CN101587970A - Electrolyte for high multiplying power lithium ion battery and preparation method thereof - Google Patents
Electrolyte for high multiplying power lithium ion battery and preparation method thereof Download PDFInfo
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- CN101587970A CN101587970A CNA2009100437243A CN200910043724A CN101587970A CN 101587970 A CN101587970 A CN 101587970A CN A2009100437243 A CNA2009100437243 A CN A2009100437243A CN 200910043724 A CN200910043724 A CN 200910043724A CN 101587970 A CN101587970 A CN 101587970A
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Abstract
The invention relates to an electrolyte for a high multiplying power lithium ion battery and preparation method thereof. The electrolyte comprises conductive lithium salts, mixed carbonic ether solvent and additives. The carbonic ether solvent without water and impurity is mixed according to a quality ratio carbonic acid ethylene eater 10-35%, propene carbonate 0-20%, methyl carbonate 25%-60%, carbonic acid methyl ethylene ester 0-35%; the conductive lithium salts are dissolved in the solvent by 0.5mol/L-1.5mol/L, adding the functional additive R[4]NBF[4]; the concentration of the additive is 0.05mol/l-1.0mol/L; R[1] and R[2] are one or one of the methyl, ethyl, propyl, butyl and methoxyl ethyl. The method for adding the functional additive in the invention enhances conductivity of the electrolyte and reduces the interface resistance between the electrolyte and the electrode to enhance the moving speed for the lithium ion battery between the electrode and the electrolyte and the multiplying power performance for the lithium ion battery.
Description
Technical field
The present invention relates to a kind of electrolyte for lithium ion battery and preparation method thereof, particularly a kind of function electrolyte that improves the lithium ion battery high rate performance and preparation method thereof.
Background technology
Lithium ion battery because have that operating voltage height, energy density are big, advantage such as memory-less effect, environmental pollution are little, become the focus of new forms of energy research.The lithium rechargeable battery both positive and negative polarity is made up of two kinds of different lithium ion inserts.During charging, Li
+Deviate from from the lattice of positive electrode, be embedded in the negative material through behind the electrolyte, positive pole is in poor lithium attitude; During discharge, Li
+Spontaneously from negative material, deviate from, turn back in the lattice of positive electrode through electrolyte.As seen electrolyte is the important component part of battery, in battery, bearing the effect of transmission charge between the both positive and negative polarity, because the power of battery is relevant with the migration rate of lithium ion between electrode, electrolyte, electrolyte and electrode interface, so electrolyte plays very big influence to the power of battery.
At present, electrolyte generally is made up of organic solvent, electric conducting lithium salt and minor amounts of additives.Organic solvent adopts big cyclic carbonate and the low linear carbonate of viscosity of dielectric constant to mix.The commercial Li-ion batteries electrolyte lithium salt mostly is LiPF
6, emerge a lot of novel lithium salts in recent years, as LiBOB, LiODFB, LiBF
3Cl etc., for the advantage of comprehensive various lithium salts, Many researchers adopts two kinds of compound or a kind of lithium salts of lithium salts to improve the performance of electrolyte as the form of additive.Z.H.Chen etc. adopt LiPF
6-LiBOB complex salt used for electrolyte is found by being added on LiPF in high power lithium ion cell
6The base electrolyte in compound LiBOB, the specific power and the cycle performance of battery all be improved (J.Electrochimica Acta, 2006,51:3322).J.Liu etc. adopt LiODFB as LiPF
6The additive of base electrolyte is found can to form more effective and stable SEI film with LiODFB as the negative terminal surface of additive battery, thus the chemical property of raising battery (J.Electrochem Comm, 2007,9:475).
The kind of additive has a lot, adopt dissimilar additives at different requirements,, generally adopt two kinds of additives in order to improve the power-performance of lithium ion battery: the one, film for additive is (as VC, ES etc.), the 2nd, conductive additive (as the micromolecule amine).Physicochemical properties such as the chemical composition of SEI film, structure, texture and stability are the keys of decision carbon in lithium ion battery negative pole/electrolyte compatibility, add film for additive and can optimize the character of negative pole interface SEI film, thereby improve the chemical property of lithium ion battery.The high conductivity of electrolyte is to reduce Li
+Migration resistance, the important assurance that improves battery rate charge-discharge performance.Conductive additive adds molecule and electrolyte ion generation complexation reaction, promotes the dissolving and the ionization of lithium salts, reduces the Stokes radius of solvation lithium ion.Improve the conductivity of electrolyte, and then improve the high rate performance of battery.
So far, complex salt electrolyte generally adopts lithium salts and lithium salts compound, and lithium salts and non-lithium salts compound rarely has report.Content of additive is difficult for too highly in the said method, otherwise may reduce the cycle performance of battery.
Summary of the invention
In order to improve the power characteristic of lithium ion battery, the invention provides a kind of electrolyte for high multiplying power lithium ion battery, it has improved the conductivity of electrolyte, reduced the interface impedance between electrode and the electrolyte, thereby improved the migration rate of lithium ion between electrode and electrolyte, and then improved the multiplying power discharging property of lithium ion battery.
The present invention is achieved by the following technical solutions.
A kind of electrolyte for high multiplying power lithium ion battery is that electric conducting lithium salt and the functional additive with structure shown in formula 1 or the formula 2 are dissolved in the solution that forms in the solvent of carbonic ester preparation, described solvent composition comprises ethylene carbonate 10～35wt%, propene carbonate 0～20wt%, dimethyl carbonate 25～60wt%, methyl ethyl carbonate 0～35wt%; The concentration of described electric conducting lithium salt is 0.5mol/L～1.5mol/L; R in the described functional additive
1And R
2Group is methyl, ethyl, propyl group, butyl, methoxy ethyl, and the concentration of described functional additive is 0.05mol/L～1.0mol/L.
Formula 1
Described electric conducting lithium salt is LiPF
6, LiBF
4, LiAsF
6, LiClO
4, LiCF
3SO
3, LiN (CF
3SO
3)
2, LiBOB, LiODFB, LiBF
3Cl, LiPF
4(C
2O
4) in one or more.
The preparation method of described electrolyte comprises the steps:
(1) with the carbonic ester removal of impurities, dewater, behind the purifying, press ethylene carbonate 10～35wt%, propene carbonate 0～20wt%, dimethyl carbonate 25～60wt%, methyl ethyl carbonate 0～35wt% is mixed with the solvent of electrolyte;
(2) in above-mentioned solvent, dissolve electric conducting lithium salt, add the functional additive with structure shown in formula 1 or the formula 2, R in the described functional additive again
1And R
2Group is methyl, ethyl, propyl group, butyl or methoxy ethyl.
Being dissolved under 10～40 ℃ of electric conducting lithium salt carried out.
Cation group can be dimethyl diethyl ammonium, dimethyl dibutyl ammonium, dimethyl dipropylammonium, dipropyl dibutyl ammonium ammonium, tetramethyl-ammonium, tetraethyl ammonium, tetrapropyl ammonium, TBuA, monomethyl triethyl ammonium, monomethyl tributyl ammonium, an ethyl tripropyl ammonium, monomethyl trimethoxy ammonium, an ethyl trimethyl ammonium, dimethylformamide dimethyl oxygen base ammonium or diethyl dimethoxy ammonium etc. in the described additive.
Used functional additive concentration is for different lithium salts and dicyandiamide solution, the optium concentration difference of additive.
Used electric conducting lithium salt and functional additive additive purity should be greater than 99.99%.
Describedly dewater, impurity removal process comprises the cosolvent method, one or more the combination in the boulton process, distillation crystallisation, molecular sieve adsorption.Used adsorbent is at least a in active carbon, calcium hydride, lithium hydride, anhydrous calcium oxide, calcium chloride, non-oxidation two phosphorus, alkali metal or the alkaline-earth metal; Described molecular sieve adsorption can adopt 3A, 4A and 5A, preferably adopts 5A or 4A.
The lithium ion battery that electrolyte of the present invention is used, its negative electrode active material comprises native graphite, electrographite, asphalt base carbon fiber, carbonaceous mesophase spherules.More excellent electrographite or the carbonaceous mesophase spherules of being chosen as.Positive active material comprises LiMn2O4, cobalt acid lithium, lithium nickelate and LiFePO4, more preferably selects LiFePO4.
The present invention has improved the degree of dissociation of electrolyte in solvent by the selection of optimization, lithium salts and the lithium salt of dicyandiamide solution, thereby has improved the conductivity of electrolyte, and then has improved the high rate performance of lithium ion battery.
The present invention is by adding a kind of novel functional additive; improved the quality of electrolyte and electrode surface interfacial film; thereby reduced the migration force of lithium ion between electrode and electrolyte; special as can effectively to protect graphite-structure in PC base electrolyte, not to be destroyed, improved the high rate performance of lithium ion battery then.
Description of drawings
Fig. 1 is the conductivity curve chart of embodiment 1, embodiment 13 and comparative example's electrolyte
A represents comparative example's 1 electrolyte;
B represents embodiment 1 function electrolyte;
C represents embodiment 13 function electrolytes.
Fig. 2 is embodiment 1, embodiment 13 and comparative example's an AC impedance comparison diagram
A represents comparative example's 1 electrolyte;
B represents embodiment 1 function electrolyte;
C represents embodiment 13 function electrolytes.
Fig. 3 is embodiment 14, embodiment 15 and comparative example's 2 a multiplying power discharging Capacity Plan
A represents comparative example's 2 electrolyte;
B represents embodiment 14 function electrolytes;
C represents embodiment 15 function electrolytes.
Fig. 4 is the multiplying power discharging curve chart of comparative example's 2 electrolyte;
Fig. 5 is the multiplying power discharging curve chart of embodiment 14 electrolyte;
Fig. 6 is the multiplying power discharging curve chart of embodiment 15 electrolyte.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but these embodiment must not be interpreted as limiting the scope of the invention.
Embodiment 1
The first step is carried out the ternary mixing with cyclic carbonate ester solvent PC, EC and linear carbonate solvent DMC, wherein PC is 18% (wt), EC is 30% (wt), and DMC is 52% (wt), by dewater in conjunction with boulton process, distillation crystallisation, 4A molecular sieve adsorption purifying, removal of impurities;
Second step was added on a certain amount of electric conducting lithium salt LiODFB in the above-mentioned solvent under 20 ℃ of conditions, and stirring is made into the electrolyte that concentration is 1.0mol/L;
The 3rd step was added a certain amount of composite electrolyte salt tetraethylammonium tetrafluoroborate (purity＞99.99%) in electrolyte, its concentration is at 0.3mol/L.
As mentioned above, the function electrolyte for preparing raising lithium ion battery high rate performance of the present invention.
With embodiment 1, just solvent is the EC of mass ratio 32%, 15% PC, 30% DMC, 23% EMC.
Embodiment 3
With embodiment 1, just solvent is the EC of mass ratio 33%, 37% DMC, 30% EMC.
With embodiment 1, just solvent is the EC of mass ratio 25%, 5% PC, 45% DMC, 25% EMC.
Embodiment 5
With embodiment 2, just electric conducting lithium salt is 0.8M LiBOB.
With embodiment 3, just electric conducting lithium salt is 1.2M LiPF
6
Embodiment 7
With embodiment 4, just electric conducting lithium salt is 1.5M LiBF
4
With embodiment 1, just electric conducting lithium salt is 0.7M LiAsO
6
Embodiment 9
With embodiment 1, just electric conducting lithium salt is 0.5M LiPF
4(C
2O
4).
With embodiment 2, just electric conducting lithium salt is 0.9M LiN (CF
3SO
3)
2
Embodiment 11
With embodiment 9, just additive is 0.8M tetrabutyl ammonium tetrafluoroborate (purity＞99.99%).
With embodiment 7, just additive is a 0.08M monomethyl trimethoxy ammonium tetrafluoroborate (purity＞99.99%).
Embodiment 13
With embodiment 5, just additive is a 0.5M monomethyl triethyl group ammonium tetrafluoroborate (purity＞99.99%).
Embodiment 14
With embodiment 6, just additive is a 0.25M dimethyl dibutyl ammonium tetrafluoroborate (purity＞99.99%).
Embodiment 15
With embodiment 7, just additive is 0.1M tetramethyl ammonium tetrafluoroborate (purity＞99.99%).
Use graphite that the function electrolyte of the foregoing description preparation assembles to lithium half-cell initial charge capacity all more than 320mAh/g, the nominal capacity of being assembled is the 063048 model LiFePO of 400mAh
4/ AG battery 1C the capacity of discharging and recharging down can reach more than the 370mAh, and it is original more than 72% that the 10C charge/discharge capacity keeps, and has good rate charge-discharge performance.
The comparative example 1
Prepare comparative example's 1 electrolyte by first, second one step process among the embodiment 1, get then among embodiment 1 and the embodiment 13 the electrolyte of preparing and comparative example's 1 electrolyte compare test.At first electrolyte is tested: water content is measured with plum Teller-Tuo benefit DL32 moisture teller, the water content＜5ppm of electrolyte.Experimentize then:
(1) conductivity test
Laboratory electrolyte as mentioned above.Adopt Switzerland's plum Teller-Tuo benefit SG3 conductivity meter, every numerical value of 5 ℃ of records, test specification is 0～45 ℃.
Comparative example 1, embodiment 1 and the conductivity of embodiment 8 electrolyte and the curve between the temperature are seen Fig. 1.
(2) constant current charge-discharge experiment
Electrolyte is for as mentioned above during experiment.Adopt button half-cell system, work electrode is for to mix after hot pressing forms in 94: 6 ratio (dry weight) with PTFE with artificial graphite sample, and barrier film is Celgard 2400.Assemble battery in the glove box that is full of high-purity Ar gas, take out the back and carry out constant current charge and discharge experiment with blue electricity (LAND) series battery test macro, the charge and discharge electric current is 0.2C, and end of charge voltage is 0.000V, and final discharging voltage is 2.000V.
Comparative example 1, embodiment 1 and embodiment 13 electrolyte first three time efficient and capacity are as shown in table 1, and wherein a represents not add comparative example's electrolyte of electrolytic salt.B represents embodiment 1 function electrolyte, and c represents embodiment 13 function electrolytes.Subscript 1,2,3 represent first, second, third circulation respectively.
Table 1
(3) AC impedance experiment
Electrolyte is for as mentioned above during experiment.As described in the half-cell manufacture method is tested as comparative example's 1 constant current charge-discharge, take out battery and carry out constant current charge and discharge experiment with blue electricity (LAND) series battery test macro, the charge and discharge electric current is 0.2C, end of charge voltage is 0.000V, final discharging voltage is 2.000V, carry out ac impedance measurement after the circulation primary, frequency range is between 10mHz～100KHz, and used instrument is the PAR2273 electrochemical workstation.The AC impedance curve chart as shown in Figure 2.
The comparative example 2
Prepare comparative example's 2 electrolyte by first, second one step process among the embodiment 9, get then that the electrolyte of preparing compares test among embodiment 14 and the embodiment 15.At first electrolyte is tested: water content is measured with plum Teller-Tuo benefit DL32 moisture teller, the water content＜5ppm of electrolyte.Experimentize then.
Rate charge-discharge test: be that embodiment 14 and embodiment 15 comparative examples 2 are described with electrolyte during experiment.Adopt 063048 type LiFePO
4The full battery of/AG is just very used LiFePO
4With binding agent and carbon black in 91: 5: 4 ratio be dissolved in the water stir after, be coated on large-scale coating machine on the two sides of smooth aluminium foil, form through hot pressing, negative pole for carbonaceous mesophase spherules and binding agent and carbon black in 94: 3: 2 ratio be dissolved in the water stir after, be coated on the smooth copper foil two sides with large-scale coating machine, form through hot pressing, barrier film is Celgard 2400, makes core through coiling and is packaged in the 063048 model box hat.Being full of the glove box fluid injection of high-purity Ar gas, seal.Carry out the constant current charge-discharge experiment with blue electricity (LAND) series battery test macro, charging current adopts 1C, and discharging current adopts 0.5C, 2C, 5C, 10C respectively, and end of charge voltage is 3.800V, and final discharging voltage is 2.200V.Comparative example 2, embodiment 14 and embodiment 15 used for electrolyte are in 063048 model LiFePO
4Multiplying power discharging capacity such as Fig. 3 in the full battery of/AG, corresponding multiplying power discharging curve such as Fig. 4, Fig. 5, Fig. 6.
Claims (7)
1, a kind of electrolyte for high multiplying power lithium ion battery, it is characterized in that, described electrolyte is that electric conducting lithium salt and the functional additive with structure shown in formula 1 or the formula 2 are dissolved in the solution that forms in the solvent of carbonic ester preparation, described solvent composition comprises ethylene carbonate 10～35wt%, propene carbonate 0～20wt%, dimethyl carbonate 25～60wt%, methyl ethyl carbonate 0～35wt%; The concentration of described electric conducting lithium salt is 0.5mol/L～1.5mol/L; R in the described functional additive
1And R
2Group is methyl, ethyl, propyl group, butyl, methoxy ethyl, and the concentration of described functional additive is 0.05mol/L～1.0mol/L.
Formula 1
Formula 2
2, electrolyte according to claim 1 is characterized in that, described electric conducting lithium salt is LiPF
6, LiBF
4, LiAsF
6, LiClO
4, LiCF
3SO
3, LiN (CF
3SO
3)
2, LiBOB, LiODFB, LiBF
3Cl, LiPF
4(C
2O
4) in one or more.
3, the preparation method of the described electrolyte of claim 1 is characterized in that, comprises the steps:
(1) with the carbonic ester removal of impurities, dewater, behind the purifying, press ethylene carbonate 10～35wt%, propene carbonate 0～20wt%, dimethyl carbonate 25～60wt%, methyl ethyl carbonate 0～35wt% is mixed with the solvent of electrolyte;
(2) in above-mentioned solvent, dissolve electric conducting lithium salt, add the functional additive with structure shown in formula 1 or the formula 2, R in the described functional additive again
1And R
2Group is methyl, ethyl, propyl group, butyl or methoxy ethyl.
4, preparation method according to claim 3 is characterized in that: the concentration of described functional additive is 0.05mol/L～1.0mol/L.
5, preparation method according to claim 3 is characterized in that: described electric conducting lithium salt is LiPF
6, LiBF
4, LiAsF
6, LiClO
4, LiCF
3SO
3, LiN (CF
3SO
3)
2, LiBOB, LiODFB, LiBF
3Cl, LiPF
4(C
2O
4) in one or more.
6, according to claim 3 or 5 described preparation methods, it is characterized in that: the concentration of described electric conducting lithium salt is 0.5mol/L～1.5mol/L.
According to claim 3 or 5 described preparation methods, it is characterized in that 7, being dissolved under 10～40 ℃ of electric conducting lithium salt carried out.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013090417A1 (en) * | 2011-12-14 | 2013-06-20 | Envia Systems, Inc. | Low temperature electrolyte for high capacity lithium based batteries |
| US8993177B2 (en) | 2009-12-04 | 2015-03-31 | Envia Systems, Inc. | Lithium ion battery with high voltage electrolytes and additives |
| CN106410274A (en) * | 2015-08-03 | 2017-02-15 | 丰田自动车株式会社 | Method for manufacturing nonaqueous electrolyte secondary cell, and cell assembly |
| US10411299B2 (en) | 2013-08-02 | 2019-09-10 | Zenlabs Energy, Inc. | Electrolytes for stable cycling of high capacity lithium based batteries |
| CN110506356A (en) * | 2017-07-26 | 2019-11-26 | 株式会社日立制作所 | Semisolid electrolyte, semisolid electrolyte, semisolid electrolyte layer and secondary cell |
| CN110828895A (en) * | 2019-11-12 | 2020-02-21 | 湖南艾威尔新能源科技有限公司 | Low-temperature-resistant lithium ion battery electrolyte and lithium ion battery |
| CN110994031A (en) * | 2019-12-19 | 2020-04-10 | 湖南美尼科技有限公司 | Fast-charging high-temperature-resistant electrolyte and preparation method thereof |
| CN111834670A (en) * | 2019-04-17 | 2020-10-27 | 中南大学 | Lithium-sulfur battery electrolyte and application thereof |
| US11973178B2 (en) | 2019-06-26 | 2024-04-30 | Ionblox, Inc. | Lithium ion cells with high performance electrolyte and silicon oxide active materials achieving very long cycle life performance |
-
2009
- 2009-06-19 CN CNA2009100437243A patent/CN101587970A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8993177B2 (en) | 2009-12-04 | 2015-03-31 | Envia Systems, Inc. | Lithium ion battery with high voltage electrolytes and additives |
| WO2013090417A1 (en) * | 2011-12-14 | 2013-06-20 | Envia Systems, Inc. | Low temperature electrolyte for high capacity lithium based batteries |
| US11121407B2 (en) | 2013-08-02 | 2021-09-14 | Zenlabs Energy, Inc. | Electrolytes for stable cycling of high capacity lithium based batteries |
| US11894518B2 (en) | 2013-08-02 | 2024-02-06 | Zenlabs Energy, Inc. | Electrolytes for stable cycling of high capacity lithium based batteries |
| US10411299B2 (en) | 2013-08-02 | 2019-09-10 | Zenlabs Energy, Inc. | Electrolytes for stable cycling of high capacity lithium based batteries |
| CN106410274B (en) * | 2015-08-03 | 2019-04-05 | 丰田自动车株式会社 | The manufacturing method and battery assembly body of nonaqueous electrolytic solution secondary battery |
| CN106410274A (en) * | 2015-08-03 | 2017-02-15 | 丰田自动车株式会社 | Method for manufacturing nonaqueous electrolyte secondary cell, and cell assembly |
| CN110506356A (en) * | 2017-07-26 | 2019-11-26 | 株式会社日立制作所 | Semisolid electrolyte, semisolid electrolyte, semisolid electrolyte layer and secondary cell |
| CN111834670A (en) * | 2019-04-17 | 2020-10-27 | 中南大学 | Lithium-sulfur battery electrolyte and application thereof |
| CN111834670B (en) * | 2019-04-17 | 2021-09-24 | 中南大学 | Lithium-sulfur battery electrolyte and application thereof |
| US11973178B2 (en) | 2019-06-26 | 2024-04-30 | Ionblox, Inc. | Lithium ion cells with high performance electrolyte and silicon oxide active materials achieving very long cycle life performance |
| CN110828895A (en) * | 2019-11-12 | 2020-02-21 | 湖南艾威尔新能源科技有限公司 | Low-temperature-resistant lithium ion battery electrolyte and lithium ion battery |
| CN110994031A (en) * | 2019-12-19 | 2020-04-10 | 湖南美尼科技有限公司 | Fast-charging high-temperature-resistant electrolyte and preparation method thereof |
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Application publication date: 20091125 |