CN107946643B - High-performance lithium battery electrolyte - Google Patents

High-performance lithium battery electrolyte Download PDF

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Publication number
CN107946643B
CN107946643B CN201711123982.3A CN201711123982A CN107946643B CN 107946643 B CN107946643 B CN 107946643B CN 201711123982 A CN201711123982 A CN 201711123982A CN 107946643 B CN107946643 B CN 107946643B
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electrolyte
battery
lithium salt
temperature
organic solvent
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CN107946643A (en
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侯荣雪
刘鹏
张民
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Hebei Shengtai Materials Co., Ltd.
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SHIJIAZHUANG SHENGTAI CHEMICAL CO Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Secondary Cells (AREA)

Abstract

The invention relates to a high-performance lithium battery electrolyte, which belongs to the technical field of lithium battery electrolytes and comprises lithium salt, an organic solvent and compounds and/or , wherein R 1 is selected from alkyl, H or F, and R 2 is selected from allyl, propargyl or benzene.

Description

High-performance lithium battery electrolyte
Technical Field
The invention belongs to the technical field of lithium battery electrolyte, and relates to a high-temperature-resistant lithium battery electrolyte. The battery electrolyte can improve the cycle performance and the recovery performance of the battery at high temperature, and the matching of the components of the battery electrolyte can effectively improve the charge and discharge performance of the lithium battery and reduce the occurrence of side reactions, thereby reducing the battery flatulence and prolonging the cycle life of the battery.
Background
The lithium ion battery has the advantages of high working voltage, high energy density, environmental friendliness, stable cycle, safety and the like, and is widely applied to various electronic devices such as notebook computers, mobile phones, MP4 and the like. However, as the capacity of batteries in electronic devices increases, higher requirements are placed on the operating voltage and energy density of lithium ion batteries. However, with the increase of the requirement of the working environment on the moisture temperature, the reaction between the electrolyte and the electrolyte is accelerated due to the excessively high moisture content in the electrolyte, and the generation of HF finally causes severe air expansion at normal temperature and high temperature, so that the cycle performance is reduced, and the performance of the battery is severely restricted.
The electrolyte is an important component of the battery, plays a role in transmitting ions between a positive electrode and a negative electrode through the inside of the battery, and has important influence on the capacity, the working temperature range, the cycle performance, the safety performance and the like of the battery. The electrolytes are generally classified into liquid electrolytes and solid electrolytes, and the following basic requirements are required to be satisfied: (1) high ionic conductivity, typically up to 1X 10-3-2×10-2S/cm; (2) high thermal stability and chemical stability, and no decomposition in a wide temperature range; (3) the electrochemical window is wide, and the stability of the electrochemical performance is kept in a wide voltage range; (4) the electrolyte has good compatibility with other parts of the battery; (5) safe, nontoxic and pollution-free.
Liquid organic electrolyte is the most commonly used, but with the continuous widening of the application range of batteries, the requirements of people on various aspects of the batteries are continuously increased, and the original electrolyte system can not meet the use requirements.
Disclosure of Invention
The invention aims to solve the problems, designs the electrolyte of the high-temperature-resistant lithium battery, and by adding the substance into the electrolyte, the electrolyte can effectively improve the charge and discharge performance of the lithium battery, increase the energy density, improve the high-low temperature cycle performance of the battery and prolong the cycle life of the battery.
The technical scheme adopted by the invention for realizing the purpose is as follows:
A high-performance lithium battery electrolyte comprises lithium salt, organic solvent and compoundAnd/orWherein R is1selected from alkyl, H or F, R2Selected from allyl, propargyl or benzene.
Compound (I)And/orThe total dosage of the electrolyte is 0.05-0.8 percent of the mass of the electrolyte.
The organic solvent comprises cyclic carbonate and/or chain carbonate. Such as ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate, and the like.
The lithium salt is selected from inorganic anionic electrolyte lithium salt and/or organic anionic electrolyte lithium salt.
The concentration of the lithium salt in the organic solvent is 1-1.5 mol/L.
Also included is 1, 2-bis (triethoxysilyl) ethane.
The invention has the beneficial effects that:
The electrolyte of the invention is added withAnd/orOn the basis of improving the formation efficiency and the fire-spreading voltage, the compound increases the solubility of solute, improves the conductivity and reduces the specific resistance, thereby prolonging the service life of the product, simultaneously improving the growth speed of an oxide film, inhibiting the hydration of the oxide film and improving the high-low temperature performance of the electrolyte.
1, 2-bis (triethoxysilyl) ethane, which is used for improving the solubility and preventing solute from crystallizing and separating out under the low-temperature condition to influence the low-temperature performance of the electrolyte; can make it possible toAnd/orThe compound has better effect and synergistic effect, can solve the problem of capacity reduction caused by long-time use of the battery, and is prepared by controlling 1, 2-bis (triethoxysilyl) ethane andand/orThe mass ratio of the compounds is 1: (0.1-0.3) to make the conductivity stable with the temperature change, meanwhile, the addition of 1, 2-bis (triethoxysilyl) ethane can further solve the swelling problem of the battery, and simultaneously can improve the chemical stability, the addition and proportion control of 1, 2-bis (triethoxysilyl) ethane can enhance the performance of lithium salt, can further reduce the resistance of the solution and increase the ionization degree of lithium ions, and simultaneously increase the ion transference number in the solution.
Addition of 1, 2-bis (triethoxysilyl) ethane andAnd/orthe discharge performance of the battery under high rate can be improved by the combined use of the compounds; meanwhile, the 1, 2-bis (triethoxysilyl) ethane is added to interact with the organic solvent, so that the solubility is improved, the reversibility of the electrode process can be improved, the falling of active substances on the electrode is reduced, the electrochemical polarization is reduced, and the cycle life of the battery is prolonged by more than 1.5 times.
Drawings
Fig. 1 is a graph of the high temperature cycling performance of a battery at 65 ℃.
Fig. 2 is a graph comparing high temperature stability of batteries.
Fig. 3 is a graph of battery impedance performance.
Wherein, laminate polymer battery 600mAh, positive pole material: 4.35V LiNi0.5Co0.2Mn0.3O2And the cathode material: silicon carbon negative electrode (Si 5%), base electrolyte: EC/EMC/DEC, LiPF61M additive VC AND, BASE is the basis, BASE + ADD is after adding the sulfonic acid additive product.
Detailed Description
the present invention will be further described with reference to the following specific examples.
Detailed description of the preferred embodiments
Example 1
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a volume ratio of 6:3: 1; LiPF with organic solvent concentration of 1mol/L6A lithium salt; ethylene glycol disulfonate accounting for 0.05 percent of the mass of the battery electrolyte.
Example 2
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a volume ratio of 4:3: 3; LiBF occupying 1.5mol/L concentration of organic solvent4A lithium salt; phenyl benzene sulfonate accounting for 0.08 percent of the mass of the battery electrolyte.
Example 3
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a volume ratio of 3:4: 3; li (CF) at an organic solvent concentration of 1.3mol/L3SO2)N2A lithium salt; allyl benzene sulfonate accounting for 0.1 percent of the mass of the battery electrolyte.
Example 4
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a volume ratio of 2:7: 1; li (CF) at an organic solvent concentration of 1.2mol/L3SO2)N2A lithium salt; 0.3 percent of propargyl benzene sulfonate in the mass of the battery electrolyte.
Example 5
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, bis (trifluoromethanol) carbonate and methyl ethyl carbonate in a volume ratio of 2:4: 4; LiPF accounting for 1.4mol/L of organic solvent6And LiBOB mixed lithium salt, LiPF6And LiBOB in a molar ratio of 3: 4; ethylene glycol ditrimethylbenzene sulfonate accounting for 0.3 percent of the mass of the battery electrolyte. Using mixed lithium salts, especially LiPF6The electrolyte can be mixed with LiBOB lithium salt for improving the electrochemical performance and the cycle performance of the electrolyte, and the LiBOB lithium salt is mixed for useThe electron delocalization effect is strong, so that the conductivity of the mixed lithium salt is high, and the improvement of the electrochemical stability and the thermal stability of the battery is facilitated.
The chemical structural formula of the ethylene glycol ditrimethylbenzene sulfonate is as follows:
Example 6
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a volume ratio of 1:6: 3; LiPF with organic solvent concentration of 1mol/L6A lithium salt; ethylene glycol disulfonate accounting for 0.05 percent of the mass of the battery electrolyte; 1, 2-bis (triethoxysilyl) ethane accounting for 0.5 percent of the electrolyte mass. Due to LiPF6The lithium salt has strong hygroscopicity, potential safety hazards are easy to generate at high temperature or high current density, the pyrolysis stability is poor, the ethylene glycol diphenyl sulfonate has better effect due to the addition of the 1, 2-bis (triethoxysilyl) ethane, the two synergistic effects can solve the problem of capacity reduction caused by long-time use of the battery, and the mass ratio of the 1, 2-bis (triethoxysilyl) ethane to the ethylene glycol diphenyl sulfonate is controlled to be 1: (0.1-0.3) to ensure that the conductivity is stable along with the change of temperature, meanwhile, the addition of the 1, 2-bis (triethoxysilyl) ethane can further solve the swelling problem of the battery and can improve the chemical stability, and the addition of the 1, 2-bis (triethoxysilyl) ethane can further reduce the resistance of the solution and increase the ionization degree of lithium ions and simultaneously increase the ion migration number in the solution.
Example 7
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, diethylene carbonate and methyl ethyl carbonate in a volume ratio of 7:2: 1; li (CF) at an organic solvent concentration of 1.0mol/L3SO2)N2and LiBMB mixed lithium salt, in which Li (CF)3SO2)N2And LiBMB in a 4:3 molar ratio; allyl benzene sulfonate accounting for 0.5 percent of the mass of the battery electrolyte; occupying the electrolyte of the battery1, 2-bis (triethoxysilyl) ethane with a mass of 1.7%. With mixed lithium salts, especially Li (CF)3SO2)N2The lithium ion battery electrolyte can be mixed with LiBMB lithium salt for use, so that the electrochemical performance and the cycle performance of the electrolyte can be improved, and the LiBMB lithium salt is mixed for use, so that the conductivity of the mixed lithium salt is high due to the strong electron delocalization effect of the LiBMB lithium salt, and the improvement of the electrochemical stability and the thermal stability of the battery is facilitated. Due to Li (CF)3SO2)N2The lithium salt is easy to generate potential safety hazard at high temperature or high current density, the pyrolysis stability is poor, the allyl benzene sulfonate can have better effect due to the addition of 1, 2-bis (triethoxysilyl) ethane, the capacity reduction problem caused by long-time use of the battery can be solved due to the synergistic effect of the lithium salt and the allyl benzene sulfonate, and the mass ratio of the 1, 2-bis (triethoxysilyl) ethane to the allyl benzene sulfonate is controlled to be 1: (0.1-0.3) to make the conductivity more stable with the change of temperature, meanwhile, the addition of 1, 2-di (triethoxysilyl) ethane can further solve the swelling problem of the battery, and can improve the chemical stability, the addition of 1, 2-di (triethoxysilyl) ethane has more effect in the composite lithium salt, and can further reduce the resistance of the solution and increase the ionization degree of lithium ions, and simultaneously increase the ion transference number in the solution.
Example 8
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of propylene carbonate, ethylene carbonate and methyl ethyl carbonate in a volume ratio of 3:2: 5; li (CF) at a concentration of 1.1mol/L in the organic solvent3SO2)3A lithium salt; ethylene glycol ditridecylbenzene sulfonate accounting for 0.8% of the mass of the battery electrolyte.
The chemical structural formula of the ethylene glycol ditridecylbenzene sulfonate is as follows:
Example 9
The high-temperature-resistant lithium ion battery electrolyte comprises an organic solvent composed of ethylene carbonate, bis (trifluoromethanol) carbonate and methyl ethyl carbonate in a volume ratio of 4:2: 4; possess ofLiPF with organic solvent concentration of 1.4mol/L6And LiBOB mixed lithium salt, LiPF6And LiBOB in a molar ratio of 3: 4; phenyl benzene sulfonate accounting for 0.3 percent of the mass of the battery electrolyte; 1, 2-bis (triethoxysilyl) ethane accounting for 1.5 percent of the mass of the battery electrolyte. Due to LiPF6The lithium salt has strong hygroscopicity, potential safety hazards are easy to generate at high temperature or high current density, the pyrolytic stability is poor, the effect of phenyl benzenesulfonate can be better due to the addition of 1, 2-bis (triethoxysilyl) ethane, the effect not only comprises better high and low temperature cycle performance, but also comprises the effect of preventing corrosion of a steel shell, the capacity reduction problem caused by long-time use of the battery can be solved due to the synergistic effect of the lithium salt and the phenyl benzenesulfonate, and the lithium salt and the phenyl benzenesulfonate are prepared by controlling the mass ratio of 1, 2-bis (triethoxysilyl) ethane to phenyl benzenesulfonate to be 1: (0.1-0.3) to ensure that the conductivity is stable along with the change of temperature, meanwhile, the addition of the 1, 2-bis (triethoxysilyl) ethane can further solve the swelling problem of the battery and can improve the chemical stability, and the addition of the 1, 2-bis (triethoxysilyl) ethane can further reduce the resistance of the solution and increase the ionization degree of lithium ions and simultaneously increase the ion migration number in the solution.
Second, performance test
1. the electrolyte disclosed by the invention is respectively assembled into batteries and then subjected to cycle performance test, and the method comprises the following steps: with LiNi0.5Co0.2Mn0.3O2The anode material is a positive electrode material, the cathode adopts a silicon-carbon cathode (Si 5%), the current collectors of the anode and the cathode are distributed into aluminum foil and copper foil, the diaphragm adopts a ceramic diaphragm to form a soft package battery, the soft package battery is assembled in a glove box after electrolyte is injected, and the test is carried out after the soft package battery is kept stand for 8 hours. The battery is activated by charging and discharging at 1/10C 3.0V to 4.45V at constant temperature of 25 ℃ at room temperature, and then the battery is charged and discharged at 1C in cycles at normal temperature. The cycle test results are shown in table 1.
TABLE 1
2. Battery discharge retention at different rates: discharging the battery to 3.0V at a constant current of 0.5C, standing for 5min, then charging to 4.4V at a constant current of 0.5C, charging at a constant voltage until the current is 0.05C, standing for 5min, and then discharging at constant currents of 0.2C, 1.5C and 2C respectively until the cut-off voltage is 3.0V. The discharge capacity under the conditions of 0.2C, 1.5C and 2C was recorded as D1, the discharge capacity under 0.2C was recorded as D0, and based on the discharge capacity under 0.2C, the discharge capacity retention rate of the battery under different rates was calculated by the formula of [ (D1-D0)/D0] × 100% (15 batteries were measured and the average value thereof was taken), and the discharge capacity retention rate under different rates of each battery under the condition of 25 ℃ was shown in table 2.
TABLE 2
3. Evaluating the low-temperature storage performance of the battery; the following table 3 shows that the battery was left to stand in a low temperature cabinet at-30 ℃ or-40 ℃ for 240min, respectively, and then the capacity retention rate of the battery was measured.
TABLE 3
4. And (3) hot box testing: the cells were tested as follows:
1) Charging the battery to 4.4V at a constant current of 1.0C, then charging at a constant voltage until the current is reduced to 0.05C, and stopping charging; 2) placing the battery in a hot box, raising the temperature from 25 ℃ to 180 ℃ at a temperature raising speed of 5 ℃/min, keeping the temperature unchanged after reaching 180 ℃, then starting timing, observing the state of the battery after 1h, and determining the standard of passing the test as follows: the batteries had no smoke, no fire, no explosion, with 10 batteries in each group. The results of the hot box test for each cell are shown in table 4. The safety performance of the battery is characterized through the hot box test.
TABLE 4
Item Post hot box test condition
Example 1 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 2 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 3 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 4 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 5 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 6 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 7 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 8 10 batteries pass through the battery pack without smoking, igniting and exploding phenomena
Example 9 All 10 batteries are connectedNo smoking, fire and explosion phenomena
5. Corrosion resistance
18650 lithium ion battery steel casings were weighed and then immersed in the lithium ion battery electrolytes for preventing corrosion of the steel casings of examples 1 to 9, 18650 lithium ion battery steel casings and the lithium ion battery electrolytes for preventing corrosion of the steel casings of examples 1 to 9 were placed in an open environment at room temperature, after 100 hours, the 18650 lithium ion battery steel casings were cleaned, dried and weighed, and the weight loss rate of the 18650 lithium ion battery steel casings was calculated, with the results shown in table 5.
TABLE 5
Item Front weight Rear weight percentage of weight loss%
Example 1 7.6589 7.6575 0.018
Example 2 7.3624 7.3610 0.019
Example 3 7.5386 7.5373 0.017
Example 4 7.6676 7.6660 0.021
Example 5 7.5743 7.5734 0.012
Example 6 7.7338 7.7331 0.009
Example 7 7.6982 7.6977 0.006
Example 8 7.7523 7.7510 0.017
Example 9 7.7948 7.7944 0.005

Claims (5)

1. The high-performance lithium battery electrolyte comprises lithium salt, organic solvent and compoundAnd/orWhereinR of (A) to (B)1Selected from alkyl, H or F;R of (A) to (B)1Selected from alkyl or F, R2Selected from allyl, propargyl or benzene;
Also included are 1, 2-bis (triethoxysilyl) ethane;
1, 2-bis (triethoxysilyl) ethane and compoundOrThe mass ratio of (1): (0.1-0.3).
2. The electrolyte for a high performance lithium battery as claimed in claim 1, wherein: compound (I)And/orThe dosage of the electrolyte is 0.05-0.8% of the mass of the electrolyte.
3. the electrolyte for a high performance lithium battery as claimed in claim 1, wherein: the organic solvent comprises cyclic carbonate and/or chain carbonate.
4. the electrolyte for a high performance lithium battery as claimed in claim 1, wherein: the lithium salt includes an inorganic anionic electrolyte lithium salt and/or an organic anionic electrolyte lithium salt.
5. The electrolyte for a high performance lithium battery as claimed in claim 1, wherein: the concentration of the lithium salt in the organic solvent is 1-1.5 mol/L.
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KR20200098335A (en) * 2019-02-12 2020-08-20 삼성전자주식회사 Lithium battery
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