CN115763960A - Silicon-based negative electrode electrolyte, preparation method and lithium ion battery thereof - Google Patents
Silicon-based negative electrode electrolyte, preparation method and lithium ion battery thereof Download PDFInfo
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- CN115763960A CN115763960A CN202211549322.2A CN202211549322A CN115763960A CN 115763960 A CN115763960 A CN 115763960A CN 202211549322 A CN202211549322 A CN 202211549322A CN 115763960 A CN115763960 A CN 115763960A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 64
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 62
- 239000010703 silicon Substances 0.000 title claims abstract description 62
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 124
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000002904 solvent Substances 0.000 claims abstract description 97
- -1 lithium hexafluorophosphate Chemical compound 0.000 claims abstract description 61
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 54
- 239000000654 additive Substances 0.000 claims abstract description 27
- 230000000996 additive effect Effects 0.000 claims abstract description 27
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims abstract description 6
- 150000003949 imides Chemical class 0.000 claims abstract description 3
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical group FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims abstract description 3
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 claims description 46
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 claims description 36
- 239000011259 mixed solution Substances 0.000 claims description 23
- VEWLDLAARDMXSB-UHFFFAOYSA-N ethenyl sulfate;hydron Chemical compound OS(=O)(=O)OC=C VEWLDLAARDMXSB-UHFFFAOYSA-N 0.000 claims description 20
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 12
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 claims description 10
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 10
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 8
- MASSZLINROTYNX-UHFFFAOYSA-N 1-(fluoromethylsulfonyl)ethane Chemical compound CCS(=O)(=O)CF MASSZLINROTYNX-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- CPOJJARBCZIKQQ-UHFFFAOYSA-N 3-trimethylsilyloxypropanenitrile Chemical compound C[Si](C)(C)OCCC#N CPOJJARBCZIKQQ-UHFFFAOYSA-N 0.000 claims description 5
- NKKMVIVFRUYPLQ-NSCUHMNNSA-N crotononitrile Chemical compound C\C=C\C#N NKKMVIVFRUYPLQ-NSCUHMNNSA-N 0.000 claims description 4
- BZWQNMUGNDAMBX-UHFFFAOYSA-N butyl butane-1-sulfonate Chemical compound CCCCOS(=O)(=O)CCCC BZWQNMUGNDAMBX-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- DWYMPOCYEZONEA-UHFFFAOYSA-L fluoridophosphate Chemical compound [O-]P([O-])(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-L 0.000 claims description 2
- LNLFLMCWDHZINJ-UHFFFAOYSA-N hexane-1,3,6-tricarbonitrile Chemical compound N#CCCCC(C#N)CCC#N LNLFLMCWDHZINJ-UHFFFAOYSA-N 0.000 claims description 2
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 230000002238 attenuated effect Effects 0.000 abstract description 2
- 150000005676 cyclic carbonates Chemical class 0.000 description 18
- QLCATRCPAOPBOP-UHFFFAOYSA-N tris(1,1,1,3,3,3-hexafluoropropan-2-yl) phosphate Chemical compound FC(F)(F)C(C(F)(F)F)OP(=O)(OC(C(F)(F)F)C(F)(F)F)OC(C(F)(F)F)C(F)(F)F QLCATRCPAOPBOP-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- MHYFEEDKONKGEB-UHFFFAOYSA-N oxathiane 2,2-dioxide Chemical compound O=S1(=O)CCCCO1 MHYFEEDKONKGEB-UHFFFAOYSA-N 0.000 description 5
- WXNUAYPPBQAQLR-UHFFFAOYSA-N B([O-])(F)F.[Li+] Chemical compound B([O-])(F)F.[Li+] WXNUAYPPBQAQLR-UHFFFAOYSA-N 0.000 description 4
- BTOQDHDEJJIDPF-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-yl dihydrogen phosphate Chemical compound OP(O)(=O)OC(C(F)(F)F)C(F)(F)F BTOQDHDEJJIDPF-UHFFFAOYSA-N 0.000 description 3
- 229910013075 LiBF Inorganic materials 0.000 description 3
- 229910013553 LiNO Inorganic materials 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 3
- IGILRSKEFZLPKG-UHFFFAOYSA-M lithium;difluorophosphinate Chemical compound [Li+].[O-]P(F)(F)=O IGILRSKEFZLPKG-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000011856 silicon-based particle Substances 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- 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 invention discloses a silicon-based negative electrode electrolyte, a preparation method and a lithium ion battery thereof, wherein the silicon-based negative electrode electrolyte comprises the following components: 17-20 parts by weight of a lithium agent, wherein the lithium agent comprises at least three of lithium hexafluorophosphate, lithium bis (difluorosulfonyl) imide, lithium bis (trifluoromethyl) sulfonyl imide, lithium bis (oxalato) borate and lithium tetrafluoroborate; 70-82.5 parts by weight of a non-aqueous primary solvent; and 0.5 to 10 parts by weight of a non-aqueous main solvent additive. The silicon-based negative electrode electrolyte can be preferably suitable for a high-silicon lithium battery system (the silicon content is more than or equal to 9%), and the problems that the electrolyte used for the silicon-based negative electrode generates gas, the circulating capacity is quickly attenuated and the like in the prior art are solved.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a silicon-based negative electrode electrolyte, a preparation method and a lithium ion battery thereof.
Background
The silicon-based material has large volume expansion, and particles can be broken in the circulation process, so that the consumption of electrolyte is increased along with the continuous recombination and repair of an SEI film. With the increasing of the silicon content, increasing the content of FEC becomes a main way to improve the electrochemical performance of the battery. However, the increase of the FEC content can cause the gas generation of the battery core to be intensified, the use safety risk of the battery is increased, and the consumption of the electrolyte is intensified along with the electrochemical processes such as circulation and the like, so that the current electrolyte cannot achieve the expected effect.
With the rapid development of lithium ion batteries, the demand for energy density is gradually increased, and silicon negative electrode materials are hot to the touch due to their high gram-capacitance (4200 mAh/g). But the charging efficiency and the cycle life times are lower, and the self-expansion rate can reach 300 percent. The main reason is that during the circulation process, the huge volume change easily causes the crushing and pulverization of silicon particles, so that an unstable SEI film is continuously generated on the crushed fresh surface, and the battery capacity is quickly attenuated. In order to alleviate the defects, a material factory reduces the influence caused by silicon expansion through nano-crystallization, pre-lithiation, pre-magnesiation and other ways, and achieves certain effect. However, the electrolyte is crucial to the wide application and popularization of the silicon negative electrode as the 'blood' of the lithium ion battery, and the improvement of the performance of the battery by the proper electrolyte is large, so that the development of the electrolyte suitable for the silicon negative electrode system becomes a problem to be solved urgently at present.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silicon-based negative electrode electrolyte capable of continuously forming a uniform, compact and stable SEI film on the negative electrode side, a preparation method and a lithium ion battery thereof, so as to solve the problems of high gas generation rate, high cycle capacity attenuation rate and the like of the electrolyte used by a silicon-based negative electrode in the prior art.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a silicon-based negative electrode electrolyte comprising:
17-20 parts by weight of a lithium agent, wherein the lithium agent comprises at least three of lithium hexafluorophosphate, lithium bis (difluorosulfonyl) imide, lithium bis (trifluoromethylsulfonyl) imide, lithium bis (oxalato) borate and lithium tetrafluoroborate;
70-82.5 parts by weight of a non-aqueous primary solvent;
and 0.5 to 10 parts by weight of a nonaqueous main solvent additive.
Further, the non-aqueous primary solvent includes a fluorinated solvent.
Further, the non-aqueous main solvent comprises one or more of fluoroethyl carbonate, dimethyl fluoro carbonate, 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether, fluoroadiponitrile, fluorinated cyclic carbonate, fluoromethyl ethyl sulfone, methylethyl carbonate, dimethyl carbonate and adiponitrile.
Further, the non-aqueous main solvent includes at least three of fluoroethyl carbonate, dimethyl fluoro carbonate, 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether, fluoroadiponitrile, fluorocyclocarbonate, fluoromethylethylsulfone, methylethyl carbonate, dimethyl carbonate, adiponitrile.
Further, the addition amount of the plurality of kinds of the nonaqueous main solvent is the same.
Further, the non-aqueous main solvent additive comprises any one or more of vinylene carbonate, propylene carbonate, 3- (trimethylsiloxy) propionitrile, 2-butenenitrile 1,3, 6-hexane, trimethyl nitrile, sulfur-containing heterocyclic borate ester, lithium nitrate, vinyl sulfate, butyl sultone and fluoro phosphate.
Further, the non-aqueous main solvent additive comprises 1, 3-propane sultone, and the addition amount of the 1, 3-propane sultone is less than 3 parts by weight. The method is used for solving the problems of high-temperature circulation, gas storage, gas generation and the like of the battery in the circulation process.
Further, the lithium agent is lithium bis (difluorosulfonimide), lithium bis (trifluoromethylsulfonimide) and lithium hexafluorophosphate.
The preparation method of the silicon-based negative electrode electrolyte comprises the following steps:
weighing 17-20 parts by weight of lithium agent, then weighing 70-82.5 parts by weight of non-aqueous main solvent, adding the lithium agent into the mixed liquid of the non-aqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the non-aqueous main solvent; and weighing 0.5-10 parts by weight of the nonaqueous main solvent additive, adding the nonaqueous main solvent additive into the mixed solution of the lithium agent and the nonaqueous main solvent, and uniformly stirring to obtain the silicon-based negative electrode electrolyte.
A lithium ion battery comprises the silicon-based negative electrode electrolyte.
The invention has the beneficial effects that:
the silicon-based negative electrode electrolyte disclosed by the invention can be better suitable for a high-silicon lithium battery system (the silicon content is more than or equal to 9%), and the problems that the gas generation of a battery core is aggravated and the use safety risk of the battery is increased due to the increase of the addition amount of FEC are solved, so that the cycle performance of the battery is improved; by continuously forming a uniform, compact and stable SEI film on the negative electrode side, the problems of high gas generation rate, high cycle capacity attenuation and the like of electrolyte used by a silicon-based negative electrode in the prior art are solved.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the 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.
Example 1
A silicon-based negative electrode electrolyte comprises 18 parts by weight of a lithium agent, 81 parts by weight of a non-aqueous main solvent and 1 part by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent includes fluorinated cyclic carbonate (FEC), fluorinated dimethyl carbonate (FDMC) and Fluorinated Ethyl Methyl Carbonate (FEMC). The non-aqueous main solvent additive includes 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris hexafluoroisopropyl phosphate (THFP), lithium difluorooxalato borate (LiDFOB).
The silicon-based negative electrode electrolyte is prepared by the following steps:
firstly, 18 parts by weight of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) are weighed 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) is not limited.
Then 27 parts by weight of fluorinated cyclic carbonate (FEC), 27 parts by weight of dimethyl Fluorocarbonate (FDMC), and 27 parts by weight of ethyl methyl Fluorocarbonate (FEMC) were weighed and mixed to be uniform, to prepare a mixed solution of a nonaqueous main solvent. Adding the lithium agent accounting for 18 parts by weight to the mixed liquid of the nonaqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the nonaqueous main solvent.
Weighing 1 part by weight of 1,3 parts of Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP) and lithium difluorooxalato borate (LiDFOB), adding the mixture into the mixed solution of the lithium agent and the nonaqueous main solvent, and uniformly stirring to obtain the silicon-based negative electrode electrolyte.
Example 2
A silicon-based negative electrode electrolyte comprises 17 parts by weight of a lithium agent, 82.5 parts by weight of a non-aqueous main solvent and 0.5 part by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent includes fluorinated cyclic carbonate (FEC), dimethyl carbonate (DMC), and Ethyl Methyl Carbonate (EMC). The non-aqueous main solvent additive includes 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris hexafluoroisopropyl phosphate (THFP), lithium difluorooxalato borate (liddob).
The silicon-based negative electrode electrolyte is prepared by the following steps:
firstly weighing 17 parts by weight of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in total 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) to (B) is not limited.
Then 27.5 parts by weight of fluorinated cyclic carbonate (FEC), 27.5 parts by weight of dimethyl carbonate (DMC) and 27.5 parts by weight of Ethyl Methyl Carbonate (EMC) were weighed and mixed uniformly to prepare a mixed solution of the non-aqueous main solvent. Adding the lithium agent accounting for 17 parts by weight to the mixed liquid of the nonaqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the nonaqueous main solvent.
Weighing 0.5 part by weight of 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP) and lithium difluoro oxalato borate (LiDFOB), adding the weighed materials into the mixed solution of the lithium agent and the non-aqueous main solvent, and uniformly stirring to obtain the silicon-based negative electrode electrolyte. In this example, specific proportions of 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), and lithium difluorooxalato borate (liddob) are not limited.
Example 3
A silicon-based negative electrode electrolyte comprises 20 parts by weight of a lithium agent, 77 parts by weight of a non-aqueous main solvent and 3 parts by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent includes fluorinated cyclic carbonate (FEC), fluorinated dimethyl carbonate (FDMC) and Fluorinated Ethyl Methyl Carbonate (FEMC). The non-aqueous main solvent additive includes 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), lithium difluoro oxalato borate (LiDFOB).
The silicon-based negative electrode electrolyte is prepared by the following steps:
first, a total of 20 parts by weight of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) were weighed 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) to (B) is not limited.
Then, 25.7 parts by weight of fluorinated cyclic carbonate (FEC), 25.7 parts by weight of fluorinated dimethyl carbonate (FDMC), and 25.7 parts by weight of Fluorinated Ethyl Methyl Carbonate (FEMC) were weighed and mixed to prepare a mixed solution of the nonaqueous main solvent. Adding the lithium agent accounting for 20 parts by weight into the mixed liquid of the non-aqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the non-aqueous main solvent.
Weighing 3 parts by weight of 1,3 parts by weight of Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD) and lithium difluoro oxalato borate (LiDFOB), adding the mixture into the mixed solution of the lithium agent and the non-aqueous main solvent, and uniformly stirring to obtain the silicon-based negative electrode electrolyte. In this example, specific proportions of 1, 3-Propanesultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), and lithium difluorooxalato borate (liddob) are not limited.
Example 4
A silicon-based negative electrode electrolyte comprises 18 parts by weight of a lithium agent, 72 parts by weight of a non-aqueous main solvent and 10 parts by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent comprises fluorinated cyclic carbonate (FEC), fluorinated adiponitrile (AND-CF) 3 ) And fluoroethyl carbonate (FEMC). The non-aqueous main solvent additive includes 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), (tris hexafluoroisopropyl) phosphate (THFP), lithium difluorooxalato borate (liddob).
The silicon-based negative electrode electrolyte is prepared by the following steps:
firstly, 18 parts by weight of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) are weighed 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) is not limited.
Then 24 parts by weight of fluorinated cyclic carbonate (FEC) AND 24 parts by weight of fluorinated adiponitrile (AND-CF) were weighed out 3 ) And 24 parts by weight of fluoroethyl carbonate (FEMC) were uniformly mixed to prepare a mixed solution of the nonaqueous main solvent. Adding the lithium agent accounting for 18 parts by weight to the mixed liquid of the nonaqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the nonaqueous main solvent.
In this example, specific proportions of 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP), lithium difluoroborate (liddob), and lithium difluoroborate (liddob) are not limited, but the amount of 1,3 Propane Sultone (PS) added should be less than 3 parts by weight.
Example 5
A silicon-based negative electrode electrolyte comprises 17 parts by weight of a lithium agent, 72 parts by weight of a non-aqueous main solvent and 10 parts by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent includes fluorinated cyclic carbonate (FEC), adiponitrile (AND), AND fluoroethyl carbonate (FEMC). The non-aqueous main solvent additive includes 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), (tris hexafluoroisopropyl) phosphate (THFP), lithium difluorooxalato borate (liddob).
The silicon-based negative electrode electrolyte is prepared by the following steps:
firstly weighing 17 parts by weight of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in total 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) to (B) is not limited.
Then, 24.3 parts by weight of fluorinated cyclic carbonate (FEC), 24.3 parts by weight of Adiponitrile (AND), AND 24.3 parts by weight of fluorinated methyl ethyl carbonate (FEMC) were weighed AND mixed uniformly to prepare a mixed solution of the nonaqueous main solvent. Adding the lithium agent accounting for 17 parts by weight to the mixed liquid of the nonaqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the nonaqueous main solvent.
In this example, specific proportions of 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP), lithium difluoroborate (liddob), and lithium difluoroborate (liddob) are not limited, but the amount of 1,3 Propane Sultone (PS) added should be less than 3 parts by weight.
Example 6
A silicon-based negative electrode electrolyte comprises 19 parts by weight of a lithium agent, 72 parts by weight of a non-aqueous main solvent and 9 parts by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium hexafluorophosphate (LiPF) 6 ) Lithium bis (oxalato) borate (LiBOB) and lithium tetrafluoroborate (LiBF) 4 ). The non-aqueous main solvent comprises 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether (D2), fluoromethylethyl sulfone (FEMS), fluoroadiponitrile (AND-CF) 3 ) And fluoroethyl carbonate (FEMC). The non-aqueous main solvent additive comprises Propylene Carbonate (PC), 3- (trimethylsiloxy) propionitrile (TMSOPN), and lithium nitrate (LiNO) 3 ) And Butane Sultone (BS).
The silicon-based negative electrode electrolyte is prepared by the following steps:
first, a total of 19 parts by weight of lithium hexafluorophosphate (LiPF) was weighed 6 ) Lithium bis (oxalato) borate (LiBOB), and lithium tetrafluoroborate (LiBF) 4 ). Lithium hexafluorophosphate (LiPF) in the present example 6 ) Lithium bis (oxalato) borate (LiBOB), and lithium tetrafluoroborate (LiBF) 4 ) The specific ratio of (A) to (B) is not limited.
Then, 18 parts by weight of 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether (D2), 18 parts by weight of fluoromethyl ethyl sulfone (FEMS) AND 18 parts by weight of fluoroadiponitrile (AND-CF) were weighed out separately 3 ) And 18 parts by weight of fluoroethyl carbonate (FEMC) were mixed uniformly to prepare a mixed solution of the nonaqueous main solvent. The lithium agent in a total of 19 parts by weight was added to the mixed solution of the nonaqueous main solvent, and the mixture was stirred uniformly to obtain a mixed solution of the lithium agent and the nonaqueous main solvent.
9 parts in total of Propylene Carbonate (PC), 3- (trimethylsiloxy) propionitrile (TMSOPN), and lithium nitrate (LiNO) were weighed 3 ) And Butyl Sultone (BS) is added into the mixed solution of the lithium agent and the non-aqueous main solvent and is uniformly stirred to obtain the silicon-based negative electrode electrolyte. In this example, propylene Carbonate (PC), 3- (trimethylsiloxy) propionitrile (TMSOPN), and lithium nitrate (LiNO) were added 3 ) The specific ratio of Butanesultone (BS) is not limited.
Example 7
A silicon-based negative electrode electrolyte comprises 20 parts by weight of lithium agent and 70 parts by weight of nonaqueous electrolyteSolvent, 10 parts by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent comprises fluorinated cyclic carbonate (FEC), fluorinated adiponitrile (AND-CF) 3 ) And fluoroethyl carbonate (FEMC). The non-aqueous primary solvent additive comprises 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP), lithium difluorophosphate (LiPF) 2 O 2 ) And 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether (D2).
The silicon-based negative electrode electrolyte is prepared by the following steps:
first, 20 parts by weight in total of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) were weighed 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) to (B) is not limited.
Then, 23.3 parts by weight of fluorinated cyclic carbonate (FEC) AND 23.3 parts by weight of fluorinated adiponitrile (AND-CF) were weighed out 3 ) And 23.3 parts by weight of fluoroethyl carbonate (FEMC) were uniformly mixed to prepare a mixed solution of the nonaqueous main solvent. Adding the lithium agent accounting for 20 parts by weight to the mixed liquid of the non-aqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the non-aqueous main solvent.
1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris hexafluoroisopropyl phosphate (THFP), lithium difluorophosphate (LiPF) were weighed out in a total of 10 parts by weight 2 O 2 ) And 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether (D2) are added into the mixed solution of the lithium agent and the nonaqueous main solvent and are uniformly stirred to obtain the silicon-based negative electrode electrolyte. In this example, 1, 3-Propanesultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP), and lithium difluorophosphate (LiPF) 2 O 2 ) And 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether (D2) are not particularly limited, but 1, 3-Propanesultone (PS) should be added in an amount of less than 3% by weightAnd (4) portions are obtained.
Example 8
A silicon-based negative electrode electrolyte comprises 19 parts by weight of a lithium agent, 72 parts by weight of a non-aqueous main solvent and 9 parts by weight of a non-aqueous main solvent additive. Wherein the lithium agent comprises lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI), and lithium hexafluorophosphate (LiPF) 6 ). The non-aqueous primary solvent includes fluorinated cyclic carbonate (FEC), dimethyl carbonate (DMC) and Ethyl Methyl Carbonate (EMC). The non-aqueous main solvent additive includes 1,3 Propane Sultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), (tris (hexafluoroisopropyl) phosphate (THFP), lithium difluorooxalato borate (LiDFOB), 2-butenenitrile (crotononitrile) 1,3, 6-Hexanetricarbonitrile (HTCN).
The silicon-based negative electrode electrolyte is prepared by the following steps:
first, 19 parts by weight in total of lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) were weighed 6 ). Lithium bis (difluorosulfonimide) (LiFSI), lithium bis (trifluoromethylsulfonimide) (LiTFSI) and lithium hexafluorophosphate (LiPF) in this example 6 ) The specific ratio of (A) to (B) is not limited.
And then respectively weighing 24 parts by weight of fluorinated cyclic carbonate (FEC), 24 parts by weight of dimethyl carbonate (DMC) and 24 parts by weight of Ethyl Methyl Carbonate (EMC) and uniformly mixing to prepare a mixed solution of the non-aqueous main solvent. The lithium agent in a total of 19 parts by weight was added to the mixed solution of the nonaqueous main solvent, and the mixture was stirred uniformly to obtain a mixed solution of the lithium agent and the nonaqueous main solvent.
In this example, specific proportions of 1,3 Propanesultone (PS), vinylene Carbonate (VC), vinyl sulfate (DTD), tris (hexafluoroisopropyl) phosphate (THFP), lithium difluorooxalato borate (liddob)/2-butenenitrile (crotononitrile), 1,3, 6-Hexanetricarbonitrile (HTCN), which amount to 9 parts by weight in total, were not limited, but the amount of 1,3 Propanesultone (PS) added should be less than 3 parts by weight, and they were added to the above-mentioned mixed solution of the lithium agent and the nonaqueous main solvent and stirred uniformly to obtain a silicon-based negative electrode electrolyte solution.
Comparative example
A prior art negative electrode electrolyte includes 18 parts by weight of lithium hexafluorophosphate (LiPF) 6 ) And a total of 82 parts by weight of a nonaqueous main solvent. Wherein the non-aqueous main solvent is a mixed solution of cyclic carbonate (EC), dimethyl carbonate (DMC) and cyclic carbonate (DEC).
The silicon-based negative electrode electrolyte is prepared by the following steps:
first, 19 parts by weight of lithium hexafluorophosphate (LiPF 6) in total was weighed, and then 27.3 parts by weight of fluorinated cyclic carbonate (FEC), 27.3 parts by weight of dimethyl carbonate (DMC) and 27.3 parts by weight of Ethyl Methyl Carbonate (EMC) were weighed and mixed uniformly to prepare a mixed solution of a nonaqueous main solvent. 18 parts by weight of lithium hexafluorophosphate (LiPF) described above 6 ) And adding the mixture into the mixed solution of the non-aqueous main solvent, and uniformly stirring to obtain the cathode electrolyte.
The performance of the silicon-based negative electrode electrolytes of examples 1 to 8 and the negative electrode electrolyte of the comparative example were respectively tested, and the test results are shown in table 1. The silicon-based negative electrode electrolytes of examples 1 to 8 were identical to the negative electrode electrolyte of the comparative example in both the number of cycles at 25 ℃ and the number of cycles at 45 ℃. Since a uniform, dense and stable SEI film can be continuously formed on the negative electrode side, the coulombic efficiency at 25 ℃ of the silicon-based negative electrode electrolytes of examples 1 to 8 is 1.5 times that at 25 ℃ of the negative electrode electrolyte of the comparative example; the 45 ℃ coulombic efficiency of the silicon-based negative electrode electrolytes of examples 1 to 8 is also obviously better than that of the negative electrode electrolyte of the comparative example at 45 ℃. Examples 1-8 the data for each example varied somewhat due to variations in the starting materials, conditions, and variations in the experimenter.
TABLE 1 circulation chart/Performance test summary sheet
The foregoing is only a preferred embodiment of the present invention, and many variations in the detailed description and the scope of the application may be made by those skilled in the art without departing from the spirit of the invention.
Claims (10)
1. A silicon-based anode electrolyte, comprising:
17-20 parts by weight of a lithium agent, wherein the lithium agent comprises at least three of lithium hexafluorophosphate, lithium bis (difluorosulfonyl) imide, lithium bis (trifluoromethylsulfonyl) imide, lithium bis (oxalato) borate and lithium tetrafluoroborate;
70-82.5 parts by weight of a non-aqueous primary solvent;
and 0.5 to 10 parts by weight of a nonaqueous main solvent additive.
2. The silicon-based anode electrolyte of claim 1, wherein the non-aqueous primary solvent comprises a fluorinated solvent.
3. The silicon-based negative electrode electrolyte of claim 1, wherein the non-aqueous main solvent comprises any one or more of fluoroethyl carbonate, dimethyl fluoro carbonate, 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether, fluoro adiponitrile, fluoro cyclic carbonate, fluoro methyl ethyl sulfone, methyl ethyl carbonate, dimethyl carbonate, and adiponitrile.
4. The silicon-based negative electrode electrolyte of claim 3, wherein the non-aqueous main solvent comprises at least three of fluoroethyl carbonate, dimethyl fluoro carbonate, 1, 2-tetrafluoroethyl-2, 3-tetrafluoropropyl ether, fluoro adiponitrile, fluoro cyclic carbonate, fluoro methyl ethyl sulfone, methyl ethyl carbonate, dimethyl carbonate, and adiponitrile.
5. The silicon-based negative electrode electrolyte of claim 4, wherein the non-aqueous primary solvents are added in the same amount.
6. The silicon-based negative electrode electrolyte of claim 1, wherein the non-aqueous main solvent additive comprises any one or more of vinylene carbonate, propylene carbonate, 3- (trimethylsiloxy) propionitrile, 2-butenenitrile, 1,3, 6-hexanetricarbonitrile, sulfur-containing heterocyclic borate esters, lithium nitrate, vinyl sulfate, butyl sultone, and fluoro phosphate.
7. The silicon-based negative electrode electrolyte of claim 6, wherein the non-aqueous main solvent additive comprises 1,3 propane sultone, and the 1,3 propane sultone is added in an amount of less than 3 parts by weight.
8. The silicon-based anode electrolyte of claim 1, wherein the lithium agent is lithium bis (difluorosulfonimide), lithium bis (trifluoromethylsulfonimide), and lithium hexafluorophosphate.
9. A method for preparing a silicon-based anode electrolyte according to any one of claims 1 to 8, comprising the steps of:
weighing 17-20 parts by weight of lithium agent, then weighing 70-82.5 parts by weight of non-aqueous main solvent, adding the lithium agent into the mixed liquid of the non-aqueous main solvent, and uniformly stirring to obtain the mixed liquid of the lithium agent and the non-aqueous main solvent; and weighing 0.5-10 parts by weight of the nonaqueous main solvent additive, adding the nonaqueous main solvent additive into the mixed solution of the lithium agent and the nonaqueous main solvent, and uniformly stirring to obtain the silicon-based negative electrode electrolyte.
10. A lithium ion battery comprising the silicon-based negative electrode electrolyte of any one of claims 1 to 8.
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