CN106816635B - A kind of electrolyte and preparation method of spinel structure nickel ion doped lithium ion battery - Google Patents
A kind of electrolyte and preparation method of spinel structure nickel ion doped lithium ion battery Download PDFInfo
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Abstract
The invention discloses the electrolyte and preparation method of a kind of spinel structure nickel ion doped lithium ion battery, the electrolyte includes: organic solvent 30-60 mass parts, lithium salts 5-15 mass parts, ionic liquid 15-30 mass parts and additive 5-10 mass parts；Using lithium ion battery prepared by electrolyte provided in an embodiment of the present invention, the capacity retention ratio after recycling 3000 times under 1C multiplying power reaches 90.33%；Capacity retention ratio after recycling 1500 times under 2C multiplying power reaches 88.5%；Capacity retention ratio after recycling 800 times under 3C multiplying power reaches 85.0%.As it can be seen that electrolyte provided by the invention after charge and discharge are multiple under high voltage, different multiplying, remains to show good cycle performance.
Description
Technical field
The present invention relates to technical field of lithium ion, in particular to a kind of spinel structure nickel ion doped lithium ion battery
Electrolyte and preparation method.
Background technique
Lithium ion battery is a kind of secondary cell, it relies primarily on lithium ion, and movement carrys out work between a positive electrode and a negative electrode.
When charging, lithium ion is embedded in cathode from positive deintercalation, by electrolyte, and cathode is in lithium-rich state；It is then opposite when electric discharge.Due to
Operating voltage height, memory-less effect, self-discharge rate is small, it is big etc. significantly with energy density to have extended cycle life because having for lithium ion battery
Advantage becomes the first choice of mancarried electronic aid battery.But with the diversification of relevant device function, equipment electricity consumption module function
Consumption also constantly rises, so that the drawbacks of existing lithium ion battery positive and negative electrode material, electrolyte and conventional batteries design also gradually
It displays；For example, there is under high voltage about spinel structure nickel ion doped lithium ion battery, the cyclicity of battery is not
It is able to satisfy the problem of existing equipment needs.
Currently, high-voltage anode material has cobalt acid lithium, nickel ion doped, lithium manganese phosphate and rich lithium-magnesium containing base layed solid-solution,
The charging voltage of above-mentioned positive electrode is in 4.5V or more.For commonly based on the electrolyte of carbonate solvent for, when filling
When piezoelectric voltage reaches 4.3V, irreversible oxidative decomposition can occur on high oxidative positive electrode surface, battery occurs swollen
Gas, so as to cause the deterioration of battery cycle life and storge quality；In order to inhibit this decomposition, those skilled in the art are electric from height
Pressure positive electrode sets out, and surface is carried out to it and is modified, and contacts in order to reduce electrolyte with the direct of positive electrode, in positive material
Expect that surface coats one layer of oxide or fluoride, play the role of barrier, high rate performance and the circulation longevity of battery are improved with this
Life.However, it is the preparation process complex process of covering material, at high cost, and it is related to the Post isothermal treatment of material, easily cause packet
The change of coating and positive electrode contact interface material component；Meanwhile the clad on high-voltage anode material surface is mostly ion
Insulator is unfavorable for the abjection of lithium ion and is embedded into, and then influences the high rate performance of battery.
Thus, it is necessary to find reasonable solution in terms of electrolyte.Why crucial electrolyte is, is because of battery
During charge and discharge, lithium ion is quickly deviate from from anode, into electrolyte, then passes through diaphragm, carries out into cathode embedding
It buries, the migration of a large amount of lithium ions needs electrolyte dynamic performance with higher, has lithium ion more in mass transport process
Small resistance to mass tranfer, it is therefore desirable to which electrolyte has better wellability, lower viscosity and the resistance of lower lithium ion transport
Power；In order to realize this purpose, the solvent that those skilled in the art generally use the high conductivity of low viscosity is arranged in pairs or groups high lithium salt
Technical solution, although the height of battery can be made gentle however, this technical solution can improve the dynamic performance of electrolyte
Degradation is stored up, the cycle life of battery is also unfavorable for；In the prior art, technical staff is no lack of by commonly based on carbonic acid
Functional additive is added in the electrolyte of ester solvent, it is still, single to meet the needs of high-voltage lithium ion batteries are to electrolyte
One additive is difficult to solve the problems, such as that electrolyte is all, it is also possible to some other problems is brought, for example, electrochemistry is compatible
Difference, battery cycle life are low, etc..
Summary of the invention
Goal of the invention of the invention is to provide the electrolyte and system of a kind of spinel structure nickel ion doped lithium ion battery
Preparation Method, not being able to satisfy equipment for cycle performance existing for existing spinel structure nickel ion doped lithium ion battery with solution needs
The technical issues of wanting.
According to a first aspect of the embodiments of the present invention, a kind of electricity of spinel structure nickel ion doped lithium ion battery is provided
Liquid is solved, the electrolyte includes:
Organic solvent 30-60 mass parts；
Lithium salts 5-15 mass parts；
Ionic liquid 15-30 mass parts；
Additive 5-10 mass parts.
Preferably, the additive includes:
At least one of vinylene carbonate and vinyl vinylene carbonate；
At least one of hexamethyldisilazane, seven methyl disilazanes, triphenyl phosphite and Trimethyl phosphite；
And at least one of biphenyl, cyclohexyl benzene and phenylene dimethyl ether.
Preferably, the anion of the ionic liquid has the following structure:
Preferably, the cation of the ionic liquid is quaternary ammonium ion, piperidines ion, pyrrolidinium ion, quaternary phosphine ion, pyrazoles
At least one of ion and imidazol ion.
Preferably, the structural formula of the quaternary ammonium ion are as follows:
The structural formula of the piperidines ion are as follows:
The structural formula of the pyrrolidinium ion are as follows:
The structural formula of the quaternary phosphine ion are as follows:
The structural formula of the pyrazolium ion are as follows:
The structural formula of the imidazol ion are as follows:
Wherein, R1~R4And R18~R21It is each independently the alkyl or replace alkyl that carbon atom number is 1~8；R5、R6、
R12、R13、R26、R31It is each independently the alkyl that carbon atom number is 1~6；R7~R11、R14~R17、R22~R25、R27~R30Respectively
From independently be hydrogen atom, halogen atom or carbon atom number be 1~6 alkyl or replace alkyl.
Preferably, the organic solvent includes ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, carbon
One of sour methyl ethyl ester, dibutyl carbonate, methyl propyl carbonate, ethyl propyl carbonic acid ester, ethyl butyl carbonate, fluorine-containing carbonic ester are several
Kind.
Preferably, the structural formula of the fluorine-containing carbonic ester are as follows:
Wherein, Rh is H or hydrocarbon chain group, Rf are H (CF2CF2)n1CH2 —、F(CF2CF2)n2CH2CH2 —Or CF3CF2CF2O
(CF(CF3)CF2O)n3CF(CF3)CH2 —, n1、n2For positive integer, n3For nonnegative integer.
Preferably, the lithium salts includes lithium hexafluoro phosphate, LiBF4, lithium perchlorate, trifluoromethyl sulfonic acid lithium, chlorination
One or more of lithium, lithium iodide, lithium aluminate, hexafluoroarsenate lithium, fluoro sulfimide lithium.
The another aspect of embodiment according to the present invention provides a kind of spinel structure nickel ion doped lithium ion battery battery
The preparation method of liquid is solved, described method includes following steps:
Organic solvent and ionic liquid are weighed, in the environment of humidity is less than 8ppm, temperature is 25 ± 1 DEG C, is had described
Solvent and the ionic liquid stir evenly, and obtain non-aqueous organic solvent；
Lithium salts is weighed, the lithium salts is slowly added into the non-aqueous organic solvent, stirring to lithium salts is completely dissolved；
Additive is weighed, the additive is slowly added into the non-aqueous organic solvent dissolved with lithium salts, stirring is quiet
It sets, obtains spinel structure nickel ion doped lithium-ion battery electrolytes.
From the above technical scheme, the present invention provides a kind of electrolysis of spinel structure nickel ion doped lithium ion battery
Liquid and preparation method, the electrolyte include organic solvent 30-60 mass parts, lithium salts 5-15 mass parts, ionic liquid 15-30 matter
Measure part, additive 5-10 mass parts；The additive include: in vinylene carbonate and vinyl vinylene carbonate at least
It is a kind of；At least one of hexamethyldisilazane, seven methyl disilazanes, triphenyl phosphite and Trimethyl phosphite；With
And at least one of biphenyl, cyclohexyl benzene and phenylene dimethyl ether；The cation of the ionic liquid preferably quaternary phosphine ion；It is described to have
Solvent is the mixture of one or more of carbonats compounds；The lithium prepared using electrolyte provided in an embodiment of the present invention
Ion battery, the capacity retention ratio after recycling 3000 times under 1C multiplying power reach 90.33%；After being recycled 1500 times under 2C multiplying power
Capacity retention ratio reach 88.5%；Capacity retention ratio after recycling 800 times under 3C multiplying power reaches 85.0%；As it can be seen that this hair
The electrolyte of bright offer remains to show good cycle performance after charge and discharge are multiple under high voltage, different multiplying.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is that the electrolyte that the embodiment of the present invention 1, embodiment 2, comparative example 1 and comparative example 2 provide is applied to point crystalline substance
1C cycle performance test chart when stone structure lithium ion battery；
Fig. 2 is that the electrolyte that the embodiment of the present invention 1, embodiment 2, comparative example 1 and comparative example 2 provide is applied to point crystalline substance
2C cycle performance test chart when stone structure lithium ion battery；
Fig. 3 is that the electrolyte that the embodiment of the present invention 1, embodiment 2, comparative example 1 and comparative example 2 provide is applied to point crystalline substance
3C cycle performance test chart when stone structure lithium ion battery.
Wherein, the 1C cyclic curve of 1- embodiment 1, the 1C cyclic curve of 2- embodiment 2, the 1C of 3- comparative example 2 recycle bent
Line, the 1C cyclic curve of 4- comparative example 1, the 2C cyclic curve of 5- embodiment 1, the 2C cyclic curve of 6- embodiment 2,7- comparative example
2 2C cyclic curve, the 2C cyclic curve of 8- comparative example 1, the 3C cyclic curve of 9- embodiment 1, the 3C circulation of 10- embodiment 2
Curve, the 3C cyclic curve of 11- comparative example 2, the 3C cyclic curve of 12- comparative example 1.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Whole description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment according to the present invention is in a first aspect, provide a kind of electricity of spinel structure nickel ion doped lithium ion battery
Liquid is solved, the electrolyte includes:
Organic solvent 30-60 mass parts；
Lithium salts 5-15 mass parts；
Ionic liquid 15-30 mass parts；
Additive 5-10 mass parts.
Preferably, the additive includes:
At least one of vinylene carbonate and vinyl vinylene carbonate；
At least one of hexamethyldisilazane, seven methyl disilazanes, triphenyl phosphite and Trimethyl phosphite；
And at least one of biphenyl, cyclohexyl benzene and phenylene dimethyl ether.
Wherein, vinylene carbonate or vinyl vinylene carbonate can be formed on lithium ion battery negative material surface
Organic solid electrolyte interface (SEI) film, can prevent the stripping problem of negative electrode material, meanwhile, guarantee the cycle performance of battery；
Hexamethyldisilazane, seven methyl disilazanes, triphenyl phosphite or Trimethyl phosphite, which can play, to be prevented in electrolyte
Organic compound combustion or explosion guarantee the safety of battery；Biphenyl, cyclohexyl benzene and phenylene dimethyl ether can be in spread of voltage or mistakes
When amount charging, the safety that is further ensured that the stability of battery performance and uses.
Preferably, the anion of the ionic liquid has the following structure:
Preferably, the cation of the ionic liquid is quaternary ammonium ion, piperidines ion, pyrrolidinium ion, quaternary phosphine ion, pyrazoles
At least one of ion and imidazol ion.
Preferably, the structural formula of the quaternary ammonium ion are as follows:
The structural formula of the piperidines ion are as follows:
The structural formula of the pyrrolidinium ion are as follows:
The structural formula of the quaternary phosphine ion are as follows:
The structural formula of the pyrazolium ion are as follows:
The structural formula of the imidazol ion are as follows:
Wherein, R1~R4And R18~R21It is each independently the alkyl or replace alkyl that carbon atom number is 1~8；R5、R6、
R12、R13、R26、R31It is each independently the alkyl that carbon atom number is 1~6；R7~R11、R14~R17、R22~R25、R27~R30Respectively
From independently be hydrogen atom, halogen atom or carbon atom number be 1~6 alkyl or replace alkyl.
The addition of ionic liquid can be such that solubility of the lithium salts in the solvent increases, reduce the viscosity of electrolyte, from
And reduce the resistance to mass tranfer of lithium ion, also make the conductivity of electrolyte higher, thus improve leaching of the electrolyte for electrode plates
Lubricant nature energy；Meanwhile the addition of ionic liquid, other compound ions and the ionic liquid in electrolyte can be made to generate network
Close, and due to the high molecular weight of ionic liquid, the battery for avoiding different batches from producing due to standing time not
Together, the layering for causing electrolyte different degrees of, to avoid the difference of the battery generation performance of different batches.
Preferably, the organic solvent includes ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, carbon
One of sour methyl ethyl ester, dibutyl carbonate, methyl propyl carbonate, ethyl propyl carbonic acid ester, ethyl butyl carbonate, fluorine-containing carbonic ester are several
Kind.
Preferably, the structural formula of the fluorine-containing carbonic ester are as follows:
Wherein, Rh is H or hydrocarbon chain group, Rf are H (CF2CF2)n1CH2 —、F(CF2CF2)n2CH2CH2 —Or CF3CF2CF2O
(CF(CF3)CF2O)n3CF(CF3)CH2 —, n1、n2For positive integer, n3For nonnegative integer.
The carbonats compounds such as included ethylene carbonate and propene carbonate in organic solvent provided by the invention
It is the solvent with high dielectric constant, is conducive to the dissolution of lithium salts, the promotion of battery high-temperature and cycle performance.
Preferably, the lithium salts includes lithium hexafluoro phosphate, LiBF4, lithium perchlorate, trifluoromethyl sulfonic acid lithium, chlorination
One or more of lithium, lithium iodide, lithium aluminate, hexafluoroarsenate lithium, fluoro sulfimide lithium.
According to another aspect of an embodiment of the present invention, a kind of spinel structure nickel ion doped lithium ion battery electrolysis is provided
The preparation method of liquid, described method includes following steps:
Organic solvent and ionic liquid are weighed, in the case where humidity is less than 8ppm, temperature is 25 ± 1 DEG C, by the organic solvent
It is stirred evenly with the ionic liquid, obtains non-aqueous organic solvent；
Lithium salts is weighed, the lithium salts is slowly added into the non-aqueous organic solvent, stirring to lithium salts is completely dissolved；
Additive is weighed, the additive is slowly added into the non-aqueous organic solvent dissolved with lithium salts, stirring is quiet
It sets, obtains spinel structure nickel ion doped lithium-ion battery electrolytes.
For the specific embodiment of the electrolyte of spinel structure nickel ion doped lithium ion battery provided by the invention, ask
Referring to following embodiment and comparative example:
Embodiment 1
In the glove box full of argon gas, by diethyl carbonate, propene carbonate and dibutyl carbonate by mass fraction point
Not Wei 15,15 and 25 mixing, be stirred continuously to uniform, being slow added into mass fraction is 25 ionic liquids, is obtained non-aqueous organic
Solvent；The trifluoromethyl sulfonic acid lithium that mass fraction is 12 is added into the non-aqueous organic solvent again, to the trifluoromethyl sulphur
After sour lithium is completely dissolved, be further continued for being added triphenyl phosphite, mass fraction that mass fraction is 2 be 3 vinylene carbonates with
And the cyclohexyl benzene that mass fraction is 3, spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing evenly.
Wherein, the ionic liquid cation Wei quaternary phosphine ion；In the glove box humidity be less than 8ppm, temperature be 25 ±
1℃。
Embodiment 2
In the glove box full of argon gas, by diethyl carbonate, propene carbonate and dibutyl carbonate by mass fraction point
Not Wei 15,15 and 25 mixing, be stirred continuously to uniform, being slow added into mass fraction is 15 ionic liquids, is obtained non-aqueous organic
Solvent；The trifluoromethyl sulfonic acid lithium that mass fraction is 12 is added into the non-aqueous organic solvent again, to the trifluoromethyl sulphur
After sour lithium is completely dissolved, be further continued for being added triphenyl phosphite, mass fraction that mass fraction is 2 be 3 vinylene carbonates with
And the cyclohexyl benzene that mass fraction is 3, spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing evenly.
Wherein, the ionic liquid cation Wei quaternary phosphine ion；In the glove box humidity be less than 8ppm, temperature be 25 ±
1℃。
Embodiment 3
In the glove box full of argon gas, by diethyl carbonate, propene carbonate and dibutyl carbonate by mass fraction point
Not Wei 15,15 and 25 mixing, be stirred continuously to uniform, being slow added into mass fraction is 20 ionic liquids, is obtained non-aqueous organic
Solvent；The trifluoromethyl sulfonic acid lithium that mass fraction is 12 is added into the non-aqueous organic solvent again, to the trifluoromethyl sulphur
After sour lithium is completely dissolved, be further continued for being added triphenyl phosphite, mass fraction that mass fraction is 2 be 3 vinylene carbonates with
And the cyclohexyl benzene that mass fraction is 3, spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing evenly.
Wherein, the ionic liquid cation Wei quaternary phosphine ion；In the glove box humidity be less than 8ppm, temperature be 25 ±
1℃。
Embodiment 4
In the glove box full of argon gas, by diethyl carbonate, propene carbonate and dibutyl carbonate by mass fraction point
Not Wei 15,15 and 25 mixing, be stirred continuously to uniform, being slow added into mass fraction is 25 ionic liquids, is obtained non-aqueous organic
Solvent；The trifluoromethyl sulfonic acid lithium that mass fraction is 12 is added into the non-aqueous organic solvent again, to the trifluoromethyl sulphur
After sour lithium is completely dissolved, be further continued for being added triphenyl phosphite, mass fraction that mass fraction is 4 be 3 vinylene carbonates with
And the cyclohexyl benzene that mass fraction is 3, spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing evenly.
Wherein, the ionic liquid cation Wei quaternary phosphine ion；In the glove box humidity be less than 8ppm, temperature be 25 ±
1℃。
It should be noted that the mass fraction that is provided into embodiment 4 of above-described embodiment 1 be 15 diethyl carbonate, matter
The propene carbonate that number is 15 and the dibutyl carbonate that mass fraction is 25 are measured as organic solvent, total mass fraction
It is 55；The organic solvent of 55 mass parts is not limited only to diethyl carbonate, the carbonic acid that the embodiment of the present invention 1 is provided to embodiment 4
The mixture of acrylic ester and dibutyl carbonate can also have other carbonats compounds substitution；For example, it may be 55 mass
Part ethylene carbonate, propene carbonate and dimethyl carbonate mixture, can also be 55 mass parts propene carbonate,
The mixture of dimethyl carbonate, diethyl carbonate and methyl ethyl carbonate can also be methyl propyl carbonate, the carbonic acid of 55 mass parts
The mixture of second propyl ester and ethyl butyl carbonate, details are not described herein.
Comparative example 1
In the glove box full of argon gas, by diethyl carbonate, propene carbonate and dibutyl carbonate by mass fraction point
Not Wei 27,30 and 31 mixing, be stirred continuously to uniform, obtain non-aqueous organic solvent；It is added again into the non-aqueous organic solvent
The trifluoromethyl sulfonic acid lithium that mass fraction is 12 obtains spinel structure nickel after the trifluoromethyl sulfonic acid lithium is completely dissolved
Manganate lithium ion battery electrolyte.
The five kinds of electrolyte provided in above-described embodiment 1 to embodiment 4 and comparative example 1, which are injected separately into capacity, is
In 60AH Soft Roll square battery, five kinds of Soft Roll square batteries with different electrolytes are obtained, wherein after injection electrolyte, note
Time of penetration is shelved needed for record, the results are shown in Table 1:
Table 1
As shown in Table 1, the electrolyte that the embodiment of the present invention 1 is provided to embodiment 4, the electrolysis liquid phase provided with comparative example 1
Than being effectively reduced for shelving penetration period needed for electrode plates, illustrating that the embodiment of the present invention 1 to embodiment 5 provides
Electrolyte constituent and mass fraction can be effectively improved the wellability of electrolyte.Wherein, embodiment 1 and embodiment 4
The time of penetration of provided electrolyte is most short, only 7h, and the time of penetration for the electrolyte that embodiment 3 provides is taken second place, and is 9h, real
Apply example 2 offer electrolyte time of penetration longest, be 12h, still, embodiment 2 compared with the time of penetration 54h of comparative example 1,
42h is reduced.
It is worth noting that, embodiment 1 to embodiment 3 the mass fraction that the difference is that only ionic liquid change
Change；The variation that the difference is that only additive mass fraction of embodiment 1 and embodiment 4；Wherein, required time of penetration is most short
Embodiment 1 and the mass fraction of ionic liquid of embodiment 4 be 25 parts, the mass fraction of 3 intermediate ion liquid of embodiment is
20 parts, the mass fraction of 4 intermediate ion liquid of embodiment is 15 parts；It can thus be seen that the leaching from electrolyte for electrode plates
From the point of view of lubricant nature angle, the mass fraction of ionic liquid is higher, and wellability is better, quality of the embodiment of the present invention for ionic liquid
Preferably 25 parts of number.
It should be noted that the addition of ionic liquid, increases solubility of the lithium salts in the solvent, reduces electrolyte
Viscosity also make the conductivity of electrolyte higher to reduce the resistance to mass tranfer of lithium ion, thus improve electrolyte for electrode
The wetting property of pole piece；Meanwhile the addition of ionic liquid, other compound ions and the ionic liquid in electrolyte can be made
Body generates complexing, and due to the high molecular weight of ionic liquid, and the battery for avoiding different batches from producing is due to placing
The difference of time, and the layering for causing electrolyte different degrees of, to avoid the difference of the battery generation performance of different batches.
It is 60AH to above-mentioned rated capacity according to the test method that GB T31484-2015 and GB T31485-2015 are provided
Above-mentioned five kinds of Soft Roll square batteries carry out cycle performance test, specifically:
The condition of cycle performance test is carried out to above-mentioned five kinds of Soft Roll square batteries are as follows:
At 25 DEG C, it is 4.95V that constant-current constant-voltage charging to voltage is carried out under 1C current value and 5.0V voltage, in 180A electricity
Constant-current discharge is carried out under flow valuve to voltage to terminate when 2.65V, is recycled 3000 times, is charged and discharged test；
At 25 DEG C, it is 4.95V that constant-current constant-voltage charging to voltage is carried out under 2C current value and 5.0V voltage, in 180A electricity
Constant-current discharge is carried out under flow valuve to voltage to terminate when 2.65V, is recycled 1500 times, is charged and discharged test；
At 25 DEG C, it is 4.95V that constant-current constant-voltage charging to voltage is carried out under 3C current value and 5.0V voltage, in 180A electricity
Constant-current discharge is carried out under flow valuve to voltage to terminate when 2.65V, is recycled 800 times, is charged and discharged test；
Obtain that the results are shown in Table 2:
Table 2
As shown in Table 2, the soft-type side's packet battery prepared using electrolyte provided by the embodiment of the present invention 1 to embodiment 4
Cycle performance compared with comparative example 1, obtained large increase, specifically, under 1C multiplying power, circulation 3000 times after, implement
The capacity highest of example 4, reaches 53.1AH；Under 2C multiplying power, after circulation 1500 times, the capacity highest of embodiment 4 reaches
51.8AH；Under 3C multiplying power, circulation 800 times after or embodiment 4 capacity highest, reach 50.5AH.
Further the capacity data in table 2 is calculated, obtains capacity retention ratio data shown in table 3:
Table 3
The capacity retention ratio data provided table 3 are analyzed, and can more intuitively be found out, the embodiment of the present invention 1 to reality
The electrolyte of the offer of example 4 is applied, compared with comparative example 1, cycle performance is greatly improved, wherein embodiment 4 is in 1C multiplying power
After lower circulation 3000 times, capacity retention ratio reaches 88.50%；After recycling 1500 times under 2C multiplying power, capacity retention ratio reaches
86.33%；After recycling 800 times under 3C multiplying power, capacity retention ratio reaches 84.17%.
The embodiment of the present invention 4 is superior to comparative example 1 and implements no matter from wellability angle, or from cycle performance angle
Example 1 is to embodiment 3, unlike comparative example 1, in the electrolyte composition that embodiment 4 provides, further include mass fraction be 25 from
Triphenyl phosphite that sub- liquid, mass fraction are 4, the hexamethylene that mass fraction is 3 vinylene carbonates and mass fraction is 3
Base benzene；Unlike embodiment 1 to embodiment 3, in the electrolyte composition that embodiment 4 provides, the mass fraction of ionic liquid
It is 25.
Embodiment 5
In the glove box full of argon gas, methyl propyl carbonate, fluorine-containing carbonic ester, propene carbonate and dibutyl carbonate are pressed
Mass fraction is respectively 10,10,15 and 25 mixing, is stirred continuously to uniform, and being slow added into mass fraction is 20 ionic liquids,
Obtain non-aqueous organic solvent；The LiBF4 and mass fraction that mass fraction is 4 is added into the non-aqueous organic solvent again
It after the LiBF4 and the lithium hexafluoro phosphate are completely dissolved is further continued for that mass fraction is added for 6 lithium hexafluoro phosphate
Vinyl vinylene carbonate, the phenylene dimethyl ether that mass fraction is 3 seven methyl disilazanes and mass fraction is 4 for 3, are stirred
Spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing uniformly.
Wherein, the cation of the ionic liquid is pyrrolidinium ion；Humidity is less than 8ppm, temperature 25 in the glove box
±1℃。
Embodiment 6
In the glove box full of argon gas, methyl propyl carbonate, fluorine-containing carbonic ester, propene carbonate and dibutyl carbonate are pressed
Mass fraction is respectively 10,10,15 and 25 mixing, is stirred continuously to uniform, and being slow added into mass fraction is 15 ionic liquids,
Obtain non-aqueous organic solvent；The LiBF4 and mass fraction that mass fraction is 4 is added into the non-aqueous organic solvent again
It after the LiBF4 and the lithium hexafluoro phosphate are completely dissolved is further continued for that mass fraction is added for 6 lithium hexafluoro phosphate
Vinyl vinylene carbonate, the phenylene dimethyl ether that mass fraction is 2 seven methyl disilazanes and mass fraction is 3 for 2, are stirred
Spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing uniformly.
Wherein, the cation of the ionic liquid is pyrrolidinium ion；Humidity is less than 8ppm, temperature 25 in the glove box
±1℃。
Embodiment 7
In the glove box full of argon gas, methyl propyl carbonate, fluorine-containing carbonic ester, propene carbonate and dibutyl carbonate are pressed
Mass fraction is respectively 10,10,15 and 25 mixing, is stirred continuously to uniform, and being slow added into mass fraction is 25 ionic liquids,
Obtain non-aqueous organic solvent；The LiBF4 and mass fraction that mass fraction is 4 is added into the non-aqueous organic solvent again
It after the LiBF4 and the lithium hexafluoro phosphate are completely dissolved is further continued for that mass fraction is added for 6 lithium hexafluoro phosphate
Vinyl vinylene carbonate, the phenylene dimethyl ether that mass fraction is 3 seven methyl disilazanes and mass fraction is 4 for 3, are stirred
Spinel structure nickel ion doped lithium-ion battery electrolytes are obtained after mixing uniformly.
Wherein, the cation of the ionic liquid is pyrrolidinium ion；Humidity is less than 8ppm, temperature 25 in the glove box
±1℃。
It should be noted that the mass fraction that is provided into embodiment 7 of above-described embodiment 5 be 10 methyl propyl carbonate, matter
Measure number be 10 fluorine-containing carbonic ester, mass fraction be 15 propene carbonate and mass fraction be 25 dibutyl carbonate
For mixture as organic solvent, total mass fraction is 60；The organic solvent of 60 mass parts is not limited only to implementation of the present invention
The mixture of methyl propyl carbonate, fluorine-containing carbonic ester, propene carbonate and dibutyl carbonate that example 5 is provided to embodiment 7, may be used also
To there is other carbonats compounds substitution；For example, it may be the diethyl carbonate of 60 mass parts, methyl ethyl carbonate and carbonic acid
The mixture of second butyl ester can also be ethylene carbonate, dimethyl carbonate, ethyl propyl carbonic acid ester and the methyl ethyl carbonate of 60 mass parts
The mixture of ester can also be the mixture of the methyl propyl carbonates of 60 mass parts, ethyl propyl carbonic acid ester and ethyl butyl carbonate, herein
It repeats no more.
Comparative example 2
In the glove box full of argon gas, methyl propyl carbonate, fluorine-containing carbonic ester, propene carbonate and dibutyl carbonate are pressed
Mass fraction is respectively 20,20,20 and 30 mixing, is stirred continuously to uniform, obtains non-aqueous organic solvent；Non-aqueous have to described again
The LiBF4 that mass fraction is 4 and the lithium hexafluoro phosphate that mass fraction is 6 are added in solvent, to the LiBF4
After being completely dissolved with the lithium hexafluoro phosphate, spinel structure nickel ion doped lithium-ion battery electrolytes are obtained.
Wherein, the cation of the ionic liquid is pyrrolidinium ion；Humidity is less than 8ppm, temperature 25 in the glove box
±1℃。
The four kinds of electrolyte provided in above-described embodiment 5 to embodiment 7 and comparative example 2, which are injected separately into capacity, is
In 60AH Soft Roll square battery, four kinds of Soft Roll square batteries with different electrolytes are obtained, wherein after injection electrolyte, note
Time of penetration is shelved needed for record, the results are shown in Table 4:
Table 4
As shown in Table 4, the electrolyte that the embodiment of the present invention 5 is provided to embodiment 7, the electrolysis liquid phase provided with comparative example 2
Than being effectively reduced for shelving penetration period needed for electrode plates, illustrating that the embodiment of the present invention 5 to embodiment 7 provides
Electrolyte constituent and mass fraction can be effectively improved the wellability of electrolyte.
Wherein, the time of penetration of electrolyte provided by embodiment 7 is most short, only 5h, the electrolyte that embodiment 5 provides
Time of penetration is taken second place, and is 6h, and the time of penetration longest for the electrolyte that embodiment 6 provides is 13h, still, embodiment 6 and comparison
The time of penetration 50h of example 2 is compared, and has reduced 37h.
It is worth noting that, embodiment 6 and embodiment 5 the difference is that, ionic liquid mass fraction and additive
The variation of mass fraction；The variation that the difference is that only ionic liquid mass fraction of embodiment 7 and embodiment 5；Wherein, institute
The mass fraction for needing the ionic liquid of the shortest embodiment 7 of time of penetration is 25 parts, the mass fraction of 5 intermediate ion liquid of embodiment
It is 20 parts, the mass fraction of 6 intermediate ion liquid of embodiment is 15 parts, it can thus be seen that from electrolyte for electrode plates
From the point of view of wellability angle, the mass fraction of ionic liquid is higher, and wellability is better, matter of the embodiment of the present invention for ionic liquid
Preferably 25 parts of number of amount.
According to GB T31484-2015 and GB T31485-2015 provide test method, to based on the above embodiment 5 to
The cycle performance of 2 four kinds of Soft Roll square batteries of embodiment 7 and comparative example is tested, specifically:
The condition of cycle performance test is carried out to above-mentioned five kinds of Soft Roll square batteries are as follows:
At 25 DEG C, it is 4.95V that constant-current constant-voltage charging to voltage is carried out under 1C current value and 5.0V voltage, in 180A electricity
Constant-current discharge is carried out under flow valuve to voltage to terminate when 2.65V, is recycled 3000 times, is charged and discharged test；
At 25 DEG C, it is 4.95V that constant-current constant-voltage charging to voltage is carried out under 2C current value and 5.0V voltage, in 180A electricity
Constant-current discharge is carried out under flow valuve to voltage to terminate when 2.65V, is recycled 1500 times, is charged and discharged test；
At 25 DEG C, it is 4.95V that constant-current constant-voltage charging to voltage is carried out under 3C current value and 5.0V voltage, in 180A electricity
Constant-current discharge is carried out under flow valuve to voltage to terminate when 2.65V, is recycled 800 times, is charged and discharged test；
Obtain that the results are shown in Table 5:
Table 5
As shown in Table 5, the soft-type side's packet battery prepared using electrolyte provided by the embodiment of the present invention 5 to embodiment 7
Cycle performance compared with comparative example 2, obtained large increase, specifically, under 1C multiplying power, circulation 3000 times after, implement
The capacity highest of example 7, reaches 54.2AH；Under 2C multiplying power, after circulation 1500 times, the capacity highest of embodiment 7 reaches
53.1AH；Under 3C multiplying power, circulation 800 times after or embodiment 7 capacity highest, reach 51.0AH.
Further the capacity data in table 5 is calculated, obtains capacity retention ratio data shown in table 6:
Table 6
The capacity retention ratio data provided table 6 are analyzed, and can more intuitively be found out, the embodiment of the present invention 5 to reality
The electrolyte of the offer of example 7 is applied, compared with comparative example 2, cycle performance is greatly improved, wherein embodiment 7 is in 1C multiplying power
After lower circulation 3000 times, capacity retention ratio reaches 90.33%；After recycling 1500 times under 2C multiplying power, capacity retention ratio reaches
88.50%；After recycling 800 times under 3C multiplying power, capacity retention ratio reaches 85.0%.
The embodiment of the present invention 7 is superior to comparative example 2 and implements no matter from wellability angle, or from cycle performance angle
Example 5 is to embodiment 6, unlike comparative example 2, in the electrolyte composition that embodiment 7 provides, further include mass fraction be 25 from
The vinyl carbon that lithium hexafluoro phosphate that LiBF4 that sub- liquid, mass fraction are 4, mass fraction are 6, mass fraction are 3
The phenylene dimethyl ether that sour vinylene, mass fraction are 3 seven methyl disilazanes and mass fraction is 4.
It can in conjunction with Fig. 1, Fig. 2 and Fig. 3 according to above-described embodiment 1 to embodiment 7 and comparative example 1 to comparative example 2
To find out, electrolyte provided by the invention under the high voltage of 5.0V, be still able to maintain good higher capacity and preferably
Cycle performance, meanwhile, electrolyte is also effectively improved the wellability of electrode plates, saves and shelves time of penetration.
From the above technical scheme, the present invention provides a kind of electrolysis of spinel structure nickel ion doped lithium ion battery
The group of liquid and preparation method, the electrolyte becomes organic solvent 30-60 mass parts, lithium salts 5-15 mass parts, ionic liquid 15-
30 mass parts, additive 5-10 mass parts；The constituent of the additive are as follows: vinylene carbonate and vinyl carbonic acid Asia second
At least one of enester；In hexamethyldisilazane, seven methyl disilazanes, triphenyl phosphite and Trimethyl phosphite
It is at least one；And at least one of biphenyl, cyclohexyl benzene and phenylene dimethyl ether；The preferred quaternary phosphine of cation of the ionic liquid
Ion；The organic solvent is the mixture of one or more of carbonats compounds；Using electricity provided in an embodiment of the present invention
The lithium ion battery of liquid preparation is solved, the capacity retention ratio after recycling 3000 times under 1C multiplying power reaches 90.33%；Under 2C multiplying power
Capacity retention ratio after circulation 1500 times reaches 88.5%；Capacity retention ratio after recycling 800 times under 3C multiplying power reaches
85.0%；As it can be seen that electrolyte provided by the invention after charge and discharge are multiple under high voltage, different multiplying, remain to show it is good
Cycle performance.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to of the invention its
Its embodiment.This application is intended to cover any variations, uses, or adaptations of the invention, these modifications, purposes or
Person's adaptive change follows general principle of the invention and including the undocumented common knowledge in the art of the present invention
Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following
Claim is pointed out.
It should be understood that the present invention is not limited to the precise structure already described above and shown in the accompanying drawings, and
And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.
Claims (7)
1. a kind of electrolyte of spinel structure nickel ion doped lithium ion battery, which is characterized in that the electrolyte includes:
Organic solvent 30-60 mass parts；
Lithium salts 5-15 mass parts；
Ionic liquid 15-30 mass parts；
Additive 5-10 mass parts；
The anion of the ionic liquid has the following structure:
The cation of the ionic liquid is quaternary ammonium ion, piperidines ion, pyrrolidinium ion, quaternary phosphine ion, pyrazolium ion and miaow
At least one of oxazolinium ion.
2. the electrolyte of spinel structure nickel ion doped lithium ion battery according to claim 1, which is characterized in that described
Additive includes:
At least one of vinylene carbonate and vinyl vinylene carbonate；
At least one of hexamethyldisilazane, seven methyl disilazanes, triphenyl phosphite and Trimethyl phosphite；
And at least one of biphenyl, cyclohexyl benzene and phenylene dimethyl ether.
3. the electrolyte of spinel structure nickel ion doped lithium ion battery according to claim 2, which is characterized in that described
The structural formula of quaternary ammonium ion are as follows:
The structural formula of the piperidines ion are as follows:
The structural formula of the pyrrolidinium ion are as follows:
The structural formula of the quaternary phosphine ion are as follows:
The structural formula of the pyrazolium ion are as follows:
The structural formula of the imidazol ion are as follows:
Wherein, R1~R4And R18~R21It is each independently the alkyl or replace alkyl that carbon atom number is 1~8；R5、R6、R12、
R13、R26、R31It is each independently the alkyl that carbon atom number is 1~6；R7~R11、R14~R17、R22~R25、R27~R30Respectively solely
It is on the spot the alkyl or replace alkyl that hydrogen atom, halogen atom or carbon atom number are 1~6.
4. the electrolyte of spinel structure nickel ion doped lithium ion battery according to claim 1, which is characterized in that described
Organic solvent includes ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, two fourth of carbonic acid
One or more of ester, methyl propyl carbonate, ethyl propyl carbonic acid ester, ethyl butyl carbonate and fluorine-containing carbonic ester.
5. the electrolyte of spinel structure nickel ion doped lithium ion battery according to claim 4, which is characterized in that described
The structural formula of fluorine-containing carbonic ester are as follows:
Wherein, Rh is H or hydrocarbon chain group, Rf are H (CF2CF2)n1CH2 —、F(CF2CF2)n2CH2CH2 —Or CF3CF2CF2O(CF
(CF3)CF2O)n3CF(CF3)CH2 —, n1、n2For positive integer, n3For nonnegative integer.
6. the electrolyte of spinel structure nickel ion doped lithium ion battery according to claim 1, which is characterized in that described
Lithium salts includes lithium hexafluoro phosphate, LiBF4, lithium perchlorate, trifluoromethyl sulfonic acid lithium, lithium chloride, lithium iodide, lithium aluminate, six
One or more of fluorine arsenic acid lithium and fluoro sulfimide lithium.
7. a kind of preparation method of spinel structure nickel ion doped lithium-ion battery electrolytes, which is characterized in that the method packet
Include following steps:
Organic solvent and ionic liquid are weighed, it, will be described organic molten in the environment of humidity is less than 8ppm, temperature is 25 ± 1 DEG C
Agent and the ionic liquid stir evenly, and obtain non-aqueous organic solvent；
Lithium salts is weighed, the lithium salts is slowly added into the non-aqueous organic solvent, stirring to lithium salts is completely dissolved；
Additive is weighed, the additive is slowly added into the non-aqueous organic solvent dissolved with lithium salts, is stirred, stands, obtains
To spinel structure nickel ion doped lithium-ion battery electrolytes；
The anion of the ionic liquid has the following structure:
The cation of the ionic liquid is quaternary ammonium ion, piperidines ion, pyrrolidinium ion, quaternary phosphine ion, pyrazolium ion and miaow
At least one of oxazolinium ion.
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