CN111200163A - EC-free lithium ion battery electrolyte suitable for high nickel-silicon-carbon system - Google Patents
EC-free lithium ion battery electrolyte suitable for high nickel-silicon-carbon system Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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Abstract
The invention discloses an EC-free lithium ion battery electrolyte suitable for a high nickel-silicon-carbon system, which relates to the technical field of lithium ion batteries and comprises electrolyte lithium salt, a non-aqueous organic solvent and an additive, wherein the additive comprises a sulfur-nitrogen compound additive A with a structure shown in a formula 1 and a conventional film-forming additive, cyclic ester in the solvent system comprises Propylene Carbonate (PC) and fluoroethylene carbonate (FEC), and linear ester comprises at least one of dimethyl carbonate, diethyl carbonate (DEC) and methyl ethyl carbonate. The electrolyte provided by the invention utilizes the synergistic effect generated by the combined use of the additive A and the conventional additive, provides the electrolyte capable of effectively improving the performance of the high-nickel-silicon-carbon system lithium ion power battery, and has good electrochemical properties such as cycle performance, rate performance, storage performance and the like under high temperature and low temperature conditions, thereby solving the problem of gas generation under high voltage of the existing high-nickel-silicon-carbon system.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to an EC-free lithium ion battery electrolyte suitable for a high nickel-silicon carbon system.
Background
With the demand of new energy automobiles on high capacity and high endurance of lithium ion batteries, higher requirements are put forward on the energy density and the safety of lithium ion power batteries.
Compare chinese patent CN201510952221.3 a lithium ion battery electrolyte and a lithium ion battery with silicon carbon cathode suitable for silicon carbon cathode, its inside is described: compared with the prior art, the lithium ion battery electrolyte comprises a non-aqueous organic solvent, lithium salt and additives, wherein the additives comprise fluoroethylene carbonate, tris (trimethylsilane) borate and a sulfate compound shown in a structural formula (1) or (2).
Compared with the chinese patent CN201810629475.5, the electrolyte of a silicon-carbon system lithium ion battery and the silicon-carbon system lithium ion battery have the following internal descriptions: the electrolyte additive comprises a nitrile compound, propylene sulfite and a tetramethyldiamine compound, and the additives act together to enable the electrolyte to form a film on the surface of a cathode, reduce the oxidation of a solvent and improve the cycle performance of a high-voltage matched silicon-carbon cathode, and the electrolyte has the charging upper limit voltage of 4.5V when being applied to a lithium ion battery and has high lithium ion conductivity; the thickness expansion and the internal resistance increase are small, and the residual capacity and the restorable capacity are high; the high and low temperature discharge has higher capacity retention rate; and the safety is high, and the problem of battery flatulence cannot be well solved because the battery is not ignited or exploded in a hot box test.
To fulfill the demand for high energy density of lithium ion batteries, high nickel-silicon carbon systems are currently considered as the most promising battery systems, however, since the electrolytes matching the high nickel-silicon carbon systems in the prior art contain mostly Ethylene Carbonate (EC), on the one hand, ethylene carbonate is unstable at high voltage; on the other hand, the high nickel material usually generates oxygen evolution phenomenon under high potential, thereby accelerating the oxidative decomposition and gas generation of EC, and finally causing poor interface stability, impedance increase and battery performance reduction of the battery.
Disclosure of Invention
The invention aims to provide an EC-free lithium ion battery electrolyte suitable for a high nickel-silicon-carbon system, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: an electrolyte suitable for a high nickel-silicon carbon system EC-free lithium ion battery, which comprises electrolyte lithium salt, a non-aqueous organic solvent and an additive, wherein the additive comprises a sulfur-nitrogen compound additive A with a structure shown in a formula I and a conventional film-forming additive; wherein, the structural formula of the sulfur-nitrogen compound additive A is shown as the formula I:
wherein R represents an alkyl group, an alkynyl group, a phenyl group, an alkoxy group, a fluorine-substituted C1-C12Any one of linear or branched alkyl groups.
The sulfur-nitrogen compound additive A with the structure of the formula I is selected from one or more of the following compounds:
the additive is one or more of propenyl-1, 3-sultone (PST), triallyl phosphate (TAP), vinyl sulfate (DTD), tris (trimethylsilane) borate (TMSB) and Vinylene Carbonate (VC) in a conventional film forming mode.
The content of the sulfur-nitrogen compound additive A with the structure of the formula I accounts for 0.1-3.0% of the total mass of the electrolyte; the content of the conventional film forming additive accounts for 3.0-5.0% of the total mass of the electrolyte; the conventional film forming additive is propenyl-1, 3-sultone and triallyl phosphate, and the contents of the propenyl-1, 3-sultone and the triallyl phosphate respectively account for 0.3-0.75% and 0.1-0.3% of the total mass of the electrolyte.
The electrolyte lithium salt is selected from one or more of lithium hexafluorophosphate, lithium difluorobis (oxalato) phosphate, lithium tetrafluorooxalato phosphate, lithium difluorophosphate, lithium bis (oxalato) borate, lithium difluorooxalato borate, lithium tetrafluoroborate, lithium bis (fluorosulfonyl) imide and lithium bis (trifluoromethanesulfonyl) imide.
The content of the lithium hexafluorophosphate accounts for 12.5-15.0% of the total mass of the electrolyte, and the content of other lithium salt compounds accounts for 0.5-3.0% of the total mass of the electrolyte; the electrolyte lithium salt is lithium hexafluorophosphate, lithium difluorophosphate and lithium difluorooxalato borate, and the contents of the lithium hexafluorophosphate, the lithium difluorophosphate and the lithium difluorooxalato borate respectively account for 12.5-14.0%, 0.5-1.0% and 0.3-0.6% of the total mass of the electrolyte.
The non-aqueous organic solvent is selected from carbonate compounds, the carbonate compounds comprise cyclic carbonate and chain carbonate, the cyclic ester in the solvent system comprises Propylene Carbonate (PC) and fluoroethylene carbonate (FEC), the linear ester comprises at least one of dimethyl carbonate (DMC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC), and the content of the PC is 20.0-40.0% of the total mass of the electrolyte; the content of the FEC accounts for 7.0-12.0% of the total mass of the electrolyte; the content of the chain carbonate accounts for 35.0-70.0% of the total mass of the electrolyte; more preferably, the non-aqueous organic solvent is PC, FEC, EMC and DEC, and the PC, FEC, EMC and DEC ratio is 2.5:1:4.5: 2.
Compared with the prior art, the invention has the beneficial effects that: (1) according to the invention, the additive A is combined with a conventional film forming additive, a compact and uniform SEI film can be formed on the surface of the silicon-carbon negative electrode, and the problem of incompatibility of PC and graphite components in the silicon-carbon negative electrode is solved;
(2) in the invention, the additive A is combined with the conventional film forming additives PST and TAP to form a stable CEI film on the surface of the NCM811 anode material, so that the NCM811 anode is protected, and the oxidation of high-valence nickel and electrolyte is reduced, thereby improving the problem of gas generation in a high-nickel-silicon carbon system;
(3) the main reduction product of sulfite groups in the additive A is a sulfur-containing organic lithium salt which has excellent Li conductivity+Ability to significantly improve low temperature performance;
(4) compared with EC system electrolyte, the electrolyte solvent of the invention selects PC and FEC, and combines additives to form a film, thus relieving the problem that PC is incompatible with graphite components in the silicon-carbon cathode. Therefore, the problem that EC is easy to oxidize to generate gas is fundamentally solved, and the electrochemical performance of the battery under the conditions of high temperature and low temperature is optimized.
In conclusion, the EC-free lithium ion battery electrolyte suitable for the high-nickel-silicon-carbon system provided by the invention has the advantages that a film with excellent performance is formed on the surface of an electrode by the synergistic effect of the sulfur-nitrogen additive A and the conventional film-forming additive, the problem of incompatibility between PC and a graphite component in a silicon-carbon negative electrode is relieved, and meanwhile, the main reduction product of sulfite groups in the additive A is a sulfur-containing organic lithium salt which has excellent Li conductivity+Ability to significantly improve low temperature performance; meanwhile, the solvent system adopts PC and FEC, so that the problem that EC is easily oxidized to generate gas is avoided, the gas generation phenomenon in a high-nickel-silicon-carbon system is effectively inhibited, the problem of fast attenuation of the soft-package high-nickel-silicon-carbon battery in the prior art under the high-temperature condition is well solved, and the application range of the high-nickel-silicon-carbon high-energy density battery is effectively expanded.
Drawings
FIG. 1 is an EIS plot of NCM 811/silicon carbon cells at 25 ℃ in electrolytes containing different additives;
FIG. 2 is a bar graph of capacity retention after storage at 55 ℃ for 7 days for NCM 811/silicon carbon batteries containing different electrolyte compositions;
FIG. 3 is a bar graph of the capacity recovery of NCM 811/silicon carbon cells containing different electrolyte compositions after 7 days of storage at 55 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
referring to fig. 1 to 3, the present invention provides a technical solution: the electrolyte for the EC-free lithium ion battery in a high nickel-silicon-carbon system is prepared by the following steps: propylene Carbonate (PC), fluoroethylene carbonate (FEC), dimethyl carbonate and diethyl carbonate (DEC) were mixed in a drying room having a dew point of-50 ℃ at a ratio of 2.5:1:4.5:2, and then 13.0 wt% of lithium hexafluorophosphate (LiPF) based on the total weight of the electrolyte was slowly added to the mixed solution6) 1.0 wt% lithium difluorophosphate (LiPO) based on the total weight of the electrolyte2F2) And 0.5 wt% of PST based on the total weight of the electrolyte, and finally 0.3 wt% of compound A (see Table 1 for specific selection of compound A), 10.0 wt% of FEC and 0.3 wt% of TAP having the structure shown in formula I based on the total weight of the electrolyte are added and uniformly stirred to obtain the lithium ion battery electrolyte of example 1.
Preparing a soft package battery: stacking the prepared positive plate, the diaphragm and the negative plate in sequence, enabling the diaphragm to be positioned between the positive plate and the negative plate, and winding to obtain a bare cell; and (3) placing the bare cell in an outer package, injecting the prepared electrolyte into the dried battery, standing, forming and grading to finish the preparation of the lithium ion soft package battery (the full battery material is a high nickel system of NCM 811/silicon carbon 4.35V).
Examples 2 to 6 and comparative examples 1 to 4:
in examples 2 to 6 and comparative examples 1 to 4, the same procedure as in example 1 was repeated, except that the electrolyte composition was changed to additives shown in Table 1.
Table 1: the composition ratios of the components of the electrolytes of examples 1-6 and comparative examples 1-4
Performance testing
Performance tests were performed on the full cells obtained in examples 2 to 6 and comparative examples 1 to 3:
(1) and (3) testing the normal-temperature cycle performance: at 25 ℃, the battery after capacity grading is charged to 4.35V at constant current and constant voltage according to 1C, the current is cut off at 0.05C, then the battery is discharged to 2.7V at constant current according to 1C, and according to the circulation, the capacity retention rate of the 1000 th cycle is calculated after 1000 cycles of charge/discharge, and the calculation formula is as follows:
the 1000 th cycle capacity retention ratio (%) (1000 th cycle discharge capacity/first cycle discharge capacity) × 100%.
(2) Thickness expansion and capacity retention and recovery rate test in 55 ℃ high-temperature storage: the method comprises the steps of firstly, circularly charging and discharging a battery for 3 times (4.35V-2.7V) at normal temperature at 0.5C, recording the discharge capacity C0 before the storage of the battery, then, charging the battery to a full state of 4.35V at constant current and constant voltage, testing the thickness d1 of the battery before the high-temperature storage by using a vernier caliper, then, storing the battery in a 55 ℃ thermostat for 7 days, taking out the battery after the storage is finished, testing the thermal thickness d2 of the stored battery, and calculating the expansion rate of the thickness of the battery after the battery is stored for 7 days at the constant temperature of 55 ℃; after the battery is cooled for 24 hours at room temperature, the battery is subjected to constant current discharge at 0.5C to 2.7V again, then the battery is subjected to constant current and constant voltage charge at 0.5C to 4.35V, the discharge capacity C1 and the charge capacity C2 after the battery is stored are recorded, and the capacity residual rate and the capacity recovery rate after the battery is stored at the constant temperature of 55 ℃ for 7 days are calculated, wherein the calculation formula is as follows:
the battery thickness expansion rate after storage at 55 ℃ for 7 days is (d2-d1)/d1 x 100 percent;
the capacity residual rate after the high-temperature storage for 7 days at 55 ℃ is C1/C0 x 100 percent;
the capacity recovery rate after 7 days of high-temperature storage at 55 ℃ is C2/C0 as 100 percent.
(3) And (3) testing the low-temperature cycle performance: under the condition of low temperature of minus 10 ℃, the battery after capacity grading is charged to 4.35V at constant current and constant voltage of 0.3C, the current is cut off at 0.05C, then the battery is discharged to 2.7V at constant current of 0.5C, and according to the cycle, the cycle capacity retention rate of 50 weeks is calculated after 50 cycles of charging/discharging. The calculation formula is as follows:
the 50 th cycle capacity retention ratio (%) (50 th cycle discharge capacity/first cycle discharge capacity) × 100%.
The results of the above performance tests are shown in table 2;
table 2: lithium ion battery electrical property test result
As can be seen from a comparison of the test results of comparative example 1 and examples 1-6 in Table 2: the sulfur-nitrogen compound additive A with the structure shown in the formula I and the conventional film forming additive have synergistic effect, and meanwhile, the PC and FEC solvent system are combined to effectively inhibit gas generation in a high nickel-silicon-carbon system, so that the problem of rapid attenuation of the soft package high nickel-silicon-carbon battery in the prior art under the high-temperature condition is well solved, and the application range of the high nickel-silicon-carbon high energy density battery is effectively expanded.
Compared with the comparative example 2 which singly uses the sulfur-nitrogen compound additive A with the structure of the formula I, the comparative example 1 which does not add the additive A with the structure of the formula I, and the comparative examples 3 and 4 which respectively add PST or TAP, the electrolyte has excellent film forming performance on the surface of an electrode and improves the electrochemical performance of the electrolyte through the synergistic film forming effect of the sulfur-nitrogen compound additive A, PST, the TAP additive and the combination of FEC.
The invention mainly aims at the EC-free lithium ion battery electrolyte suitable for a high nickel-silicon carbon system, (1) the additive A in the invention is combined with a conventional film forming additive, a compact and uniform SEI film can be formed on the surface of a silicon carbon cathode, and the problem of incompatibility of PC and graphite components in the silicon carbon cathode is relieved;
(2) in the invention, the additive A is combined with the conventional film forming additives PST and TAP to form a stable CEI film on the surface of the NCM811 anode material, so that the NCM811 anode is protected, and the oxidation of high-valence nickel and electrolyte is reduced, thereby improving the problem of gas generation in a high-nickel-silicon carbon system;
(3) the main reduction product of sulfite groups in the additive A is a sulfur-containing organic lithium salt which has excellent Li conductivity+Ability to significantly improve low temperature performance;
(4) compared with EC system electrolyte, the electrolyte solvent of the invention selects PC and FEC, and combines additives to form a film, thus relieving the problem that PC is incompatible with graphite components in the silicon-carbon cathode. Therefore, the problem that EC is easy to oxidize to generate gas is fundamentally solved, and the electrochemical performance of the battery under the conditions of high temperature and low temperature is optimized.
In conclusion, the EC-free lithium ion battery electrolyte suitable for the high-nickel-silicon-carbon system provided by the invention has the advantages that a film with excellent performance is formed on the surface of an electrode by the synergistic effect of the sulfur-nitrogen additive A and the conventional film-forming additive, the problem of incompatibility between PC and a graphite component in a silicon-carbon negative electrode is relieved, and meanwhile, the main reduction product of sulfite groups in the additive A is a sulfur-containing organic lithium salt which has excellent Li conductivity+Ability to significantly improve low temperature performance; meanwhile, the solvent system adopts PC and FEC, so that the problem that EC is easily oxidized to generate gas is avoided, the gas generation phenomenon in a high-nickel-silicon-carbon system is effectively inhibited, the problem of fast attenuation of the soft-package high-nickel-silicon-carbon battery in the prior art under the high-temperature condition is well solved, and the application range of the high-nickel-silicon-carbon high-energy density battery is effectively expanded.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The EC-free lithium ion battery electrolyte suitable for the high nickel-silicon-carbon system is characterized in that: the electrolyte comprises electrolyte lithium salt, a non-aqueous organic solvent and additives, wherein the additives comprise a sulfur-nitrogen compound additive A with a structure shown in a formula I and a conventional film-forming additive; wherein, the structural formula of the sulfur-nitrogen compound additive A is shown as the formula I:
wherein R represents an alkyl group, an alkynyl group, a phenyl group, an alkoxy group, a fluorine-substituted C1-C12Any one of linear or branched alkyl groups.
2. The electrolyte applicable to the high nickel-silicon-carbon system EC-free lithium ion battery according to claim 1 is characterized in that: the sulfur-nitrogen compound additive A with the structure of the formula I is selected from one or more of the following compounds:
3. the electrolyte applicable to the high nickel-silicon-carbon system EC-free lithium ion battery according to claim 2 is characterized in that: the additive is selected from one or more of propenyl-1, 3-sultone, triallyl phosphate, vinyl sulfate, tris (trimethylsilane) borate and vinylene carbonate.
4. The electrolyte applicable to the high nickel-silicon-carbon system EC-free lithium ion battery according to claim 3 is characterized in that: the content of the sulfur-nitrogen compound additive A with the structure of the formula I accounts for 0.1-3.0% of the total mass of the electrolyte; the content of the conventional film forming additive accounts for 3.0-5.0% of the total mass of the electrolyte; the conventional film forming additive is propenyl-1, 3-sultone and triallyl phosphate, and the contents of the propenyl-1, 3-sultone and the triallyl phosphate respectively account for 0.3-0.75% and 0.1-0.3% of the total mass of the electrolyte.
5. The electrolyte applicable to the high nickel-silicon-carbon system EC-free lithium ion battery according to claim 1 is characterized in that: the electrolyte lithium salt is selected from one or more of lithium hexafluorophosphate, lithium difluorobis (oxalato) phosphate, lithium tetrafluorooxalato phosphate, lithium difluorophosphate, lithium bis (oxalato) borate, lithium difluorooxalato borate, lithium tetrafluoroborate, lithium bis (fluorosulfonyl) imide and lithium bis (trifluoromethanesulfonyl) imide.
6. The electrolyte applicable to the high nickel-silicon-carbon system EC-free lithium ion battery according to claim 5 is characterized in that: the content of the lithium hexafluorophosphate accounts for 12.5-15.0% of the total mass of the electrolyte, and the content of other lithium salt compounds accounts for 0.5-3.0% of the total mass of the electrolyte; the electrolyte lithium salt is lithium hexafluorophosphate, lithium difluorophosphate and lithium difluorooxalato borate, and the contents of the lithium hexafluorophosphate, the lithium difluorophosphate and the lithium difluorooxalato borate respectively account for 12.5-14.0%, 0.5-1.0% and 0.3-0.6% of the total mass of the electrolyte.
7. The electrolyte applicable to the high nickel-silicon-carbon system EC-free lithium ion battery according to claim 1 is characterized in that: the non-aqueous organic solvent is selected from carbonate compounds, the carbonate compounds comprise cyclic carbonate and chain carbonate, the cyclic ester in the solvent system comprises propylene carbonate and fluoroethylene carbonate, and the linear ester comprises at least one of dimethyl carbonate, diethyl carbonate and ethyl methyl carbonate; the content of the propylene carbonate accounts for 20.0-40.0% of the total mass of the electrolyte; the content of the fluoroethylene carbonate is 7.0-12.0% of the total mass of the electrolyte, the content of the chain carbonate is 35.0-70.0% of the total mass of the electrolyte, the non-aqueous organic solvent is propylene carbonate and fluoroethylene carbonate, ethyl methyl carbonate and diethyl carbonate, and the ratio of the propylene carbonate to the fluoroethylene carbonate to the ethyl methyl carbonate to the diethyl carbonate is 2.5:1:4.5: 2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112635830A (en) * | 2020-12-21 | 2021-04-09 | 惠州亿纬锂能股份有限公司 | EC-free lithium ion battery electrolyte and application thereof |
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Application publication date: 20200526 |