CN113745661B - High-voltage electrolyte matched with ternary cathode material lithium ion battery - Google Patents
High-voltage electrolyte matched with ternary cathode material lithium ion battery Download PDFInfo
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Abstract
The invention discloses a high-voltage electrolyte matched with a ternary anode material lithium ion battery, which comprises lithium fluorophosphate, lithium difluorooxalate phosphate, a non-aqueous solvent, a cathode film-forming additive ethylene vinylene carbonate and an anode film-forming additive diisopropyl cyano phosphine. The diisopropyl cyano phosphine can inhibit the decomposition of the electrolyte under high voltage, so that the electrolyte can keep stable performance when working under higher voltage, and an interface film which is stable under high voltage is formed. The ethylene vinylene carbonate promotes lithium difluorooxalate phosphate to decompose to form lithium fluoride which is uniformly embedded into the SEI film, the formed SEI film has low impedance and good conductivity, and the low-temperature performance and the cycle life of the battery are improved; when the lithium ion battery prepared by the high-voltage electrolyte matched with the ternary cathode material lithium ion battery is used under the charge cut-off voltage of 4.5V, the lithium ion battery still has good cycle performance, high-temperature performance and low-temperature performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a high-voltage electrolyte matched with a ternary cathode material lithium ion battery.
Background
Lithium ion batteries dominate the high energy application market. With the continuous increase of energy density of lithium ion batteries, conventional LiNi1/3Co1/3Mn1/3O2（NCM111）、LiNi0.5Co0.2Mn0.3O2(NCM 523) and other medium-low nickel ternary materials cannot meet the requirement of high specific energy batteries, and two methods are mainly used for improving the capacity of the ternary materials: increasing nickel content and increasing charge cut-off voltage. However, increasing the nickel content increases the difficulty of preparing ternary materials and increases the manufacturing cost, so in recent years, increasing the charge voltage of materials such as NCM111 and NCM523 has become the mainstream method for increasing the energy density of batteries.
At the usual lower charge cut-off potential (e.g.. ltoreq.4.3V vs Li | Li+) The lithium extracted by NCM is limited. Improvement ofAn important method for improving the specific capacity of the low-nickel (Ni is less than or equal to 60%) NCM positive electrode is to improve the charge cut-off voltage of the battery so that the lithium removal degree of the battery is higher. However, in the battery under high voltage, due to the change of the structure of the positive electrode material, the change of the electrolyte interface, and the like, the capacity attenuation of the battery is severe, for example, when the charge cut-off voltage of the lithium ion battery is increased to 4.5V, the cycle performance of the lithium ion battery is obviously deteriorated, and the high-temperature performance and the low-temperature performance of the battery are also poor.
Disclosure of Invention
The purpose of the invention is as follows: the high-voltage electrolyte matched with the ternary cathode material lithium ion battery is provided, so that the lithium ion battery still has good cycle performance, high-temperature performance and low-temperature performance when being used under the charge cut-off voltage of up to 4.5V.
The technical scheme of the invention is as follows:
a high-voltage electrolyte matched with a ternary anode material lithium ion battery comprises a lithium salt, a non-aqueous solvent, a cathode film-forming additive and an anode film-forming additive; the lithium salt comprises lithium hexafluorophosphate and lithium difluorooxalate phosphate, the negative electrode film forming additive is ethylene vinylene carbonate, the positive electrode film forming additive is diisopropyl cyanophosphine, and the structural formula of the diisopropyl cyanophosphine is as follows:
(ii) a The mass of the negative electrode film-forming additive accounts for 0.3-2% of the total mass of the electrolyte, and the mass of the positive electrode film-forming additive accounts for 0.5-3% of the total mass of the electrolyte.
The high-voltage electrolyte of the lithium ion battery matched with the ternary cathode material contains the cathode film-forming additive, and the cathode film-forming additive, namely the diisopropylcyanophosphine, can inhibit the oxidative decomposition of the electrolyte under high voltage, widens the working voltage window of the electrolyte, and ensures that the lithium ion battery prepared from the electrolyte keeps stable performance when working under higher voltage. In addition, the positive electrode electrolyte interfacial film (CEI film for short) containing phosphorus formed by the diisopropylcyanophosphine has good stability on the surface of the positive electrode, and the direct contact between the electrode and the electrolyte can be effectively reduced even under high voltage, so that the decomposition of the electrolyte is effectively inhibited, and the dissolution of transition metal ions and the damage of a positive electrode material are weakened.
The negative electrode film forming additive ethylene vinylene carbonate can be decomposed at 1.35V in the formation and charging process of the battery, and an organic negative electrode electrolyte interface film (SEI film for short) is formed on a graphite negative electrode, and the organic SEI film can effectively obstruct and filter electrolyte organic molecules combined with lithium ions, effectively prevent solvated lithium ions from contacting with negative electrode graphite and being embedded into an interlayer structure of the graphite, and prevent the electrolyte from being gradually decomposed at the negative electrode in the circulating process through solvated lithium ion forms. Also, such an organic SEI film has a large resistance, which causes lithium ions to be reduced on the surface of a negative electrode and to precipitate lithium when the battery is used at low temperatures, resulting in deterioration of low-temperature performance of the battery. The ethylene vinylene carbonate can promote the rupture of the fluorophosphate bond in the lithium difluorooxalate, the negative electrode film-forming additive ethylene vinylene carbonate and the lithium difluorooxalate are simultaneously used in the electrolyte of the invention, lithium fluoride formed by the cleavage of a fluorophosphate bond in lithium difluorooxalato phosphate can be inserted into the SEI film containing P-O-C and uniformly distributed while the vinylene carbonate forms the organic SEI film, so that the content of inorganic components in the formed organic SEI film is higher, the formed SEI film formed by orderly combining the inorganic components and the organic components is more stable, the SEI film containing the lithium fluoride has better ion conductivity and lower impedance, can effectively prevent the electrolyte from directly contacting with the cathode, and the conductivity is good, lithium ions are not easy to be separated out on the surface of the negative electrode to form lithium dendrites, and the low-temperature performance of the battery is improved. In addition, the lithium difluorooxalate phosphate can also effectively reduce the viscosity of the electrolyte and improve the conductivity of the electrolyte. Lithium hexafluorophosphate and lithium difluorooxalato phosphate are used simultaneously, so that an SEI film and a CEI film which are stable and fast in lithium ion conduction and contain inorganic and organic components can be formed on the positive electrode and the negative electrode synergistically, side reactions of the interface of the battery during working under high voltage are reduced, and the cycle life of the ternary positive electrode material during use under high voltage is effectively prolonged.
The mass of the negative electrode film forming additive accounts for 0.3-2% of the total mass of the electrolyte. 0.3 to 2 percent of the negative electrode film forming additive can form a complete and effective SEI film and can not remain in the electrolyte too much.
Preferably, the mass of lithium hexafluorophosphate in the lithium salt accounts for 13.0% of the total mass of the electrolyte, and the mass of lithium difluorooxalato phosphate accounts for 0.5% -2.5% of the total mass of the electrolyte. The proportion of 13.0 percent of lithium hexafluorophosphate and 0.5 to 2.5 percent of lithium difluorooxalate phosphate is kept, so that the inlaying proportion of the formed lithium fluoride inorganic component and the organic SEI film is proper and uniform.
Preferably, the nonaqueous solvent is a cyclic carbonate or a linear carbonate.
Preferably, the linear carbonate is a mixture of ethyl methyl carbonate and diethyl carbonate.
Preferably, the nonaqueous solvent is a mixture of ethyl methyl carbonate and diethyl carbonate in a mass ratio of 1:5: 7. The non-aqueous solvent prepared according to the proportion has lower content of ethylene carbonate, is beneficial to low-temperature charge and discharge of the battery, and improves the low-temperature performance of the battery; and the mixed use of the three can improve the thermodynamic stability of the electrolyte under high voltage and has good conductivity.
The invention has the beneficial effects that:
according to the high-voltage electrolyte matched with the ternary cathode material lithium ion battery, the cathode film forming additive of the diisopropyl cyanophosphine can inhibit the oxidative decomposition of the electrolyte under high voltage, so that the electrolyte can keep stable performance when working under higher voltage, and an interface film which is still stable under high voltage can be formed on the surface of the cathode, thereby weakening the dissolution of transition metal and the damage of the cathode material. The ethylene vinylene carbonate serving as a negative electrode film forming additive promotes the fluorine phosphorus bond in the lithium difluorooxalate to be broken, and the formed lithium fluoride is uniformly embedded into an SEI film containing P-O-C, so that the formed stable SEI film with sequentially combined inorganic and organic components has low impedance and good conductivity, the low-temperature performance of the battery is improved, and the cycle life of the battery is prolonged; therefore, the high-voltage electrolyte of the lithium ion battery prepared by the high-voltage electrolyte of the matched ternary cathode material lithium ion battery still has good cycle performance, high-temperature performance and low-temperature performance when the high-voltage electrolyte of the lithium ion battery is used under the charge cut-off voltage of 4.5V.
Detailed Description
The present invention will be described in detail with reference to examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
1. Preparing a high-voltage electrolyte matched with a ternary cathode material lithium ion battery:
in a glove box (with the water content less than 0.1ppm and the oxygen content less than 0.1ppm) filled with argon, ethylene carbonate, ethyl methyl carbonate and diethyl carbonate are uniformly mixed according to the mass ratio of 1:5:7 to prepare a non-aqueous solvent, 0.5 percent of diisopropylcyanophosphine, 1.0 percent of ethylene vinylene carbonate and 1.5 percent of lithium difluorobis (oxalato) phosphate based on the total mass of the electrolyte are added into the non-aqueous solvent, then 13.0 percent of lithium hexafluorophosphate based on the total mass of the electrolyte is slowly added into the non-aqueous solvent, and the mixture is stirred until the lithium hexafluorophosphate is completely dissolved, so that the high-voltage electrolyte matched with the ternary cathode material lithium ion battery is obtained.
2. Battery fabrication
And injecting the prepared high-voltage electrolyte matched with the ternary anode material lithium ion battery into a 2Ah soft package lithium ion battery cell with an anode material of NCM523 and an anode material of artificial graphite, wherein the addition amount of the electrolyte is 10g, sealing for the first time, standing at 45 ℃ for 24 hours, forming by using a high-temperature clamp, sealing for the second time, and grading to prepare the soft package lithium ion battery.
Examples 2 to 7
The high-voltage electrolyte matched with the ternary cathode material lithium ion battery is prepared by the same method as the embodiment 1, and the distribution ratio of each component in the electrolyte of each embodiment is shown in table 1. The electrolyte prepared in each example is prepared into soft package lithium ion batteries with the same model by the same method and the same electrolyte adding amount as those in example 1.
Comparative examples 1 to 3
Preparing an electrolyte and manufacturing a battery:
the proportions of the components of the electrolyte in each proportion are shown in table 1. The electrolytes prepared in each proportion are respectively prepared into soft package lithium ion batteries with the same model by adopting the same method and the same electrolyte adding amount as the embodiment 1, and the soft package lithium ion batteries with the same model are prepared by adopting the same method and the same electrolyte adding amount as the embodiment 1.
TABLE 1 compositions and proportions of the components of the electrolytes of examples 1-7 and comparative examples 1-3
| Group of | Lithium salt | Non-aqueous solvent | Diisopropylcyanophosphine | Ethylene vinylene carbonate |
| Example 1 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 0.5% | 1.0% |
| Example 2 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 1.5% | 1.0% |
| Example 3 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 3.0% | 1.0% |
| Example 4 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 1.5% | 0.3% |
| Example 5 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 1.5% | 2.0% |
| Example 6 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 0.5 percent | EC/EMC/DEC=1/5/7 | 1.5% | 1.0% |
| Example 7 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 2.5 percent | EC/EMC/DEC=1/5/7 | 1.5% | 1.0% |
| Comparative example 1 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 0 | 1.0% |
| Comparative example 2 | Lithium hexafluorophosphate: 13.0% lithium difluorooxalate phosphate: 1.5 percent | EC/EMC/DEC=1/5/7 | 1.5% | 0 |
| Comparative example 3 | Lithium hexafluorophosphate: 13.0 percent | EC/EMC/DEC=1/5/7 | 1.5% | 1.0% |
(EC in Table 1 is abbreviated as ethylene carbonate, EMC is abbreviated as ethyl methyl carbonate, and DEC is abbreviated as diethyl carbonate.)
And (3) testing the battery performance:
the soft-packed lithium ion batteries prepared in examples 1 to 7 and comparative examples 1 to 3 described above were subjected to the following tests:
(1) and (3) testing the normal-temperature cycle performance: charging the prepared battery to 4.5V at a constant current of 0.5C and then to 4.5V at a constant voltage at 25 ℃, wherein the cut-off current of the constant voltage charging is 0.01C; then discharged to 3.0V at a constant current of 0.5C. After 600 cycles of charge and discharge according to the above charge and discharge system, the capacity retention rate at the 600 th cycle was calculated. The calculation formula is as follows:
capacity retention ratio (%) at 600 cycles = (600-cycle discharge capacity/1-cycle discharge capacity) × 100%.
(2) And (3) testing the high-temperature storage performance: charging the prepared battery to 4.5V at 25 ℃ with a constant current of 0.5C, and then charging with a constant voltage of 4.5V, wherein the cut-off current of the constant voltage charging is 0.01C; then, the discharge was performed at a constant current of 0.5C to 3.0V, and the discharge capacity was recorded and was regarded as the initial capacity. Charging to 4.5V at a constant current of 0.5C, and then charging at a constant voltage of 4.5V, wherein the cut-off current of the constant voltage charging is 0.01C; and then placing the battery in a 60 ℃ oven for 10 days, taking out the battery after the storage is finished, cooling the battery to 25 ℃, discharging to 3.0V at 25 ℃ at 0.5 ℃, and recording the measured discharge capacity of the battery as the retention capacity of the battery. The charge and discharge were continued at 25 ℃ for 1 cycle at 0.5C (4.5-3.0V), and the discharge capacity was recorded as the recovery capacity.
Battery capacity retention (%) = retention capacity/initial capacity × 100%;
battery capacity recovery (%) = recovered capacity/initial capacity × 100%.
(3) And (3) testing low-temperature discharge performance: charging the prepared battery to 4.5V at a constant current of 0.5C at 25 ℃, and then charging at a constant voltage of 4.5V, wherein the cut-off current of the constant voltage charging is 0.01C; then discharging to 3.0V at 0.2C, recording the discharge capacity, and recording the discharge capacity as the initial discharge capacity; and continuously charging to 4.5V at a constant current of 0.5C, then charging at a constant voltage of 4.5V, wherein the cut-off current of constant voltage charging is 0.01C, placing the battery in a low-temperature box at the temperature of-30 ℃ for standing for 4h, discharging to 3.0V at the temperature of-30 ℃ at 0.2C, and recording the discharge capacity, namely the low-temperature discharge capacity.
Low-temperature discharge capacity retention (%) — low-temperature discharge capacity/initial discharge capacity × 100%.
The results of the above tests are shown in table 2.
Table 2 performance test data of lithium ion batteries prepared in each example and comparative example
As can be seen from table 2: in the examples 1, 2 and 3, the positive film-forming additive diisopropyl cyanophosphine is added, while in the comparative example 1, the diisopropyl cyanophosphine is not added, and under the condition that the content of the negative film-forming additive ethylene vinylene carbonate is the same, the capacity retention rate of the battery prepared in the comparative example 1 at the time of cycling at 25 ℃ for 600 times is at least reduced by 28.42 percent; the capacity retention rate at high temperature is reduced by at least 17.37 percent, and the capacity recovery rate is reduced by at least 16.54 percent; and the low-temperature capacity retention rate is also reduced. This shows that diisopropyl cyanophosphine as film forming additive for positive electrode improves the cycle performance at normal temperature and reduces the capacity attenuation when the prepared electrolyte is used at the charge cut-off voltage of up to 4.5V; and improved high temperature storage performance when used at charge cut-off voltages of up to 4.5V. In examples 4 and 5 and comparative example 2, the positive film-forming additive diisopropylcyanophosphine is added, while in comparative example 2, ethylene vinylene carbonate is not added, under the condition that the content of the positive film-forming additive diisopropylcyanophosphine is the same, the capacity retention rate at 600 th time of 25 ℃ circulation of the battery prepared in comparative example 2 is at least reduced by 25.48%, and the high-temperature storage performance and the low-temperature discharge capacity retention rate are also reduced.
In addition, the difference between the electrolyte of comparative example 3 and the electrolyte of example 2 and examples 6-7 is only the lithium salt, only one lithium hexafluorophosphate is used in the electrolyte of comparative example 3, and 13.0 percent of lithium hexafluorophosphate and 0.5 percent to 2.5 percent of lithium difluorooxalate phosphate are added in the electrolyte of example 2 and examples 6-7, and the two lithium salts are used in combination, so that the normal temperature cycle performance, the high temperature storage performance and the low temperature discharge capacity retention rate of the prepared lithium ion battery are improved. Therefore, the stable SEI film formed by orderly combining inorganic and organic components is simultaneously used for the lithium hexafluorophosphate and the lithium difluorooxalate phosphate, the lithium difluorooxalate lithium battery has good lithium ion conductivity of an inorganic film structure and good mechanical toughness of an organic film, the side reaction of a negative electrode interface is effectively inhibited, and the cycle performance of the battery is improved.
According to the high-voltage electrolyte matched with the ternary cathode material lithium ion battery, decomposition of the electrolyte when the battery is used under high voltage can be effectively inhibited through the cathode film forming additive diisopropyl cyanophosphine, so that the battery keeps stable performance when used under higher charging voltage; the negative electrode film forming additive ethylene vinylene carbonate can promote lithium difluorooxalate phosphate to form lithium fluoride which is inserted into a decomposition product of the ethylene vinylene carbonate to form an SEI film with low impedance, good conductivity and good mechanical toughness, and lithium hexafluorophosphate enables the electrolyte to have higher conductivity.
The high-voltage electrolyte of the lithium ion battery matched with the ternary cathode material is stable in use and not easy to decompose at high temperature and high voltage by simultaneously using the diisopropylcyanophosphine, the ethylene vinylene carbonate and the lithium difluorooxalate phosphate; and the conduction impedance of lithium ions in the battery is small, the battery is not easy to precipitate lithium when used at low temperature, and the high-temperature performance and the low-temperature performance of the battery are good while the battery has good cycle performance.
It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features related to the embodiments of the present invention described above may be combined with each other as long as they do not conflict with each other.
Claims (5)
1. The high-voltage electrolyte matched with the ternary anode material lithium ion battery is characterized by comprising a lithium salt, a non-aqueous solvent, a cathode film-forming additive and an anode film-forming additive; the lithium salt comprises lithium hexafluorophosphate and lithium difluorooxalate phosphate, the negative electrode film forming additive is ethylene vinylene carbonate, the positive electrode film forming additive is diisopropyl cyanophosphine, and the structural formula of the diisopropyl cyanophosphine is as follows:
(ii) a The mass of the negative electrode film-forming additive accounts for 0.3-2% of the total mass of the electrolyte, and the mass of the positive electrode film-forming additive accounts for 0.5-3% of the total mass of the electrolyte.
2. The high voltage electrolyte of a matched ternary positive electrode material lithium ion battery as claimed in claim 1, wherein the mass of lithium hexafluorophosphate in the lithium salt accounts for 13.0% of the total mass of the electrolyte, and the mass of lithium difluorooxalato phosphate accounts for 0.5% -2.5% of the total mass of the electrolyte.
3. The high voltage electrolyte of a matched ternary positive electrode material lithium ion battery of claim 1, wherein the non-aqueous solvent is a cyclic carbonate or a linear carbonate.
4. The high voltage electrolyte of a matched ternary positive electrode material lithium ion battery of claim 3, wherein said linear carbonate is a mixture of ethyl methyl carbonate and diethyl carbonate.
5. The high-voltage electrolyte of the matched ternary cathode material lithium ion battery as claimed in claim 2, wherein the non-aqueous solvent is a mixture of ethylene carbonate, ethyl methyl carbonate and diethyl carbonate in a mass ratio of 1:5: 7.
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