CN112687956A - Non-aqueous electrolyte of lithium battery and lithium ion battery based on same - Google Patents
Non-aqueous electrolyte of lithium battery and lithium ion battery based on same Download PDFInfo
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Abstract
The invention relates to a non-aqueous electrolyte of a lithium battery and a lithium ion battery based on the non-aqueous electrolyte, wherein the characteristic that the number of central atoms of lithium difluorobis (oxalate) phosphate of a lithium salt additive is large is utilized to be matched with the characteristic that fluorobenzene improves the infiltration capacity of the electrolyte, the oxidation potential of a mixed electrolyte of fluorobenzene and lithium difluorobis (oxalate) phosphate is controlled, the film forming additive can be decomposed at a negative electrode and is kept stable at a positive electrode, so that the effect of the low-impedance film forming additive is better exerted, materials are protected, lithium precipitation is inhibited, the thickness and the stability of a surface film of the electrode are controlled, the increase of the cycle impedance can be inhibited in the long term, and the performances of low-impedance increase and long cycle at different.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a non-aqueous electrolyte of a lithium battery and the lithium ion battery based on the non-aqueous electrolyte.
Background
The lithium ion battery has the advantages of high specific energy, no memory effect, long cycle life and the like, so that the lithium ion battery is generally applied to the field of 3C consumer electronics products such as mobile phones and notebook computers, and in addition, along with the rapid development of new energy automobiles, the application of the lithium ion battery in the fields of power and energy storage is more and more common. With the increase of the endurance mileage of the electric vehicle and the gradual decrease of national subsidies, the requirement on the energy density of the power battery is higher and higher, and at present, the effective methods are to improve the voltage and the compaction density of the electrode active material and select a proper electrolyte.
In order to increase the capacity of the battery, the use of a high-voltage cathode material is an effective way to increase the capacity density of the lithium ion battery, and at high voltage, the electrolyte is easily decomposed, the additive is gradually reduced, the internal resistance of the battery is increased and a large amount of heat is generated along with the continuous charging of the battery, and the cycle life is generally deteriorated after many charging and discharging cycles.
Therefore, it is particularly important to develop more and more novel electrolytes matched with high-voltage cathode materials.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a non-aqueous electrolyte of a lithium battery, which realizes the control of the thickness and stability of a surface film of an electrode by using lithium difluorobis (oxalato) phosphate and fluorobenzene as additives, and further realizes the performance of low impedance growth and long cycle at different temperatures.
The first object of the present invention is to provide a nonaqueous electrolytic solution for a lithium battery, comprising an electrolyte lithium salt, a nonaqueous organic solvent and an additive, characterized in that the additive comprises fluorobenzene and lithium difluorobis (oxalato) phosphate;
the oxidation potential of the fluorobenzene and lithium difluorobis (oxalato) phosphate mixed electrolyte is 4.35-5.1V, and the reduction potential is 0.1-0.5V.
Further, the additive also comprises one or more of 1, 3-propane sultone, fluoroethylene carbonate, ethylene sulfate and vinylene carbonate.
Further, the content of the electrolyte lithium salt is 10-20% of the total mass of the electrolyte.
Further, the electrolyte lithium salt is selected from lithium hexafluorophosphate (LiPF)6) Lithium difluorophosphate (LiPO)2F2) Lithium bis (fluorosulfonylimide) (LiFSI) or bis (trifluoromethanesulfonylimide)Lithium amine (LiTFSI), lithium tetrafluoroborate (LiBF)4) One or more of them.
Further, the non-aqueous organic solvent is selected from one or more of a linear carbonate solvent, a cyclic carbonate solvent, a carboxylic acid ester solvent, and a fluorinated carbonate solvent.
Further, the straight-chain carbonate solvent is selected from one or more of ethyl methyl carbonate, dimethyl carbonate and diethyl carbonate; the cyclic carbonate solvent is selected from one or more of ethylene carbonate and propylene carbonate; the carboxylic ester solvent is selected from one or more of ethyl acetate, ethyl propionate, methyl propionate, propyl butyrate and propyl acetate; the fluorinated carbonate solvent is selected from one or more of fluorinated ethylene carbonate, 1, 2-difluoroethylene carbonate, methyl trifluoroethyl carbonate and bis trifluoroethyl carbonate.
The second purpose of the invention is to provide the application of the electrolyte in the preparation of a lithium ion battery, wherein the charging voltage of the lithium ion battery is less than 5.5V.
A third object of the present invention is to provide a lithium ion battery comprising: a positive electrode, a negative electrode, a separator between the positive electrode and the negative electrode, and the electrolyte;
the positive electrode includes a positive electrode active material;
the negative electrode comprises a negative current collector and a negative diaphragm arranged on the negative current collector, and the negative diaphragm comprises a negative active material, a negative conductive agent and a binder.
Further, the positive active material is selected from one or more of lithium cobaltate, lithium nickelate, lithium manganate, lithium vanadate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel manganese oxide, lithium cobalt manganese manganate, lithium-rich manganese-based material and ternary positive material, and the structural formula of the ternary positive material is LiNi1-x-y-zCoxMnyAlzO2Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and x + y + z is more than or equal to 0 and less than or equal to 1.
Further, the negative active material is selected from one or more of artificial graphite, natural graphite, silicon-oxygen compound, silicon-based alloy and active carbon; the negative electrode conductive agent is selected from one or more of acetylene black, conductive carbon black, carbon fiber, carbon nanotube and Ketjen black.
Further, the kind of the diaphragm is not particularly limited and may be selected according to actual requirements. Preferably, the diaphragm comprises a base film and a nano alumina coating coated on the base film, wherein the base film is at least one of PP, PE and PET, and the thickness of the nano alumina coating is 1.0-6.0 μm.
In the invention, the high-voltage non-aqueous electrolyte refers to a non-aqueous electrolyte suitable for a lithium ion battery under a high-voltage condition, and the high voltage specifically refers to a charging voltage of 4.1-5.5V.
The matching principle and the action of all substances in the lithium ion battery electrolyte are as follows:
in the process of charging and discharging of the lithium ion battery, main components and additives in the electrolyte can be decomposed and polymerized on the surfaces of a positive electrode and a negative electrode, and a polymer with large molecular weight can be separated out on the surface of the electrode and wraps the generated inorganic lithium salt to form a solid electrolyte membrane which can isolate the electrolyte and can conduct ions. The electrolyte formed by the electrolyte solvent is thick and loose, and is difficult to protect and isolate the electrolyte, so that the electrolyte can be thickened continuously, the battery impedance is increased, and continuous electrolyte loss is brought. According to the invention, the characteristic that the lithium difluorobis (oxalate) phosphate as a lithium salt additive has a large number of central atoms is utilized, the characteristic that fluorobenzene improves the infiltration capacity of an electrolyte is matched for use, the oxidation potential of fluorobenzene and lithium difluorobis (oxalate) phosphate mixed electrolyte is controlled, the film forming additive can be decomposed at a negative electrode, and the film forming additive can be kept stable at a positive electrode, so that the effect of the low-impedance film forming additive is better exerted, materials are protected, lithium precipitation is inhibited, the thickness and the stability of a surface film of an electrode are controlled, the increase of the circulating impedance can be inhibited in a long term, and the low-impedance increase and long-circulating performance at different temperatures.
By the scheme, the invention at least has the following advantages:
according to the invention, the characteristic that the lithium difluorobis (oxalate) phosphate as a lithium salt additive has a large number of central atoms is utilized, the characteristic that fluorobenzene improves the infiltration capacity of an electrolyte is matched for use, the oxidation potential of fluorobenzene and lithium difluorobis (oxalate) phosphate mixed electrolyte is controlled, the film forming additive can be decomposed at a negative electrode, and the film forming additive can be kept stable at a positive electrode, so that the effect of the low-impedance film forming additive is better exerted, materials are protected, lithium precipitation is inhibited, the thickness and the stability of a surface film of an electrode are controlled, the increase of the circulating impedance can be inhibited in a long term, and the low-impedance increase and long-circulating performance at different temperatures.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a preferred embodiment of the present invention and is described in detail below.
Detailed Description
In the present invention, the electrolyte solution includes an electrolyte lithium salt selected from lithium hexafluorophosphate (LiPF), a non-aqueous organic solvent and an additive6) Lithium difluorophosphate (LiPO)2F2) Lithium bis (fluorosulfonylimide) (LiFSI), lithium bis (trifluoromethanesulfonylimide) (LiTFSI), and lithium tetrafluoroborate (LiBF)4) The non-aqueous organic solvent is selected from one or more of a straight-chain carbonate solvent, a cyclic carbonate solvent, a carboxylic ester solvent and a fluorinated carbonate solvent, and the additive comprises 1, 3-propane sultone PS, difluorophenyl FB and difluorobis lithium oxalate phosphate LiODFP; the lithium fluobenzene and difluoro-bis-oxalate phosphate mixed electrolyte has an oxidation potential of 4.35-5.1V and a reduction potential of 0.1-0.5V, and further comprises one or more of fluoroethylene carbonate FEC, ethylene sulfate DTD and vinylene carbonate VC.
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The lithium ion secondary battery of the present invention is prepared by:
LiNi as positive electrode active material0.5Co0.2Mn0.3O2(LNCM), conductive agent acetylene black and adhesive polyvinylidene fluoride (PVDF) according to the mass ratio of 95: 3: 2Fully stirring and uniformly mixing the mixture in an N-methylpyrrolidone solvent system, coating the mixture on an aluminum foil, drying and cold pressing the mixture to obtain the positive pole piece, wherein the compaction density of the positive pole piece is 3.45g/cm3。
Fully stirring and uniformly mixing a negative active material graphite, a conductive agent acetylene black, a binder Styrene Butadiene Rubber (SBR) and a thickening agent sodium carboxymethyl cellulose (CMC) in a deionized water solvent system according to a mass ratio of 96: 2: 1, coating the mixture on a Cu foil, drying and cold pressing to obtain a negative pole piece, wherein the compaction density of the negative pole piece is 1.65g/cm3。
Polyethylene (PE) with the thickness of 9 mu m is taken as a base film, and a nano aluminum oxide coating layer with the thickness of 3 mu m is coated on the base film to obtain the diaphragm.
And stacking the positive and negative pole pieces and the diaphragm made of polyethylene in a negative pole, diaphragm, positive pole and diaphragm mode, and ending with the negative pole to obtain the bare cell.
And (3) carrying out hot pressing on the naked electric core to ensure that polyvinylidene fluoride (PVDF) on the surface of the diaphragm bonds the pole pieces together. And (3) welding the lugs of the hot-pressed bare cell, placing the bare cell in an aluminum plastic film with a punched pit, and carrying out hot-melt packaging to obtain the pre-packaged battery with a liquid injection port. And (3) placing the pre-packaged battery in a vacuum furnace for fully baking and drying, injecting corresponding electrolyte from the liquid injection port, and packaging the liquid injection port in a vacuum environment to obtain the secondary battery.
The secondary battery of the present invention can be tested by the following method:
(1) initial discharge capacity and cycle test of secondary battery
The prepared battery is aged and placed on a clamp, the activated battery is charged to 4.3V at 25 ℃ by using a current of 1C, the voltage is constant to 0.05C, the battery is discharged to 2.8V by using 1C, and the discharge capacity is recorded. And recording initial DCR of the battery after the first circle of discharge, then performing a cycle test until the discharge capacity of the battery is 80% of the first circle of capacity, and recording the DCR, the increase rate of the DCR, the number of turns of the battery reaching 80% SOH (state of health of the battery) and the change of gas production volume of the battery after the cycle is finished.
Wherein the change in the direct current resistance of the secondary battery and the volume of the generated gas are measured by the following methods, respectively:
(i) direct Current Resistance (DCR) test of secondary battery
When the battery is discharged to 50% SOC (state of charge, reflecting the residual capacity of the battery) at a specified temperature by 1C current, the current is increased to 4C and kept for 30s, the difference between the updated stable voltage and the original platform voltage is detected, and the ratio of the value to the 3C current value is the direct current resistance of the battery. And comparing the DCR after the cycle is ended with the DCR at the beginning of the cycle to obtain the increase rate of the DCR.
(ii) Volume change test of gas generated by secondary battery
Fixing the secondary battery with a string, completely soaking the secondary battery in water at 25 ℃, recording the weight difference before and after soaking, and converting the weight difference into the volume difference according to the density of the water at 25 ℃.
(2) Capacity recovery test of secondary battery at 60 deg.C
After aging treatment of examples 5, 6, 7 and comparative example 2, the activated battery was charged to 4.3V at 25 ℃ with a current of 1C and was constant-voltage to a current of 0.05C. The secondary battery was placed in an environment at 60 ℃ for 60 days, and the capacity recovery rate was recorded for 60 days.
(3) Cycle test of secondary battery at 60 deg.C
After aging treatment of examples 5, 6 and 7 and comparative examples 2 and 3, the activated cell was charged to 4.25V at 60 ℃ with a current of 1C, and was constant-voltage to a current of 0.05C, and then discharged to 3.0V at 1C, and the discharge capacity was recorded. And recording initial DCR of the battery after the first circle of discharge, then performing a cycle test until the discharge capacity of the battery is 80% of the first circle of capacity, and recording the DCR, the increase rate of the DCR and the gas production volume change of the battery after the cycle is finished.
Low temperature discharge test
The full-state battery after capacity separation was discharged to 3.0V at 25 ℃ at 1C, and the initial discharge capacity was recorded as DC (25 ℃). Then, the mixture was charged to 4.2V at 25 ℃ at a constant current and a constant voltage of 1C, and the current was cut off at 0.05C. The temperature is reduced to minus 20 ℃ and the mixture is kept for 4 hours, then the mixture is discharged to 3.0V at 1C, and the discharge capacity DC (-20 ℃) is recorded. The low-temperature discharge capacity retention rate was 100% DC (-20 ℃)/DC (25 ℃).
The corresponding electrolyte above was prepared according to the following examples:
example 1:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 12% of LiPF6 and 1.5% of LiPO which are calculated according to the total mass of the finished electrolyte2F21% LiFSI, 0.5% VC, 0.5% PS, 5% FB and 0.5% LiODFP, and uniformly mixing to obtain the electrolyte, wherein the oxidation potential of the mixed electrolyte of fluorobenzene and lithium difluorobis (oxalate) phosphate is between 4.45V, and the reduction potential is 0.2V.
Comparative example 1:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 12% of LiPF6 and 1.5% of LiPO which are calculated according to the total mass of the finished electrolyte2F21% LiFSI, 2% VC and 0.5% PS, and uniformly mixing to obtain the electrolyte.
Comparative example 2:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 12% of LiPF6 and 1.5% of LiPO which are calculated according to the total mass of the finished electrolyte2F21% LiFSI, 0.5% VC, 0.5% PS and 10% FB, and uniformly mixing to obtain the electrolyte.
Comparative example 3:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 12% of LiPF6 and 1.5% of LiPO which are calculated according to the total mass of the finished electrolyte2F21% LiFSI, 0.5% VC, 0.5% PS and 1% LiODFP, and uniformly mixing to obtain the electrolyte.
The results of the electrical property tests of the different lithium ion batteries in example 1 and comparative examples 1 to 3 are shown in table 1, and the charge cut-off voltage of each lithium ion secondary battery was 4.4V. The result shows that the lithium difluorobis (oxalate) phosphate and fluorobenzene are used in a matching manner, the effect of the low-impedance film forming additive can be more effectively exerted, and the performances of low-impedance growth and long circulation at different temperatures are realized.
TABLE 1 test results of electrical properties of different lithium ion batteries
Example 2:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 12% of LiPF6 and 1% of LiPO which are calculated according to the total mass of the finished electrolyte2F21% LiFSI, 1% LiTFSI, 1.5% DTD, 0.5% VC, 1% PS, 10% FB and 0.5% LiODFP, and uniformly mixing to obtain an electrolyte, wherein the oxidation potential of the mixed electrolyte of fluorobenzene and lithium difluorobis (oxalate) phosphate is between 4.58V, and the reduction potential is 0.3V.
Example 3:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 6 parts of EMC, 1 part of DEC and 4 parts of PC/Add into a non-aqueous organic solvent, and adding 13% LiPF6 and 1% LiPO which are obtained according to the total mass of the finished electrolyte2F2、0.4％LiBF4And uniformly mixing 0.5% of DTD, 0.5% of VC, 1% of PS, 15% of FB and 0.5% of LiODFP to obtain the electrolyte, wherein the oxidation potential of the mixed electrolyte of fluorobenzene and lithium difluorobis (oxalato) phosphate is 4.81V, and the reduction potential is 0.2V.
Example 4:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 13% of LiPF6 and 1% of LiPO which are calculated according to the total mass of the finished electrolyte2F2And 0.5% of LiODFB, 3% of FEC, 0.5% of PS, 5% of FB and 0.5% of LiODFP, and uniformly mixing to obtain the electrolyte, wherein the oxidation potential of the mixed electrolyte of fluorobenzene and lithium difluorobis (oxalate) phosphate is 4.55V, and the reduction potential is 0.1V.
Comparative example 4:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 5 parts of EMC and 2 parts of DEC to obtain a non-aqueous organic solvent, and adding 13% of LiPF6 and 1% of LiPO which are calculated according to the total mass of the finished electrolyte2F23% of FEC, 1% of PS and 0.5% of LiODFB, and uniformly mixing to obtain the electrolyte.
Comparative example 5:
the preparation steps of the electrolyte are as follows:
mixing 3 parts of EC, 6 parts of EMC, 1 part of DEC and 4 parts of PC/Add into a non-aqueous organic solvent, and adding 13.5 percent LiPF6 and 1 percent LiPO which are calculated according to the total mass of the finished electrolyte2F2、0.4％LiBF40.5% of DTD, 0.5% of VC and 0.5% of PS are uniformly mixed to obtain the electrolyte.
The results of the electrical property tests of the different lithium ion batteries of examples 2 to 4 and comparative examples 4 and 5 are shown in table 2, and the charge cut-off voltage of each lithium ion secondary battery was 4.4V. The results also indicate that.
TABLE 2 test results of electrical properties of different lithium ion batteries
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A non-aqueous electrolyte for a lithium battery, comprising an electrolyte lithium salt, a non-aqueous organic solvent and an additive, wherein the additive comprises fluorobenzene and lithium difluorobis (oxalato) phosphate;
the oxidation potential of the fluorobenzene and lithium difluorobis (oxalato) phosphate mixed electrolyte is 4.35-5.1V, and the reduction potential is 0.1-0.5V.
2. The nonaqueous electrolytic solution of claim 1, wherein the additive further comprises one or more of 1, 3-propanesultone, fluoroethylene carbonate, ethylene sulfate, and vinylene carbonate.
3. The high-voltage nonaqueous electrolytic solution of claim 1, wherein the content of the electrolytic lithium salt is 10 to 20% by mass of the total mass of the electrolytic solution.
4. The nonaqueous electrolytic solution of claim 2, wherein the electrolyte lithium salt is one or more selected from lithium hexafluorophosphate, lithium difluorophosphate, lithium bis-fluorosulfonylimide, lithium bis-trifluoromethanesulfonylimide, and lithium tetrafluoroborate.
5. The nonaqueous electrolytic solution of claim 1, wherein the nonaqueous organic solvent is one or more selected from a linear carbonate-based solvent, a cyclic carbonate-based solvent, a carboxylic acid-based solvent, and a fluorinated carbonate-based solvent.
6. The nonaqueous electrolytic solution of claim 5, wherein the linear carbonate-based solvent is one or more selected from ethyl methyl carbonate, dimethyl carbonate, and diethyl carbonate; the cyclic carbonate solvent is selected from one or more of ethylene carbonate and propylene carbonate; the carboxylic ester solvent is selected from one or more of ethyl acetate, ethyl propionate, methyl propionate, propyl butyrate and propyl acetate; the fluorinated carbonate solvent is selected from one or more of fluorinated ethylene carbonate, 1, 2-difluoroethylene carbonate, methyl trifluoroethyl carbonate and bis trifluoroethyl carbonate.
7. Use of the nonaqueous electrolytic solution according to any one of claims 1 to 6 for producing a lithium ion battery, wherein a charging voltage of the lithium ion battery is 5.5V or less.
8. A lithium ion battery, comprising: a positive electrode, a negative electrode, a separator between the positive electrode and the negative electrode, and the nonaqueous electrolytic solution of any one of claims 1 to 6;
the positive electrode includes a positive electrode active material;
the negative electrode comprises a negative current collector and a negative diaphragm arranged on the negative current collector, and the negative diaphragm comprises a negative active material, a negative conductive agent and a binder.
9. The lithium ion battery of claim 8, wherein the positive active material is selected from one or more of lithium cobaltate, lithium nickelate, lithium manganate, lithium vanadate, lithium iron phosphate, lithium iron manganese phosphate, lithium nickel manganate, lithium cobalt manganate, lithium manganese rich-based material and ternary positive material, and the ternary positive material has a structural formula of LiNi1-x-y-zCoxMnyAlzO2Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and x + y + z is more than or equal to 0 and less than or equal to 1.
10. The lithium ion battery of claim 8, wherein the negative active material is selected from one or more of artificial graphite, natural graphite, silicon-oxygen compound, silicon-based alloy and activated carbon; the negative electrode conductive agent is selected from one or more of acetylene black, conductive carbon black, carbon fiber, carbon nanotube and Ketjen black.
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| CN116072829A (en) * | 2021-11-02 | 2023-05-05 | 宁德时代新能源科技股份有限公司 | Positive electrode active material, method for preparing same, lithium ion battery including same, battery module, battery pack, and power device |
| CN117096442A (en) * | 2023-09-26 | 2023-11-21 | 三一红象电池有限公司 | Lithium ion battery electrolyte and lithium ion battery |
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