CN105336985A - High-rate Li-ion electrolyte - Google Patents
High-rate Li-ion electrolyte Download PDFInfo
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- CN105336985A CN105336985A CN201410384626.7A CN201410384626A CN105336985A CN 105336985 A CN105336985 A CN 105336985A CN 201410384626 A CN201410384626 A CN 201410384626A CN 105336985 A CN105336985 A CN 105336985A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses high-rate Li-ion battery electrolyte, belonging to high-rate Li-ion electrolyte for Li-ion batteries. According to the technical scheme, the high-rate Li-ion battery electrolyte comprises conductive Li salt, a mixed carbonic ester solvent and additives, wherein the conductive Li salt is lithium hexafluorophosphate, the mixed carbonic ester solvent comprises ethylene carbonate, propylene carbonate, dimethyl carbonate and ethyl methyl carbonate, the additives include a film forming additive and a surfactant. The high-rate Li-ion battery electrolyte comprises the following components in percentage by mass: lithium hexafluorophosphate: 13-16.0%; ethylene carbonate: 15-35%; propylene carbonate: 0-15%; dimethyl carbonate:30-60%; ethyl methyl carbonate:0-20%; the film forming additive: 2.5-5%; and the surfactant: 0.5-3%. All the raw materials used in the invention are well-commercialized, abundant in source and low in price; the rate capacity of the Li-ion battery.
Description
Technical field
The present invention relates to the electrolyte of battery, specifically a kind of high multiplying power lithium ion electrolyte of lithium battery.
Background technology
Operating voltage is high, specific energy is high owing to having for lithium ion battery, have extended cycle life, with the feature such as environmental friendliness and memory-less effect, obtain and develop rapidly, become the new lover of energy field.Lithium rechargeable battery is made up of both positive and negative polarity, electrolyte, barrier film, wherein the positive pole of lithium ion battery is can the transistion metal compound of deintercalate lithium ions, negative pole is can material with carbon element, the carbon-silicon composite material of deintercalate lithium ions, or other can the material such as phosphorus, sulphur of deintercalate lithium ions, during charging, lithium ion is deviate from from the lattice of positive electrode, enter in electrolyte bulk solution, through the SEI film on barrier film and negative material surface, be finally diffused in negative material; During electric discharge, lithium ion deintercalation from negative material body out, turns back in positive electrode by antipodal path during charging.Therefore from lithium ion battery operation principle, electrolyte is the important component part of lithium ion battery, its effect is except providing lithium ion mobility environment, also to the formation important of electrode surface SEI film, and lithium ion battery power depend on lithium concentration, lithium ion in positive/negative plate body diffusion rate, the migration rate of lithium ion in electrolyte bulk solution, lithium ion through the interface compatibility of barrier film migration rate, lithium ion and SEI film and interface impedance.It can thus be appreciated that the power-performance of electrolyte to lithium ion battery has vital effect.
Lithium-ion battery electrolytes is made up of solvent, electric conducting lithium salt, additive three part.Solvent is generally mixed by low viscosity, lower boiling linear carbonate, carboxylate and high viscosity, high boiling cyclic carbonate, electric conducting lithium salt mostly is business-like LiPF
6, other novel conductive lithium salts is as LiBOB, LiSO
3cF
3, Li (CF
3sO
2) N, Li (CF3SO
2)
3mostly be lithium carbonate and carry out use, can help in embodying to form stable SEI film at LiFePO 4, ternary, LiMn2O4 as added LiBOB3%, improving the performance of circulation and gram volume, but LiBOB and positive pole material of lithium cobalt acid react and inapplicable, additive is primarily of film for additive, surfactant, anti-overcharge additive, the compositions such as conductive additive, additive is by many types, different additive is used to improve battery performance for different system, two kinds of additives are generally used: one for high-rate lithium battery, film for additive is (as VC, PS etc.), two, surfactant, the object adding these two kinds of additives is except the interface in order to improve electrolyte and SEI film, reduce the impedance of SEI film, also soak pole piece to accelerate electrolyte, barrier film and improve the migration environment of lithium ion when heavy-current discharge in electrolyte bulk solution and diffusional environment in pole piece, and then improve the high rate performance of lithium ion battery, and these two kinds of additive levels can not be too high, otherwise the performances such as the circulation of battery can be affected, also cost can be increased.
Summary of the invention
The present invention, in order to overcome the deficiencies in the prior art, provides a kind of high multiplying power lithium ion electrolyte, its objective is the problem that raw material is single, price is high solving existing high multiplying power lithium ion electrolyte and use.
In order to solve above-mentioned technical problem, the basic technical scheme that the present invention proposes is: a kind of high multiplying power lithium ion battery electrolyte, comprise electric conducting lithium salt, mixed carbonic acid ester solvent and additive, described electric conducting lithium salt is lithium hexafluoro phosphate, described mixed carbonic acid ester solvent comprises ethylene carbonate, propene carbonate, dimethyl carbonate and methyl ethyl carbonate, and described additive comprises film for additive and surfactant; According to mass percent:
Lithium hexafluoro phosphate: 13 ~ 16.0%;
Ethylene carbonate: 15 ~ 35%;
Propene carbonate: 0 ~ 15%;
Dimethyl carbonate: 30 ~ 60%;
Methyl ethyl carbonate: 0 ~ 20%;
Film forming agent: 2.5 ~ 5%;
Surfactant: 2 ~ 3%.
In high multiplying power lithium ion electrolyte of the present invention, each component is as follows according to mass percent,
Lithium hexafluoro phosphate: 13 ~ 16.0%;
Ethylene carbonate: 20 ~ 35%;
Propene carbonate: 0 ~ 10%;
Dimethyl carbonate: 30 ~ 50%;
Methyl ethyl carbonate: 10 ~ 20%;
Film forming agent: 2.5 ~ 5%;
Surfactant: 2 ~ 2.5%.
In high multiplying power lithium ion electrolyte of the present invention, the addition of described surfactant is 2.4%.
In high multiplying power lithium ion electrolyte of the present invention, described film forming agent is at least one in unsaturated carbon acid esters, halocarbonate, cyclic sulfates, sulphonic acid ester, unsaturated sulfone or dioxide.
In high multiplying power lithium ion electrolyte of the present invention, described film forming agent comprises at least one in chloroethylene carbonate ester, carbonic acid chloropropene ester, vinylene carbonate, vinylethylene carbonate, sulfonic acid propiolactone, sulfonic acid butyrolactone, sulfuric acid vinyl ester, sulfuric acid in alkene ester, ethylene sulfite, propylene sulfite, diphenyl sulphone (DPS), vinyl sulfone, phenyl vinyl sulfone, carbon dioxide or sulfur dioxide.
In high multiplying power lithium ion electrolyte of the present invention, described surfactant is ethyl acetate.
In high multiplying power lithium ion electrolyte of the present invention, the addition of described ethyl acetate is 2.4%.
The invention has the beneficial effects as follows:
1, raw material selected by the present invention are all ripe business-like, and abundance is cheap;
2, suitable solvent kind, suitable additive is selected, and be equipped with suitable solvent burden ratio, additive formula and electric conducting lithium salt proportioning, electric conducting lithium salt can fully be dissociated in mixed carbonic acid ester solvent, make lithium ion energy fully solvation, to obtain high concentration ion state lithium salts and lithium ion mobility environment well, simultaneously electrolyte can also the stable performance of negative pole embedding lithium carbon material surface, surface energy is low, impedance is little SEI film, thus improve the high rate performance of lithium ion battery;
3, in the present invention, ethyl butyrate elected as by surfactant, except source and price advantage, ethyl butyrate add the surface tension that greatly can also reduce electrolyte, thus greatly can accelerate the speed that electrolyte soaks pole piece and barrier film, save lithium ion battery ageing and ageing time in actual production, enhance productivity, the cryogenic property of electrolyte can also be improved simultaneously.
Accompanying drawing explanation
Fig. 1 is the rate discharge curves of embodiment one to embodiment nine in 534312520C3200mah test battery;
Fig. 2 is embodiment ten and the rate discharge curves of embodiment 11 in 704312520C3700 test battery;
Fig. 3 is the rate discharge curves of embodiment 10 three to embodiment 14 in 954513530C5000mah test battery.
In accompanying drawing, C1 represents embodiment one, C2 and represents embodiment two, so analogizes; Wherein, 10-1# represents the 1# test of embodiment ten, corresponding with table 4, so analogizes.
Specific embodiment
In order to better understand technical scheme of the present invention, below will be described in detail technical scheme of the present invention by specific embodiment, but should not limit the scope of the invention with this.
Invention will be described technical scheme of the present invention with 14 specific embodiments.The experiment purpose of the present embodiment one to embodiment nine is test different solvents systems, and different additive system and different solvents and additive formula are on the impact of high rate performance; And specific embodiment ten, specific embodiment 11 are in order to whether test surfaces interpolation ethyl butyrate is obvious to the effect reducing electrolyte surface tension force, quickening electrolyte soaks pole piece, and the impact on battery high rate performance, wherein normal temperature ageing 48h after embodiment ten battery liquid-filling, and ageing 36h after battery liquid-filling in embodiment 11.Last embodiment 12, embodiment 13, embodiment 14 are to test same dicyandiamide solution, same additive system, different solvents proportioning, and different electric conducting lithium salt content is on the impact of battery high rate performance.
Basic experiment situation below involved by specific embodiment:
1, the layoutprocedure of electrolyte is as follows:
At normal temperature and pressure about relative humidity 1ppm, and under the environment of inert gas, by even for the mixed carbonate ester solvent of purity all more than 99.95%, in this mixed carbonic acid ester solvent, dissolve electric conducting lithium salt lithium hexafluoro phosphate (LiPF
6), this lithium hexafluoro phosphate average mark adds for three times, 2 ~ 3 hours time intervals at every turn added, and adds fully to shake up afterwards, finally adds additive.
2, the method for testing of experimental data:
Measure the conductivity of high multiplying power lithium ion electrolyte with conductivity meter, the moisture in high multiplying power lithium ion electrolyte is determined in coulomb Ka Shi method deep pool, the acidity in acid base titration test high multiplying power lithium ion electrolyte.
3, selected test lithium ion battery
Positive electrode active materials selected by the present invention is preferably LiFePO 4 and cobalt acid lithium, and selected negative active core-shell material is preferably Delanium and carbonaceous mesophase spherules; Selected test battery is the battery of 20C30C, and used in battery barrier film is individual layer PP, PE barrier film of high porosity or the composite diaphragm of PP and PE.Test battery selected by the present invention is flexible package square battery, test battery selected by specific embodiment 1 to specific embodiment 9 is 534312520C3200mah, wherein 53 is cell thickness 5.3mm, 43 is cell widths 43mm, 125 is battery length 125mm, 20C refers to this battery lasts 20C and discharges, and 3200mah is this battery design nominal capacity is 3200mah; Specific embodiment 10 is 704312520C3700mah with the test battery selected by specific embodiment 11; Specific embodiment 12, specific embodiment 13, test battery selected by specific embodiment 14 are 954513530C5000mah.
4, the multiplying power method of testing of the finished product of lithium ion battery:
The first, 1C electric current constant-current constant-voltage charging is to 4.2V, and cut-off current is 0.02C electric current;
The second, static 5min;
Three, 1C constant-current discharge is to 3.0V, discharge capacity during record 1C constant-current discharge;
Four, static 5min;
Five, 1C electric current constant-current constant-voltage charging is to 4.2V, and cut-off current is 0.02C electric current;
Six, according to lithium ion battery design discharge-rate and battery design nominal capacity, calculate lithium ion battery multiplying power discharging electric current, record battery multiplying power discharging capacity, multiplying power discharging initial voltage, multiplying power discharging time, calculate multiplying power discharging capacity ratio=multiplying power discharging capacity/1C discharge capacity, the multiplying power discharging magnitude of voltage of multiplying power discharging mean voltage corresponding to the half of multiplying power discharging time.
Embodiment one
At normal temperature and pressure about relative humidity 1ppm, and under the environment of inert gas, the ethylene carbonate 31.9% of purity all more than 99.95%, dimethyl carbonate 43.7%, methyl ethyl carbonate 8.4% are mixed; Electric conducting lithium salt 13.4%LiPF is dissolved again in this mixed carbonic acid ester solvent
6, this LiPF
6average mark adds for three times, 2.5 hours time intervals at every turn added, and adds fully to shake up afterwards, finally adds additive propane sultone 1.7%, vinylene carbonate 0.84%.
Embodiment two
Compared with embodiment one, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: ethylene carbonate 32.8%, dimethyl carbonate 42.9%, methyl ethyl carbonate 8.4%.
Embodiment three
Compared with embodiment one, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: ethylene carbonate 33.6%, dimethyl carbonate 42.0%, methyl ethyl carbonate 8.4%.
Embodiment four
Compared with embodiment one, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: ethylene carbonate 34.5%, dimethyl carbonate 42.9%, methyl ethyl carbonate 6.7%.
Embodiment five
Compared with embodiment one, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: ethylene carbonate 34.9%, dimethyl carbonate 45%, methyl ethyl carbonate 4.2%.
Embodiment six
At normal temperature and pressure about relative humidity 1ppm, and under the environment of inert gas, by the ethylene carbonate 30% of purity all more than 99.95%, dimethyl carbonate 48.3%, propene carbonate 5% mixes; Electric conducting lithium salt 13.3%LiPF is dissolved again in this mixed carbonic acid ester solvent
6, this LiPF
6average mark adds for three times, 2.5 hours time intervals at every turn added, and adds fully to shake up afterwards, finally adds additive propane sultone 2.5%, vinylene carbonate 0.83%.
Embodiment seven
Compared with embodiment six, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: ethylene carbonate 30.8%, dimethyl carbonate 47.5%, propene carbonate 5%.
Embodiment eight
Compared with embodiment six, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: 31.7% ethylene carbonate, dimethyl carbonate 46.7%, propene carbonate 5%.
Embodiment nine
Compared with embodiment six, the difference of the present embodiment is mixed carbonic acid ester solvent to replace with: ethylene carbonate 32.5%, dimethyl carbonate 45.8%, propene carbonate 5%.
Embodiment ten
Ethylene carbonate 30.8%, propene carbonate 5%, dimethyl carbonate 43.3%, methyl ethyl carbonate 4.2% mix, then dissolve electric conducting lithium salt 13.3%LiPF in this mixed carbonic acid ester solvent
6, average mark adds for three times, 2.5 hours time intervals at every turn added, and adds fully to shake up afterwards, finally adds additive propane sultone 2.5%, vinylene carbonate 0.83%, normal temperature ageing 48h after lithium ion battery liquid injection.
Embodiment 11
Ethylene carbonate 30.1%, propene carbonate 4.9%, dimethyl carbonate 42.3%, methyl ethyl carbonate 4.1% add highly purified ethyl butyrate 2.4% after mixing; Electric conducting lithium salt 13.3%LiPF is dissolved again in this mixed carbonic acid ester solvent
6, this LiPF
6average mark adds for three times, 2.5 hours time intervals at every turn added, and adds fully to shake up afterwards, finally adds additive propane sultone 2.4%, vinylene carbonate 0.81%, normal temperature ageing 36h after battery liquid-filling body;
Embodiment 12
Ethylene carbonate 28.5%, propene carbonate 4.9%, dimethyl carbonate 43.9%, methyl ethyl carbonate 4.1%, ethyl butyrate 2.4%, 13.3%LiPF6,2.4% propane sultone, 0.81 vinylene carbonate %.
Embodiment 13
Ethylene carbonate 30.1%, propene carbonate 4.9%, dimethyl carbonate 42.7%, methyl ethyl carbonate 4.1%, ethyl butyrate 2.4%, 12.9%LiPF
6, 2.4% propane sultone, 0.81 vinylene carbonate %.
Embodiment 14
Ethylene carbonate 28.5%, propene carbonate 4.9%, dimethyl carbonate 44.3%, methyl ethyl carbonate 4.1%, ethyl butyrate 2.4%, 13.3%LiPF
6, 2.4% propane sultone, 0.81 vinylene carbonate %.
According to above-mentioned method of testing, the moisture of the electrolyte of embodiment one to embodiment nine, fluohydric acid content and conductivity are as shown in table 1; The electric property of embodiment one to embodiment nine is as shown in table 2; The moisture of the electrolyte of embodiment ten to embodiment 14, fluohydric acid content and conductivity are as shown in table 3; The electric property of embodiment ten to embodiment 14 is as shown in table 4.
Table 1
| Moisture (ppm) | Fluohydric acid content (ppm) | Conductivity (ms/cm) | |
| Embodiment one | 7.5 | 18.2 | 11.2 |
| Embodiment two | 8.2 | 19.6 | 10.9 |
| Embodiment three | 7.4 | 20.4 | 10.7 |
| Embodiment four | 6.5 | 17.3 | 10.8 |
| Embodiment five | 7.1 | 18.3 | 11.5 |
| Embodiment six | 8.3 | 22.1 | 11.4 |
| Embodiment seven | 10.1 | 21.5 | 11.2 |
| Embodiment eight | 8.6 | 20.8 | 11.3 |
| Embodiment nine | 9.8 | 19.5 | 10.8 |
Table 2
Table 3
| Moisture (ppm) | Fluohydric acid content (ppm) | Conductivity (ms/cm) | |
| Embodiment ten | 8.2 | 20.3 | 11.2 |
| Embodiment 11 | 9.3 | 21.4 | 11 |
| Embodiment 12 | 7.8 | 19.2 | 11.3 |
| Embodiment 13 | 8.4 | 17.5 | 11.1 |
| Embodiment 14 | 7.6 | 18.5 | 11 |
Table 4
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-described embodiment and revise.Therefore, the present invention is not limited to specific embodiment disclosed and described above, also should fall in the protection range of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (7)
1. a high multiplying power lithium ion battery electrolyte, comprise electric conducting lithium salt, mixed carbonic acid ester solvent and additive, described electric conducting lithium salt is lithium hexafluoro phosphate, described mixed carbonic acid ester solvent comprises ethylene carbonate, propene carbonate, dimethyl carbonate and methyl ethyl carbonate, it is characterized in that: described additive comprises film for additive and surfactant; According to mass percent:
Lithium hexafluoro phosphate: 13 ~ 16.0%;
Ethylene carbonate: 15 ~ 35%;
Propene carbonate: 0 ~ 15%;
Dimethyl carbonate: 30 ~ 60%;
Methyl ethyl carbonate: 0 ~ 20%;
Film forming agent: 2.5 ~ 5%;
Surfactant: 2 ~ 3%.
2. high multiplying power lithium ion electrolyte as claimed in claim 1, is characterized in that: each component is as follows according to mass percent,
Lithium hexafluoro phosphate: 13 ~ 16.0%;
Ethylene carbonate: 20 ~ 35%;
Propene carbonate: 0 ~ 10%;
Dimethyl carbonate: 30 ~ 50%;
Methyl ethyl carbonate: 10 ~ 20%;
Film forming agent: 2.5 ~ 5%;
Surfactant: 2 ~ 2.5%.
3. high multiplying power lithium ion electrolyte as claimed in claim 1 or 2, is characterized in that: the addition of described surfactant is 2.4%.
4. high multiplying power lithium ion electrolyte as claimed in claim 1 or 2, is characterized in that: described film forming agent comprises at least one in unsaturated carbon acid esters, halocarbonate, cyclic sulfates, sulphonic acid ester, unsaturated sulfone or dioxide.
5. high multiplying power lithium ion electrolyte as claimed in claim 4, is characterized in that: described film forming agent comprises at least one in alkene ester, ethylene sulfite, propylene sulfite, diphenyl sulphone (DPS), vinyl sulfone, phenyl vinyl sulfone, carbon dioxide in chloroethylene carbonate ester, carbonic acid chloropropene ester, vinylene carbonate, vinylethylene carbonate, sulfonic acid propiolactone, sulfonic acid butyrolactone, sulfuric acid vinyl ester, sulfuric acid or sulfur dioxide.
6. high multiplying power lithium ion electrolyte as claimed in claim 1 or 2, is characterized in that: described surfactant is ethyl acetate.
7. high multiplying power lithium ion electrolyte as claimed in claim 6, is characterized in that: the addition of described ethyl acetate is 2.4%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328999A (en) * | 2016-11-29 | 2017-01-11 | 河南省法恩莱特新能源科技有限公司 | High-rate electrolyte of lithium-ion battery |
| CN108232302A (en) * | 2017-12-30 | 2018-06-29 | 国联汽车动力电池研究院有限责任公司 | A kind of high concentration lithium salt electrolyte suitable for silicon-based anode lithium ion battery |
| EP3352276A1 (en) * | 2017-01-20 | 2018-07-25 | Optimum Battery Co., Ltd. | Electrolyte for lithium ion battery and lithium ion battery including the same |
| CN108376800A (en) * | 2018-02-02 | 2018-08-07 | 江苏海基新能源股份有限公司 | The electrolyte and lithium ion battery of high-temperature lithium ion battery cycle performance can be improved |
| CN113381067A (en) * | 2020-03-10 | 2021-09-10 | 荣盛盟固利新能源科技有限公司 | High-safety electrolyte of high-energy-density soft package battery and high-energy-density soft package battery |
| CN114566706A (en) * | 2022-01-19 | 2022-05-31 | 湖北亿纬动力有限公司 | Lithium battery electrolyte and lithium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106328999A (en) * | 2016-11-29 | 2017-01-11 | 河南省法恩莱特新能源科技有限公司 | High-rate electrolyte of lithium-ion battery |
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| CN113381067A (en) * | 2020-03-10 | 2021-09-10 | 荣盛盟固利新能源科技有限公司 | High-safety electrolyte of high-energy-density soft package battery and high-energy-density soft package battery |
| CN114566706A (en) * | 2022-01-19 | 2022-05-31 | 湖北亿纬动力有限公司 | Lithium battery electrolyte and lithium battery |
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