CN103311571A - Lithium ion secondary battery and electrolyte thereof - Google Patents
Lithium ion secondary battery and electrolyte thereof Download PDFInfo
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- CN103311571A CN103311571A CN2013101910175A CN201310191017A CN103311571A CN 103311571 A CN103311571 A CN 103311571A CN 2013101910175 A CN2013101910175 A CN 2013101910175A CN 201310191017 A CN201310191017 A CN 201310191017A CN 103311571 A CN103311571 A CN 103311571A
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Abstract
The invention discloses a lithium ion secondary battery and an electrolyte thereof. The electrolyte comprises lithium salt, a non-water solvent and an addition agent, wherein the addition agent comprises linear borate; the mass percentage of the linear borate in the electrolyte is 0.2-5%. Compared with the prior art, the lithium ion secondary battery and the electrolyte have the advantages that the linear borate is added into the electrolyte of the lithium ion secondary battery, so that the high-temperature performance of the battery is obviously improved, the expanding time for reaching the same thickness is obviously prolonged when the battery is stored at a high temperature, and the actual utilization of the battery is easy to realize.
Description
Technical field
The invention belongs to field of lithium ion secondary, more particularly, the present invention relates to a kind of lithium rechargeable battery and electrolyte thereof.
Background technology
With respect to lead-acid battery, Ni-MH battery, nickel-cadmium cell, lithium rechargeable battery has higher energy density and longer cycle life, has been widely used at present consumer electronics field.Because the applied environment of consumption electronic product is varied, therefore for satisfying actual needs, lithium rechargeable battery need to have preferably high-temperature behavior, can not expand after being mainly manifested in long-term use.This is because consumption electronic product has frivolous characteristics mostly, is used for placing the limited space of lithium rechargeable battery, and the obvious expansion of battery will strut the shell of consumption electronic product and affect normal use.
High temperature storage is an important test of lithium rechargeable battery, its way is after lithium rechargeable battery is completely filled, be positioned in the baking oven of uniform temperature, the most often test is 60 degrees centigrade, the some days test battery one-tenth-value thickness 1/10s in every interval, and the thickness value that increases compared with initial value, the ratio General Requirements is less than 10%.
But along with becoming increasingly abundant of consumption electronic product function, its requirement to energy content of battery density is more and more higher.The use voltage that improves battery can improve the energy density of battery significantly, has reduced simultaneously also the high-temperature storage performance of battery, so that the easier flatulence of battery.For example, high temperature storage 4.2V battery system in order is designed into 4.3V, 4.4V or more during high voltage, the current potential of negative electrode can be higher, also easier at high temperature reacting with electrolyte and cause obvious cell thickness to expand.
In view of this, necessaryly provide a kind of lithium rechargeable battery and electrolyte thereof with good properties at high temperature.
Summary of the invention
The object of the invention is to: a kind of lithium rechargeable battery and electrolyte thereof with good properties at high temperature is provided.
In order to realize the foregoing invention purpose, the inventor finds to add a small amount of linear borate in electrolyte of lithium-ion secondary battery through concentrating on studies, and can obviously improve the high-temperature behavior of battery.Accordingly, the invention provides a kind of electrolyte of lithium-ion secondary battery, it comprises lithium salts, nonaqueous solvents and additive, wherein, additive package vinculum borate, the mass percent of linear borate in electrolyte is 0.2%～5%.
The mass percent of linear borate is restricted to 0.2%～5% the reason that accounts for electrolyte to be: content is less than 0.2% the time, and the inhibition that when high temperature storage cell thickness is expanded is not obvious; When content greater than 5% the time, can obviously reduce the conductivity of electrolyte, reduce approximately 0.7mS/cm, so that affect the volumetric properties of battery.
As a kind of improvement of electrolyte of lithium-ion secondary battery of the present invention, described linear borate is one or more in butyl borate, triproylborate, the triethyl borate, is preferably butyl borate.
As a kind of improvement of electrolyte of lithium-ion secondary battery of the present invention, described nonaqueous solvents is selected from any two kinds or two or more combinations in propene carbonate, ethylene carbonate, methyl ethyl carbonate, the diethyl carbonate.
A kind of improvement as electrolyte of lithium-ion secondary battery of the present invention, described additive also comprises vinylene carbonate, fluorinated ethylene carbonate, 1, in the 3-propane sultone any one or multiple, these additives mainly are the formation for the SEI film of anode graphite.
As a kind of improvement of electrolyte of lithium-ion secondary battery of the present invention, described lithium salts is LiPF
6
In order to realize the foregoing invention purpose, the present invention also provides a kind of lithium rechargeable battery, and it comprises positive plate, negative plate, is interval in the barrier film between positive plate and the negative plate, and electrolyte, wherein, electrolyte is the described electrolyte that contains linear borate of above arbitrary paragraph.
Compared with prior art, the present invention is by adding linear borate in electrolyte of lithium-ion secondary battery, improve significantly the high-temperature behavior of battery, so that battery reaches the time of same thickness expansion when high temperature storage obvious prolongation has been arranged, be conducive to the actual use of battery.
Description of drawings
Below in conjunction with the drawings and specific embodiments, lithium rechargeable battery of the present invention and electrolyte thereof are elaborated.
Fig. 1 is the linear volt-ampere test result comparison diagram of electrolyte of lithium-ion secondary battery in Comparative Examples 1 and the embodiment of the invention 1.
Fig. 2 is the change curve of lithium rechargeable battery thickness swelling in 4.4V, 60 ℃ of storing process in Comparative Examples 1 and the embodiment of the invention 1.
Fig. 3 is the change curve of lithium rechargeable battery open circuit voltage in 4.4V, 60 ℃ of storing process in Comparative Examples 1 and the embodiment of the invention 1.
Fig. 4 is partly the fill state EIS comparison diagram of lithium rechargeable battery before 4.4V, 60 ℃ of storages in Comparative Examples 1 and the embodiment of the invention 1.
Fig. 5 is partly the fill state EIS comparison diagram of lithium rechargeable battery after 4.4V, 60 ℃ of storages in Comparative Examples 1 and the embodiment of the invention 1.
Fig. 6 is 45 ℃ of cycle performance test result figure of lithium rechargeable battery in the Comparative Examples 1.
Fig. 7 is 45 ℃ of cycle performance test result figure of lithium rechargeable battery in the embodiment of the invention 1.
Fig. 8 is voltage curve and the current curve comparison diagram of lithium rechargeable battery in charging process in Comparative Examples 1 and the embodiment of the invention 1.
Fig. 9 is the temperature curve comparison diagram of lithium rechargeable battery in charging process in Comparative Examples 1 and the embodiment of the invention 1.
Embodiment
In order to make goal of the invention of the present invention, technical scheme and useful technique effect more clear, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be understood that, the embodiment that describes in this specification only is in order to explain the present invention, is not in order to limit the present invention.
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 1% vinylene carbonate (VC) and mass ratio and be 2% butyl borate, make electrolyte of lithium-ion secondary battery.
The preparation of positive plate: with positive pole material of lithium cobalt acid (LiCoO
2), conductive agent acetylene black, binding agent polyvinylidene fluoride (PVDF) is after 96:2:2 fully mixes in the 1-METHYLPYRROLIDONE dicyandiamide solution in mass ratio, is coated on the plus plate current-collecting body Al paper tinsel drying and cold pressing and obtain positive plate.
The preparation of negative plate: be after graphite, conductive agent acetylene black, binding agent butadiene-styrene rubber (SBR), thickener sodium carboxymethylcellulose (CMC) fully mix in the deionized water solvent system according to mass ratio 94:2:2:2 with negative material, be coated on the negative current collector Cu paper tinsel, drying and colding pressing obtains negative plate.
The preparation of barrier film: with the PE porous polymer film as barrier film.
The preparation of lithium rechargeable battery: the positive plate, barrier film, the negative plate that make are placed in order, barrier film is in plays buffer action between the positive/negative plate, and coiling is obtained naked battery core; Naked battery core is packaged in the packaging bag, the electrolyte of above-mentioned preparation is injected into removes in the battery of moisture after dry, through encapsulate, leave standstill, change into, the operation such as shaping, obtain the flexible packing lithium ion secondary battery that operating voltage range is 3.0～4.4V.
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 2% 1,3-propane sultone (PS) and mass ratio are 0.2% butyl borate, make electrolyte of lithium-ion secondary battery.
Among the embodiment 2, the preparation of the preparation of positive plate, the preparation of negative plate, barrier film, and the preparation of lithium rechargeable battery is all substantially the same manner as Example 1, repeats no more.
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 4% fluorinated ethylene carbonate (FEC) and mass ratio and be 5% butyl borate, make electrolyte of lithium-ion secondary battery.
Among the embodiment 3, the preparation of the preparation of positive plate, the preparation of negative plate, barrier film, and the preparation of lithium rechargeable battery is all substantially the same manner as Example 1, repeats no more.
Embodiment 4
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 0.5% vinylene carbonate (VC), 2% fluorinated ethylene carbonate (FEC) and mass ratio and be 3% triproylborate, make electrolyte of lithium-ion secondary battery.
Among the embodiment 4, the preparation of the preparation of positive plate, the preparation of negative plate, barrier film, and the preparation of lithium rechargeable battery is all substantially the same manner as Example 1, repeats no more.
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 1% vinylene carbonate (VC), 1% fluorinated ethylene carbonate (FEC), 2% 1,3-propane sultone (PS) and mass ratio are 4% triethyl borate, make electrolyte of lithium-ion secondary battery.
Among the embodiment 5, the preparation of the preparation of positive plate, the preparation of negative plate, barrier film, and the preparation of lithium rechargeable battery is all substantially the same manner as Example 1, repeats no more.
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 1% vinylene carbonate (VC), 3% 1,3-propane sultone (PS), 1% triethyl borate and 1% butyl borate make electrolyte of lithium-ion secondary battery.
Among the embodiment 6, the preparation of the preparation of positive plate, the preparation of negative plate, barrier film, and the preparation of lithium rechargeable battery is all substantially the same manner as Example 1, repeats no more.
Comparative Examples 1
The preparation of electrolyte: with propene carbonate (PC), ethylene carbonate (EC) and diethyl carbonate (DEC) according to the 1:1:1(mass ratio) ratio mix, be made into the LiPF of 1mol/L
6Electrolyte; Then, add again mass ratio and be 1% vinylene carbonate (VC), make electrolyte of lithium-ion secondary battery.
In the Comparative Examples 1, the preparation of the preparation of positive plate, the preparation of negative plate, barrier film, and the preparation of lithium rechargeable battery is all substantially the same manner as Example 1, repeats no more.
Performance test
The linear volt-ampere test of electrolyte: take the Pt electrode as work electrode, the lithium sheet is for to electrode and reference electrode, sweep speed 1mV/s scans 4.5V from Open Circuit Potential, the electrolyte of embodiment 1 and Comparative Examples 1 is carried out linearity volt-ampere test, and the result as shown in Figure 1.As can be seen from the figure, the oxidation current that embodiment 1 has added the electrolyte of butyl borate obviously dies down, and shows that butyl borate is conducive to reduce oxidation reaction.
The key property test of battery:
A) after tested, the battery capacity of the embodiment of the invention and Comparative Examples distributes substantially in same level, and the impedance of 1000Hz also is in same level;
B) multiplying power test: probe temperature is normal temperature; Charging modes be the 0.5C constant current charge to 4.4V, then the 4.4V constant voltage is to 0.05C; Discharge is respectively with 0.5C, 1C, 1.5C, 2C discharge; Take 0.5C as reference point, the capability retention of battery when obtaining different discharge-rate.The test result demonstration, the capability retention the when 1C of Comparative Examples 1,1.5C, 2C is respectively 97%, 91%, 79%, and the respective value of embodiment 1 is 97%, 86%, 69%.From numerical value, the high rate performance of battery of the present invention slightly descends, reason may be that butyl borate has played inhibition to a certain degree in the film forming on pole piece surface to the transmission of lithium ion, therefore so that during high magnification 2C capacity loss more, but it is less to descend when 1C and 1.5C, little on the practical application impact;
C) self discharge test: with battery with the 0.5C constant current charge to 3.875V, then constant voltage is to 0.05C; Take off from test machine, left standstill 24 hours, the test open circuit voltage; And then left standstill 48 hours, again measure open circuit voltage; At last with the difference of the open circuit voltage that records for twice divided by 48, obtain the numerical value in order to the characterizing battery self-discharge performance.Result's demonstration, Comparative Examples 1 is 0.016mV/h; Embodiment 1 is 0.024mV/h.Although the self discharge numerical value of battery of the present invention increases to some extent, all less than general requirements value 0.080mV/h.
The high temperature storage test: the battery of Comparative Examples 1, embodiment 1 is respectively got 3, and the 0.5C constant current charge is to 4.4V at normal temperatures, and constant voltage is taken off the battery that is namely completely filled to 0.05C from the charging machine again.Then the thickness of battery placed battery 60 ℃ of baking ovens before the test storage, measured thickness (heat is surveyed) and the open circuit voltage of battery every 3 days.Be calculated as follows thickness swelling, thickness swelling=(after the storage before the thickness-storage the thickness)/front thickness of storage, respectively to mapping memory time, its result is as shown in Figures 2 and 3 with thickness swelling and open circuit voltage.
Can find out from Fig. 2, embodiment 1 contains the battery of additive boric acid tributyl, and its thickness swelling in the time of 30 days is 10% only, is significantly less than 35% of Comparative Examples 1 battery.This shows that butyl borate has significantly improvement effect for battery in the memory property under the 4.4V, 60 ℃.
Can find out from Fig. 3, Comparative Examples 1 is identical with the initial potential of the battery of embodiment 1, all is why 4.37V(is lower than 4.4V, is because the effect of polarization); Thereafter 3 days, 6 days, 9 days ... the battery open circuit voltage that can see embodiment 1 boronic acid containing tributyl falls lowlyer, its reason be butyl borate at high temperature with the electrode effect, so that cathode potential reduces, lower current potential can reduce the generation of side reaction, thereby is conducive to reduce the aerogenesis situation.
In addition, the battery after the storage is carried out 0.5C be discharged to 3.0V, its capacity is the residual capacity after the storage; The 0.5C constant current charge is to 4.4V again, and constant voltage is to 0.05C, and 0.5C is discharged to 3.0V, and this discharge capacity is reversible capacity; The 0.5C constant current charge is to 3.875V again, and constant voltage is to 0.05C, and then the test cross flow impedance is composed (EIS); Capacity before residual capacity and reversible capacity and the storage is divided by, obtains residual capacity conservation rate and reversible capacity conservation rate.The result shows, the residual capacity conservation rate of Comparative Examples 1 and reversible capacity conservation rate be respectively 69.0% and the numerical value of 83.9%, embodiment 1 be respectively 66.9% and 83.6%.As seen, the battery remaining retention capacity conservation rate of embodiment 1 boronic acid containing tributyl is low, this also just under the high temperature butyl borate with the electrode effect so that the reflection of cathode potential reduction; The reversible capacity conservation rate of battery reduces very little, shows that butyl borate just acts on electrode interface, improves the effect of electrolyte and electrode, but very little on the impact of battery material body.
Moreover, from the variation of storage front and back battery EIS, can infer that also butyl borate reduces the mechanism of action of electrode interface side reaction.Fig. 4 for the storage before the EIS comparison diagram of battery when partly filling state, on scheming, can find out Comparative Examples 1(curve 41) and embodiment 1(curve 42) battery EIS curve overlap fully; Fig. 5 for storage after the EIS comparison diagram of battery when partly filling state, on scheming, can find out embodiment 1(curve 52) Rct of the battery of boronic acid containing tributyl is less.This shows in 60 ℃ of storing process, because the effect of butyl borate, it is less that the battery electrode interface side reaction of embodiment 1 occurs.
The cycle performance test: Fig. 6 and Fig. 7 are respectively 45 ℃ of cycle performance test result figure of battery among Comparative Examples 1 and the embodiment 1.Can find out on scheming, the battery capacity conservation rate of embodiment 1 is slightly low, but basically with Comparative Examples 1 still in same level.
Over-charging test: to 6V, then constant voltage is 1 hour with the current charges of 2C, checks that battery is whether on fire etc.Fig. 8 is battery charging process voltage curve and the current curve comparison diagram of Comparative Examples 1 and embodiment 1; Fig. 9 is the temperature curve comparison diagram of the battery charging process of Comparative Examples 1 and embodiment 1.Can find out on scheming, reach when completely filling, the battery temperature of Comparative Examples 1 is up to more than 800 ℃, and this moment, battery occured on fire; And the battery maximum temperature of embodiment 1 only is 83 ℃, and battery was in 6V constant voltage 1 hour, and just flatulence does not occur on fire.This shows that butyl borate is conducive to improve the over-charge safety performance of battery.
In kind the battery of embodiment 2-6 is done high temperature storage test, after storage in 30 days, thickness swelling is respectively 28%, 6%, 13%, 16% and 15% to the battery that the result shows embodiment 2-6 at 60 ℃, 4.4V, all less than the thickness swelling value of Comparative Examples 1.
In addition, in kind the battery of embodiment 2-6 is done above-mentioned various other tests, the numerical value of test result and Comparative Examples 1 is similar, repeats no more herein.
To sum up above all test results add butyl borate in the electrolyte when improving battery high-temperature memory property and over-charging as can be known, almost do not cause the deterioration of other performance, have therefore effectively improved the combination property of battery.
The according to the above description announcement of book and instruction, those skilled in the art in the invention can also carry out suitable change and modification to above-mentioned execution mode.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should fall in the protection range of claim of the present invention modifications and changes more of the present invention.In addition, although used some specific terms in this specification, these terms do not consist of any restriction to the present invention just for convenience of description.
Claims (6)
1. an electrolyte of lithium-ion secondary battery comprises lithium salts, nonaqueous solvents and additive, it is characterized in that: described additive package vinculum borate, the mass percent of linear borate in electrolyte is 0.2%～5%.
2. electrolyte of lithium-ion secondary battery according to claim 1, it is characterized in that: described linear borate is one or more in butyl borate, triproylborate, the triethyl borate, is preferably butyl borate.
3. electrolyte of lithium-ion secondary battery according to claim 1, it is characterized in that: described nonaqueous solvents is selected from any two kinds or two or more combinations in propene carbonate, ethylene carbonate, methyl ethyl carbonate, the diethyl carbonate.
4. electrolyte of lithium-ion secondary battery according to claim 3, it is characterized in that: described additive also comprises vinylene carbonate, fluorinated ethylene carbonate, 1, in the 3-propane sultone any one or multiple.
5. electrolyte of lithium-ion secondary battery according to claim 1, it is characterized in that: described lithium salts is LiPF
6
6. a lithium rechargeable battery comprises positive plate, negative plate, is interval in the barrier film between positive plate and the negative plate, and electrolyte, it is characterized in that: described electrolyte is each described electrolyte that contains linear borate in the claim 1 to 5.
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Cited By (6)
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| CN105047995A (en) * | 2015-09-22 | 2015-11-11 | 宁德新能源科技有限公司 | Electrolyte, lithium ion battery comprising same and preparation method of lithium ion battery |
| CN105355976A (en) * | 2015-11-13 | 2016-02-24 | 华南师范大学 | An electrolyte containing a tripropylborate additive, a preparing method thereof and applications of the electrolyte |
| CN105390747A (en) * | 2015-11-13 | 2016-03-09 | 华南师范大学 | Trimethyl borate additive-containing electrolyte solution, preparation method therefor and application thereof |
| CN111106384A (en) * | 2018-10-29 | 2020-05-05 | 中国科学院福建物质结构研究所 | Electrolyte matched with high-nickel anode lithium ion battery |
| CN111525190A (en) * | 2020-04-29 | 2020-08-11 | 远景睿泰动力技术(上海)有限公司 | Electrolyte and lithium ion battery |
| CN111697265A (en) * | 2020-05-15 | 2020-09-22 | 湖南博信新能源科技有限公司 | LNCM manganese ternary lithium ion battery electrolyte, lithium battery and preparation method thereof |
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| CN105047995A (en) * | 2015-09-22 | 2015-11-11 | 宁德新能源科技有限公司 | Electrolyte, lithium ion battery comprising same and preparation method of lithium ion battery |
| CN105047995B (en) * | 2015-09-22 | 2018-05-08 | 宁德新能源科技有限公司 | Lithium ion battery of electrolyte including the electrolyte and preparation method thereof |
| CN105355976A (en) * | 2015-11-13 | 2016-02-24 | 华南师范大学 | An electrolyte containing a tripropylborate additive, a preparing method thereof and applications of the electrolyte |
| CN105390747A (en) * | 2015-11-13 | 2016-03-09 | 华南师范大学 | Trimethyl borate additive-containing electrolyte solution, preparation method therefor and application thereof |
| CN111106384A (en) * | 2018-10-29 | 2020-05-05 | 中国科学院福建物质结构研究所 | Electrolyte matched with high-nickel anode lithium ion battery |
| CN111106384B (en) * | 2018-10-29 | 2021-02-12 | 中国科学院福建物质结构研究所 | Electrolyte matched with high-nickel anode lithium ion battery |
| CN111525190A (en) * | 2020-04-29 | 2020-08-11 | 远景睿泰动力技术(上海)有限公司 | Electrolyte and lithium ion battery |
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| CN111697265A (en) * | 2020-05-15 | 2020-09-22 | 湖南博信新能源科技有限公司 | LNCM manganese ternary lithium ion battery electrolyte, lithium battery and preparation method thereof |
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Application publication date: 20130918 |