CN102082292B - High-temperature lithium ion battery electrolyte and lithium ion battery - Google Patents
High-temperature lithium ion battery electrolyte and lithium ion battery Download PDFInfo
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- CN102082292B CN102082292B CN2010106036189A CN201010603618A CN102082292B CN 102082292 B CN102082292 B CN 102082292B CN 2010106036189 A CN2010106036189 A CN 2010106036189A CN 201010603618 A CN201010603618 A CN 201010603618A CN 102082292 B CN102082292 B CN 102082292B
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Abstract
The invention discloses a high-temperature lithium ion battery electrolyte and a lithium ion battery. The electrolyte is prepared by uniformly mixing electrolyte salts, a nonaqueous organic solvent, a high-temperature film-forming additive and high-temperature gas generation inhibiting additives, wherein the high-temperature film-forming additive is lithium bis(oxalate) borate (LiBOB); the LiBOB accounts for 0.2-3% by mass of the mixed lithium salt solution formed by the electrolyte salts and the nonaqueous organic solvent; the high-temperature gas generation inhibiting additive is one or two of ionic liquid and phthalic anhydride, and accounts for 0.8-9% by mass of the mixed lithium salt solution; and the total content of the added high-temperature film-forming additive and high-temperature gas generation inhibiting additives accounts for 1-11% by mass of the mixed lithium salt solution. The lithium ion battery comprises a cathode, an anode, a diaphragm and the high-temperature lithium ion battery electrolyte. The invention has the advantage of reasonable design, the steps in the preparation processes are simple and convenient to implement, and the prepared electrolyte and the lithium ion battery have excellent comprehensive performance.
Description
Technical field
The present invention relates to a kind of lithium-ion battery electrolytes and use the lithium ion battery of this electrolyte, especially relate to a kind of high temperature modification lithium-ion battery electrolytes and lithium ion battery.
Background technology
In recent years, because the pressure of environmental pollution and energy shortage forces each state all at the energy of seeking new green, environmental protection and sustainable development.The high-capacity environment-protecting lithium ion battery that occurs the nineties in 20th century since the energy density that it had high, have extended cycle life, the operating voltage advantages of higher, make it become one of electrical source of power that attracts most attention.Yet Along with people's deepens continuously to the understanding of battery service condition, finds that the use of battery under a lot of situation all is being higher than under the condition of normal temperature, and when moving, battery is because heating can cause temperature to rise to about 45 ℃ like notebook computer; And GPS uses battery; Because long term exposure in the sun; Temperature tends to reach about 80 ℃; Working under the hot conditions or storing requires harshlyer to the job stability of battery system and storage stability, make to have caused attention to improving the electrical property and the high temperature storage performance of battery under hot conditions in the industry.
Under hot environment, a series of variations can take place in lithium-ion battery system.Positive electrode is because active higher, together with electrolyte generation oxidation reaction, thereby influences the performance of lithium ion battery.When negative material changed at lithium ion battery, the surface can form the SEI film, and when being in hot environment, the SEI film can dissolve and destroyed, thereby influenced cycle performance and the capacity performance etc. of battery.Particularly the lithium manganate material of one of popular positive electrode of power lithium battery because the dissolving of Mn aggravation causes the decay of circulation volume to accelerate, is the bottleneck that limits its large-scale application under hot conditions always.Simultaneously, when battery stored in hot environment for a long time, volatilization or reduction decomposition can take place in electrolyte, cause battery " inflatable ", may cause safety problems such as battery explosion.
Therefore; Face to face during Lingao temperature service condition, the design of lithium-ion battery electrolytes must be considered the compatibility between the lithium ion battery plus-negative plate material and electrolyte under the hot environment; Reduce the probability that electrolyte reacts with both positive and negative polarity, and improve the stability of SEI film.The researcher is arranged through adding a certain amount of special additive in the industry at present, can solve the inflatable problem of battery to a certain extent, but but seriously influenced the electrical property of battery at normal temperature and high temperature.
In addition, ionic liquid has lot of advantages: most of ionic liquids all exist with liquid form in wider temperature range, are applied in the serviceability temperature scope that can enlarge battery in the battery; Ion liquid vapour pressure is zero, and is also non-volatile under higher temperature, can solve the problem of electrokinetic cell high temperature inflatable; Viscosity is low, and thermal capacitance is big, and some ionic liquid is all stable to water, air, is prone to handle; Preparation is than being easier to, and cost of material is cheap etc.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned deficiency of the prior art, provides that a kind of processing and preparing is easy, cost is low and high temperature performance and electrical property equal excellent high-temperature type lithium-ion battery electrolytes and lithium ion battery.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is: a kind of high temperature modification lithium-ion battery electrolytes and lithium ion battery; Comprise the mixing lithium salt solution that forms by electrolytic salt and the even mixed preparing of non-aqueous organic solvent; It is characterized in that: also comprise the high temperature film for additive and inhibition high temperature aerogenesis additive that evenly are blended in the said mixing lithium salt solution; Said high temperature film for additive is biethyl diacid lithium borate LiBOB, and biethyl diacid lithium borate LiBOB is 0.2%～3% with said mass percent of mixing between the lithium salt solution; Said inhibition high temperature aerogenesis additive is one or both in ionic liquid and the phthalic anhydride, and said inhibition high temperature aerogenesis additive is 0.8%～9% with said mass percent of mixing between the lithium salt solution, and said ion liquid chemical formula does
R=CH wherein
2CH
3, CH
2CH
2CH
3Or CH
2CH
2CH
2CH
3And said ionic liquid should be ionic liquid EMI-TFSI, ionic liquid PMI-TFSI or ionic liquid BMI-TFSI mutually; The gross mass of adding the high temperature film for additive and suppressing high temperature aerogenesis additive be 1%～11% with mass percent between the said solution quality that mixes lithium salt solution.
Above-mentioned a kind of high temperature modification lithium-ion battery electrolytes; It is characterized in that: said electrolytic salt is one or both in lithium hexafluoro phosphate, LiBF4, biethyl diacid lithium borate and the lithium trifluoromethanesulp,onylimide, and said electrolytic salt and the said non-aqueous organic solvent amount of substance concentration of mixing lithium salt solution that forms that evenly is mixed is 0.8mol/L～1.4mol/L.
Above-mentioned a kind of high temperature modification lithium-ion battery electrolytes; It is characterized in that: the mixed solvent of said non-aqueous organic solvent for evenly mixing by ethylene carbonate, propene carbonate and diethyl carbonate, and the volume ratio of ethylene carbonate, propene carbonate and diethyl carbonate ratio is 2～5: 1～3: 3～6.
Above-mentioned a kind of high temperature modification lithium-ion battery electrolytes is characterized in that: said electrolytic salt is a lithium hexafluoro phosphate.
Simultaneously; The present invention also provides a kind of high comprehensive performance and has had the lithium ion battery of good high-temperature storage performance, high temperature cyclic performance and low temperature performance; Comprise positive pole, negative pole and barrier film, it is characterized in that: also comprise the high temperature modification lithium-ion battery electrolytes.
Above-mentioned a kind of high temperature modification lithium ion battery is characterized in that: said positive pole is processed by cobalt acid lithium or lithium manganate material, and said negative pole is processed by material with carbon element, and said barrier film is processed by the porous polyolefin material.
Above-mentioned a kind of high temperature modification lithium ion battery is characterized in that: said lithium ion battery is square flexible packing lithium ion battery.
The present invention compared with prior art has the following advantages:
1, the manufacture method step of electrolyte and lithium ion battery is simple and workable, makes easily the high comprehensive performance of prepared electrolyte and lithium ion battery.The lithium ion battery of making is as positive pole by cobalt acid lithium material or lithium manganate material; Native graphite, carbonaceous mesophase spherules material with carbon elements such as (MCMB) are as negative pole; The porous polyolefin compound is as barrier film, and adopts lamination or winding method to process the square flexible packing lithium ion battery.
2, prepared electrolyte has excellent low temperature performance, has the discharge capability that under-30 ℃ of temperature conditions, carries out regular picture.
3, prepared electrolyte has higher high temperature discharge performance, under high temperature (55 ℃, the 0.2C discharge) condition, has 98.3% discharge ratio.
4, prepared electrolyte has the high temperature storage performance of superelevation; The gas that electrolyte volatilization or reduction decomposition produce when storing in order to suppress the battery long term high temperature effectively; The present invention has used the good ionic liquid of thermal stability as high temperature additive; Utilize its higher boiling point of 300 ℃, almost do not have advantages such as vapour pressure, no combustibility and high conductivity; And add an amount of phthalic anhydride, through the collaborative use of the two, improved the high temperature storage performance of battery under this electrolyte system effectively.The battery that uses this invention institute preparing electrolyte is being shelved 48h and after shelving 4h under 100 ℃ under 85 ℃, battery is inflatable not all, and has higher capability retention and capacity restoration rate, is respectively 85% and 95%, and the internal resistance rate of change of battery is also less in addition.
5, prepared electrolyte has excellent normal-temperature circulating performance.
6, reasonable in design; Manner of formulation is flexible and practical value is high; Popularizing application prospect is extensive; It is the main body solvent that its solvent adopts higher boiling point, high-flash, high-k and low viscous ring-type or linear carbonate class, can improve burning-point, boiling point, the decomposition temperature of electrolyte system so greatly, and then improves the thermal stability and the fail safe of electrolyte system.Simultaneously, be LiPF in order to improve main salt
6The stability of base electrolyte system, the present invention has introduced novel electrolytes salt LiBOB as film for additive.At present, one of problem of restriction LiMn2O4 electrokinetic cell development is that battery inducing capacity fading under hot environment is very fast, and K.Amine research shows that the mechanism of high temperature inducing capacity fading mainly is LiPF
6Decomposition has produced HF acid, and sour environment has been accelerated Mn
3+Disproportionation and the dissolving of Mn, destroyed the composition structure of SEI film simultaneously, and used LiBOB base electrolyte can improve the stability of SEI film greatly, reduce the output of HF simultaneously, improve the high temperature cyclic performance of battery.To sum up, the present invention efficiently solves the high temperature capacity attenuation problem of lithium manganate battery, has high temperature cyclic performance preferably.
In sum; The present invention is reasonable in design, preparation method's step simple, realize convenient and prepared electrolyte and lithium ion battery high comprehensive performance; It adopts higher boiling point, high-k and low viscous solvent is base solvent; Adopt the good electrolytic salt LiBOB of high temperature cyclic performance and thermal stability as film for additive; Adopt outstanding ionic liquid of thermal stability and phthalic anhydride as high temperature additive, suppressed the aerogenesis phenomenon in the battery high-temperature storage process effectively, make the lithium ion battery that uses electrolyte of the present invention on the basis that does not influence the normal temperature electrical property; Have 100 ℃ high temperature storage performance and 60 ℃ high temperature cyclic performance, and take into account-30 ℃ of low temperature performances under the temperature conditions.
Through accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is for going out the test result sketch map that cobalt acid lithium battery carries out the test of normal temperature 1C cycle performance to the present invention is prepared.
Fig. 2 is for going out the test result sketch map that cobalt acid lithium battery carries out the test of high temperature 1C cycle performance to the present invention is prepared.
Fig. 3 is for going out the test result sketch map that the manganese cobalt acid lithium battery carries out the test of high temperature 1C cycle performance to the present invention is prepared.
Fig. 4 is for going out the test result sketch map that cobalt acid lithium battery carries out high low temperature performance test to the present invention is prepared.
Embodiment
The invention discloses a kind of high temperature modification lithium-ion battery electrolytes; Comprise the mixing lithium salt solution that forms by electrolytic salt and the even mixed preparing of non-aqueous organic solvent; Also comprise the high temperature film for additive and inhibition high temperature aerogenesis additive that evenly are blended in the said mixing lithium salt solution; Said high temperature film for additive is biethyl diacid lithium borate LiBOB, and biethyl diacid lithium borate LiBOB is 0.2%～3% with said mass percent of mixing between the lithium salt solution; Said inhibition high temperature aerogenesis additive is one or both in ionic liquid and the phthalic anhydride, and said inhibition high temperature aerogenesis additive is 0.8%～9% with said mass percent of mixing between the lithium salt solution, and said ion liquid chemical formula does
R=CH wherein
2CH
3, CH
2CH
2CH
3Or CH
2CH
2CH
2CH
3And said ionic liquid should be ionic liquid EMI-TFSI, ionic liquid PMI-TFSI or ionic liquid BMI-TFSI mutually; The gross mass of adding the high temperature film for additive and suppressing high temperature aerogenesis additive be 1%～11% with mass percent between the said solution quality that mixes lithium salt solution, said ion liquid purity is pure for analysis.
In the actual fabrication process; Said electrolytic salt is one or both in lithium hexafluoro phosphate, LiBF4, biethyl diacid lithium borate and the lithium trifluoromethanesulp,onylimide, and said electrolytic salt and the said non-aqueous organic solvent amount of substance concentration of mixing lithium salt solution that forms that evenly is mixed is 0.8mol/L～1.4mol/L.The mixed solvent of said non-aqueous organic solvent for evenly mixing by ethylene carbonate, propene carbonate and diethyl carbonate, and the ratio of the volume ratio between ethylene carbonate, propene carbonate and the diethyl carbonate is 2～5: 1～3: 3～6.
In addition, the disclosed high temperature modification lithium ion battery of the present invention comprises positive pole, negative pole and barrier film, also comprises the high temperature modification lithium-ion battery electrolytes simultaneously.
Embodiment 1
In the present embodiment, during preparation electrolyte: (the H in being full of the glove box of argon gas of elder generation
2O content＜10ppm); Is that 3: 1: 3 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1mol/L after evenly mixing.Simultaneously; In said mixing lithium salt solution; Add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution, can according to actual needs biethyl diacid lithium borate LiBOB be adjusted accordingly in 0.2%～3% scope with said mass percent of mixing between the lithium salt solution in the actual fabrication process; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive; And to add ionic liquid EMI-TFSI be 3% with the be made into mass percent of mixing between the lithium salt solution; Can said inhibition high temperature aerogenesis additive be adjusted accordingly in 0.8%～9% scope with said mass percent of mixing between the lithium salt solution according to the concrete needs of reality in the actual fabrication process, and interpolation high temperature film for additive and the gross mass that suppresses high temperature aerogenesis additive are controlled in 1%～11% scope with mass percent between the said solution quality that mixes lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, the electrolytic salt that is adopted (specifically is lithium hexafluoro phosphate LiPF
6During actual fabrication; Can be according to the concrete needs of reality; Select for use in lithium hexafluoro phosphate, LiBF4, biethyl diacid lithium borate and the lithium trifluoromethanesulp,onylimide one or both as electrolytic salt, wherein the performance of lithium hexafluoro phosphate is the most excellent, is commercialization lithium ion battery lithium salts commonly used; Therefore, select lithium hexafluoro phosphate LiPF in the present embodiment for use
6Be main salt.Simultaneously, during actual fabrication, can be according to actual needs, select for use in ionic liquid and the phthalic anhydride one or both as suppressing high temperature aerogenesis additive.
When the high temperature modification lithium-ion battery electrolytes that utilization is mixed with is made cobalt acid lithium ion battery, should make the positive pole, negative pole and the barrier film that constitute lithium ion battery respectively.In the present embodiment; Said positive pole is processed by cobalt acid lithium material; Said negative pole is processed by material with carbon element; Said barrier film is processed by the porous polyolefin material, and said lithium ion battery is that square flexible packing lithium ion battery and its are formed by a plurality of lamination closed assemblies, also can adopt conventional winding method to make during the actual fabrication lithium ion battery.
When making positive pole, be solvent with N-dimethyl pyrrolidone (NMP), active material is cobalt acid lithium (LiCoO
2), conductive agent is super conductive carbon black (Super P), the NMP adding proportion is between 40%～65%.In the present embodiment, the mass percent of making used each raw material of anode sizing agent should be mutually: LiCoO
2: Super P: PVDF (Kynoar): NMP=94: 3: 3: 60.At first with LiCoO
2, Super P, PVDF and NMP be mixed with anode sizing agent according to design proportion, again the anode sizing agent for preparing is uniformly coated on the collector aluminium foil afterwards and through drying, roll-in and die-cut after, just accomplish the making of positive plate.
When making negative pole, the preparation of cathode size is consistent with anodal preparation steps, is solvent with water, and active material is a modified graphite, and conductive agent is super conductive carbon black (Super P), and bonding agent is the mixture of SBR and CMC, and the water adding proportion is between 90%～120%.Thereby preparation is during cathode size, with modified graphite, Super P, SBR, CMC and H
2O is mixed with cathode size according to design proportion, again the cathode size for preparing is coated on the copper foil of affluxion body afterwards and through drying, roll-in and die-cut after, just accomplish the making of negative plate.Among the embodiment, the mass percent of making used each raw material of cathode size should be mutually: modified graphite: Super P: SBR: CMC: H
2O=93: 3: 2: 2: 110.
At last; Die-cut good positive plate, negative plate and barrier film stacked gradually by the order of barrier film, negative plate, barrier film, positive plate, barrier film and negative plate from the bottom to top be combined into electric core; The electric core that is combined into utilizes aluminium pole ears and nickel lug to carry out ultrasonic bonding; The electric core that has welded is put in the aluminum-plastic packaged shell of square; After injecting above-mentioned high temperature modification lithium-ion battery electrolytes for preparing and sealing behind 80 ℃ of baking 24h, just making battery size is the cobalt acid lithium ion battery of 403465S, and the design capacity of battery is 1000mAh with electric core.
In addition, when utilizing the high temperature modification lithium-ion battery electrolytes that is mixed with to make manganate lithium ion battery, should make the positive pole, negative pole and the barrier film that constitute lithium ion battery respectively.In the present embodiment, said positive pole is processed by lithium manganate material, and said negative pole is processed by material with carbon element, and said barrier film is processed by the porous polyolefin material, and said lithium ion battery is that square flexible packing lithium ion battery and its are formed by a plurality of lamination closed assemblies.
When making positive pole, be solvent with N-dimethyl pyrrolidone (NMP), active material is spinel lithium manganate (LiMn
2O
4), conductive agent is super conductive carbon black (Super P) and anodal graphite agent (KS6), the NMP adding proportion is between 40%～65%.In the present embodiment, the mass percent of making used each raw material of anode sizing agent should be mutually: LiMn
2O
4: Super P: KS6: PVDF: NMP=91: 3: 2: 4: 60.At first with LiMn
2O
4, Super P, KS6, PVDF and NMP be mixed with anode sizing agent according to design proportion, again the anode sizing agent for preparing is uniformly coated on the collector aluminium foil afterwards and through drying, roll-in and die-cut after, just accomplish the making of positive plate.
When making negative pole, the preparation of cathode size is consistent with anodal preparation steps, is solvent with water, and active material is a modified graphite, and conductive agent is super conductive carbon black (Super P), and bonding agent is the mixture of SBR and CMC, and the water adding proportion is between 90%～120%.Thereby preparation is during cathode size, with modified graphite, Super P, SBR, CMC and H
2O is mixed with cathode size according to design proportion, again the cathode size for preparing is coated on the copper foil of affluxion body afterwards and through drying, roll-in and die-cut after, just accomplish the making of negative plate.Among the embodiment, the mass percent of making used each raw material of cathode size should be mutually: modified graphite: Super P: SBR: CMC: H
2O=93: 3: 2: 2: 110.
At last; Die-cut good positive plate, negative plate and barrier film stacked gradually by the order of barrier film, negative plate, barrier film, positive plate, barrier film and negative plate from the bottom to top be combined into electric core; The electric core that is combined into utilizes aluminium pole ears and nickel lug to carry out ultrasonic bonding; The electric core that has welded is put in the aluminum-plastic packaged shell of square; Electric core after injecting above-mentioned high temperature modification lithium-ion battery electrolytes for preparing and sealing behind 80 ℃ of baking 24h, just make the manganate lithium ion battery that battery size is 553465MS, and the design capacity of battery is 1000mAh.
Embodiment 2
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: be full of the glove box (H of argon gas
2In the O content＜10ppm); Is that 3: 1: 5 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.1mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 0.5% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid BMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid BMI-TFSI be 5% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 3
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 1: 1: 1 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 0.8mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 2% with the be made into mass percent of mixing between the lithium salt solution; Add additive package that ionic liquid PMI-TFSI and phthalic anhydride mix again as suppressing high temperature aerogenesis additive; And to add ionic liquid PMI-TFSI be 5% with the be made into mass percent of mixing between the lithium salt solution, to add phthalic anhydride be 4% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 4
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 3: 2: 5 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution; Add additive package that ionic liquid EMI-TFSI and phthalic anhydride mix again as suppressing high temperature aerogenesis additive; And to add ionic liquid EMI-TFSI be 5% with the be made into mass percent of mixing between the lithium salt solution, to add phthalic anhydride be 3% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 5
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 1: 1: 1 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 2% with the be made into mass percent of mixing between the lithium salt solution; Add additive package that ionic liquid EMI-TFSI and phthalic anhydride mix again as suppressing high temperature aerogenesis additive; And to add ionic liquid EMI-TFSI be 3% with the be made into mass percent of mixing between the lithium salt solution, to add phthalic anhydride be 2% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 6
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 3: 2: 3 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.2mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution; Add additive package that ionic liquid PMI-TFSI, ionic liquid BMI-TFSI and phthalic anhydride mix again as suppressing high temperature aerogenesis additive; And to add ionic liquid PMI-TFSI be 3% with the be made into mass percent of mixing between the lithium salt solution; To add ionic liquid BMI-TFSI be 2% with the be made into mass percent of mixing between the lithium salt solution, to add phthalic anhydride be 2% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
During actual fabrication, go out the good characteristic of high temperature modification lithium-ion battery electrolytes for checking the present invention is prepared, also done following three contrast tests simultaneously:
Contrast test one, in being full of the glove box of argon gas (H
2O＜10ppm), solvent ethylene carbonate (EC) and Methylethyl carbonic ester (EMC) are that 1: 1 mixed is even according to volume ratio, and add the LiPF of certain mass
6, be mixed with the electrolyte that concentration is 1mol/L, add mass percent simultaneously and be 2% vinylene carbonate (VC), treat electrolytic salt LiPF
6Fully after the dissolving, leave standstill 24h, promptly obtain contrasting electrolyte one.
Contrast test two, in being full of the glove box of argon gas (H
2O＜10ppm) is that 1: 1: 1 mixed is even with solvent ethylene carbonate (EC), dimethyl carbonate (DMC) and Methylethyl carbonic ester (EMC) according to volume ratio, and adds the LiPF of certain mass
6, be mixed with the electrolyte that concentration is 1mol/L, add mass percent simultaneously and be 1% film for additive vinylene carbonate (VC) and mass percent and be 2% 1.3-propane sultone (PS), leave standstill 24h, promptly obtain contrasting electrolyte two.
Contrast test three, in being full of the glove box of argon gas (H
2O＜10ppm) is that 1: 1: 1 mixed is even with solvent ethylene carbonate (EC), propene carbonate (PC) and Methylethyl carbonic ester (EMC) according to volume ratio, and adds the LiPF of certain mass
6, be mixed with the electrolyte that concentration is 1mol/L, adding mass percent simultaneously and be 2% film for additive vinylene carbonate (VC) and mass percent is 3%1.3-propane sultone (PS), leaves standstill 24h, promptly obtains contrasting electrolyte three.
At first, three kinds of electrolyte that make in six kinds of high temperature modification lithium-ion battery electrolytes being made among the embodiment 1-6 and three contrast tests are carried out the test of normal temperature 1C cycle performance:
Tester: Neware charge-discharge test appearance;
Probe temperature: ambient temperature is a room temperature, is specially 25 ℃;
Charging modes: constant-current constant-voltage charging is to 4.2V, cut-off current 0.03CmA;
Discharge mode: constant-current discharge is to 3.0V;
Charging and discharging currents: 1.0C.
Finally draw the six kinds of high temperature modification lithium-ion battery electrolytes being made among the embodiment 1-6 and the normal-temperature circulating performance test result of three contrast test electrolyte and see table 1:
Table 1 electrolyte normal-temperature circulating performance test result contrast table
Secondly, three kinds of electrolyte that make in six kinds of high temperature modification lithium-ion battery electrolytes being made among the embodiment 1-6 and three contrast tests are carried out the test of high temperature 1C cycle performance:
Tester: Neware charge-discharge test appearance;
Probe temperature: 60 ℃;
Test battery: cobalt acid lithium battery;
Charging modes: constant-current constant-voltage charging is to 4.2V, cut-off current 0.03CmA;
Discharge mode: constant-current discharge is to 3.0V;
Charging and discharging currents: 1.0C;
Finally draw the six kinds of high temperature modification lithium-ion battery electrolytes being made among the embodiment 1-6 and the high temperature cyclic performance test result of three contrast test electrolyte and see table 2:
Table 2 electrolyte high temperature cyclic performance test result contrast table
Afterwards, two kinds of electrolyte that make in six kinds of high temperature modification lithium-ion battery electrolytes being made among the embodiment 1-3 and contrast test one and 2 two contrast tests of contrast test are carried out the test of high temperature 1C cycle performance:
Tester: Neware charge-discharge test appearance;
Probe temperature: 60 ℃;
Test battery: lithium manganate battery;
Charging modes: constant-current constant-voltage charging is to 4.2V, cut-off current 0.03CmA;
Discharge mode: constant-current discharge is to 3.0V;
Charging and discharging currents: 1.0C;
The high temperature cyclic performance test result that finally draws two kinds of electrolyte that make in six kinds of high temperature modification lithium-ion battery electrolytes being made among the embodiment 1-3 and contrast test one and 2 two contrast tests of contrast test is seen table 3:
Table 3 electrolyte high temperature cyclic performance test result contrast table
Then, three kinds of high temperature modification lithium-ion battery electrolytes that made in embodiment 3,5 and 6 are carried out the high temperature storage performance test:
The storage condition: under the full power state, shelve the regular hour in certain temperature, specific as follows:
Shelve under 60 ℃ of temperature conditions 60 days, shelving 48h under 85 ℃ of temperature conditions and under 100 ℃ of temperature conditions, shelving 4h three times test;
Test battery: cobalt acid lithium battery;
Test mode: storage is cooled to room temperature after finishing, and it is carried out the 1.0C discharge, and its discharge capacity is the maintenance capacity, carries out 1.0C three weeks circulation again, and the 3rd all discharge capacities are designated as recovery capacity; Conservation rate=maintenance capacity/initial capacity, recovery rate=recovery capacity/initial capacity;
The high temperature storage The performance test results that finally draws two kinds of electrolyte that make in three kinds of high temperature modification lithium-ion battery electrolytes being made in embodiment 3,5 and 6 and contrast test one and 2 two contrast tests of contrast test is seen table 4:
Table 4 electrolyte high temperature storage The performance test results contrast table
At last, three kinds of high temperature modification lithium-ion battery electrolytes that made among the embodiment 1-3 are carried out high low temperature performance test:
Tester: climatic chamber;
Probe temperature: 55 ℃/-10 ℃/-30 ℃;
Test battery: cobalt acid lithium battery;
Charging modes: after room temperature left standstill 2h, constant-current constant-voltage charging was to 4.2V, cut-off current 0.03CmA;
Discharge mode: after under probe temperature, leaving standstill 8h, constant-current discharge is to 3.0V;
Charging and discharging currents: charging 1.0C/ discharge 0.2C.
The high low temperature performance test result that finally draws three kinds of high temperature modification lithium-ion battery electrolytes that made among the embodiment 1-3 is seen table 5:
The high low temperature performance test result of table 5 electrolyte contrast table
Embodiment 7
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 3: 3: 4 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 2mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 0.2% with the be made into mass percent of mixing between the lithium salt solution; Add additive package that ionic liquid PMI-TFSI and phthalic anhydride mix again as suppressing high temperature aerogenesis additive; And to add ionic liquid PMI-TFSI be 1% with the be made into mass percent of mixing between the lithium salt solution, to add phthalic anhydride be 0.5% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 8
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 3: 1: 5 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.6mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 0.4% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 3% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 9
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 3: 3: 5 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.4mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 0.2% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 0.8% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 2: 1: 3 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.4mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1.5% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 4% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 11
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 5: 3: 6 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.2mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 4% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 12
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 4: 3: 4 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.2mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 4% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 13
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 4: 2: 5 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.2mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 4% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
Embodiment 14
In the present embodiment, different with embodiment 1 is: during preparation electrolyte: (H in being full of the glove box of argon gas earlier
2O content＜10ppm); Is that 5: 2: 6 mixed is evenly processed non-aqueous organic solvent with solvent ethylene carbonate (EC), propene carbonate (PC) and diethyl carbonate (DEC) according to volume ratio, and the electrolytic salt that in made non-aqueous organic solvent, adds respective quality again (specifically is lithium hexafluoro phosphate LiPF
6), be mixed with the mixing lithium salt solution that amount of substance concentration is 1.2mol/L after evenly mixing.Simultaneously, in said mixing lithium salt solution, add earlier biethyl diacid lithium borate LiBOB as the high temperature film for additive and to add biethyl diacid lithium borate LiBOB be 1% with the be made into mass percent of mixing between the lithium salt solution; Add ionic liquid EMI-TFSI again as suppressing high temperature aerogenesis additive, and to add ionic liquid EMI-TFSI be 4% with the be made into mass percent of mixing between the lithium salt solution.Treat that electrolytic salt (is lithium hexafluoro phosphate LiPF
6) fully after the dissolving, leave standstill 24h, promptly obtain the high temperature modification lithium-ion battery electrolytes.
In the present embodiment, utilize the manufacture method step of the high temperature modification lithium-ion battery electrolytes making lithium ion battery that is mixed with all identical with embodiment 1 with material requested.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalent structure that above embodiment did according to the present invention, all still belongs in the protection range of technical scheme of the present invention.
Claims (5)
1. high temperature modification lithium-ion battery electrolytes; Comprise the mixing lithium salt solution that forms by electrolytic salt and the even mixed preparing of non-aqueous organic solvent; It is characterized in that: also comprise the high temperature film for additive and inhibition high temperature aerogenesis additive that evenly are blended in the said mixing lithium salt solution; Said high temperature film for additive is biethyl diacid lithium borate LiBOB, and biethyl diacid lithium borate LiBOB is 0.2%～3% with said mass percent of mixing between the lithium salt solution; Said inhibition high temperature aerogenesis additive is two kinds of ionic liquid and phthalic anhydrides, and said inhibition high temperature aerogenesis additive is 0.8%～9% with said mass percent of mixing between the lithium salt solution, and said ion liquid chemical formula does
R=CH wherein
2CH
3, CH
2CH
2CH
3Or CH
2CH
2CH
2CH
3And said ionic liquid should be ionic liquid EMI-TFSI, ionic liquid PMI-TFSI or ionic liquid BMI-TFSI mutually; The gross mass of adding the high temperature film for additive and suppressing high temperature aerogenesis additive be 1%～11% with mass percent between the said solution quality that mixes lithium salt solution; The mixed solvent of said non-aqueous organic solvent for evenly mixing by ethylene carbonate, propene carbonate and diethyl carbonate, and the volume ratio between ethylene carbonate, propene carbonate and the diethyl carbonate is 2～5 ︰, 1～3 ︰ 3～6.
2. according to the described a kind of high temperature modification lithium-ion battery electrolytes of claim 1; It is characterized in that: said electrolytic salt is one or both in lithium hexafluoro phosphate, LiBF4, biethyl diacid lithium borate and the lithium trifluoromethanesulp,onylimide, and said electrolytic salt and the said non-aqueous organic solvent amount of substance concentration of mixing lithium salt solution that forms that evenly is mixed is 0.8mol/L～1.4mol/L.
3. according to the described a kind of high temperature modification lithium-ion battery electrolytes of claim 2, it is characterized in that: said electrolytic salt is a lithium hexafluoro phosphate.
4. a lithium ion battery that utilizes high temperature modification lithium-ion battery electrolytes as claimed in claim 1 to process comprises positive pole, negative pole and barrier film, it is characterized in that: also comprise the high temperature modification lithium-ion battery electrolytes; Said positive pole is processed by cobalt acid lithium or lithium manganate material, and said negative pole is processed by material with carbon element, and said barrier film is processed by the porous polyolefin material.
5. according to the described a kind of high temperature modification lithium ion battery of claim 4, it is characterized in that: said lithium ion battery is square flexible packing lithium ion battery.
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| JP6966276B2 (en) * | 2017-09-27 | 2021-11-10 | 太陽誘電株式会社 | Electrolytes for electrochemical devices and electrochemical devices |
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| CN107910587B (en) * | 2017-12-08 | 2020-08-04 | 广州天赐高新材料股份有限公司 | Lithium secondary battery electrolyte and lithium secondary battery |
| CN111463486B (en) * | 2018-12-20 | 2023-08-01 | 江西普瑞森新能源科技有限公司 | Lithium ion battery electrolyte |
| CN109935908B (en) * | 2019-04-02 | 2022-02-08 | 合肥工业大学 | Low-concentration lithium salt electrolyte and lithium secondary battery comprising same |
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| CN114976239A (en) * | 2022-05-31 | 2022-08-30 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-safety lithium ion battery electrolyte suitable for full sea depth |
| CN116848692A (en) * | 2022-07-15 | 2023-10-03 | 宁德时代新能源科技股份有限公司 | Secondary battery, battery module, battery pack, and power consumption device |
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