CN109786809B - Electrolyte and secondary battery - Google Patents
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Abstract
The invention provides an electrolyte suitable for a silicon anode material, which comprises a nonaqueous solvent, lithium salt and an additive, and is characterized in that the additive contains an additive X, and the general formula of the additive X is
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to lithium ion battery electrolyte.
Background
The lithium ion negative electrode material is in the most critical link in the lithium ion battery industry at present, and the negative electrode material accounts for 25% -28% of the total cost of the lithium battery according to the cost proportion of the lithium ion battery, and is researched and developed relative to the positive electrode material. The lithium ion battery cathode material mainly comprises carbon materials, oxides of transition metals, alloy materials, silicon materials and other silicon-containing materials, nitrides of transition metals containing lithium and lithium titanate materials. Silicon materials have extremely high theoretical specific capacity, but have low first efficiency, especially the continuous shrinkage and expansion of the materials in the process of removing lithium ions are easy to cause particle breakage, so that the capacity of the cycling process is reduced continuously, meanwhile, an unstable SEI film on the silicon negative electrode material is gradually thickened in the cycling process, polarization is increased, larger mechanical stress is caused, the electrode structure is damaged, and a film forming additive in the existing electrolyte can also expand and shrink along with the silicon negative electrode material in the charging and discharging processes, so that the protective film is damaged continuously, the SEI film is required to be repaired continuously in the cycling process, a large amount of active lithium is consumed, the SEI film is increased in a transitional manner, and the cycling performance is reduced.
Disclosure of Invention
In order to solve the technical problems, the invention provides an electrolyte suitable for a silicon negative electrode material, which is characterized in that the electrolyte contains an additive X, the additive X is polymerized in a battery cell to form polysilaborons, and the polysilaborons are coated on the surface of the silicon negative electrode material to protect the polysilaborons, so that the transitional reaction of the electrolyte and the silicon negative electrode material is avoided, and the cycle performance of the silicon negative electrode material is effectively improved.
The invention provides an electrolyte, which comprises a nonaqueous solvent, lithium salt and an additive, wherein the additive contains an additive X with a general formula of,
in the general formula, R1, R2, R3, R4, R5 and R6 are independently C1-C8 alkyl or alkoxy or phenyl.
Further, the additive X comprises 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexamethoxy-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaethyl-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaphenyl-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2, 6-tetramethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2, 6-tetraethoxy-4, 6-disilazane-2, 6-tetrabromone, 3, 6-tetraethoxy-4, 8-tetrabromone, 4, 6-tetrabromone-2, 6-tetraethoxy-4, 6-tetrabromone-2, 6-tetrabromone;
further, the additive contains other additives besides the additive X, wherein the other additives comprise one or more of vinyl sulfate, vinyl sulfite, fluoroethylene carbonate, lithium bissulfonylimide, lithium difluorophosphate, tri (trimethylsilyl) phosphate and unsaturated phosphate;
further, the nonaqueous solvent is one or a mixture of more than one of cyclic carbonate and chain carbonate,
further, the cyclic carbonate mainly comprises one or more of ethylene carbonate, propylene carbonate and fluoroethylene carbonate, and the chain carbonate mainly comprises one or more of dimethyl carbonate, diethyl carbonate, methylethyl carbonate, methylpropyl carbonate, ethyl acetate, methyl acetate and propyl acetate;
the lithium salt is one or a mixture of more of lithium hexafluorophosphate, lithium difluorosulfimide and lithium difluorooxalato borate.
The invention also provides a secondary battery, which comprises a positive plate, a negative plate, a diaphragm and electrolyte, wherein the diaphragm is arranged between the positive plate and the negative plate, and the electrolyte is the electrolyte with the characteristics.
Detailed Description
The invention provides an electrolyte, which comprises a nonaqueous solvent, lithium salt and an additive, wherein the additive contains an additive X with a general formula of,in the general formula, R1, R2, R3, R4, R5 and R6 are independently C1-C8 alkyl or alkoxy or phenyl.
Further, the additive X comprises 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexamethoxy-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaethyl-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaphenyl-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2, 6-tetramethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilazane-4, 8-diboronic cyclooctane, 2, 6-tetraethoxy-4, 6-disilazane-2, 6-tetrabromone, 3, 6-tetraethoxy-4, 8-tetrabromone, 4, 6-tetrabromone-2, 6-tetraethoxy-4, 6-tetrabromone-2, 6-tetrabromone;
specifically, the mass percentage of the additive X in the lithium battery electrolyte is 0.01-10%. Preferably, the mass percentage of the additive X in the lithium battery electrolyte is 0.1-2%.
Further, the additive contains other additives besides the additive X, wherein the other additives comprise one or more of vinyl sulfate, vinyl sulfite, fluoroethylene carbonate, lithium bissulfonylimide, lithium difluorophosphate, tri (trimethylsilyl) phosphate and unsaturated phosphate; the mass percentage of the other additives in the lithium battery electrolyte is 0.01-10%.
Further, the nonaqueous solvent is one or a mixture of more than one of cyclic carbonate and chain carbonate,
further, the cyclic carbonate mainly comprises one or more of ethylene carbonate, propylene carbonate and fluoroethylene carbonate, and the chain carbonate mainly comprises one or more of dimethyl carbonate, diethyl carbonate, methylethyl carbonate, methylpropyl carbonate, ethyl acetate, methyl acetate and propyl acetate;
the lithium salt is one or a mixture of more of lithium hexafluorophosphate, lithium difluorosulfimide and lithium difluorooxalato borate, and the molar concentration of the lithium salt in the lithium battery electrolyte is 0.01-2 mol/L. Preferably, the molar concentration of the lithium salt is 0.5-1.3 mol/L.
Example 1
And (3) manufacturing a battery:
preparing a positive electrode: the positive electrode active material LiNi0.8Co0.1Mn0.1O2 (lithium nickel cobalt manganese) and the conductive agent acetylene black (SuperP) are mixed, N-methyl pyrrolidone (NMP) binder polyvinylidene fluoride glue solution (PVDF) is added into a stirring tank, and the mixture is stirred fully until the mixture is uniform, wherein the mass ratio of the positive electrode active material to the conductive agent to the binder is (95:3.5:1.5). And coating the obtained slurry on an aluminum foil, baking, rolling and cutting to obtain the positive electrode plate.
Preparing a negative electrode: the mixture of the negative electrode active material silicon oxide and graphite, the conductive agent SuperP, the Polyimide (PI) binder and deionized water are added into a stirring tank and stirred fully until uniform, wherein the ratio of the active material to the conductive agent to the binder is (93:3:4). And coating the obtained slurry on a copper foil, baking, rolling and cutting to obtain the negative electrode plate.
Preparing an electrolyte: in a glove box filled with argon (H2O is less than 10ppm, O2 is less than 1 ppm), taking a certain amount of mixed liquid of propylene carbonate, fluoroethylene carbonate, diethyl carbonate and methyl ethyl carbonate (mass ratio is 3:2:2:3), adding an additive of ethylene sulfate into the mixed liquid, wherein the addition amount is 3% of the total mass, then adding 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilyl-4, 8-diboronic cyclooctane accounting for 1.5% of the total mass of the electrolyte into the electrolyte, and finally slowly adding LiPF6 accounting for 12.5% of the total mass (about 1M) into the mixed liquid to obtain the electrolyte.
Preparation of the battery: and stacking the prepared positive and negative pole pieces and the isolating film according to the sequence of the positive pole, the isolating film and the negative pole, ensuring that the isolating film is positioned between the positive and negative pole pieces, winding, hot-pressing and shaping, welding the pole lugs to obtain a bare cell, performing top side sealing by using an aluminum plastic film, baking the cell at 85 ℃ for 24 hours after the end, injecting electrolyte, and performing the working procedures of negative pressure packaging, standing, forming, shaping and the like to obtain the battery of the embodiment 1.
Example 2
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disiloxane-4, 8-diboronic cyclooctane in example 1 was replaced with 2,2,4,6,6,8-hexamethoxy-1, 3,5, 7-tetraoxy-2, 6-disiloxane-4, 8-diboronic cyclooctane in a mass fraction of 1.5%.
A battery was prepared by the method of example 1;
example 3
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane in example 1 was replaced with 2,2,4,6,6,8-hexaethyl-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane in a mass fraction of 1.5%.
A battery was prepared by the method of example 1;
example 4
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane in example 1 was replaced with 2,2,4,6,6,8-hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane in a mass fraction of 1.5%.
A battery was prepared by the method of example 1;
example 5
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disiloxane-4, 8-diboronic cyclooctane in example 1 was replaced with 2,2,4,6,6,8-hexaphenyl-1, 3,5, 7-tetraoxy-2, 6-disiloxane-4, 8-diboronic cyclooctane in a mass fraction of 1.5%.
A battery was prepared by the method of example 1;
example 6
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane in example 1 was replaced with 1.5% by mass of 2, 6-tetramethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane.
A battery was prepared by the method of example 1;
example 7
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane in example 1 was replaced with 1.5% by mass of 2, 6-tetraethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane.
A battery was prepared by the method of example 1;
example 8
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane in example 1 was replaced with 1.5% by mass of 2, 6-tetramethoxy-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane.
A battery was prepared by the method of example 1;
a battery was prepared by the method of example 1;
example 9
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disiloxane-4, 8-diboronic cyclooctane in example 1 was replaced with 2,2,4,6,6,8-hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disiloxane-4, 8-diboronic cyclooctane in a mass fraction of 3%.
A battery was prepared by the method of example 1;
comparative example 1
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1, except that 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane of example 1 was not added.
A battery was prepared by the method of example 1;
comparative example 2
Preparing a positive electrode sheet by the method of example 1;
preparing a negative electrode sheet by the method of example 1;
an electrolyte was prepared by the method of example 1 except that no additive was added;
a battery was prepared by the method of example 1;
cycle life experiment: the batteries obtained in examples 1 to 9 and comparative examples 1 to 2 were subjected to charge and discharge tests at 25℃and a charge and discharge rate of 1C/1C in a range of 2.7 to 4.2V, respectively, and initial capacities and capacities after 500cls were recorded.
Capacity retention = capacity after 500cls per initial capacity 100% and the results are given in the table below.
| Vinyl sulfate content (%) | Additive X | Additive X content (%) | Capacity retention @500cls (%) | |
| Example 1 | 3 | 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane | 1.5 | 76 |
| Example 2 | 3 | 2,2,4,6,6,8-Hexamethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic acid cyclooctane | 1.5 | 82 |
| Example 3 | 3 | 2,2,4,6,6,8-Hexaethyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane | 1.5 | 78 |
| Example 4 | 3 | 2,2,4,6,6,8-Hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic acid cyclooctane | 1.5 | 79 |
| Example 5 | 3 | 2,2,4,6,6,8-hexaphenyl-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane | 1.5 | 74 |
| Example 6 | 3 | 2, 6-tetramethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilyl-4, 8-diboronic cyclooctane | 1.5 | 77 |
| Example 7 | 3 | 2, 6-tetraethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilicon-4, 8-diboronic cyclooctane | 1.5 | 77 |
| Example 8 | 3 | 2, 6-tetramethoxy-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane | 1.5 | 81 |
| Example 9 | 3 | 2,2,4,6,6,8-Hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic acid cyclooctane | 3 | 82 |
| Comparative example 1 | 3 | - | 0 | 68 |
| Comparative example 2 | 0 | - | 0 | 57 |
As is apparent from the table, the secondary battery containing additive X in the electrolyte has a significantly higher capacity retention than the secondary battery without additive X, and additive X is 2,2,4,6,6,8-hexamethoxy-1, 3,5, 7-tetraoxy-2, 6-disilane-4, 8-diboronic cyclooctane with a content of 1.5% and the capacity retention is the highest, but the table is provided only as examples, but the invention within the spirit of the present invention is included in the claims of the present invention.
Claims (6)
1. An electrolyte comprising a nonaqueous solvent, a lithium salt and an additive, wherein the additive comprises an additive X of the formula
Wherein R1, R2, R3, R4, R5 and R6 are independently C1-C8 alkyl or alkoxy, phenyl;
the mass percentage of the additive X in the lithium battery electrolyte is 0.01-10%.
2. The electrolyte of claim 1 wherein the additive X comprises a plurality of 2,2,4,6,6,8-hexamethyl-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexamethoxy-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaethyl-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaethoxy-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2,2,4,6,6,8-hexaphenyl-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2, 6-tetramethyl-4, 8-ethoxy-1, 3,5, 7-tetraoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2, 6-tetraethoxy-2, 6-disilo-4, 8-diboronic cyclooctane, 2, 6-tetraethoxy-4, 8-dioxio-2, 6, 7-tetraboro-4, 8-tetraboro-dioxie-2, 6, 7-tetraoxy-4, 6-dioxido-tetraboro-2, 6-tetraboro-dio-2, 6-tetraboro-2.
3. The electrolyte of claim 1 wherein the additive comprises, in addition to additive X, other additives including one or more of vinyl sulfate, vinyl sulfite, fluoroethylene carbonate, lithium bissulfonylimide, lithium difluorophosphate, tris (trimethylsilyl) phosphate, and unsaturated phosphate.
4. The electrolyte of claim 1, wherein the nonaqueous solvent is one or a mixture of a cyclic carbonate and a chain carbonate.
5. The electrolyte of claim 1, wherein the lithium salt is one or a mixture of lithium hexafluorophosphate, lithium difluorosulfonimide, and lithium difluorooxalato borate.
6. A secondary battery comprising a positive electrode sheet, a negative electrode sheet, a separator interposed between the positive and negative electrodes, and an electrolyte, wherein the electrolyte is the electrolyte according to any one of claims 1 to 5.
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| CN101939874A (en) * | 2008-03-05 | 2011-01-05 | 株式会社杰士汤浅国际 | Non-aqueous electrolyte battery |
| CN103518284A (en) * | 2011-05-09 | 2014-01-15 | 新神户电机株式会社 | Nonaqueous electrolyte solution and lithium ion battery |
| CN103730263A (en) * | 2013-12-27 | 2014-04-16 | 深圳新宙邦科技股份有限公司 | Organic electrolytic solution for super capacitor and super capacitor |
| CN106129473A (en) * | 2016-09-18 | 2016-11-16 | 珠海市赛纬电子材料股份有限公司 | A kind of nonaqueous electrolytic solution of silicon-based anode lithium ion battery |
| CN108598461A (en) * | 2018-04-25 | 2018-09-28 | 欣旺达电子股份有限公司 | Electrolyte and lithium ion battery |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101939874A (en) * | 2008-03-05 | 2011-01-05 | 株式会社杰士汤浅国际 | Non-aqueous electrolyte battery |
| CN103518284A (en) * | 2011-05-09 | 2014-01-15 | 新神户电机株式会社 | Nonaqueous electrolyte solution and lithium ion battery |
| CN103730263A (en) * | 2013-12-27 | 2014-04-16 | 深圳新宙邦科技股份有限公司 | Organic electrolytic solution for super capacitor and super capacitor |
| CN106129473A (en) * | 2016-09-18 | 2016-11-16 | 珠海市赛纬电子材料股份有限公司 | A kind of nonaqueous electrolytic solution of silicon-based anode lithium ion battery |
| CN108598461A (en) * | 2018-04-25 | 2018-09-28 | 欣旺达电子股份有限公司 | Electrolyte and lithium ion battery |
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