CN109935907A - Application, electrolysis additive, lithium ion battery and its electrolyte of silicon substrate sulfuric ester - Google Patents
Application, electrolysis additive, lithium ion battery and its electrolyte of silicon substrate sulfuric ester Download PDFInfo
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- CN109935907A CN109935907A CN201910212512.7A CN201910212512A CN109935907A CN 109935907 A CN109935907 A CN 109935907A CN 201910212512 A CN201910212512 A CN 201910212512A CN 109935907 A CN109935907 A CN 109935907A
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- additive
- electrolyte
- silicon substrate
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- ion battery
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to application, electrolysis additive, lithium ion battery and its electrolyte of a kind of silicon substrate sulfuric ester, silicon substrate sulfuric ester has the structure such as logical formula (I):R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.The silicon substrate sulfuric ester is film for additive, SEI interfacial film can be generated in the positive and negative polar decomghtion of battery core in battery forming process, compared to the additive of double silicon substrate sulfuric esters, the silicon substrate sulfuric ester of the structure can be melted at lower voltages, to generate the lower SEI interfacial film of impedance, and then improve battery core high temperature, cycle performance while, there is superior cryogenic property, and the production gas situation of battery core can also be effectively inhibited.In addition, the silicon substrate sulfuric ester has good normal temperature storage stability, so advantageously reducing the production cost of battery core, production efficiency is improved.
Description
Technical field
The present invention relates to battery technology fields, application, electrolysis additive, lithium more particularly to a kind of silicon substrate sulfuric ester
Ion battery and its electrolyte.
Background technique
The electrolyte of lithium ion battery is mainly made of anode, cathode, electrolyte.In lithium ion battery first charge-discharge mistake
(formation process is also referred to as in battery preparation technique) in journey, a series of electrochemical reactions occur for electrode material and electrolyte, raw
It is secondary anti-so as to reduce electrolyte at the passivation layer for being covered on electrode material surface, i.e. solid electrolyte interface (SEI) film
It answers, extends the circulation of battery core, improve the multiplying power of battery core, improve the high temperature performance of battery core.Film for additive refers to: in electrolyte
Middle additive amount is few, can preferentially react in electrode surface, and reaction product is covered on electrode surface, and then forms excellent SEI film
A substance.
The film for additive of current electrolysis liquid have VC (vinylene carbonate), VEC (vinyl ethylene carbonate), PS (1,
The third sultone of 3-), PST (1-propene-1,3-sulfonic acid lactone) etc., but be difficult keeping lithium ion battery in practical applications
On the basis of cycle performance, the high temperature performance of lithium ion battery is combined.
Summary of the invention
Based on this, it is necessary to provide a kind of electrolysis additive, be used for the electrolyte of lithium ion battery, can keep
On the basis of the cycle performance of lithium ion battery, makes lithium ion battery while there is preferable high temperature performance.
Correspondingly, it there is a need to provide a kind of compound and preparing the new opplication in electrolysis additive, i.e. silicon substrate sulfuric acid
Ester is preparing the application in electrolysis additive.
One aspect of the present invention provides a kind of silicon substrate sulfuric ester and is preparing the application in electrolysis additive, described
Silicon substrate sulfuric ester has the structure such as logical formula (I):
Wherein, R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.
The silicon substrate sulfuric ester is film for additive, can generate SEI circle in the positive and negative polar decomghtion of battery core in battery forming process
Facial mask can be used separately as electrolysis additive, can also be applied in combination with other electrolysis additives, and then can answer extensively
In electrolyte for various electrolyte lithium salts.The present inventor the study found that compared to double silicon substrate sulfuric esters additive, the knot
The silicon substrate sulfuric ester of structure can be melted at lower voltages, to generate the lower SEI interfacial film of impedance, and then improved
While the high temperature of battery core, cycle performance, there is superior cryogenic property, and the production gas feelings of battery core can also be effectively inhibited
Condition.For inventor further to mechanism study, this may be by the structure of the silicon substrate sulfuric ester there is stronger asymmetry to cause
's.In addition, there is the silicon substrate sulfuric ester good normal temperature storage stability to mention so advantageously reducing the production cost of battery core
High efficiency.
R in one of the embodiments,1~R4The halogen atom with 1~3 C atom is each independently to replace or do not take
The alkyl in generation.
R in one of the embodiments,1~R4It is methyl.
It is still another aspect of the present invention to provide a kind of electrolysis additives, contain additive A；The additive A is silicon
Base sulfuric ester, the silicon substrate sulfuric ester have the structure such as logical formula (I):
Wherein, R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.
It in one of the embodiments, further include additive B, the additive B is di-oxalate lithium borate, difluorophosphoric acid boron
At least one of sour lithium and difluorine oxalic acid boracic acid lithium.
In one of the embodiments, further include addition of C, the addition of C be vinylene carbonate, polystyrene,
At least one of polystyrene-divinylbenzene microspheres and vinyl ethylene carbonate.
It is still another aspect of the present invention to provide a kind of electrolyte for lithium ion battery, including electrolyte lithium salt, You Jirong
Agent and electrolysis additive described in any of the above embodiments.
In one of the embodiments, in the electrolyte for lithium ion battery, the mass content of the additive A is
1%~10%；
When the electrolysis additive further includes additive B, in the electrolyte for lithium ion battery, the addition
The mass content of agent B is 0.5%~5%；
When the electrolysis additive further includes addition of C, in the electrolyte for lithium ion battery, the addition
The mass content of agent C is 0.5%~5%.
The electrolyte lithium salt is selected from lithium hexafluoro phosphate, lithium perchlorate, two (trifluoromethyls in one of the embodiments,
Sulphonyl) at least one of imine lithium and imidodisulfuryl fluoride lithium salt.
It is still another aspect of the present invention to provide a kind of lithium ion battery, electrolyte is lithium described in any of the above embodiments
Ion battery electrolyte.
Specific embodiment
To facilitate the understanding of the present invention, below will to invention is more fully described, and give it is of the invention compared with
Good embodiment.But the invention can be realized in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
The present invention provides the silicon substrate sulfuric esters of an embodiment to prepare the application in electrolysis additive, silicon substrate sulfuric acid
Ester has the structure such as logical formula (I):
Wherein, R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.
The silicon substrate sulfuric ester is film for additive, can generate SEI circle in the positive and negative polar decomghtion of battery core in battery forming process
Facial mask can be used separately as electrolysis additive, can also be applied in combination with other electrolysis additives, and then can answer extensively
In electrolyte for various electrolyte lithium salts.The present inventor the study found that compared to double silicon substrate sulfuric esters additive, the knot
The silicon substrate sulfuric ester of structure can be melted at lower voltages, to generate the lower SEI interfacial film of impedance, and then improved
While the high temperature of battery core, cycle performance, there is superior cryogenic property, and the production gas feelings of battery core can also be effectively inhibited
Condition.For inventor further to mechanism study, this may be by the structure of the silicon substrate sulfuric ester there is stronger asymmetry to cause
's.
In recent years, sulfuric acid vinyl ester (DTD) is widely applied as additive, but sulfuric acid vinyl ester itself
Stability is bad, therefore the electrolyte for adding DTD needs cryo-conservation, and in the infiltration of the high temperature of battery production, high-temperature clamp
The processes such as chemical conversion, activation need to be adjusted temperature, increase the cost of production, while affecting battery core production efficiency.And
The silicon substrate sulfuric ester of above-mentioned logical formula (I) structure has good normal temperature storage stability, so advantageously reduce the production of battery core
Cost improves production efficiency.
It is understood that the halogen atom in the alkyl that halogen atom replaces is fluorine atom, bromine atom, chlorine atom or iodine atom.
R in one of the embodiments,1~R4It is each independently the alkyl with 1~5 C atom.
In one embodiment, R1~R4It is methyl.
An embodiment of the present invention additionally provides a kind of electrolysis additive, contains additive A.Wherein additive A is upper
State the silicon substrate sulfuric ester with the structure such as logical formula (I):
Wherein, R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.
The lithium-ion electrolyte additive further includes additive B in one of the embodiments, and additive B is double oxalic acid
Lithium borate (LiBOB), difluorophosphate (LiPO2F2At least one of) and difluorine oxalic acid boracic acid lithium (LiODFB).Further
Ground, additive B are di-oxalate lithium borate (LiBOB) and difluorophosphate (LiPO2F2At least one of).
The lithium-ion electrolyte additive further includes addition of C, and addition of C is film for additive.Addition of C includes but not
It is limited to vinylene carbonate (VC), PS (the third sultone of 1,3-), PST (1- propylene -1,3- sultones) and vinyl carbonic acid second
At least one of enester (VEC).
The mass parts ratio of additive A, additive B and addition of C is (1~10) in one of the embodiments: (0.5
~5): (0.5~5).Preferably, the mass parts ratio of additive A, additive B and addition of C is (1~5): (0.5~5):
(0.5~5).Further, the mass parts ratio of additive A, additive B and addition of C is (1~2): (0.5~5): (0.5
~5).
The present invention also provides a kind of electrolyte for lithium ion battery of an embodiment, including it is electrolyte lithium salt, organic
Solvent and any of the above-described electrolysis additive.
In one of the embodiments, electrolyte lithium salt include but is not limited to bis- (fluorosulfonyl) imide lis (LiFSI),
At least one of lithium hexafluoro phosphate, lithium perchlorate, two (trimethyl fluoride sulfonyl) imine lithiums.
Organic solvent is selected from ethylene carbonate (EC), propene carbonate (PC), butylene carbonate in one of the embodiments,
Ester (BC), dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), methyl propyl carbonate, gamma-butyrolacton
(GBL), methyl acetate (MA), ethyl acetate (EA), propyl acetate (EP), butyl acetate, ethyl propionate, propyl propionate and propionic acid
At least one of butyl ester.
In one of the embodiments, in electrolyte for lithium ion battery, the mass content of additive A is 1%~
10%.Preferably, in electrolyte for lithium ion battery, the mass content of additive A is 1%~5%.Further, in lithium
In ion battery electrolyte, the mass content of additive A is 1%~2%.
It in one of the embodiments, further include additive B, the quality of additive B in electrolyte for lithium ion battery
Content is 0.5%~5%.It in one of the embodiments, further include addition of C in electrolyte for lithium ion battery, addition
The mass content of agent C is 0.5%~5%.
The present invention also provides the lithium ion battery of an embodiment, electrolyte is that any of the above-described kind of lithium ion battery is used
Electrolyte.Specifically, lithium ion battery includes that anode, cathode and the electrolyte between anode and cathode, the electrolyte are
Any of the above-described kind of electrolyte for lithium ion battery.
The following are specific embodiments.
1) preparation of electrolyte
The electrolyte of embodiment 1-8 and comparative example 1-6 are prepared by the following method:
It is in mass ratio EC:DEC:EMC by ethylene carbonate (EC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC)
=3:2:5 is mixed, and it is 0.8mol/L that lithium hexafluoro phosphate to molar concentration, which is then added, and additive is then added and is mixed to get
Electrolyte.Additive types and its content in the electrolyte of each embodiment and comparative example show in table 1, wherein additive
Ratio is to account for the ratio of the total weight of the electrolyte.
The additive and its content of table 1 embodiment 1-10 and comparative example 1-4
It should be pointed out that bis- (trimethyl silicon substrate) sulfuric esters added by comparative example 6 are different from the present invention in above-mentioned table 1
Additive A, structure is as follows:
2) preparation of positive plate
By the mass ratio mixing nickle cobalt lithium manganate (LiNi of 95.5:2:1:1.50.5Co0.2Mn0.3), Super-P (lead by little particle
Electric carbon black), CNT (Carbon Nanotube, carbon nanotube) and PVDF (Kynoar), then disperse them in NMP
In (N-Methyl pyrrolidone), the lower stirring of de-airing mixer effect obtains anode sizing agent to stable uniform；Anode sizing agent is uniform
Coated on the aluminium foil with a thickness of 16 μm；Aluminium foil is transferred to in 120 DEG C of convection oven dry 2h after room temperature is dried, then
By being cold-pressed, being die cut to obtain positive plate.
3) preparation of negative electrode tab
By the quality of 95.5:1.5:1:2 than admixed graphite, Super-P (little particle conductive black), SBR (butadiene-styrene rubber)
With CMC (carboxymethyl cellulose), then disperses them in deionized water, obtain negative electrode slurry；Negative electrode slurry is uniformly applied
It overlays on the copper foil with a thickness of 8 μm；Copper foil is transferred to in 120 DEG C of convection oven dry 2h after room temperature is dried, is then passed through
Cross cold pressing, cross cutting obtains negative electrode tab.
4) preparation of lithium ion battery
Positive plate, negative electrode tab and diaphragm are obtained into naked battery core by lamination process, after battery core is put into pack case, injection
Electrolyte, then successively seal, lithium ion battery is obtained through processes, production such as standing, hot cold pressing, chemical conversion, partial volumes.
Illustrate the performance test process and test result of lithium ion battery below:
(1) normal-temperature circulating performance is tested
By lithium ion battery at 25 DEG C with 1C constant-current charge to 4.6V after, constant-voltage charge to cut-off current be 0.05C, so
A charge and discharge cycles are denoted as to 3.0V with 1C constant-current discharge afterwards.Then 200 circulations are carried out according to above-mentioned condition.Lithium ion
Capacity retention ratio (%)=(discharge capacity of the 200th circulation/discharge capacity for the first time) × 100% after battery 200 times circulations.
(2) high temperature cyclic performance is tested
By lithium ion battery at 45 DEG C with 1C constant-current charge to 4.6V after, constant-voltage charge to cut-off current be 0.05C, so
A charge and discharge cycles are denoted as to 3.0V with 1C constant-current discharge afterwards.Then 800 circulations are carried out according to above-mentioned condition.Lithium ion
Capacity retention ratio (%)=(discharge capacity of the 800th circulation/discharge capacity for the first time) × 100% after battery 800 times circulations.
(3) high-temperature storage performance is tested
Room temperature 1C constant-current constant-voltage charging ends to 4.6V, 0.05C, and then 1C constant-current discharge, 3V cut-off, circulation calculate three times
Average size is initial capacity C0, the volume for testing lithium ion battery is V0；Room temperature 1C constant-current constant-voltage charging is to 4.6V, 0.05C sections
Only, it is then placed in high temperature test cabinet and stores 7 days for 60 DEG C, take out the volume of test lithium ion battery and be denoted as Vn, volume expansion
Rate (%)=(Vn-V0)/V0；
After room temperature shelves 5h, 1C constant-current discharge to 3V records discharge capacity C1, charged percentage=C1/C0；Room temperature 1C
Constant-current constant-voltage charging ends to 4.6V, 0.05C, and then 1C constant-current discharge, 3V cut-off, record restore capacity C2；Restore percentage
=C2/C0。
(4) cryogenic property is tested
At 25 DEG C, lithium ion battery is charged to 4.6V with 1C constant current constant voltage, then with 1C constant-current discharge to 3.0V, record
Discharge capacity.Then 1C constant current constant voltage is charged to 4.6V, and 0.05C cut-off is placed in -20 DEG C of environment after shelving for 24 hours, 1C constant current is put
Electricity records discharge capacity to 2.4V.
- 20 DEG C of low temperature discharging efficiency value=1C discharge capacity (- 20 DEG C)/1C discharge capacity (25 DEG C) × 100%.
The test result of 2 Examples 1 to 8 of table and comparative example 1~6
As known from Table 2: comparing comparative example 1~6, the lithium ion battery of Examples 1 to 8 is in normal temperature circulation, high temperature circulation, height
Gentle storage, low temperature discharge etc. are all greatly improved, and the lithium ion battery of comparative example 1, comparative example 2~6 is interior
Resistance is respectively less than Examples 1 to 8.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of silicon substrate sulfuric ester is preparing the application in electrolysis additive, which is characterized in that the silicon substrate sulfuric ester has
The structure of such as logical formula (I):
Wherein, R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.
2. application as described in claim 1, which is characterized in that R1~R4It is former to be each independently the halogen with 1~3 C atom
The substituted or unsubstituted alkyl of son.
3. application as described in claim 1, which is characterized in that R1~R4It is methyl.
4. a kind of electrolysis additive, which is characterized in that contain additive A；The additive A is silicon substrate sulfuric ester, the silicon
Base sulfuric ester has the structure such as logical formula (I):
Wherein, R1~R4It is each independently the substituted or unsubstituted alkyl of halogen atom with 1~5 C atom.
5. electrolysis additive as claimed in claim 4, which is characterized in that further include additive B, the additive B is double
At least one of Lithium bis (oxalate) borate, difluorophosphoric acid lithium borate and difluorine oxalic acid boracic acid lithium.
6. electrolysis additive as described in claim 4 or 5, which is characterized in that further include addition of C, the addition of C is
At least one of vinylene carbonate, polystyrene, polystyrene-divinylbenzene microspheres and vinyl ethylene carbonate.
7. a kind of electrolyte for lithium ion battery, which is characterized in that including electrolyte lithium salt, organic solvent and such as claim 4
~6 described in any item electrolysis additives.
8. electrolyte for lithium ion battery as claimed in claim 7, which is characterized in that in the electrolyte for lithium ion battery
In, the mass content of the additive A is 1%~10%；
When the electrolysis additive further includes additive B, in the electrolyte for lithium ion battery, the additive B
Mass content be 0.5%~5%；
When the electrolysis additive further includes addition of C, in the electrolyte for lithium ion battery, the addition of C
Mass content be 0.5%~5%.
9. electrolyte for lithium ion battery as claimed in claim 7 or 8, which is characterized in that the electrolyte lithium salt is selected from six
Lithium fluophosphate, lithium perchlorate, two (trimethyl fluoride sulfonyl) at least one of imine lithiums and imidodisulfuryl fluoride lithium salt.
10. a kind of lithium ion battery, which is characterized in that its electrolyte is such as the described in any item lithium-ion electrics of claim 7~9
Pond electrolyte.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910212512.7A CN109935907A (en) | 2019-03-20 | 2019-03-20 | Application, electrolysis additive, lithium ion battery and its electrolyte of silicon substrate sulfuric ester |
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| CN201910212512.7A CN109935907A (en) | 2019-03-20 | 2019-03-20 | Application, electrolysis additive, lithium ion battery and its electrolyte of silicon substrate sulfuric ester |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111082146A (en) * | 2020-01-21 | 2020-04-28 | 大同新成新材料股份有限公司 | Electrolyte taking propylene carbonate as main solvent |
| CN111293362A (en) * | 2020-04-08 | 2020-06-16 | 河南华瑞高新材料有限公司 | Electrolyte suitable for nickel-manganese system |
| CN112054238A (en) * | 2020-09-11 | 2020-12-08 | 山东海科新源材料科技股份有限公司 | Cyclic sulfate additive containing silica chain segment, electrolyte containing cyclic sulfate additive and lithium ion battery |
-
2019
- 2019-03-20 CN CN201910212512.7A patent/CN109935907A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111082146A (en) * | 2020-01-21 | 2020-04-28 | 大同新成新材料股份有限公司 | Electrolyte taking propylene carbonate as main solvent |
| CN111293362A (en) * | 2020-04-08 | 2020-06-16 | 河南华瑞高新材料有限公司 | Electrolyte suitable for nickel-manganese system |
| CN112054238A (en) * | 2020-09-11 | 2020-12-08 | 山东海科新源材料科技股份有限公司 | Cyclic sulfate additive containing silica chain segment, electrolyte containing cyclic sulfate additive and lithium ion battery |
| CN112054238B (en) * | 2020-09-11 | 2021-10-22 | 山东海科新源材料科技股份有限公司 | Cyclic sulfate additive containing silica chain segment, electrolyte containing cyclic sulfate additive and lithium ion battery |
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Application publication date: 20190625 |