage of current consumer electronics, electric automobiles and power grids, and the development technology obtains the Nobel chemical prize in 2019. Due to the increasing demand for high energy density, has high theoretical capacity (3860mAh g) -1 ) And a low reduction potential (-3.04V, compared to a standard hydrogen electrode) are considered to be the optimal negative electrode for next generation batteries.However, the incompatibility of highly active lithium metal with conventional liquid electrolytes tends to cause lithium dendrite formation on the surface of the negative electrode, resulting in short circuit or explosion of the battery. Solid electrolytes can effectively reduce the growth of lithium dendrites compared to liquid electrolytes and possess the inherent advantages of a wide operating temperature range and no electrolyte leakage. The intensive research project has included the research of all solid-state lithium metal batteries, of which the research of solid-state electrolytes is the key. The solid polymer electrolyte is one of solid electrolytes, and has excellent mechanical flexibility and producibility. However, commercial application of solid polymer electrolytes still faces a key challenge: battery failure due to lithium dendrite growth.
Researchers have provided a range of strategies to eliminate dendrite growth, including building three-dimensional bodies, optimizing electrolyte additives, and building artificial protective layers. Among them, conditioning or reconstructing a Solid Electrolyte (SEI) layer is a simple and effective method. The SEI component is mainly derived from the products of the reduction of the electrolyte by the lithium negative electrode during cycling. These reduction products can help to regulate lithium ion kinetics, allow lithium ions to diffuse uniformly through the SEI layer, and optimize flux distribution of lithium ions during deposition/stripping, thereby inhibiting formation of dendritic nucleation. Furthermore, dendrite growth is driven by a strong electric field around the crystal nuclei, the intensity of which corresponds to the dielectric response of the upper part of the dendrite tip. Therefore, a protective layer with a high dielectric constant can effectively shield the potential, helping to slow down the directional movement of lithium ions near the nucleation of dendrites, thereby greatly affecting the lithium deposition behavior at high current densities.
Disclosure of Invention
The composite solid electrolyte with silicon nitride as an additive is developed and designed, the silicon nitride introduced by the invention can improve the interface chemistry of the lithium metal cathode, can effectively inhibit the growth condition of lithium dendrite under large current, and greatly improves the rate capability and cycle performance of the battery; in addition, the silicon nitride introduced by the invention is an inorganic ceramic material with high thermal stability, and is beneficial to improving the flame retardant property of the solid electrolyte; thereby solving the problems of lithium dendrite growth and poor thermal stability faced by polymer electrolytes.
According to a first aspect of the present invention, there is provided a composite solid electrolyte membrane comprising an organic polymer body, a lithium ion conductor, and a nano silicon nitride powder.
Preferably, the nano silicon nitride powder is amorphous nano silicon nitride powder, alpha crystal phase silicon nitride powder or beta crystal phase silicon nitride powder.
Preferably, the mass ratio of the organic polymer main body to the lithium ion conductor to the nano silicon nitride powder is (50-80): (10-40): (1-10).
Preferably, the organic polymer body is at least one of polyethylene oxide, polyvinylidene fluoride-hexafluoropropylene copolymer, and polyacrylonitrile.
Preferably, the lithium ion conductor is at least one of lithium hexafluorophosphate, lithium difluorooxalate borate, lithium dioxalate borate, lithium bistrifluoromethylsulfonyl imide and lithium bistrifluorosulfonimide.
Preferably, the particle size of the nano silicon nitride powder is less than 200 nm.
According to another aspect of the present invention, there is provided a method for producing any one of the composite solid electrolyte membranes, comprising the steps of:
(1) dispersing an organic polymer and a lithium salt in an organic solvent, and uniformly mixing to obtain mixed slurry;
(2) adding nano silicon nitride powder into the mixed slurry obtained in the step (1);
(3) and (3) pouring the slurry obtained in the step (2) onto a mould, and drying in vacuum to obtain the composite solid electrolyte membrane.
Preferably, the mass ratio of the organic polymer to the lithium salt to the nano silicon nitride powder is (50-80): (10-40): (1-10).
Preferably, the organic polymer body is at least one of polyethylene oxide, polyvinylidene fluoride-hexafluoropropylene copolymer and polyacrylonitrile;
the lithium ion conductor is at least one of lithium hexafluorophosphate, lithium difluoro oxalate borate, lithium bis (trifluoromethyl) sulfonyl imide and lithium bis (fluoro) sulfonyl imide.
According to another aspect of the present invention, there is provided a use of any one of the composite solid electrolyte membranes for a solid electrolyte of a lithium metal battery.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
(1) the silicon nitride in the present invention, especially amorphous silicon nitride, has a sufficient number of unsaturated bonds (N) 3 ≡Si·,Si 2 N), these unsaturated bonds can grab the positive and negative charges that move on the silicon nitride surface, thereby changing the charge distribution (space charge polarization) on the silicon nitride surface. This space charge polarization helps to increase the dielectric constant of the amorphous silicon nitride. Under the condition of external connection of large current, the high dielectric constant is helpful for shielding the electric field effect, so that the uniform deposition of lithium ions on the surface of lithium metal is induced, and the growth of lithium dendrite is inhibited. Silicon nitride can also be reduced in situ by lithium metal to LiSi during cycling 2 N 3 The Li-Si-N channel formed in situ has a lower lithium ion transmission energy barrier and a faster ion transmission rate, and can effectively conduct lithium ions, so that the transmission path of the lithium ions on an SEI layer of a negative electrode is regulated. In addition, local overheating during operation of lithium batteries can cause the batteries to burn. The good heat resistance of the silicon nitride can improve the flame retardant property of the electrolyte, so that the safety and reliability of the battery operation are improved.
(2) The amorphous silicon nitride introduced by the invention can improve the interface chemistry of the lithium metal cathode, can effectively inhibit the growth condition of lithium dendrite under large current, and greatly improves the rate capability and cycle performance of the battery.
(3) The silicon nitride introduced by the invention has good heat resistance, and is beneficial to improving the flame retardant property of the solid electrolyte, so that the safety coefficient of the battery is improved.
(4) The silicon nitride introduced by the invention is economic and environment-friendly, and utilizes the requirement of commercial development.
(5) The multifunctional inorganic ceramic additive is introduced, so that the cycle life and the safety performance of the battery are improved, and the commercial application of the polymer composite electrolyte is possible.
Drawings
Fig. 1 is a graph showing the values of dielectric constants of electrolyte membranes prepared in example 1.
Fig. 2 a scanning electron microscope picture of the electrolyte membrane prepared in example 2.
Fig. 3 is the cycle capacity of the Li-Li symmetric cell of the electrolyte membrane prepared in example 2.
FIG. 4 is a graph showing the flame retardancy performance of the electrolyte membrane prepared in example 3.
Fig. 5 is a graph showing the cycle performance of the solid electrolyte membrane-matched lithium iron phosphate all-solid-state lithium metal battery prepared in example 3 at a current of 1C.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention relates to a composite solid electrolyte membrane of a multifunctional additive, which comprises an organic polymer main body, a lithium ion conductor and silicon nitride powder.
In some embodiments, the mass of the organic polymer is 50 to 80 wt% of the total mass of the solid electrolyte; the lithium ion conductor accounts for 10-40 wt% of the total mass of the solid electrolyte; the silicon nitride powder accounts for 1-10 wt% of the total mass of the solid electrolyte.
In some embodiments, the organic polymer is one or a mixture of polyethylene oxide (PEO), polyvinylidene fluoride (PVDF), polyvinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP), and Polyacrylonitrile (PAN) in any mass ratio.
In some embodiments, the lithium ion conductor is one or more of lithium hexafluorophosphate (LiPF6), lithium difluorooxalato borate (liddob), lithium dioxaoxalato borate (LiBOB), lithium bistrifluoromethylsulfonylimide (LiTFSi), lithium bistrifluorosulfonylimide (LiFSi).
In some embodiments, the inorganic ceramic powder is amorphous silicon nitride nanopowder with a particle size of less than 200 nm.
The preparation method of the composite solid electrolyte membrane comprises the following steps:
(1) dispersing organic polymer and lithium salt in the solid electrolyte membrane in an organic solvent according to a formula ratio, and stirring for 4-24h at the temperature of 30-80 ℃;
(2) adding silicon nitride into the mixed slurry obtained in the step (1) according to the formula ratio, and continuously stirring for 4-24 hours at the temperature of 30-80 ℃;
(3) pouring the mixed slurry obtained in the step (2) onto a polytetrafluoroethylene mold, and coating by adopting a scraper with a gap of 50-500 um; transferring the mould to a vacuum oven, and drying in vacuum for 8-48h at the temperature of 40-90 ℃ to obtain the composite solid electrolyte membrane.
In some embodiments, the organic solvent in step (1) is one or a mixture of two or more of acetonitrile, N-methylpyrrolidone and N, N-dimethylformamide in any mass ratio.
Example 1
A composite solid electrolyte membrane and a preparation method and application thereof are as follows:
(1) 0.5g of polyethylene oxide (PEO) and 0.3g of lithium bistrifluoromethylsulfonyl imide (LiTFSi) were weighed in a small volume flask, then 10mL of acetonitrile was added thereto, and magnetically stirred at 30 ℃ for 4 h;
(2) adding 0.05g of alpha crystal phase silicon nitride particles into the mixed slurry in the step (1), and continuously stirring for 8 h;
(3) and (3) uniformly coating the mixed slurry obtained in the last step on a polytetrafluoroethylene mould by using a scraper with a gap of 200um, transferring the mould to an oven, and performing vacuum drying at 40 ℃ for 24 hours to obtain the composite polymer electrolyte membrane.
Example 2
A composite solid electrolyte membrane and a preparation method and application thereof are as follows:
(1) weighing 0.5g of polyvinylidene fluoride-hexafluoropropylene copolymer (PVDF-HFP) and 0.2g of lithium bis (oxalato) borate (LiBOB) in a glove box, adding 10mL of N, N-Dimethylformamide (DMF), and magnetically stirring at 60 ℃ for 8 h;
(2) adding 0.2g of alpha crystal phase silicon nitride particles into the mixed slurry in the step (1), and continuously stirring for 8 h;
(3) and (3) uniformly coating the mixed slurry obtained in the last step on a polytetrafluoroethylene mould by using a scraper with a clearance of 300 mu m, transferring the mould to an oven, and performing vacuum drying at 80 ℃ for 24 hours to obtain the composite polymer electrolyte membrane.
Example 3
A composite solid electrolyte membrane and a preparation method and application thereof are as follows:
(1) weighing 0.5g of polyvinylidene fluoride (PVDF), 0.3g of lithium bistrifluoromethylsulfonylimide (LiTFSi) and 0.2g of lithium bis (oxalato) borate (LiBOB) in a glove box, adding 10mL of N, N-Dimethylformamide (DMF) therein, and magnetically stirring at 50 ℃ for 4 hours;
(2) adding 0.1g of amorphous silicon nitride particles into the mixed slurry in the step (1), and continuing stirring for 8 hours;
(3) and (3) uniformly coating the mixed slurry obtained in the last step on a polytetrafluoroethylene mould by using a scraper with a clearance of 300 mu m, transferring the mould to an oven, and performing vacuum drying at 80 ℃ for 24 hours to obtain the composite polymer electrolyte membrane.
Example 4
A composite solid electrolyte membrane and a preparation method and application thereof are as follows:
(1) 0.54g of polyvinylidene fluoride (PVDF), 0.36g of lithium bis (fluorosulfonyl) imide (LiFSI) and 0.1g of lithium difluoro (oxalato) borate (LiDFOB) were weighed in a glove box into a small-volume flask, 10mL of N-methylpyrrolidone (NMP) was then added thereto, and magnetic stirring was carried out at 60 ℃ for 8 hours;
(2) adding 0.05g of amorphous silicon nitride particles into the mixed slurry in the step (1), and continuing stirring for 8 hours;
(3) and (3) uniformly coating the mixed slurry obtained in the last step on a polytetrafluoroethylene mould by using a scraper with a clearance of 300 mu m, transferring the mould to an oven, and performing vacuum drying at 90 ℃ for 24 hours to obtain the composite polymer electrolyte membrane.
Fig. 1 is a value of dielectric constant of the electrolyte membrane prepared in example 1.
Fig. 2 is a scanning electron microscope picture of the electrolyte membrane prepared in example 2, showing a flat and dense membrane surface.
Fig. 3 is the cycle capacity of the Li-Li symmetric cell of the electrolyte membrane prepared in example 2.
The electrolyte membrane prepared in example 3 was tested for flame retardancy, and as shown in fig. 4, the electrolyte membrane self-extinguished within 2 seconds, indicating that the electrolyte membrane prepared according to the present invention has high safety.
The electrolyte membrane prepared in example 3 is used as a solid electrolyte, lithium iron phosphate (LFP) is used as a positive electrode, and lithium metal is used as a negative electrode, and the test result is shown in fig. 5, and as can be seen from fig. 5, the all-solid-state lithium metal battery can stably circulate 500 cycles at a current of 1C, the height of the cycle retention rate is 86.5%, and the coulombic efficiency is maintained at 99.7% or more.
To summarize: the excellent performance of the electrolyte membrane shown in the embodiments 1 to 3 shows that the composite electrolyte membrane of the multifunctional additive provided by the invention can be used for a lithium metal solid-state battery, and the lithium metal battery assembled by the electrolyte membrane can inhibit the growth of lithium dendrites and prolong the cycle life of the battery; in addition, the flame retardant property of the solid electrolyte is beneficial to improving the safety performance of the battery, and is convenient for practical commercial application.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A composite solid electrolyte membrane is characterized by comprising an organic polymer main body, a lithium ion conductor and nano silicon nitride powder.
2. The composite solid electrolyte membrane according to claim 1, wherein the nano silicon nitride powder is an amorphous nano silicon nitride powder, an alpha crystalline phase silicon nitride powder, or a beta crystalline phase silicon nitride powder.
3. The composite solid electrolyte membrane according to claim 1 or 2, wherein the mass ratio of the organic polymer body, the lithium ion conductor and the nano silicon nitride powder is (50-80): (10-40): (1-10).
4. The composite solid electrolyte membrane according to claim 1, wherein the organic polymer body is at least one of polyethylene oxide, polyvinylidene fluoride-hexafluoropropylene copolymer, and polyacrylonitrile.
5. The composite solid electrolyte membrane according to claim 1, wherein the lithium ion conductor is at least one of lithium hexafluorophosphate, lithium difluorooxalato borate, lithium dioxalate borate, lithium bistrifluoromethylsulfonyl imide, and lithium bistrifluorosulfonimide.
6. The composite solid electrolyte membrane according to claim 1 or 2, wherein the nano silicon nitride powder has a particle size of less than 200 nm.
7. The method for producing a composite solid electrolyte membrane according to any one of claims 1 to 6, comprising the steps of:
(1) dispersing an organic polymer and a lithium salt in an organic solvent, and uniformly mixing to obtain mixed slurry;
(2) adding nano silicon nitride powder into the mixed slurry obtained in the step (1);
(3) and (3) pouring the slurry obtained in the step (2) onto a mould, and drying in vacuum to obtain the composite solid electrolyte membrane.
8. The method for producing a composite solid electrolyte membrane according to claim 7, wherein the mass ratio of the organic polymer to the lithium salt to the nano silicon nitride powder is (50-80): (10-40): (1-10).
9. The method for producing a composite solid electrolyte membrane according to claim 7 or 8, wherein the organic polymer body is at least one of polyethylene oxide, polyvinylidene fluoride-hexafluoropropylene copolymer, and polyacrylonitrile;
the lithium ion conductor is at least one of lithium hexafluorophosphate, lithium difluoro oxalate borate, lithium bis (trifluoromethyl) sulfonyl imide and lithium bis (fluoro) sulfonyl imide.
10. Use of a composite solid electrolyte membrane according to any one of claims 1 to 6 for a solid electrolyte of a lithium metal battery.
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