CN109786809A - A kind of electrolyte and secondary cell - Google Patents
A kind of electrolyte and secondary cell Download PDFInfo
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- CN109786809A CN109786809A CN201910129380.1A CN201910129380A CN109786809A CN 109786809 A CN109786809 A CN 109786809A CN 201910129380 A CN201910129380 A CN 201910129380A CN 109786809 A CN109786809 A CN 109786809A
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Abstract
The present invention provides a kind of electrolyte of suitable silicium cathode material, including including nonaqueous solvents, lithium salts and additive, which is characterized in that the additive contains additive X, and the general formula of the additive X is
Description
Technical field
The present invention relates to technical field of lithium ion more particularly to a kind of lithium-ion battery electrolytes.
Background technique
Ion cathode material lithium is currently in the link of most critical in lithium ion battery industry, by lithium ion battery cost ratio
Example, negative electrode material accounts for the 25% ~ 28% of lithium battery totle drilling cost, and relative to positive electrode, the research of negative electrode material is in the ascendant.Meet
Chemical potential is lower, cyclic specific capacity is high, coulombic efficiency is high, has good electronic conductivity and ionic conductivity, stability
High, resourceful, cheap, manufacturing process is simple, safety, the negative electrode material of green non-pollution are substantially not present at present, because
This research energy density is high, has a safety feature, is cheap, the novel anode material that material is easy to get becomes the task of top priority, existing rank
Section, lithium ion battery negative material mainly has carbon material, the oxide of transition metal, alloy material, silicon materials and other are siliceous
Material, the nitride and lithium titanate material of the transition metal containing lithium.Silicon materials due to high theoretical specific capacity in recent years
It is concerned, but its first charge discharge efficiency is low, especially material continuous convergent-divergent during deintercalate lithium ions is easy to make
At Particle Breakage, lead to the continuous decline of cyclic process capacity, meanwhile, unstable SEI film is being circulated throughout on silicium cathode material
Progressive additive in journey, polarization increase, cause biggish mechanical stress, destroy electrode structure, along in existing electrolyte
Film for additive also can constantly be destroyed, lead with expansion and contraction of the silicium cathode material in charge and discharge process, protective film
It causes it to need constantly to repair SEI film in the circulating cycle, consumes a large amount of active lithium, and SEI film transition is caused to increase, thus into causing
Cycle performance reduces.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of electrolyte of suitable silicium cathode material, it is characterized in that
Contain additive X in the electrolyte, additive X polymerize in battery core forms Polyborosiloxane, is coated on silicium cathode material table
Protection is formed in face of it, the transient response of electrolyte Yu silicium cathode material is avoided, effectively improves the cycle performance of silicium cathode material.
A kind of electrolyte provided by the invention, including nonaqueous solvents, lithium salts and additive, the additive contain additive
The general formula of X, the additive X is,R1 in general formula, R2, R3, R4, R5, R6 are independently the alkane of C1 ~ C8
Base or alkoxy, phenyl.
Further, the additive X includes 2,2,4,6,6,8- vegolysens, 3,5,7- tetra- oxygen -2,6-, bis- silicon -4,8-
Hypoboric acid cyclooctane, four oxygen -2,6- of 2,2,4,6,6,8- hexa methoxy -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,2,
Four oxygen -2,6- of 4,6,6,8- Hexaethyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, six ethyoxyl -1 2,2,4,6,6,8-,
Tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, four oxygen -2,6- two of 2,2,4,6,6,8- hexaphenyl -1,3,5,7-
Silicon -4,8- hypoboric acid cyclooctane, two silicon -4,8- of 2,2,6,6- tetramethyl -4,8- ethyoxyl four oxygen -2,6- of -1,3,5,7-, two boron
Sour cyclooctane, four oxygen -2,6- of 2,2,6,6- tetraethyl -4,8- ethyoxyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,
Four oxygen -2,6- of 2,6,6- tetramethoxy -4,8- ethyoxyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane；
Further, also contain other additives in the additive in addition to containing additive X, other described additives include sulphur
Vinyl acetate, ethylene sulfite, fluorinated ethylene carbonate, double sulfimide lithiums, difluorophosphate, three (trimethyl silicane) phosphoric acid
Ester, the mixing of one or more of unsaturated phosphate ester；
Further, the nonaqueous solvents is the mixing of one or more of cyclic carbonate and linear carbonate,
Further, the cyclic carbonate mainly include ethylene carbonate, propene carbonate, fluoro ethylene carbonate one kind or
Several mixing, the linear carbonate mainly include dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, second
Acetoacetic ester, the mixing of one or more of methyl acetate, propyl acetate；
The lithium salts is the mixing of one or more of lithium hexafluoro phosphate, double fluorine sulfimide lithiums, difluorine oxalic acid boracic acid lithium.
The present invention also provides a kind of secondary cells, include positive plate, negative electrode tab, the diaphragm and electricity being interval between positive and negative anodes
Liquid is solved, the electrolyte is the electrolyte comprising features described above.
Specific embodiment
A kind of electrolyte provided by the invention, including nonaqueous solvents, lithium salts and additive, the additive contain additive
The general formula of X, the additive X is,, R1, R2, R3 in general formula, R4, R5, R6 is independently, C1 ~ C8's
Alkyl or alkoxy, phenyl.
Further, the additive X includes 2,2,4,6,6,8- vegolysens, 3,5,7- tetra- oxygen -2,6-, bis- silicon -4,8-
Hypoboric acid cyclooctane, four oxygen -2,6- of 2,2,4,6,6,8- hexa methoxy -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,2,
Four oxygen -2,6- of 4,6,6,8- Hexaethyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, six ethyoxyl -1 2,2,4,6,6,8-,
Tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, four oxygen -2,6- two of 2,2,4,6,6,8- hexaphenyl -1,3,5,7-
Silicon -4,8- hypoboric acid cyclooctane, two silicon -4,8- of 2,2,6,6- tetramethyl -4,8- ethyoxyl four oxygen -2,6- of -1,3,5,7-, two boron
Sour cyclooctane, four oxygen -2,6- of 2,2,6,6- tetraethyl -4,8- ethyoxyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,
Four oxygen -2,6- of 2,6,6- tetramethoxy -4,8- ethyoxyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane；
Specifically, mass percent of the additive X in the lithium battery electrolytes is 0.01 ~ 10%.Preferably, institute
Stating mass percent of the additive X in the lithium battery electrolytes is 0.1 ~ 2%.
Further, also contain other additives, other described additive packets in the additive in addition to containing additive X
Include sulfuric acid vinyl ester, ethylene sulfite, fluorinated ethylene carbonate, double sulfimide lithiums, difluorophosphate, three (trimethyl silicanes)
Phosphate, the mixing of one or more of unsaturated phosphate ester；Matter of other the described additives in the lithium battery electrolytes
Measuring percentage is 0.01 ~ 10%.
Further, the nonaqueous solvents is the mixing of one or more of cyclic carbonate and linear carbonate,
Further, the cyclic carbonate mainly include ethylene carbonate, propene carbonate, fluoro ethylene carbonate one kind or
Several mixing, the linear carbonate mainly include dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, methyl propyl carbonate, second
Acetoacetic ester, the mixing of one or more of methyl acetate, propyl acetate；
The lithium salts is the mixing of one or more of lithium hexafluoro phosphate, double fluorine sulfimide lithiums, difluorine oxalic acid boracic acid lithium,
Molar concentration in the lithium battery electrolytes is 0.01 ~ 2 mol/L.Preferably, the molar concentration of the lithium salts be 0.5 ~
1.3 mol/L。
Embodiment 1
Battery production:
Anode preparation: by positive electrode active materials LiNi0.8Co0.1Mn0.1O2 (lithium nickel cobalt manganese) and conductive agent acetylene black
(SuperP) it mixing, N-Methyl pyrrolidone (NMP) binder polyvinylidene fluoride glue (PVDF) is added in agitator tank,
With all strength be stirred until homogeneous, wherein positive electrode active materials, conductive agent, binder mass ratio be (95:3.5:1.5).By what is obtained
Slurry is coated on aluminium foil, and baking, roll-in obtains anode pole piece after cut-parts.
Cathode preparation: negative electrode active material is aoxidized to mixture, the conductive agent SuperP of sub- silicon and graphite, polyimides
(PI) binder and deionized water are added into agitator tank, are stirred until homogeneous with all strength, wherein active material, conductive agent and bonding
The ratio of agent is (93:3:4).Obtained slurry is coated on copper foil, baking, roll-in obtains cathode pole piece after cut-parts.
Electrolyte preparation: in the glove box of applying argon gas (H2O < 10ppm, O2 < 1ppm), a certain amount of propylene carbonate is taken
Ester, fluorinated ethylene carbonate, diethyl carbonate, methyl ethyl carbonate (mass ratio 3:2:2:3) mixed liquor, are added into mixed liquor and add
Adding agent sulfuric acid vinyl ester, additional amount accounts for the 3% of gross mass, the 2,2 of electrolyte total amount 1.5% is then added into the electrolyte again,
4,6,6,8- vegolysens, 3,5,7- tetra- oxygen -2,6-, bis- silicon -4,8- hypoboric acid cyclooctane, are finally slowly added into mixed liquor
Account for about 1 M of gross mass 12.5%() LiPF6, obtain electrolyte.
The preparation of battery: the positive and negative anodes pole piece of preparation and isolation film are folded according to anode, isolation film, cathode sequence,
Ensure that isolation film is between positive and negative anodes pole piece, then wind, hot pressing shaping, soldering polar ear obtains naked battery core, utilizes aluminum plastic film
Carry out top side seal, after battery core is toasted at 85 DEG C for 24 hours, injection electrolyte, encapsulated by negative pressure, stand, chemical conversion, shaping
Etc. processes obtain the battery of embodiment 1.
Embodiment 2
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,4,6,6, the 8- hexa methoxies-of mass fraction 1.5%
Tetra- oxygen -2,6- of 1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace embodiment 1 in 2,2,4,6,6,8- vegolysen, 3,
Tetra- oxygen -2,6- of 5,7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Embodiment 3
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,4,6,6,8- Hexaethyl -1 of mass fraction 1.5%,
Tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace embodiment 1 in 2,2,4,6,6,8- vegolysen, 3,5,
Tetra- oxygen -2,6- of 7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Embodiment 4
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,4,6,6,8- six ethyoxyls-of mass fraction 1.5%
Tetra- oxygen -2,6- of 1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace embodiment 1 in 2,2,4,6,6,8- vegolysen, 3,
Tetra- oxygen -2,6- of 5,7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Embodiment 5
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,4,6,6,8- hexaphenyl -1 of mass fraction 1.5%,
Tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace embodiment 1 in 2,2,4,6,6,8- vegolysen, 3,5,
Tetra- oxygen -2,6- of 7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Embodiment 6
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,6,6- tetramethyl -4,8- second of mass fraction 1.5%
Oxy-1, tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace the 2,2,4,6,6,8- hexamethyl-in embodiment 1
Tetra- oxygen -2,6- of 1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Embodiment 7
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,6,6- tetraethyl -4,8- second of mass fraction 1.5%
Oxy-1, tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace the 2,2,4,6,6,8- hexamethyl-in embodiment 1
Tetra- oxygen -2,6- of 1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Embodiment 8
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,6,6- tetramethoxies -4,8- of mass fraction 1.5%
Four oxygen -2,6- of ethyoxyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replaces the 2,2,4,6,6,8- pregnancy in embodiment 1
Four oxygen -2,6- of base -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Battery is prepared using the method for embodiment 1；
Embodiment 9
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that with 2,2,4,6,6,8- six ethyoxyl -1 of mass fraction 3%,
Tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane replace embodiment 1 in 2,2,4,6,6,8- vegolysen, 3,5,
Tetra- oxygen -2,6- of 7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Comparative example 1
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that not adding 2,2,4,6,6, the 8- hexamethyls-in embodiment 1
Tetra- oxygen -2,6- of 1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane.
Battery is prepared using the method for embodiment 1；
Comparative example 2
Anode pole piece is prepared using the method for embodiment 1；
Cathode pole piece is prepared using the method for embodiment 1；
Electrolyte is prepared using the method for embodiment 1, the difference is that not adding any additive；
Battery is prepared using the method for embodiment 1；
Cycle life experiment: by embodiment 1 ~ 9 and 1 ~ 2 gained battery of comparative example respectively under the conditions of 25 DEG C with the charge and discharge of 1C/1C
Electric multiplying power carries out charge-discharge test, record initial capacity and the capacity after circulation 500cls within the scope of 2.7 ~ 4.2V.
Capacity/initial capacity * 100% after capacity retention ratio=circulation 500cls, acquired results see the table below.
| Sulfuric acid ethylene Ester content (%) | Additive X | Additive X Content (%) | Capacity retention ratio@ 500cls(%) | |
| Embodiment 1 | 3 | 2,2,4,6,6,8- vegolysen, tetra- oxygen -2,6- of 3,5,7- Two silicon -4,8- hypoboric acid cyclooctane | 1.5 | 76 |
| Embodiment 2 | 3 | Four oxygen -2 2,2,4,6,6,8- hexa methoxy -1,3,5,7-, Bis- silicon -4,8- hypoboric acid cyclooctane of 6- | 1.5 | 82 |
| Embodiment 3 | 3 | Four oxygen -2,6- of 2,2,4,6,6,8- Hexaethyl -1,3,5,7- Two silicon -4,8- hypoboric acid cyclooctane | 1.5 | 78 |
| Embodiment 4 | 3 | Four oxygen -2 six ethyoxyl -1,3,5,7- of 2,2,4,6,6,8-, Bis- silicon -4,8- hypoboric acid cyclooctane of 6- | 1.5 | 79 |
| Embodiment 5 | 3 | Four oxygen -2,6- of 2,2,4,6,6,8- hexaphenyl -1,3,5,7- Two silicon -4,8- hypoboric acid cyclooctane | 1.5 | 74 |
| Embodiment 6 | 3 | 2,2,6,6- tetramethyl -4,8- ethyoxyl -1,3,5,7- four Two silicon -4,8- hypoboric acid cyclooctane of oxygen -2,6- | 1.5 | 77 |
| Embodiment 7 | 3 | 2,2,6,6- tetraethyl -4,8- ethyoxyl -1,3,5,7- four Two silicon -4,8- hypoboric acid cyclooctane of oxygen -2,6- | 1.5 | 77 |
| Embodiment 8 | 3 | 2,2,6,6- tetramethoxy -4,8- ethyoxyl -1,3,5,7- Four oxygen -2,6-, two silicon -4,8- hypoboric acid cyclooctane | 1.5 | 81 |
| Embodiment 9 | 3 | Four oxygen -2 six ethyoxyl -1,3,5,7- of 2,2,4,6,6,8-, Bis- silicon -4,8- hypoboric acid cyclooctane of 6- | 3 | 82 |
| Comparative example 1 | 3 | - | 0 | 68 |
| Comparative example 2 | 0 | - | 0 | 57 |
As seen from table, the capacity retention ratio of the secondary cell containing additive X in electrolyte is apparently higher than without additive X
Secondary cell, additive X is 2,2,4,6,6,8- hexa methoxies -1,3, and 5,7- tetra- oxygen -2,6-, bis- silicon -4,8- hypoboric acid ring is pungent
Alkane, the capacity retention ratio highest that content is 1.5% are only merely to provide several embodiments, but be not limited to the above embodiment party in table
Formula, all inventions within the scope of spirit of that invention are all contained in the claims in the present invention protection scope.
Claims (6)
1. a kind of electrolyte provided by the invention, including nonaqueous solvents, lithium salts and additive, which is characterized in that the additive
Containing additive X, the general formula of the additive X is, R1, R2, R3 in general formula, R4, R5, R6 is independent
For alkyl or alkoxy, the phenyl of C1 ~ C8.
2. a kind of electrolyte as described in claim 1, which is characterized in that the additive X includes 2,2,4,6,6,8-
Vegolysen, tetra- oxygen -2,6- of 3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,2,4,6,6,8- hexa methoxy -1,3,5,7- four
Two silicon -4,8- hypoboric acid cyclooctane of oxygen -2,6-, four oxygen -2,6- of 2,2,4,6,6,8- Hexaethyl -1,3,5,7-, two silicon -4,8- two
Boric acid cyclooctane, six ethyoxyl -1,3,5,7- of 2,2,4,6,6,8-, four oxygen -2,6-, two silicon -4,8- hypoboric acid cyclooctane, 2,2,4,
Four oxygen -2,6- of 6,6,8- hexaphenyl -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,2,6,6- tetramethyl -4,8- ethoxy
Four oxygen -2,6- of base -1,3,5,7-, two silicon -4,8- hypoboric acid cyclooctane, 2,2,6,6- tetraethyl -4,8- ethyoxyl -1,3,5,7-
Four oxygen -2,6-, two silicon -4,8- hypoboric acid cyclooctane, four oxygen -2,6- of 2,2,6,6- tetramethoxy -4,8- ethyoxyl -1,3,5,7-
One of two silicon -4,8- hypoboric acid cyclooctane or a variety of mixing.
3. a kind of electrolyte as described in claim 1, which is characterized in that in the additive in addition to containing additive X
Also contain other additives, other described additives include sulfuric acid vinyl ester, ethylene sulfite, and fluorinated ethylene carbonate is double
Sulfimide lithium, difluorophosphate, three (trimethyl silicane) phosphates, the mixing of one or more of unsaturated phosphate ester.
4. a kind of electrolyte as described in claim 1, which is characterized in that the nonaqueous solvents is cyclic carbonate and chain carbon
The mixing of one or more of acid esters.
5. a kind of electrolyte as described in claim 1, which is characterized in that the lithium salts is lithium hexafluoro phosphate, double fluorine sulphonyl Asia
The mixing of one or more of amine lithium, difluorine oxalic acid boracic acid lithium.
6. including positive plate, negative electrode tab, the diaphragm being interval between positive and negative anodes and electrolysis the present invention also provides a kind of secondary cell
Liquid, the electrolyte are the electrolyte comprising claim 1-5 any one.
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| CN114430066A (en) * | 2020-10-13 | 2022-05-03 | 中国石油化工股份有限公司 | Electrolyte and lithium ion battery containing same |
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