CN109921092B - Non-aqueous electrolyte of silicon-based negative electrode lithium ion battery and silicon-based negative electrode lithium ion battery containing electrolyte - Google Patents
Non-aqueous electrolyte of silicon-based negative electrode lithium ion battery and silicon-based negative electrode lithium ion battery containing electrolyte Download PDFInfo
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Abstract
The invention relates to the technical field of lithium ion batteries, and discloses a silicon-based negative electrode lithium ion battery non-aqueous electrolyte and a silicon-based negative electrode lithium ion battery containing the same. The non-aqueous electrolyte solution of the silicon-based negative electrode lithium ion battery comprises electrolyte lithium salt, a non-aqueous organic solvent and a film-forming additive, wherein the film-forming additive contains a silicon-based compound shown in a formula (I) structure and/or a conventional negative electrode film-forming additive. The silicon-based additive can form a layer of uniform and elastic protective film on the surface of the silicon-based negative electrode material, reduces the oxidation reaction of electrolyte on the surface of the battery material, and improves the normal-temperature cycle performance, the high-temperature cycle performance and the high-temperature storage performance of the silicon-based negative electrode lithium ion battery.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to a silicon-based negative electrode lithium ion battery non-aqueous electrolyte and a silicon-based negative electrode lithium ion battery with the electrolyte.
Background
The lithium ion battery has the advantages of high working voltage, high energy density, long service life, wide working temperature range, environmental friendliness and the like, and is widely applied to the fields of 3C digital products, electric tools, electric automobiles and the like. In recent years, with the rapid development of global economy, mobile electronic devices, particularly lighter and thinner smart phones, have come into the underground spray development, and people have made higher demands on the energy density of lithium ion batteries.
The energy density of the lithium ion battery is improved by the following common methods: firstly, the working voltage of the anode material is improved, and the problem that partial solvent or additive in the electrolyte is oxidized and decomposed on the surface of the anode material under high voltage is solved, so that the service life of the lithium ion battery is greatly shortened; ② silicon-based materials with higher discharge capacity (theoretical gram capacity of silicon: 4200mAh/g, theoretical gram capacity of graphite: 372mAh/g) were used.
However, compared with a carbon-based negative electrode material, the silicon-based material has obvious defects, for example, the silicon-based material has a huge volume effect in the room-temperature or high-temperature cycle process, which can cause the expansion of the negative electrode sheet to cause poor adhesion between the negative electrode material and the current collector; on the other hand, the expansion of silicon base can cause the SEI film on the negative electrode interface to be cracked and recombined in the battery cycle process, thereby causing the reduction and decomposition of electrolyte, the aggravation of by-products and the deterioration of the battery cycle performance.
In order to solve the problems in the application of silicon-based negative electrode materials, from the perspective of electrolytes, current research is mainly focused on developing new suitable additives and solvents. Although the conventional additives such as fluoroethylene carbonate (FEC) can improve the electrochemical performance of the silicon-based negative electrode lithium ion battery to a great extent, the addition of too much FEC causes the deterioration of the high-temperature performance of the battery, and the addition of a small amount of FEC causes the influence on the room-temperature cycle performance of the battery. At present, the commercialized electrolyte of the silicon-based negative electrode lithium ion battery is not mature, and the development of a new film-forming additive for solving the problems is not easy.
Disclosure of Invention
The invention aims to overcome the defects of the background technology and provides the non-aqueous electrolyte of the silicon-based negative electrode lithium ion battery and the silicon-based negative electrode lithium ion battery containing the non-aqueous electrolyte.
In order to achieve the purpose, the nonaqueous electrolyte solution of the silicon-based negative electrode lithium ion battery comprises electrolyte lithium salt, a nonaqueous organic solvent and a film-forming additive, wherein the film-forming additive contains a silicon-based compound shown in a structure of a formula (I):
wherein R is selected from alkyl, alkenyl, alkynyl, H atom, F atom, fluorine-containing alkyl and phenyl with 1-4 carbon atoms, the fluorine-containing atom number of the terminal group in the fluorine-containing alkyl is 0-3, and the fluorine-containing atom number of other carbon atoms is 0-2.
Preferably, the film forming additive further comprises a conventional negative electrode film forming additive, wherein the conventional negative electrode film forming additive is selected from one or more of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC), Vinyl Ethylene Carbonate (VEC), 1, 3-Propane Sultone (PS), 1, 3-propane sultone (1,3-PST), vinyl sulfite (ES), tris (trimethylsilane) phosphate (TMSP), tris (trimethylsilane) borate (TMSB), and Methylene Methanedisulfonate (MMDS).
Preferably, the mass of the fluoroethylene carbonate accounts for the total mass of the electrolyte
5.0-10.0%, wherein the mass of the ethylene carbonate or the 1, 3-propylene sultone accounts for 0.01-1.2% of the total mass of the electrolyte.
More preferably, the film-forming additive contains vinylene carbonate, 1, 3-propane sultone, fluoroethylene carbonate and tris (trimethylsilane) borate, or contains vinylene carbonate, 1, 3-propane sultone, fluoroethylene carbonate, tris (trimethylsilane) borate and vinylethylene carbonate; more preferably, the film forming additive contains vinylene carbonate, 1, 3-propane sultone, fluoroethylene carbonate and tris (trimethylsilane) borate, and the addition amounts thereof are respectively 1.0%, 10.0% and 1.5% of the total mass of the electrolyte; or vinylene carbonate, 1, 3-propane sultone, fluoroethylene carbonate, tris (trimethylsilane) borate and vinylethylene carbonate, and the addition amounts thereof are 1.0%, 10.0%, 1.5% and 0.5% of the total mass of the electrolyte, respectively.
Preferably, the silicon-based compound having the structure of formula (i) is selected from one or more of compounds 1-6:
preferably, the mass of the silicon-based compound having the structure of formula (i) is 0.01% to 3.0%, for example 0.9% to 1.1%, and as a further example 1% of the total mass of the electrolyte.
More preferably, the mass of the film forming additive accounts for 0.5-15.0% of the total mass of the electrolyte.
Preferably, the electrolyte lithium salt is lithium hexafluorophosphate (LiPF)6) Lithium bis (fluorosulfonyl) imide (LiFSI), lithium difluorophosphate (LiPO)2F2) And lithium difluorooxalato borate (liddob), such as a mixed lithium salt of lithium hexafluorophosphate and lithium difluorophosphate, or a mixed lithium salt of lithium hexafluorophosphate, lithium difluorosulfonimide and lithium difluorophosphate, or a mixed lithium salt of lithium hexafluorophosphate, lithium difluorophosphate and lithium difluorooxalato borate.
Preferably, the addition amount of the electrolyte lithium salt is 13.0-17.5% of the total mass of the electrolyte.
Further preferably, the electrolyte lithium salt is a mixed lithium salt of lithium hexafluorophosphate and lithium difluorophosphate, and the addition amounts of the lithium hexafluorophosphate and the lithium difluorophosphate respectively account for 15.0 wt% and 1.0 wt% of the total mass of the electrolyte; or a mixed lithium salt of lithium hexafluorophosphate, lithium bis (fluorosulfonyl) imide and lithium difluorophosphate, wherein the addition amounts of the lithium hexafluorophosphate, the lithium bis (fluorosulfonyl) imide and the lithium difluorophosphate respectively account for 15.0%, 2.0% and 1.0% of the total mass of the electrolyte; or a mixed lithium salt of lithium hexafluorophosphate, lithium difluorophosphate and lithium difluorooxalato borate, wherein the addition amounts of the lithium hexafluorophosphate, the lithium difluorophosphate and the lithium difluorooxalato borate respectively account for 15.0%, 1.0% and 1.0% of the total mass of the electrolyte.
Preferably, the non-aqueous organic solvent comprises cyclic carbonate and chain carbonate, preferably, the cyclic carbonate is selected from one or more of ethylene carbonate and propylene carbonate, and the chain ester is selected from one or more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, bis (2,2, 2-trifluoroethyl) carbonate and methyl trifluoroethyl carbonate.
Preferably, the addition amount of the cyclic carbonate accounts for 20.0-45.0% of the total mass of the electrolyte, wherein the addition amount of the propylene carbonate accounts for 5.0-20.0% of the total mass of the electrolyte.
More preferably, the non-aqueous organic solvent includes ethylene carbonate, diethyl carbonate and ethyl methyl carbonate, and the ethylene carbonate, the diethyl carbonate and the ethyl methyl carbonate are mixed in a mass ratio of 20: 15: 15: 50 are mixed.
The invention also provides a silicon-based negative lithium ion battery which comprises a cathode pole piece, an anode pole piece, a separation film arranged between the cathode pole piece and the anode pole piece and the non-aqueous electrolyte of the silicon-based negative lithium ion battery.
Preferably, the cathode plate comprises an aluminum foil current collector and a cathode membrane, and the anode plate comprises a copper foil current collector and an anode membrane.
Preferably, the cathode membrane includes a cathode active material, a conductive agent, and a binder, and the anode membrane includes an anode active material, a conductive agent, and a binder.
Further preferably, the cathode active material is LiNi1-x-y-zCoxMnyAlzO2Or LiAmBnPO4Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, m is more than or equal to 0 and less than or equal to 1, n is more than or equal to 0 and less than or equal to 1, and x + y + z is more than or equal to 0 and less than or equal to 1, A, B represents.
Further preferably, the anode active material is nano silicon, silicon alloy, SiOwSilicon carbon composite material compounded with graphite, preferably, the SiOwIs a silicon oxide, a silicon oxide or other silicon-based material.
The invention has the advantages that:
1. the negative electrode film forming additive (especially fluoroethylene carbonate) is reduced on the surface of the negative electrode material in preference to the solvent to form an excellent interface protective film, so that the reaction of the electrode material and the electrolyte is reduced; meanwhile, the formed solid electrolyte membrane has low impedance, which is beneficial to improving the internal dynamic characteristics of the lithium ion battery;
2. the silicon-based additive shown in the structure of formula (I) can form a layer of uniform and elastic protective film on the surface of a silicon-based negative electrode material, so that the oxidation reaction of electrolyte on the surface of a battery material is reduced; in the additive, a silicon-group-containing functional group preferentially reacts with a silicon-based negative electrode material to be embedded into the negative electrode material, and the tail part of the additive forms a film longitudinally, so that the formed SEI film has higher toughness;
3. the negative electrode film forming additive (especially fluoroethylene carbonate) and the silicon-based additive shown in the structure of the formula (I) act together, so that the risk of FEC high-temperature gas generation can be reduced to a certain extent, and the high-temperature cycle performance and the high-temperature storage performance of the battery are improved; and other auxiliary conventional additives are added, so that the SEI film can be better modified, and the performance of the battery is improved.
4. In the invention, novel conductive lithium salts of lithium bis (fluorosulfonyl) imide, lithium difluorophosphate and lithium difluorooxalato borate with good film forming characteristics are added, compared with the case of singly using LiPF6And various novel film-forming lithium salts are combined for use, so that the high-low temperature performance, the rate capability and the long cycle performance of the power battery are improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
As used herein, the terms "comprises," "comprising," "includes," "including," "contains," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
Preparing electrolyte: in a glove box filled with argon, ethylene carbonate, diethyl carbonate and ethyl methyl carbonate are mixed according to the mass ratio of EC: PC: DEC: EMC 20: 15: 15: 50, and then 15.0 wt% of lithium hexafluorophosphate and 1.0 wt% of LiPO were slowly added to the mixed solution2F2And finally, adding 1.0 wt% of silicon-based compound (shown in table 1) shown in the formula (I) based on the total weight of the electrolyte, and uniformly stirring to obtain the lithium ion battery electrolyte of the example 1.
Examples 2 to 14 and comparative examples 1 to 9
As shown in Table 1, examples 2 to 14 and comparative examples 1 to 9 were the same as example 1 except that the components of the electrolyte were added in the proportions shown in Table 1.
TABLE 1 composition ratios of the components of the electrolytes of examples 1-14 and comparative examples 1-9
Effects of the embodiment
Injecting the prepared lithium ion battery electrolyte into the fully dried artificial graphite material/LiNi0.6Co0.2Mn0.2O2In the battery, the battery is subjected to conventional capacity grading after standing at 45 ℃, high-temperature clamp formation and secondary sealing.
1) And (3) testing the normal-temperature cycle performance of the battery: at 25 ℃, the battery after capacity grading is charged to 4.2V at constant current and constant voltage according to 1C, the current is cut off at 0.05C, then the battery is discharged to 2.8V 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 (%) was (1000 th cycle discharge capacity/first cycle discharge capacity) × 100%;
2) thickness expansion and capacity residual rate test at constant temperature of 60 ℃: firstly, the battery is placed at normal temperature and is circularly charged and discharged for 1 time (4.2V-2.8V) at 0.5C, and the discharge capacity C before the battery is stored is recorded0Then charging the battery to 4.2V full-voltage state with constant current and constant voltage, and using vernier caliper to test the thickness d of the battery before high-temperature storage1(the two diagonals of the battery are respectively connected through a straight line, and the intersection point of the two diagonals is a battery thickness test point), then the battery is placed in a 60 ℃ incubator for storage for 7 days, and after the storage is finished, the battery is taken out and the thermal thickness d of the stored battery is tested2Calculating the expansion rate of the thickness of the battery after the battery is stored for 7 days at a constant temperature of 60 ℃; after the battery is cooled for 24 hours at room temperature, the battery is discharged to 2.8V at constant current of 0.5C again, and the discharge capacity C after the battery is stored is recorded1And calculating the capacity residual rate of the battery after being stored for 7 days at the constant temperature of 60 ℃, wherein the calculation formula is as follows: thickness expansion rate of battery after 7 days of storage at 60 ═ d2-d1)/d1100% of the total weight; the residual capacity rate after 7 days of constant temperature storage at 60 ℃ is C1/C0*100％；
3) And (3) testing the 45 ℃ cycle performance of the battery: at the temperature of 45 ℃, the battery after capacity grading is charged to 4.2V at constant current and constant voltage according to 1C, the current is cut off at 0.05C, then the battery is discharged to 2.8V at constant current according to 1C, and according to the circulation, the circulation capacity retention rate of 800 weeks is calculated after 800 cycles of charging/discharging, and the calculation formula is as follows: the 800 th cycle capacity retention (%) was (800 th cycle discharge capacity/first cycle discharge capacity) × 100%.
The results of the electrical property tests of the lithium ion battery electrolytes of examples 1 to 14 and comparative examples 1 to 9 are shown in table 2.
Table 2 results of electrical property test of electrolytes for lithium ion batteries in examples 1 to 14 and comparative examples 1 to 9
The comparison of the electrical performance test results of comparative example 1 and examples 1-6 in Table 2 shows that: the novel film-forming additive can obviously improve the cycle performance of the battery and the capacity retention rate after high-temperature storage, and can speculate that the silicon-based additive can form a layer of uniform and tough protective film on the surface of a silicon-based negative electrode material, and the protective film can effectively relieve the pulverization and cracking of the material caused by the expansion and contraction of a silicon-carbon material in the charging and discharging processes.
The comparison of the electrical property test results of example 1 and example 2 in table 2 shows that: example 1 electrical performance is better than example 2 because the unsaturated carbon-carbon triple bond film quality is not as good as the unsaturated carbon-carbon double bond charge, which is very likely to be great in the resistance of acetylenic materials to film formation.
The comparison of the results of the electrical property tests of example 11 and example 13 in table 2 shows that: the electrical property of the example 13 is better than that of the example 11, the unsaturated bond-containing material VEC is added into the example 13, the material has good film forming stability on a negative electrode and good toughness, can adapt to the expansion and contraction of a silicon-based material, and simultaneously the VEC can well improve the high-temperature performance of the battery.
The results of the electrical property tests of example 1, example 7 and example 8 in table 2 are compared to see that: the amount of compound 1 added to the novel additive is preferably about 1.0%. When the addition amount is too small, the novel additive has poor film forming quality on a silicon-based negative electrode, so that the electrical property of the battery can not meet the requirement. When the amount is too large, the additive in the non-film-forming portion is very harmful to the storage performance of the battery.
The comparison of the results of the electrical property tests of comparative examples 2-5 in table 2 shows that: the fluoroethylene carbonate (FEC) can obviously improve the cycle performance of the silicon-based negative electrode lithium ion battery, but the high-temperature cycle performance and the high-temperature storage performance of the battery are deteriorated along with the increase of the FEC content.
A comparison of the results of the electrical property tests of examples 1-8 and examples 9-14 in Table 2 shows that: the silicon-based novel additive is used alone, the requirement of the electrical performance of the battery cannot be completely met, other types of additives are required to be added, and the additives have interaction and improve the electrical performance of the battery together.
Further, compared with the use of LiPF alone6As the conductive lithium salt, the novel conductive lithium salt lithium difluorophosphate with good film forming characteristics is added in the embodiments 1 to 14, and the combined use of various novel film forming lithium salts effectively improves the cycle performance and the high-temperature storage performance of the silicon-based negative electrode lithium ion battery.
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 (5)
1. The nonaqueous electrolyte solution for the silicon-based negative electrode lithium ion battery comprises electrolyte lithium salt, a nonaqueous organic solvent and a film-forming additive, and is characterized in that the film-forming additive contains a silicon-based compound, and the structural formula of the silicon-based compound is shown as a compound 1:
the non-aqueous organic solvent is ethylene carbonate, propylene carbonate, diethyl carbonate and ethyl methyl carbonate, and the mass ratio of the ethylene carbonate to the propylene carbonate to the diethyl carbonate to the ethyl methyl carbonate is 20: 15: 15: 50, and the addition amount of the compound 1 accounts for 1.0 percent of the total mass of the electrolyte;
the lithium salt consists of lithium hexafluorophosphate, lithium difluorosulfonimide and lithium difluorophosphate, the addition amounts of the lithium hexafluorophosphate, the lithium difluorosulfonimide and the lithium difluorophosphate respectively account for 15.0%, 2.0% and 1.0% of the total mass of the electrolyte, and the film forming additive also contains a conventional negative electrode film forming additive which is vinylene carbonate, 1, 3-propane sultone, fluoroethylene carbonate and tris (trimethylsilane) phosphate, and the addition amounts of the vinylene carbonate, the 1, 3-propane sultone, the fluoroethylene carbonate and the tris (trimethylsilane) phosphate respectively account for 1.0%, 10.0% and 1.5% of the total mass of the electrolyte; or the conventional negative electrode film forming additive is vinylene carbonate, 1, 3-propane sultone, fluoroethylene carbonate, tris (trimethylsilane) phosphate and ethylene carbonate, and the addition amounts of the vinylene carbonate, the 1, 3-propane sultone, the fluoroethylene carbonate, the tris (trimethylsilane) phosphate and the ethylene carbonate respectively account for 1.0%, 10.0%, 1.5% and 0.5% of the total mass of the electrolyte.
2. A silicon-based negative electrode lithium ion battery, which is characterized by comprising a cathode pole piece, an anode pole piece, a separation film arranged between the cathode pole piece and the anode pole piece and the non-aqueous electrolyte of the silicon-based negative electrode lithium ion battery in claim 1.
3. The silicon-based negative lithium ion battery of claim 2, wherein the cathode plate comprises an aluminum foil current collector and a cathode membrane, and the anode plate comprises a copper foil current collector and an anode membrane.
4. The silicon-based negative lithium ion battery according to claim 3, wherein the cathode membrane comprises a cathode active material, a conductive agent and a binder, and the anode membrane comprises an anode active material, a conductive agent and a binder.
5. The silicon-based negative electrode lithium ion battery according to claim 4, wherein the cathode active material is LiNi1-x-y-zCoxMnyAlzO2Or LiAmBnPO4Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, m is more than or equal to 0 and less than or equal to 1, n is more than or equal to 0 and less than or equal to 1, and x + y + z is more than or equal to 0 and less than or equal to 1, A, B represents.
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| CN117154187B (en) * | 2023-10-30 | 2024-06-18 | 宁德时代新能源科技股份有限公司 | Battery cell, battery and electricity utilization device |
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| KR20140038979A (en) * | 2011-05-09 | 2014-03-31 | 신코베덴키 가부시키가이샤 | Nonaqueous electrolyte solution and lithium ion battery |
| CN105428701B (en) * | 2015-12-21 | 2018-02-09 | 东莞新能源科技有限公司 | A kind of electrolyte and the lithium ion battery including the electrolyte |
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| CN109417200A (en) * | 2016-07-01 | 2019-03-01 | 中央硝子株式会社 | Non-aqueous electrolyte additive, non-aqueous electrolyte and nonaqueous electrolyte secondary battery using the additive |
| CN108987804A (en) * | 2018-07-18 | 2018-12-11 | 石家庄圣泰化工有限公司 | Application of the nitrile compounds of silicone-containing base in battery electrolyte |
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