CN115692844A - Sodium secondary battery and electrolyte - Google Patents
Sodium secondary battery and electrolyte Download PDFInfo
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- CN115692844A CN115692844A CN202211133321.XA CN202211133321A CN115692844A CN 115692844 A CN115692844 A CN 115692844A CN 202211133321 A CN202211133321 A CN 202211133321A CN 115692844 A CN115692844 A CN 115692844A
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- 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 relates to the technical field of sodium ion batteries, and discloses an electrolyte for a sodium secondary battery, which comprises a sodium salt, a solvent and an electrolyte additive with the following structural formula:
Description
Technical Field
The invention belongs to the technical field of sodium ion batteries, and particularly relates to a sodium secondary battery and electrolyte.
Background
Among the novel battery systems, sodium-ion batteries are considered to be one of the most competitive next-generation rechargeable batteries due to their low cost and abundant sodium resources in nature. Sodium is electrochemically and chemically in the same group as Li, so sodium-ion batteries (SIBs) can follow the path of success for lithium-ion batteries. In addition, aluminum replaces copper as a negative current collector of the sodium ion battery, and the overall weight of the battery can be significantly reduced, thereby effectively increasing the energy density of the battery. Based on these advantages, advanced cathodes and anodes with various morphologies and compositionally elaborated designs have been successfully developed, many of which have been demonstrated to have great commercial application potential. Among them, higher energy density and lower price of sodium ion batteries are constantly pursued by researchers.
Currently, the positive electrode material of commercial sodium ion batteries can increase the energy density of the sodium ion battery by increasing the charging voltage. However, with the increase of the upper limit voltage, commercial positive electrode materials such as sodium vanadium phosphate materials suffer from poor high-temperature storage and serious cycle gassing. On one hand, the newly developed coating or doping technology is not perfect, and on the other hand, the matching problem of the electrolyte is solved, and the conventional electrolyte can be oxidized and decomposed on the surface of the battery anode under the high voltage of 4.3V, and particularly under the high temperature condition, the oxidative decomposition of the electrolyte can be accelerated, and meanwhile, the deterioration reaction of the anode material is promoted.
The sodium salt film-forming additive is one of the important components of electrolyte additive for sodium secondary battery. The excellent sodium salt film forming additives such as NaDFOB, naFSI and NaTFSI can form a protective film on the surface of the electrode, the protective film is insoluble in an organic solvent, sodium ions are allowed to be freely inserted into and removed from the electrode, solvent molecules are not allowed to pass through, and the damage of the electrode caused by further reaction of the organic electrolyte and the electrode can be effectively prevented, so that the normal-temperature cycle performance and the high-temperature and low-temperature performance of the battery are improved. More importantly, the use of film-forming additives is simpler and cheaper than the relatively complex and expensive modification of material coatings.
For example, chinese patent 201811353637.3 discloses an electrolyte for a lithium metal battery, which comprises the following components: a lithium salt, an additive and a non-aqueous solvent; the additive is NaBOB, naTFSI, naFSI, naPF 6 、NaBF 4 、 (C 3 H 3 NaO 2 ) n ，Na 2 SO 4 、Mg(FSI) 2 、Mg(TFSI) 2 One or more of KFSI and KTFSI; the concentration of the additive in the electrolyte for the lithium metal battery is 0.2-0.5 mol/L; the non-aqueous solvent is one or more of carbonate organic solvents, phosphate organic solvents and ether organic solvents.
The electrolyte in the invention can form an SEI interface layer on the surface of the metal lithium cathode in the process of constant current charging and discharging, thereby improving the safety performance of the battery, the utilization rate of the battery and the cycling stability.
However, the performance of the film forming additive varies due to the difference of the type and the proportion, so that the sodium ion battery is one of the main research directions of future batteries, and in order to further improve the comprehensive performance of the sodium ion battery, particularly the cycle performance, the high-temperature storage performance and the like, an electrolyte additive with better performance needs to be developed and applied to the sodium ion battery.
The Chinese patent 201711033014.3 discloses a lithium titanate battery electrolyte with low gas production; the organic solvent is a mixture of dimethyl carbonate, ethyl chlorocarbonate, tri (trimethylsilyl) phosphate and chain carboxylate, and the mass ratio of the solvent to the solvent is 1-1.6; the self-care ratio of the lithium salt to the organic solvent is 10-15%; the additive is at least one of sodium benzoate, ethylene diamine tetraacetic acid and 10-hydroxy-2-decenoic acid; the lithium titanate battery of the present invention has a small gas production amount, has high safety, can improve charge and discharge cycle characteristics, and can suppress gas generation during high-temperature storage.
The electrolyte additive such as sodium benzoate is adopted to improve the performance of the electrolyte, so that the comprehensive performance of the lithium battery is further improved, and the sodium ion battery can be used as reference, but the sodium ion battery directly has performance difference, and the electrolyte suitable for the sodium ion battery is obtained by corresponding further improvement.
Disclosure of Invention
One of the purposes of the invention is to provide an electrolyte suitable for sodium secondary, which can improve the cycle performance, high-temperature storage performance and low-temperature discharge performance of a sodium ion battery under high voltage;
another object of the present invention is to provide a sodium secondary battery which is capable of effectively reducing surface activity of an electrode at a high voltage, suppressing elution of vanadium and occurrence of side reactions between the electrode and an electrolyte, and increasing a conduction rate of sodium ions, thereby improving cycle performance, high-temperature storage performance, and low-temperature discharge performance of the battery at a high voltage (4.5V).
In order to achieve the above object, the present invention provides an electrolyte for a sodium secondary battery, comprising a sodium salt, a solvent, and an electrolyte additive of the following structural formula:
preferably, the electrolyte additive comprises the electrolyte additive with the structural formula and also comprises an auxiliary additive, wherein the auxiliary additive is lithium bis (oxalato) borate and/or tri (trimethylsilyl) borate.
Preferably, the electrolyte additive with the structural formula (I) accounts for 0.1-1.0% of the total mass of the sodium salt and the solvent.
In the electrolyte, the mass sum of the electrolyte additive and the auxiliary additive accounts for 0.1-5% of the total mass of the sodium salt and the solvent.
In the electrolyte, the sodium salt is sodium hexafluorophosphate, and the concentration of the sodium salt in the electrolyte is 0.5-1.5 mol/L.
In the present invention, it is not excluded that the sodium salt is wholly or partially one or more of sodium nitrate, sodium perchlorate, sodium difluorophosphate, sodium bisoxalato borate, sodium difluorooxalato borate, sodium bistrifluoromethylsulfonimide and sodium bisfluorosulfonimide.
In the present invention, the sodium salt may also be a combination of sodium hexafluorophosphate and one or more of sodium nitrate, sodium perchlorate, sodium difluorophosphate, sodium bisoxalate, sodium difluorooxalate, sodium bistrifluoromethylsulfonylimide and sodium bistrifluorosulfonimide in any proportion.
In the above-mentioned electrolytic solution, the solvent includes any one or more of a chain carbonate-based compound and a cyclic carbonate-based compound.
In the implementation process, the chain carbonate compound and the cyclic carbonate compound can be compounded in any proportion, and the change trend of the electrolyte of the invention is not influenced decisively.
Preferably, the cyclic carbonates include ethylene carbonate and/or propylene carbonate.
Preferably, the chain carbonates may be any one or more selected from dimethyl carbonate, diethyl carbonate and ethyl methyl carbonate.
Specifically, the solvent may be any combination of one or more of ethylene carbonate, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, propylene carbonate, ethyl acetate, butyl acetate, gamma-butyrolactone, propyl propionate, difluoroethyl acetate, and ethyl 2, 2-trifluoroacetate;
the invention also provides a sodium secondary battery which comprises a positive electrode made of sodium vanadium phosphate, a negative electrode made of hard carbon and the electrolyte.
In addition, the positive electrode material of the present invention may be selected from Na x CoO 2 、Na x MnO 2 、NaNi 0.33 Fe 0.33 Mn 0.33 O 2 、 NaFePO 4 、NaCoPO 4 、Na 3 V 2 (PO 4 ) 3 One or more of (a); the negative electrode material is selected from one or more of soft carbon, hard carbon, sodium titanate and metal capable of forming an alloy with sodium.
Advantageous effects
Compared with the prior art, the invention has the following beneficial effects:
(1) The compound with the specific structural formula is used as an electrolyte additive, acetate and sodium ions can generate coordination, so that a layer of stable interfacial film can be formed among additive molecules to coat the surfaces of a positive electrode and a negative electrode, and the stable structure combined with a benzene ring has higher thermodynamic stability;
(2) The compound with a specific structural formula is used as an electrolyte additive and is mixed with lithium bis (oxalato) borate and/or tri (trimethylsilane) borate to form a new electrolyte formula, so that a synergistic effect can be generated, the circulation performance, the high-temperature storage performance and the low-temperature discharge performance of the sodium-ion battery under high voltage are improved, and the sodium-ion battery has better performance;
(3) The electrolyte has more excellent performance by the mass ratio of the specific electrolyte additive, and the effects of effectively improving the cycle performance, high-temperature storage performance and low-temperature discharge performance of the sodium-ion battery under high voltage are effectively improved.
(4) When the electrolyte is used for a sodium secondary battery taking sodium vanadium phosphate as a positive electrode and hard carbon as a negative electrode, the surface activity of the electrode can be effectively reduced, the dissolution of vanadium and the occurrence of side reactions between the electrode and the electrolyte are inhibited, and the conduction rate of sodium ions is improved, so that the cycle performance, the high-temperature storage performance and the low-temperature discharge performance of the battery under high voltage (4.5V) are improved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without any creative effort, fall within the protection scope of the present invention.
Example 1
A sodium secondary battery specifically comprises the following preparation steps:
(1) Preparing an electrolyte: ethylene Carbonate (EC), diethyl carbonate (DEC) and Ethyl Methyl Carbonate (EMC) were mixed at a mass ratio of EC: DEC: EMC =1 6 ) And (3) enabling the concentration of sodium salt in the electrolyte to reach 1M, and adding an electrolyte additive accounting for 0.1% of the total mass of the sodium salt and the solvent after the sodium salt is completely dissolved, wherein the electrolyte additive is the electrolyte additive with the structural formula (I).
(2) Preparing a positive plate: uniformly mixing sodium vanadium phosphate, a conductive agent SuperP, a bonding agent PVDF and a Carbon Nano Tube (CNT) according to a mass ratio of 95.3; and then trimming, cutting into pieces, slitting, drying for 4 hours at 85 ℃ under a vacuum condition after slitting, and welding the tabs to prepare the sodium ion battery positive plate meeting the requirements.
(3) Preparing a negative plate: preparing hard carbon, a conductive agent SuperP, a thickening agent CMC and a binding agent SBR (styrene butadiene rubber emulsion) into slurry according to the mass ratio of 95.5.
(4) Preparing a sodium ion battery: preparing the positive plate, the negative plate and the diaphragm prepared by the process into a sodium-ion battery with the thickness of 4.7mm, the width of 55mm and the length of 60mm by a lamination process, baking the sodium-ion battery for 10 hours at 75 ℃, and injecting the electrolyte; after standing for 24 hours, the mixture was charged to 4.5V with a constant current of 0.lC (180 mA), and then charged at a constant voltage of 4.5V until the current dropped to 0.05C (90 mA); then discharging to 3.0V at 0.2C (180 mA), repeating the charging and discharging for 2 times, finally charging the battery to 3.8V at 0.2C (180 mA), and completing the battery manufacturing.
Example 2
Substantially the same as in example 1 except that the electrolyte additive was 0.2% by mass based on the total mass of the sodium salt and the solvent.
Example 3
Substantially the same as in example 1 except that the electrolyte additive was 0.5% by mass based on the total mass of the sodium salt and the solvent.
Example 4
The same as example 1 except that the electrolyte additive was 1% by mass based on the total mass of the sodium salt and the solvent.
Example 5
The electrolyte additive is a mixture of a compound shown in a structural formula (I) and lithium bis (oxalato) borate, and is 0.2% of the additive and 0.3% of the additive, which are basically the same as those in example 1.
Example 6
The electrolyte additive was a mixture of the compound represented by the formula (I) and tris (trimethylsilyl) borate, and was added in an amount of 0.2% and 0.3% in the same manner as in example 1.
Example 7
The electrolyte additive is basically the same as the electrolyte additive in the embodiment 1, except that the electrolyte additive is a mixture of a compound shown in a structural formula (I), lithium bis (oxalato) borate and tris (trimethylsilyl) borate, and the weight ratio of the three components is 4:3, the total amount of the three is 0.5 percent.
Example 8
Same as example 3 except that the solvent is EC PC: DEC: EMC = 1.
Example 9
Same as example 3 except that the solvent was EC: DMC: EMC = 1.
Comparative examples the following comparative compounds were used:
comparative example 1
Essentially the same as example 2, except that the electrolyte additive was comparative compound 1.
Comparative example 2
Essentially the same as example 2, except that the electrolyte additive was comparative compound 2.
Comparative example 3
Substantially the same as example 2, except that the electrolyte additive was comparative compound 3.
Comparative example 4
Substantially the same as in example 5 except that the electrolyte additive was lithium bis (oxalato) borate, which was equivalent to 0.5% by mass of the total mass of the sodium salt and the solvent.
Comparative example 5
The same as example 6 except that the electrolyte additive was tris (trimethylsilane) borate ester, which corresponded to 0.5% by mass of the total mass of the sodium salt and the solvent.
Comparative example 6
Substantially the same as in example 7 except that the electrolyte additive was a mixture of tris (trimethylsilane) borate ester and lithium bis (oxalato) borate, each of which corresponded to 0.25% by weight of the total mass of the sodium salt and the solvent.
Comparative example 7
Substantially the same as example 2 except that the electrolyte additive was NaDFOB.
Comparative example 8
Essentially the same as example 2 except that the electrolyte additive was NaTFSI.
Comparative example 9
Essentially the same as example 2, except that the electrolyte additive was NaFSI.
Performance test
Sodium ion battery performance test
Test method 1:
25 ℃ 0.5C/0.5C Normal temperature cycle test: charging to 4.5V at 25 deg.C under 0.5C constant current, charging at constant voltage of 4.5V to 0.05C cut-off current, and discharging at 0.5C constant current to obtain discharge capacity C 0 Repeating the charging and discharging steps for 400 weeks to obtain a discharge capacity C at 400 weeks 400 Capacity retention ratio = C 400 /C 0 *100％。
The test method 2:
capacity retention test at 60 ℃ for 14 days: charging to 4.5V at 25 deg.C under 0.5C constant current, charging at constant voltage of 4.5V to 0.05C cut-off current, and discharging at 0.5C constant current to obtain discharge capacity C 0 Charging at 25 deg.C with 0.5C constant current to 4.5V and constant voltage of 4.5V to cutoff current of 0.05C, transferring the battery to 60 deg.C, standing for 14 days, and discharging at 0.5C constant current to obtain discharge capacity C 1 Capacity retention = C at 60 ℃ storage for 14 days 1 /C 0 *100％。
Test method 3:
-10 ℃ low temperature discharge test: charging to 4.5V at 25 deg.C under 0.5C constant current, charging at constant voltage of 4.5V to 0.05C cut-off current, and discharging at 0.5C constant current to obtain discharge capacity C 0 . Charging to 4.5V at constant current of 0.5C and charging to cutoff current of 0.05V at constant voltage of 4.5V at 25 deg.C, transferring the battery to-10 deg.C, standing for 240min, and discharging at constant current of 0.5C to obtain discharge capacity C 2 Discharge rate at-10 ℃ C = C 2 /C 0 *100％。
The above examples 1 to 7 and comparative examples 1 to 13 were tested for the normal temperature cycle performance, the high temperature cycle performance and the low temperature discharge performance of the sodium ion battery by the above three test methods, and the results are shown in table 1:
table 1: sodium ion battery performance test results
As can be seen from the data in table 1:
1. as can be seen from the comparison between the example 2 and the comparative examples 1 to 3, the amount of formate is obviously improved on the electrochemical performance, and the compound shown in the structural formula (I) has a great improvement on the electrochemical performance of the electrolyte when being used as an electrolyte additive;
2. as can be seen from the comparison between the example 2 and the comparative examples 7 to 9, the compound shown in the structural formula (I) as the electrolyte additive has more excellent effect of improving the electrochemical performance of the electrolyte compared with other conventional electrolyte additives;
3. as can be seen from the comparison between the example 5 and the comparative example 4, the compound shown in the structural formula (I) and the lithium bis (oxalato) borate generate a synergistic effect, so that the effects of the cycle performance, the high-temperature storage performance and the low-temperature discharge performance of the sodium-ion battery under high voltage are improved, and the sodium-ion battery has better performance;
4. as can be seen from the comparison between the example 6 and the comparative example 5, the compound shown in the structural formula (I) and the tris (trimethylsilane) borate generate a synergistic effect, so that the effects of the cycle performance, the high-temperature storage performance and the low-temperature discharge performance of the sodium-ion battery under high voltage are improved, and the sodium-ion battery has better performance;
5. as can be seen from comparison between example 7 and comparative example 6, after the compound shown in the structural formula (I) is mixed with lithium bis (oxalato) borate and tri (trimethylsilyl) borate, the synergistic effect is obviously improved in the electrochemical performance of the electrolyte compared with the mixing of the lithium bis (oxalato) borate and the tri (trimethylsilyl) borate.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. An electrolyte for a sodium secondary battery comprises a sodium salt and a solvent, and is characterized by further comprising an electrolyte additive with the following structural formula:
2. the electrolyte for a sodium secondary battery according to claim 1, further comprising an auxiliary additive which is lithium bis (oxalato) borate and/or tris (trimethylsilyl) borate.
3. The electrolyte for a sodium secondary battery according to claim 2, wherein the electrolyte additive of the structural formula (I) is 0.1 to 1.0% by mass of the total mass of the sodium salt and the solvent.
4. The electrolyte for sodium secondary batteries according to any one of claims 1 to 3, wherein the sum of the mass of the electrolyte additive and the mass of the auxiliary additive accounts for 0.1 to 5% of the total mass of the sodium salt and the solvent.
5. The electrolyte for a sodium secondary battery according to claim 4, wherein the sodium salt is sodium hexafluorophosphate, and the concentration of the sodium salt in the electrolyte is 0.5mol/L to 1.5mol/L.
6. The electrolyte for a sodium secondary battery according to claim 4, wherein the solvent includes any one or more of chain and cyclic carbonate-based compounds.
7. The electrolyte for a sodium secondary battery according to claim 6, wherein the cyclic carbonates include ethylene carbonate and/or propylene carbonate.
8. The electrolyte for a sodium secondary battery according to claim 6, wherein the chain carbonates are any one or more of dimethyl carbonate, diethyl carbonate, and ethyl methyl carbonate.
9. A sodium secondary battery comprising a positive electrode of a material of sodium vanadium phosphate and a negative electrode of a material of hard carbon, characterized by further comprising the electrolyte of any one of claims 1 to 8.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116779969A (en) * | 2023-07-13 | 2023-09-19 | 华南师范大学 | Sodium ion battery electrolyte, sodium ion battery and method for improving performance of sodium ion battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116779969A (en) * | 2023-07-13 | 2023-09-19 | 华南师范大学 | Sodium ion battery electrolyte, sodium ion battery and method for improving performance of sodium ion battery |
| CN116779969B (en) * | 2023-07-13 | 2024-01-23 | 华南师范大学 | Sodium ion battery electrolyte, sodium ion battery and method for improving performance of sodium ion battery |
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