CN115732756B - Electrolyte and secondary battery using same - Google Patents

Electrolyte and secondary battery using same Download PDF

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CN115732756B
CN115732756B CN202111017997.8A CN202111017997A CN115732756B CN 115732756 B CN115732756 B CN 115732756B CN 202111017997 A CN202111017997 A CN 202111017997A CN 115732756 B CN115732756 B CN 115732756B
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electrolyte
compounds
lithium
imide
fluorosulfonyl
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CN115732756A (en
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陈黎
刘春彦
王志涛
王婷婷
甘朝伦
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Zhangjiagang Guotai Huarong New Chemical Materials Co Ltd
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Zhangjiagang Guotai Huarong New Chemical Materials Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The present invention relates to an electrolyte and a secondary battery including the same. In order to solve the problem that the existing electrolyte cannot simultaneously give consideration to the high-low temperature cycle performance, the quick charge performance and the service life of a lithium secondary battery and effectively inhibit the impedance growth of the battery under different charge states, the electrolyte comprises 2.0-10.0% of lithium bis (fluorosulfonyl) imide and the total mass of the electrolyteThe carboxylate derivatives shown, R1 and R2 are independently C 1 ‑C 6 Alkyl orWherein G is 1 Is a bond, C 1 ‑C 5 Alkylene or a heteroatom-containing substituent, G 2 Is C 1 ‑C 5 Alkyl or a heteroatom-containing substituent, and G 1 、G 2 At least one of R1 and R2 is a heteroatom-containing substituent

Description

Electrolyte and secondary battery using same
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to an electrolyte and a secondary battery containing the same.
Background
With the increasing emphasis of energy crisis, new energy automobiles in the newly developed strategic industry bring greater opportunity for the development of lithium ion batteries. The electrolyte is an important component in the lithium ion battery, plays a role in conducting electrons between the anode and the cathode of the lithium ion battery, and can be composed of a solvent, lithium salt and an additive.
In order to improve the comprehensive performance of the lithium ion battery, a method for screening electrolyte lithium salt and additives is commonly used at present. CN112736278A is used for reasonably designing the area size of the positive electrode lug to ensure that the concentration C of lithium bis (fluorosulfonyl) imide in the electrolyte LiFSI Area S with positive tab Positive tab The proportion is controlled at [0.1,40 ]]In the interval range of (2), the corrosion of aluminum foil is avoided or reduced under the condition that LiFSI is contained in the electrolyte, even the aluminum foil corrosion phenomenon is not seen more than 2000 times of cyclic charge and discharge, the production cost is reduced, and meanwhile, the dynamic performance and the low-temperature performance of the battery are improved. CN112259790a discloses a dianion high concentration electrolyte comprising bis-fluorosulfonyl imide (FSI - ) And bis (trifluoromethanesulfonyl) imide (TFSI - ). Further, the electrolyte of the patent comprises a low-viscosity organic solvent, lithium salt, and ion plastic crystal and/or ionic liquid as flame retardant, and FSI is provided in the electrolyte of the patent - And TFSI - Anions can effectively inhibit corrosion of aluminum foil of positive current collector and formation of lithium dendrite, and FSI - And TFSI - The dianion can act on the positive electrode and the negative electrode cooperatively, so that the cycle performance of the battery is effectively improved.
Although the performance of the lithium ion battery is improved to a certain extent by the method, the method has certain limitation, and the impedance growth of the battery under different charge states can not be effectively restrained while the high-low temperature cycle performance, the quick charge performance and the service life of the lithium secondary battery are simultaneously considered.
Disclosure of Invention
The invention aims to provide an electrolyte capable of improving the cycle life and the quick charge performance of a lithium ion battery at high and low temperatures and inhibiting the increase of internal resistance of the battery under different charge states, and a secondary battery containing the electrolyte.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the invention provides an electrolyte, comprising a lithium salt, an organic solvent and an additive, wherein the lithium salt comprises lithium bis (fluorosulfonyl) imide, and the lithium bis (fluorosulfonyl) imide accounts for 2.0-10.0% of the total mass of the electrolyte;
the additive comprises a carboxylic ester derivative, wherein the carboxylic ester derivative is one or more of compounds shown as a structural formula (I), and the structural formula (I) is
R1 and R2 are independently C 1 -C 6 Alkyl orWherein G is 1 Is a bond, C 1 -C 5 Alkylene or a heteroatom-containing substituent, G 2 Is C 1 -C 5 Alkyl or a heteroatom-containing substituent, and G 1 、G 2 At least one of R1 and R2 is a heteroatom-containing substituent>
The bond means G 1 Is a single bond between two carbon atoms, not an atom, i.e. when G1 is a bond,is->
Preferably, the heteroatom-containing substituent has the formula-R 3 OR 4 ，-OR 4 ，-R 3 SR 4 ，-SR 4 ，-S i R 4 R 5 R 6 or-R 3 S i R 4 R 5 R 6 Wherein R is 3 Is C 1 -C 5 Alkylene group, R 4 、R 5 、R 6 Independently C 1 -C 5 An alkyl group.
Further preferably, said R 3 Is C 1 -C 3 Alkylene group, R 4 、R 5 、R 6 Independently C 1 -C 3 An alkyl group.
Further preferably, one of R1 and R2 is C 1 -C 6 Straight chain alkyl, the other isThe G is 1 、G 2 One of which is a heteroatom-containing substituent.
According to some specific and preferred embodiments, the carboxylate derivatives are selected from one or more of the following structural formulae:
preferably, the carboxylate derivative accounts for 0.01% -5.0% of the total mass of the electrolyte.
Further preferably, the carboxylate derivative accounts for 0.1% -2% of the total mass of the electrolyte.
Preferably, the mass ratio of the carboxylic ester derivative to the lithium bis (fluorosulfonyl) imide is 1:2.5-10.
Further preferably, the mass ratio of the carboxylic acid ester derivative to the lithium bis (fluorosulfonyl) imide is 1:2.8-9.8.
The lithium salt also comprises other lithium salts, and the other lithium salts are LiPF 6 、LiBF 4 、LiAsF 6 、LiClO 4 、LiCF 3 SO 3 、 LiC 4 F 9 SO 3 、Li(CF 3 SO 2 ) 2 N、Li(CF 3 SO 2 ) 3 C、Li(C 6 F 5 ) 4 B、Li(C 2 F 5 SO 2 ) 2 N、LiBF 3 C 2 F 5 、LiPF 3 (C2F 5 ) 3 One or more of the following.
According to a specific and preferred embodiment, the other lithium salt is LiPF 6 。
Preferably, the other lithium salt accounts for 5-25% of the total mass of the electrolyte.
Further preferably, the other lithium salt accounts for 6% -20% of the total mass of the electrolyte.
Still more preferably, the other lithium salt accounts for 10% -20% of the total mass of the electrolyte.
Preferably, the mass ratio of the lithium bis (fluorosulfonyl imide) to the other lithium salts is 1:0.5-8.
Further preferably, the mass ratio of the lithium bis (fluorosulfonyl imide) to the other lithium salt is 1:0.8-5.
Preferably, the electrolyte further comprises other additives, wherein the other additives are one or more of cyclic carbonates, sulfonates, sultones, sulfates, sulfites, benzene-containing compounds, halogenated compounds, nitrile compounds, boron-containing compounds, cyclic ether compounds, phosphazene compounds, phosphates, phosphites, amine compounds, isocyanate compounds, silicon-containing compounds, lithium salt-type compounds and fluoroether compounds containing double bonds.
Further preferred, such other additives include, but are not limited to, vinylene carbonate, ethylene carbonate, fluoroethylene carbonate, methylene methane disulfonate, ethylene sulfate, ethylene sulfite, 1, 3-propane sultone, 1, 3-dioxane, biphenyl, cyclohexylbenzene, t-butylbenzene, t-pentylbenzene, m-fluorotoluene, 3, 4-difluorotoluene, 4-bromo-2-fluoroanisole, p-fluorotoluene, p-xylene, 1, 2-dimethoxy-4-nitrobenzene, N-phenylmaleimide, pentafluoroanisole, 2, 5-di-t-butyl, 1, 4-dimethoxybenzene, adiponitrile, hexanetrinitrile, succinonitrile, N-butylamine, alkanolamine, ethanolamine, N-dicyclohexylcarbodiimide, N-diethyltrimethylsilane, hexamethyldisilazane, hexaethyldisilazane, hexapropyldisilazane, triphenyl phosphate, adiponitrile, pimelic nitrile, ethoxypentafluoro-phosphazene, lithium difluoroborate, lithium bis (3, 3-trifluoromethylphosphite), lithium bis (3, 3-tetrafluoro) 2, 3-bis (1, 3-tetrafluoro) 3-diphosphonitrile, 1, 3-bis (3-tetrafluoro) silane, 3-tetrafluoro (1, 3-tetrafluoro) phosphate, 3-bis (3-propyl) phosphate, or a plurality of such as these additives.
Still further preferably, the other additive is fluoroethylene carbonate and/or ethylene sulfate.
According to some embodiments, the other additive is a combination of fluoroethylene carbonate and ethylene sulfate in a mass ratio of 6-10:1.
Preferably, the other additives account for 0.5% -15% of the total mass of the electrolyte.
Further preferably, the other additives account for 1.0% -10% of the total mass of the electrolyte.
Still more preferably, the other additive accounts for 3.0% -6.0% of the total mass of the electrolyte.
Preferably, the organic solvent is one or more of carbonic ester, carboxylic ester, ether and sulfone.
Further preferably, the carbonate comprises a fluorocarbonate.
Further preferably, the carboxylic acid ester comprises a fluorinated carboxylic acid ester.
Further preferably, the ether comprises a fluoroether.
Further preferably, the sulfone comprises one or more of sulfoxide, fluoro sulfone and fluoro sulfoxide.
Still more preferably, the organic solvent is two or more of dimethyl carbonate, diethyl carbonate, ethylene carbonate, propylene carbonate, methyl ethyl carbonate, ethylene glycol dimethyl ether, r-butyrolactone, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl propionate, propyl propionate, butyl propionate, methyl butyrate, ethyl butyrate, sulfolane, methyl ethyl sulfone, dimethyl sulfoxide, fluoroethylene carbonate, difluoroethylene carbonate, trifluoroethyl carbonate, fluoroethyl sulfone, tetrafluoroethyl tetrafluoropropyl ether.
According to some embodiments, the organic solvent is a mixture of ethylene carbonate, diethyl carbonate, and methylethyl carbonate.
More specifically, the mass ratio of the ethylene carbonate to the diethyl carbonate to the methyl ethyl carbonate is (0.8-2) 1 (2-5).
Preferably, the organic solvent accounts for 50% -85% of the total electrolyte.
Further preferably, the organic solvent accounts for 70% -85% of the total electrolyte.
The second aspect of the invention also provides a lithium ion battery, which comprises the electrolyte.
Specifically, the lithium ion battery comprises a shell, a battery core and the electrolyte, wherein the battery core and the electrolyte are contained in the shell.
More specifically, the battery cell comprises a positive electrode, a negative electrode and a separator between the positive electrode and the negative electrode.
More specifically, the positive electrode comprises a positive electrode current collector and a positive electrode material positioned on the surface of the positive electrode current collector, wherein the positive electrode material comprises a positive electrode active substance, a positive electrode conductive agent and a positive electrode binder, and the positive electrode active substance can be LiCoO 2 、 LiNi 0.5 Mn 1.5 O 4 、LiNiPO 4 、LiCoPO 4 、Li 3 V 2 (PO 4 ) 3 、LiNi 1-y-z Co y Mn z O 2 、LiNi 1-y-z Co y Al z O 2 Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0, z is more than or equal to 0, and y+z is more than or equal to 1.
According to some embodiments, the positive electrode active material is LiCoO 2 (LCO)/LiNi 0.8 Co 0.1 Mn 0.1 O 2 (NCM811)。
According to some embodiments, the positive electrode conductive agent is acetylene black or carbon nanotubes, and the positive electrode binder is polyvinylidene fluoride.
Specifically, the negative electrode comprises a negative electrode current collector and a negative electrode material positioned on the surface of the negative electrode current collector, wherein the negative electrode material comprises a negative electrode active substance and a negative electrode binder, and the negative electrode material can also optionally comprise a negative electrode conductive agent.
More specifically, the negative electrode conductive agent and the positive electrode conductive agent may be the same or different, and are all conductive agents commonly used in the art.
More specifically, the negative electrode active material and the negative electrode binder may be negative electrode active materials and negative electrode binders conventionally used in the art, and for example, the negative electrode active materials may be lithium metal, metal oxides, lithium aluminum alloys, graphite, modified carbon materials, silicon oxides, and silicon carbon.
According to some embodiments, the negative electrode active material is graphite.
Specifically, the separator layer is a separator layer conventionally used in the art.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the invention, the carboxylic ester derivative additive with the structural formula (I) and the lithium bis (fluorosulfonyl) imide accounting for 2.0-10.0% of the total mass of the electrolyte are added into the electrolyte through researches, so that the cycle life and the quick charge performance of the lithium ion battery at high and low temperatures can be improved, the internal resistance of the battery at different charge states is inhibited from increasing, the components and the proportion of the electrolyte are further optimized, and the normal-temperature and high-temperature cycle performance, the quick charge performance and the cycle performance of the lithium secondary battery at different charge states are further improved. The electrolyte and the secondary battery have wide commercial prospect.
Detailed Description
The invention is further described below with reference to examples. The present invention is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions which are not noted are conventional conditions in the industry. The technical features of the various embodiments of the present invention may be combined with each other as long as they do not collide with each other.
The existing lithium battery electrolyte additive can improve the performance of a lithium ion battery to a certain extent, but has certain limitation, and can not effectively inhibit the impedance growth of the battery under different charge states while simultaneously considering the high-low temperature cycle performance, the quick charge performance and the service life of the lithium secondary battery. According to the electrolyte containing the electrolyte salt of LiFSI with higher concentration, on one hand, the positive and negative electrode film forming characteristics of the carboxylic ester derivative are improved by the LiFSI with higher concentration, the lithium ion migration rate in the charge and discharge process is improved, on the other hand, the positive electrode current collector corrosion and negative electrode lithium dendrite formation caused by LiSSI are inhibited by the carboxylic ester derivative, the cycle life of the lithium ion battery at high and low temperatures is improved by the synergistic use of the two compounds, the quick charge performance of the lithium battery is improved, the impedance growth of the lithium battery in different charge states is inhibited, and the cycle performance in different charge states is improved.
Preparation of electrolyte:
embodiments of the invention battery electrolytes were formulated in a glove box according to the formulations described in table 1. Wherein the substances mentioned in the table are named Ethylene Carbonate (EC), diethyl carbonate (DEC), ethylmethyl carbonate (EMC), fluoroethylene carbonate (FEC), and ethylene sulfate (DTD)
TABLE 1
The additives referred to in table 1 are as follows:
preparation of the battery:
the electrolytes obtained in comparative examples 1 to 18 and examples 1 to 13 were injected into the same batch of positive electrode LiNi 0.8 Co 0.1 Mn 0.1 O 2 (NCM 811) in a 1Ah polymer pouch cell having a negative electrode of a silicon oxide material (silicon content: 12%), the capacity retention (pre-cycle capacity/post-cycle capacity) of the cell after 500 weeks of a 1C charge-discharge cycle at 25℃and 60℃at a voltage of 4.2V was tested, as shown in Table 2; the test cells were charged at normal temperature 5C for 4.2V and then discharged at 0.2C to a capacity of 2.75V, see table 3; the internal resistance values of the cells at 50% SOC (battery charge retention) and 20% SOC (battery charge retention) were tested and are shown in Table 4
Experimental results:
TABLE 2
TABLE 3 Table 3
As can be seen from tables 2 and 3, when lithium bis (fluorosulfonyl) imide accounting for 2.0% -10.0% of the total mass of the electrolyte is contained under the conditions of low temperature and high temperature, the carboxylate derivatives shown by S1-S7 are added into the electrolyte, and the capacity retention rate after 25 ℃/500 weeks, the capacity retention rate after 60 ℃/500 weeks and the 0.2C discharge capacity after 5C charge are all improved, so that the cycle performance is better under the high and low temperature state. Wherein the capacity retention rate is as high as 80.25% after 25 ℃/500 weeks, 62.87% after 60 ℃/500 weeks, and 0.2C discharge capacity is as high as 0.658Ah after normal temperature 5C charging in example 1.
TABLE 4 Table 4
/>
As can be seen from table 4, when lithium bisfluorosulfonyl imide was contained in an amount of 2.0% to 10.0% by weight based on the total mass of the electrolyte, the carboxylic acid ester derivatives shown in S1 to S7 were added to the electrolyte, and the internal resistance value of 50% soc (battery charge retention rate) and the internal resistance value of 20% soc (battery charge retention rate) were both greatly reduced as compared with the comparative examples, and the cycle performance was greatly lowered. Wherein the internal resistance values of 50% SOC (battery charge retention) and 20%% SOC (battery charge retention) in example 1 were as low as 16.24mΩ and 40.09mΩ, respectively.
As can be seen from the combination of tables 2 to 4, the battery performance of the examples of the present invention is superior to that of the batteries prepared in the comparative examples. The carboxylate derivative additive shown in S1-S7 and the lithium bis (fluorosulfonyl) imide accounting for 2.0-10.0% of the total mass of the electrolyte are synergistic, so that the cycle life of the lithium ion battery at high and low temperatures can be improved, the quick charge performance of the lithium battery is improved, the impedance growth of the lithium battery in different charge states is inhibited, the cycle performance in different charge states is improved, and the prepared battery has excellent comprehensive performance.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, but are not intended to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.

Claims (9)

1. An electrolyte comprising lithium salt, an organic solvent and an additive, characterized in that: the lithium salt comprises lithium bis (fluorosulfonyl) imide, wherein the lithium bis (fluorosulfonyl) imide accounts for 2.0-10.0% of the total mass of the electrolyte;
the additive comprises a carboxylic ester derivative, wherein the carboxylic ester derivative is one or more of compounds shown as a structural formula (I), and the structural formula (I) is，
R1 and R2 are independently C 1 -C 6 Alkyl orWherein G is 1 Is a bond, C 1 -C 5 Alkylene or a heteroatom-containing substituent, G 2 Is C 1 -C 5 Alkyl or a heteroatom-containing substituent, and G 1 、G 2 At least one of R1 and R2 is a heteroatom-containing substituent>，
The structural formula of the substituent group containing the hetero atom is-R 3 OR 4 ，-OR 4 ，-R 3 SR 4 ，-SR 4 ，-S i R 4 R 5 R 6 or-R 3 S i R 4 R 5 R 6 Wherein R is 3 Is C 1 -C 5 Alkylene group, R 4 、R 5 、R 6 Independently C 1 -C 5 An alkyl group.
2. The electrolyte of claim 1, wherein: the carboxylic ester derivative is selected from one or more of substances shown in the following structural formulas:、/>、、/>、 />、/>、/>。
3. the electrolyte according to claim 1 or 2, characterized in that: the carboxylate derivative accounts for 0.01% -5.0% of the total mass of the electrolyte.
4. The electrolyte according to claim 1 or 2, characterized in that: the mass ratio of the carboxylic ester derivative to the lithium bis (fluorosulfonyl) imide is 1:2.5-10.
5. The electrolyte of claim 1, wherein: the lithium salt also comprises other lithium salts, and the other lithium salts are LiPF 6 、LiBF 4 、LiAsF 6 、LiClO 4 、LiCF 3 SO 3 、LiC 4 F 9 SO 3 、Li(CF 3 SO 2 ) 2 N、Li(CF 3 SO 2 ) 3 C、Li(C 6 F 5 ) 4 B、Li(C 2 F 5 SO 2 ) 2 N 、LiBF 3 C 2 F 5 、LiPF 3 (C2F 5 ) 3 One or more of (a)The method comprises the steps of carrying out a first treatment on the surface of the The other lithium salt accounts for 5% -25% of the total mass of the electrolyte.
6. The electrolyte according to claim 5, wherein: the mass ratio of the lithium bis (fluorosulfonyl) imide to the other lithium salts is 1:0.5-8.
7. The electrolyte of claim 1, wherein: the electrolyte also comprises other additives, wherein the other additives are one or more of cyclic carbonates, sulfonates, sultones, sulfates, sulfites, benzene-containing compounds, halogenated compounds, nitrile compounds, boron-containing compounds, cyclic ether compounds, phosphazene compounds, phosphate esters, phosphites, amine compounds, isocyanate compounds, silicon-containing compounds, lithium salt-type compounds and fluoroether compounds containing double bonds; the other additives account for 0.5-15% of the total mass of the electrolyte.
8. The electrolyte of claim 1, wherein: the organic solvent is one or more of carbonic ester, carboxylic ester, ether and sulfone; the organic solvent accounts for 50% -85% of the total amount of the electrolyte.
9. The utility model provides a lithium ion battery, includes electric core and electrolyte, its characterized in that: the electrolyte is the electrolyte according to any one of claims 1 to 8.
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