CN118610009A - Electrolyte containing lithium salt additive and preparation and application thereof - Google Patents
Electrolyte containing lithium salt additive and preparation and application thereof Download PDFInfo
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- CN118610009A CN118610009A CN202410580413.5A CN202410580413A CN118610009A CN 118610009 A CN118610009 A CN 118610009A CN 202410580413 A CN202410580413 A CN 202410580413A CN 118610009 A CN118610009 A CN 118610009A
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- lithium salt
- electrolyte
- salt additive
- low
- electrolyte containing
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 74
- 229910003002 lithium salt Inorganic materials 0.000 title claims abstract description 58
- 159000000002 lithium salts Chemical class 0.000 title claims abstract description 58
- 239000000654 additive Substances 0.000 title claims abstract description 55
- 230000000996 additive effect Effects 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 11
- 239000003990 capacitor Substances 0.000 claims abstract description 9
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 8
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 229910013188 LiBOB Inorganic materials 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 6
- 229910013870 LiPF 6 Inorganic materials 0.000 claims description 4
- 229910013063 LiBF 4 Inorganic materials 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 230000004913 activation Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- WXNUAYPPBQAQLR-UHFFFAOYSA-N B([O-])(F)F.[Li+] Chemical compound B([O-])(F)F.[Li+] WXNUAYPPBQAQLR-UHFFFAOYSA-N 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 229910013075 LiBF Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- UBQYURCVBFRUQT-UHFFFAOYSA-N N-benzoyl-Ferrioxamine B Chemical compound CC(=O)N(O)CCCCCNC(=O)CCC(=O)N(O)CCCCCNC(=O)CCC(=O)N(O)CCCCCN UBQYURCVBFRUQT-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000005678 chain carbonates Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010351 charge transfer process Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 150000005676 cyclic carbonates Chemical class 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- -1 lithium tetrafluoroborate Chemical compound 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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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
- Y02E60/13—Energy storage using capacitors
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- Secondary Cells (AREA)
Abstract
The invention relates to an electrolyte containing a lithium salt additive, and preparation and application thereof, wherein the electrolyte comprises lithium salt, the lithium salt additive and a low-temperature solvent, the lithium salt additive is LiDFOB, liBF 4 or LiBOB, and the low-temperature solvent is a mixture of ethylene carbonate, ethylmethyl carbonate and toluene. Compared with the prior art, the invention can effectively solve the problems of low-temperature performance attenuation and the like of the lithium ion capacitor.
Description
Technical Field
The invention belongs to the technical field of electrolyte, and relates to electrolyte containing a lithium salt additive, and preparation and application thereof.
Background
Lithium Ion Capacitor (LIC) is a novel power type energy storage device, which adopts a lithium ion battery (Lithium-ion battery, LIB) intercalation reaction cathode and a super capacitor physical adsorption anode, has the advantages of high energy density of the lithium ion battery and long cycle life of the super capacitor, most hopefully meets the automobile 48V power performance requirement of the United states advanced battery consortium (United STATES ADVANCED Battery Consortium, USABC), and is gradually applied in the scenes of energy regeneration, power assistance, energy storage and the like, but the problem of performance attenuation at low temperature limits the further application development of the LIC.
Different application scenarios have different requirements on the operating temperature range of the power supply device, for example, the consumer electronics field generally requires that the operating temperature range is-20-60 ℃; in the field of automobiles, the automobile is required to be capable of being stored at a low temperature of-20 or-30 ℃ and being charged and discharged at a low-rate current density, and meanwhile, the automobile is stable in performance when being stored at 60 ℃ and the capacity retention rate is required to be higher than 80% after 200 circles of cycles when being cycled at a high temperature; when the battery is applied to the fields of national defense and military industry and the like, the battery is required to be stored at the temperature of minus 40 ℃ and charged and discharged at the low multiplying power of 0.2 ℃, the capacity retention rate is higher than 80% after being stored at the temperature of 70 ℃ for 48 hours, and the expansion rate of the battery is required to be lower than 5% if the battery is used; in the aerospace field, where temperature requirements are more stringent, it is sometimes even required that the battery be capable of charge and discharge at low temperatures of-80 ℃ at low current densities.
LIC has inherited the problem of serious performance decay at low temperatures of LIB, rather than EDLC, and has little research on LIC's low-temperature electrolyte, fortunately, reference can be made to LIB's low-temperature electrolyte research, and meanwhile, LIC is also noted to be different in electrode materials, energy storage mechanisms and the like and LIB.
In a battery system, electrolyte conducts ions, forms an SEI film on the surfaces of an anode and a cathode, has an important influence on the low-temperature performance of the battery, and comprises a binary or multi-element solvent system formed by a cyclic carbonate and a chain carbonate organic solvent which are mixed together according to a certain proportion, a main solvent with a high dielectric constant and a cosolvent with low viscosity, lithium salt, typically LiPF 6, with the concentration of typically 1mol/L, and in recent years, researches on ultra-concentrated lithium salt electrolyte, an additive necessary for improving the performance of the battery and the like are also carried out. However, the existing electrolyte is difficult to meet the low-temperature performance requirement of LIC.
Disclosure of Invention
The invention aims to provide electrolyte containing a lithium salt additive, and preparation and application thereof, so as to solve the problems of low-temperature performance attenuation and the like of a lithium ion capacitor.
The aim of the invention can be achieved by the following technical scheme:
One of the technical schemes of the invention provides an electrolyte containing a lithium salt additive, which comprises lithium salt, the lithium salt additive and a low-temperature solvent, wherein the lithium salt additive is LiDFOB (lithium difluoroborate), liBF 4 (lithium tetrafluoroborate) or LiBOB (lithium oxalato borate), and the low-temperature solvent is a mixture of ethylene carbonate, ethylmethyl carbonate and toluene.
Further, the lithium salt is LiPF 6.
Further, the concentration of the lithium salt in the electrolyte is 1.1 to 1.3mol/L.
Further, the concentration of the lithium salt in the electrolyte was 1.2mol/L.
Further, the concentration of the lithium salt additive in the electrolyte is 0.08-0.12 mol/L.
Further, the concentration of the lithium salt additive in the electrolyte is 0.1mol/L.
Further, the volume ratio of the ethylene carbonate to the methyl ethyl carbonate to the toluene is 1: (0.8-1.2): (2.5-3.5). Further, the volume ratio of the ethylene carbonate to the methyl ethyl carbonate to the toluene is 1:1:3.
The second technical scheme of the invention provides a preparation method of the electrolyte containing the lithium salt additive, wherein the lithium salt and the lithium salt additive are weighed and mixed with a low-temperature solvent to obtain the electrolyte.
The third technical scheme of the invention provides application of electrolyte containing lithium salt additive in lithium ion capacitors. When the low-temperature electrolyte is applied to a lithium ion capacitor, the low-temperature performance of the lithium ion capacitor can be effectively improved.
According to the invention, the distribution and arrangement of lithium salt in the electrolyte are improved by optimizing the lithium salt additive and adopting the specific low-temperature solvent for compounding with the lithium salt additive, so that the low-temperature performance of the device is improved.
Drawings
FIG. 1 shows charge and discharge curves of the first two cycles of HC half-cell formation for different electrolytes at room temperature;
FIG. 2 is a graph of differential capacity for HC half-cell formation using different electrolytes;
FIG. 3 is a graph showing EIS of HC negative electrode as a function of voltage during first charge at room temperature using three electrode button;
FIG. 4 is a graph showing the rate performance of HC half-cells using different electrolytes at different temperatures;
FIG. 5 is a graph showing the rate performance of LIC full cells using different electrolytes at-20deg.C;
FIG. 6 is a graph showing the HC negative electrode impedance measured with a three electrode button cell at 0.4V at different temperatures;
Fig. 7 is a graph of impedance data obtained by EIS curve fitting and an arrhenii Wu Sigong equation fitting.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, unless otherwise indicated, the starting materials or processing techniques are all conventional commercially available in the art.
Example 1:
The electrolyte containing the lithium salt additive in the embodiment consists of lithium salt, the lithium salt additive and a low-temperature solvent, wherein the lithium salt additive is LiDFOB, the concentration of the lithium salt additive is 0.1mol/L, the low-temperature solvent is formed by mixing ethylene carbonate, methyl ethyl carbonate and toluene according to the volume ratio of 1:1:3, the lithium salt is LiPF 6, the concentration of the lithium salt is 1.2mol/L, and the obtained electrolyte is E5.
Example 2:
In comparison with example 1, the same procedure was followed except that the lithium salt additive was replaced with LiBF 4, and the resulting electrolyte was designated as E6.
Example 3:
in comparison with example 1, which is largely identical except that the lithium salt additive is replaced by LiBOB, the resulting electrolyte is designated as E7.
Comparative example 1:
in comparison with example 1, the electrolyte was obtained, which was designated as E1, except that no lithium salt additive was added.
FIG. 1 shows charge and discharge curves of the first two cycles of formation of an electrolyte HC half cell containing a lithium salt additive at room temperature, the HC half cell containing the additive electrolyte E5-E7 exhibits a larger discharge plateau in the voltage range of 0.75-1.0V when charged for the first time than E1, and the irreversible capacities of the E5-E7 electrolyte HC half cell are 104.7, 98.8 and 120.8mAh/g, respectively.
Fig. 2 is a graph of differential capacity obtained according to fig. 1, and it can be seen from fig. 2 that the peak potentials corresponding to the different electrolytes are different in addition to the common peak around about 0.25V. For E1, the curve has two smaller peaks at about 0.65 and 0.85V. For electrolytes with both additives, liDFOB and LiBOB, which have coincident peaks at about 0.84V, the curve for the LiDFOB-containing electrolyte is steeper than the curve for the LiBOB-containing electrolyte at voltages below 0.84V. For an electrolyte containing LiBF 4, the curve has two smaller peaks at about 0.78 and 0.97V, with peak voltages higher than E1. Of the 3 salt additives, liBF 4 had the highest coulombic efficiency for the first circle, followed by LiBOB and LiBOB.
Fig. 3 is a graph showing EIS of HC negative electrode as a function of voltage during first charge at room temperature, measured using three electrode button. When charged from an open state to 0.9 or 0.8V, the impedance change is small, remains substantially at a high level, and the EIS curve starts to become regular. When charged to 0.6V, the impedance is significantly reduced by orders of magnitude compared to when at high potential. When charging is continued to 0.4V, the impedance is again significantly reduced by orders of magnitude. Thereafter, the decreasing trend begins to slow down. As the charging proceeds, the impedance further decreases when charging to 0.2V, reaching a minimum at 0.01V.
As can be seen from fig. 3 (b, d, f) for lithium salt additives, the trend exhibited by the 3 additive cells is different. For LiDFOB and LiBF 4, the impedance changes less than 0.01V at voltages below 0.6V, and the first semicircle is slightly larger than the second semicircle, and the second semicircle and overall impedance begin to increase at voltages above 0.6V. For LiBOB, it can be seen that its first semicircle is always larger than the second semicircle. It is noted that at the end of the initial charge, the different electrolyte HC impedances are E1, E6, E5, E7 in order from small to large, but as the discharge proceeds, the E1 electrolyte HC impedance increases significantly with increasing voltage, while the E5 electrolyte HC impedance is substantially unchanged, and during the discharge, the HC impedances are E6, E1, E5, E7 in order from small to large.
Fig. 4 is a graph showing the rate performance of HC half cells using different electrolytes at different temperatures. As can be seen from fig. 4, the rate performance of HC is improved when the electrolyte containing the additive is used, compared with the electrolyte containing no additive, and even at-40 ℃, the electrolyte HC half cell containing no additive has no capacity, and the electrolyte HC half cell containing LiBF 4 or lifob still has certain performance. Of the 3 salt additives, liBF 4 exhibited the best rate performance at different temperatures, as shown in fig. 4 (a-d), the performance of the HC half cell containing the LiBF ob electrolyte was inferior to LiBF 4, even slightly superior to LiBF 4 at-20 ℃, while the performance of LiBOB was worse than the former two, and the cell had no capacity at-40 ℃ as the cell without the additive electrolyte. In general, liBF 4 and LiBOB have a certain effect on improving battery performance, liBF 4 has the best effect on improving performance at different temperatures, liBOB times, and LiBOB has a poor effect on improving low temperature performance.
Fig. 5 is a graph showing the rate performance of an LIC full cell using different electrolytes at-20 ℃. As can be seen from FIG. 5, the gradient of the performance distribution of LIC using different electrolytes is more remarkable at-20deg.C, and, unlike the LiDFOB-containing electrolyte HC half cell of FIG. 4 (c), the LiBF 4 electrolyte performance is significantly better than that of LiDFOB-containing electrolyte HC half cell of FIG. 4 (c), the discharge specific capacity of the LIC full cell is mainly limited to AC positive electrode rather than HC negative electrode, and for AC positive electrode, anion adsorption and desorption are mainly performed at charge and discharge, possibly becauseThe ion size is smaller than DFOB - ions, and the pore size distribution of the electrolyte is coordinated with that of the AC, so that in the LIC full battery, the performance of the LiBF 4 electrolyte is obviously better than that of LiDFOB. From the performance data of full and half cells, we infer that the improvement of LIC low temperature performance by lifob is probably mainly from its anionsThe portion of the ion.
The influence of all additives on LIC performance can be comprehensively compared, and other additives except LiBOB can improve the LIC multiplying power performance to different degrees at normal temperature, and the effects are as follows: liBF 4 and LiDFOB, but the additive has an improvement effect on the low-temperature performance of LIC, the ordering is that LiBF 4、LiDFOB.LiBF4 has the best effect, and for HC half batteries, the specific capacity of about 57mAh/g is still maintained at the current density of 0.02A/g even at the temperature of minus 40 ℃; for LIC full cells, the specific capacity was about 18.5mAh/g at a current density of 0.02A/g at-20deg.C, and the capacity retention was 62.71% compared to the same current density at room temperature.
Fig. 6 shows the resistance of the HC negative electrode at 0.4V at different temperatures measured with a three electrode button cell. As can be seen from fig. 6, although the HC half-cell containing LiBOB electrolyte has the highest irreversible capacity in the first cycle of formation, it has a poor impedance-reducing effect, much less than the case of the lipob and LiBF 4, at 25 c, the impedance is even higher than without the additive, and as the temperature decreases, the effect of decreasing the impedance gradually emerges, but still far less than LiDFOB and LiBF 4.
Fig. 7 (a) and (b) are SEI film resistance and charge transfer resistance data at different temperatures at 0.4V for an HC negative electrode fitted according to an equivalent circuit model. And further bringing the impedance data obtained by fitting into an Arrhenius formula, and obtaining activation energy data of two impedance corresponding processes, as shown in (c) and (d) of FIG. 7. In the process of the diffusion of the desolvated lithium ions through the SEI film, the activation energy of the four electrolytes is 7.65, 18.81, 23.90 and 48.44kJ/mol respectively. For the charge transfer process corresponding to R ct, the activation energy is obviously larger than that of the former, and the activation energy of the four electrolytes is 66.18, 59.98, 57.53 and 63.71kJ/mol respectively.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. The electrolyte containing the lithium salt additive is characterized by comprising lithium salt, the lithium salt additive and a low-temperature solvent, wherein the lithium salt additive is LiDFOB, liBF 4 or LiBOB, and the low-temperature solvent is a mixture of ethylene carbonate, ethylmethyl carbonate and toluene.
2. The electrolyte containing a lithium salt additive according to claim 1, wherein the lithium salt is LiPF 6.
3. The electrolyte containing a lithium salt additive according to claim 1, wherein the concentration of the lithium salt in the electrolyte is 1.1 to 1.3mol/L.
4. The electrolyte containing a lithium salt additive according to claim 1, wherein the concentration of the lithium salt in the electrolyte is 1.2mol/L.
5. The electrolyte containing lithium salt additive according to claim 1, wherein the concentration of the lithium salt additive in the electrolyte is 0.08-0.12 mol/L.
6. The electrolyte containing a lithium salt additive according to claim 5, wherein the concentration of the lithium salt additive in the electrolyte is 0.1mol/L.
7. The electrolyte containing lithium salt additive according to claim 1, wherein the volume ratio of the ethylene carbonate, the ethylmethyl carbonate and the toluene is 1: (0.8-1.2): (2.5-3.5).
8. The electrolyte containing lithium salt additive according to claim 7, wherein the volume ratio of the ethylene carbonate, the ethylmethyl carbonate and the toluene is 1:1:3.
9. The method for preparing an electrolyte containing a lithium salt additive according to any one of claims 1 to 8, wherein the lithium salt and the lithium salt additive are weighed and mixed with a low-temperature solvent to obtain the electrolyte.
10. Use of an electrolyte comprising a lithium salt additive according to any one of claims 1-8 in a lithium ion capacitor.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410580413.5A CN118610009A (en) | 2024-05-11 | 2024-05-11 | Electrolyte containing lithium salt additive and preparation and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410580413.5A CN118610009A (en) | 2024-05-11 | 2024-05-11 | Electrolyte containing lithium salt additive and preparation and application thereof |
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| CN118610009A true CN118610009A (en) | 2024-09-06 |
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| CN202410580413.5A Pending CN118610009A (en) | 2024-05-11 | 2024-05-11 | Electrolyte containing lithium salt additive and preparation and application thereof |
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