CN102394314A - Lithium ion battery electrolyte and lithium ion secondary battery - Google Patents
Lithium ion battery electrolyte and lithium ion secondary battery Download PDFInfo
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- CN102394314A CN102394314A CN2011103904023A CN201110390402A CN102394314A CN 102394314 A CN102394314 A CN 102394314A CN 2011103904023 A CN2011103904023 A CN 2011103904023A CN 201110390402 A CN201110390402 A CN 201110390402A CN 102394314 A CN102394314 A CN 102394314A
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- ion battery
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- carbonate
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the technical field of battery, and discloses a lithium ion battery electrolyte and a lithium ion secondary battery. The lithium ion battery electrolyte contains electrolyte salts, a non-aqueous organic solvent, and an additive; the additive comprises a silane phosphate ester additive which accounts for 0.01%-20% of the total weight of the lithium ion battery electrolyte. the lithium ion secondary battery comprises the lithium ion battery electrolyte. By adding the silane phosphate ester additive into the lithium ion battery electrolyte, the invention obviously increases the cycle performance and low temperature discharge performance of the lithium ion battery.
Description
Technical field
The present invention relates to a kind of lithium-ion battery electrolytes and lithium rechargeable battery, particularly a kind of lithium-ion battery electrolytes that can improve lithium ion battery cycle performance and low temperature performance and the lithium rechargeable battery made from this electrolyte.
Background technology
In recent years, because the pressure of environmental pollution and energy shortage forces various countries to strive to find the energy of new green, environmental protection, sustainable development.The lithium ion battery that occurs the nineties in 20th century is widely used as compact power so that its voltage is high, specific energy is high, have extended cycle life, characteristics such as discharge performance is stable, environmental protection.Expansion along with the lithium ion battery applications field; Requirement to battery performance also improves constantly, in some special occasions, such as military affairs, space flight, aviation etc.; Performance requirement to lithium ion battery is more harsh, and these performance requirements are mainly reflected in cycle performance, cryogenic property and the fail safe.Lithium-ion battery electrolytes is one of key factor of these performances of decision.
Lithium ion battery with two kinds can embedding/compound that takes off lithium is as the both positive and negative polarity active material, present business-like positive active material is generally the transition metal oxide material, like cobalt acid lithium, lithium nickelate, ternary material, LiFePO 4, spinel lithium manganate etc.; Negative electrode active material is generally graphite-like (comprising native graphite and Delanium) and carbonaceous mesophase spherules MCMB etc.; Electrolyte plays a part to carry and conduction current in lithium ion battery, is the bridge that connects both positive and negative polarity.
Electrolyte generally with non-water organosilane ester as solvent, with LiPF
6, LiBF
4, LiBOB and LiN (SO
2CF
3)
2Deng lithium salts as solute.The composition of electrolyte is the key factor of decision lithium ion battery cycle life, high rate performance, temperature discharge performance and security performance.
Electrolyte solvent commonly used has propene carbonate PC, ethylene carbonate EC, dimethyl carbonate DMC, diethyl carbonate DEC, methyl ethyl carbonate EMC etc.The commercialization lithium-ion battery electrolytes mainly contains binary or ternary system at present; Cyclic carbonate EC, PC etc. have bigger dielectric constant and polarity, the lithium salts that can fully dissociate, but its viscosity is bigger; Reduce the coefficient of conductivity of lithium ion in the electrolyte, be unfavorable for the raising of conductivity; And viscositys such as linear carbonate DMC, DEC, EMC are lower, can reduce the viscosity that contains cyclic carbonate electrolyte as cosolvent, improve electrolytic conductivity.
PC is as the organic solvent commonly used of lithium-ion battery electrolytes; In battery charge and discharge process along with the embedding of Li+; And the embedding carbon negative pole material; The special construction of PC can cause material to be peeled off causing the battery capacity decay, and battery cycle life shortens, and therefore commercially at present generally adopts EC base electrolyte with lithium-ion battery electrolytes.In battery initial charge process, EC can form the SEI film with protective effect in carbon negative terminal surface reduction decomposition, stops electrolyte further to decompose.But EC fusing point higher (36 ℃) is a solid under the normal temperature, and this causes ethylene carbonate EC base electrolyte fusing point higher relatively again, has reduced the cryogenic property of lithium ion battery.
For cycle performance and the cryogenic property that guarantees battery; Can optimize the content of EC, PC; In electrolyte, add vinylene carbonate VC, fluorinated ethylene carbonate FEC isopreference simultaneously in the film for additive of EC reduction, promptly through improving electrolytic conductivity and optimizing cycle performance and the low temperature performance that SEI film character improves battery.
Summary of the invention
The present invention is directed to the problem that has cycle performance and low temperature performance deficiency in the lithium rechargeable battery, provide a kind of and can improve functional lithium-ion battery electrolytes of lithium ion battery cycle performance and low temperature performance and the lithium rechargeable battery made from this electrolyte.Said functional lithium-ion battery electrolytes is meant the mixed system with certain ionic conductivity that is added with a small amount of functional additive that the organic solvent that is dissolved with lithium salts or ORGANIC SOLVENT MIXTURES form.
The present invention is achieved in that a kind of lithium-ion battery electrolytes, includes electrolytic salt, non-aqueous organic solvent and additive; Comprise the silanes phosphate ester additive that accounts for lithium-ion battery electrolytes total weight 0.01%～20% in the said additive; The structural formula of said silanes phosphate ester additive is following:
Wherein, R
1～R
9Be C
mH
n, 1≤m≤6,1≤n≤13.
Wherein, said electrolytic salinity is 0.4M～2M.
Said electrolytic salt is selected from LiPF
6, LiClO
4, LiBF
4, LiAsF
6, LiCFSO
3, LiN (SO
2CF
3)
2, among the LiBOB, LiODFB one or more.
Described non-aqueous organic solvent includes but not limited to carbonates, carboxylic acid esters, ether solvent or ketones solvent.Said non-aqueous organic solvent includes a kind of cyclic carbonate and a kind of chain (linearity) carbonic ester at least, and various components in proportions are adjusted according to the lithium ion battery performance demands when mixing use; Said cyclic carbonate is selected from one or both among PC, the EC; Said linear carbonate is selected from one or more in DMC, DEC, EMC, MPC, EA, propyl formate, the propyl acetate.
Preferably, said silanes phosphate ester additive accounts for 0.2%～5% of lithium-ion battery electrolytes total weight.
Described lithium-ion battery electrolytes can also comprise other additives, like film for additive, overcharging additive or flame-retardant additive etc.; Film for additive commonly used can be selected from vinylene carbonate VC, propane sultone PS, fluorinated ethylene carbonate FEC, ethylene thiazolinyl vinylene VEC; Overcharging additive can be selected from biphenyl BP, cyclohexyl benzene CHB, fluorotoluene, fluorodiphenyl FBP etc.; Mostly flame-retardant additive is phosphoric acid ester or phosphine nitrence class material.
The present invention also aims to provide a kind of lithium rechargeable battery, comprise foregoing lithium-ion battery electrolytes.In addition; Also include the transition metal oxide that contains lithium as positive electrode active materials that can store reversiblely/discharge lithium ion; Can store reversiblely/discharge the carbonaceous material as negative active core-shell material of lithium ion, and place the porous septum between positive pole and the negative pole.
Lithium rechargeable battery of the present invention includes but are not limited to square lithium ion battery, cylindrical lithium ion battery, polymer Li-ion battery in form.
The silane phosphoric acid ester additive that provides among the present invention; Can on the negative pole of lithium ion battery, reduce and form thin and fine and close SEI film; Therefore in lithium-ion battery electrolytes, add silane phosphoric acid ester additive, can obviously improve cycle performance, the low temperature performance of lithium ion battery.
Description of drawings
Fig. 1 is the cyclic voltammetric collection of illustrative plates of button half-cell among the embodiment 1
Fig. 2 is the ac impedance spectroscopy of button half-cell among the embodiment 1;
Fig. 3 is the normal-temperature circulating performance curve of the battery of electrolyte 3, electrolyte 4 and electrolyte 12 compositions;
Fig. 4 is 0 ℃ of cyclic curve that electrolyte 13 and electrolyte 6 are formed battery.
Embodiment
Below in conjunction with instance substantive distinguishing features of the present invention and advantage are further described, but the present invention is not limited to listed embodiment.
The present invention is through in non-aqueous electrolyte for lithium ion cell, adding a kind of structural formula silanes phosphate ester additive as follows, to improve the cycle performance and the low temperature performance of lithium ion battery.
Wherein, R
1～R
9Be C
mH
n, 1≤m≤6,1≤n≤13.
This silanes phosphate ester additive can preferentially form the SEI film in negative terminal surface, and the SEI membrane impedance that forms is less.
The non-aqueous organic solvent that is adopted in the embodiment of the invention is that EC, DEC, EMC and lithium salts are LiPF
6, embodiment all operates in less than-40 ℃ dry environment at dew point.
EC, EMC, DEC is even according to 1: 1: 1 mixed of volume ratio, slowly add lithium salts LiPF
6Being mixed with concentration is the non-water organic electrolyte of 1M, makes electrolyte 1, in electrolyte 1, adds three (trimethyl silane) phosphate TMSP that accounts for this electrolyte total weight 2wt%, is mixed with electrolyte 2.
The negative plate that with lithium sheet and Delanium is active material is as two electrodes, and porous polyolefin compound barrier film is as barrier film, as electrolyte, makes the button half-cell with the electrolyte 1 of preparation and electrolyte 2.
Carry out cyclic voltammetric (CV) test with 0.5mV/S speed, test result is seen Fig. 1, can see obviously that TMSP forms the SEI film in negative terminal surface prior to solvent EC reduction; And the half-cell (graphite is in embedding lithium attitude) of discharge attitude carried out AC impedance (EIS) test, the result is as shown in Figure 2.It is thus clear that the electric liquid that adds TMSP has less SEI membrane impedance and electron transfer impedance at the skin covering of the surface that negative terminal surface forms.
Is that 3: 4: 3 mixed is even with EC, EMC, DEC according to volume ratio, slowly adds lithium salts LiPF
6Being mixed with concentration is the non-water organic electrolyte of 1M, in the electrolyte of preparation, adds three (trimethyl silane) phosphate according to the ratio that accounts for this electrolyte total weight 0.5wt%, 1wt%, 5wt% respectively, makes electrolyte 3, electrolyte 4, electrolyte 5.
Embodiment 3
Is that 3: 7 mixed is even with EC, DEC according to volume ratio, slowly adds lithium salts LiPF
6Being mixed with concentration is the non-water organic electrolyte of 1M, and the fluorinated ethylene carbonate FEC that in the electrolyte of preparation, adds three (tri-phenyl-silane) phosphates and 2wt% ratio according to the ratio that accounts for this electrolyte total weight 1wt%, 10wt%, 15wt% respectively makes electrolyte 6, electrolyte 7, electrolyte 8.
Is that 1: 1: 1 mixed is even with EC, EMC, DEC according to volume ratio, slowly adds lithium salts LiPF
6Being mixed with concentration is the non-water organic electrolyte of 1M; In the electrolyte of preparation, add the biphenyl BP of three (triethyl silicane) phosphates and 0.5wt% ratio respectively according to the ratio that accounts for this electrolyte total weight 0.5wt%, 3wt%, 5wt%, make electrolyte 9, electrolyte 10, electrolyte 11.
Comparative example 1
This comparative example is used for explaining the preparation of prior art lithium-ion battery electrolytes.
Respectively according to embodiment 2, embodiment 3, embodiment 4 preparing electrolyte, but the additive of neither interpolation aforementioned structural formula makes electrolyte 12, electrolyte 13, electrolyte 14.
Present embodiment is used to explain the making of lithium rechargeable battery of the present invention.
The preparation of negative pole: in homogenate equipment; Use N-methyl pyrrolidone NMP as solvent; The Delanium of 94.5wt% is mixed with the acetylene black of 2wt% and the Kynoar PVDF of 3.5wt%; Use coating device that it evenly is coated on the Copper Foil of 8 μ m, obtain negative plate through after rolling, shear, drying.
Anodal preparation: in homogenate equipment; Use N-methyl pyrrolidone NMP as solvent; 96wt% cobalt acid lithium is mixed with the acetylene black of 2wt% and the PVDF of 2wt%, use coating device base evenly to be coated on the aluminium foil of 15 μ m, obtain positive plate through after rolling, shear, drying.
With positive pole, negative pole and PE membrane coil coiled utmost point group, and the assembling square lithium ion battery.Inject the electrolyte of embodiment 2, embodiment 3, embodiment 4, comparative example 1 preparation, place behind the 24h with the 0.2C current charges to 4.2V, the 4.2V constant voltage charge is reduced to 20mA up to electric current and is ended then; Aging after 7 days, carry out reprocessing according to the 0.5C electric current; Battery is made and is finished.
Battery performance test
(1) normal-temperature circulating performance
The lithium ion battery of making among the embodiment 5 is done the normal temperature loop test on the Arbin battery test system; Test parameter is that 1C is discharged to 3V; 1C charges to 4.2V; 4.2V constant voltage charge ends to 20mA, so circulates for 300 weeks, the initial capacity of recording cell and maintenance capacity (the 301st discharge capacity) see the following form.
Visible by last table data, silanes phosphate ester additive provided by the invention can obviously improve the normal-temperature circulating performance of battery, and along with the increase of addition, 300 times circulation back capability retention increases.
(2) 0 ℃ of cycle performances
The lithium ion battery of making among the embodiment 5 is done 0 ℃ of loop test on the Arbin battery test system; Test parameter is that 0.5C is discharged to 3V; 0.5C charge to 4.2V; Constant voltage 4.2V charges to 20mA to be ended, and so circulates 10 times, and cell thickness variation and battery initial capacity (0 ℃ of following the 1st discharge capacity) and maintenance capacity (the 10th discharge capacity) see the following form before and after the record circulation.
Because negative pole the lithium phenomenon occurs analysing and can cause the battery bulging, can see that by this table silanes phosphate ester additive provided by the invention can obviously improve low temperature performance in the low temperature cyclic process, suppress the bulging of battery in the low temperature cyclic process.
Claims (6)
1. a lithium-ion battery electrolytes includes electrolytic salt, non-aqueous organic solvent and additive; It is characterized in that, comprise the silanes phosphate ester additive that accounts for lithium-ion battery electrolytes total weight 0.01%-20% in the said additive; The structural formula of said silanes phosphate ester additive is following:
Wherein, R1-R9 is C
mH
n, 1≤m≤6,1≤n≤13.
2. lithium-ion battery electrolytes according to claim 1 is characterized in that, said electrolytic salinity is 0.4M-2M.
3. lithium-ion battery electrolytes according to claim 1 and 2 is characterized in that said electrolytic salt is selected from LiPF
6, LiClO
4, LiBF
4, LiAsF
6, LiCFSO
3, LiN (SO
2CF
3)
2, among the LiBOB, LiODFB one or more.
4. lithium-ion battery electrolytes according to claim 1 is characterized in that said non-aqueous organic solvent includes cyclic carbonate and linear carbonate; Said cyclic carbonate is selected from one or both in propene carbonate (PC), the ethylene carbonate (EC); Said linear carbonate is selected from one or more in dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), carbonic acid first propyl ester (MPC), ethyl acetate (EA), propyl formate, the propyl acetate.
5. lithium-ion battery electrolytes according to claim 1 is characterized in that said silanes phosphate ester additive accounts for the 0.2%-5% of lithium-ion battery electrolytes total weight.
6. a lithium rechargeable battery is characterized in that, includes the lithium-ion battery electrolytes of claim 1-5 described in each.
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|---|---|---|---|
| CN2011103904023A CN102394314A (en) | 2011-11-30 | 2011-11-30 | Lithium ion battery electrolyte and lithium ion secondary battery |
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|---|---|---|---|
| CN2011103904023A CN102394314A (en) | 2011-11-30 | 2011-11-30 | Lithium ion battery electrolyte and lithium ion secondary battery |
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Family
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103597647A (en) * | 2012-04-30 | 2014-02-19 | 株式会社Lg化学 | Electrolyte additive, lithium secondary battery and non-aqueous electrolyte comprising additive |
| CN105789698A (en) * | 2016-03-04 | 2016-07-20 | 深圳新宙邦科技股份有限公司 | Non-aqueous electrolyte of lithium ion battery and lithium ion battery |
| CN106099186A (en) * | 2016-07-12 | 2016-11-09 | 华南师范大学 | A kind of high pressure corrosion resistant erosion electrolyte and preparation method and application |
| CN106328993A (en) * | 2015-06-17 | 2017-01-11 | 深圳市沃特玛电池有限公司 | Electrolyte used for lithium iron phosphate high-magnification lithium ion battery |
| CN106356559A (en) * | 2016-10-11 | 2017-01-25 | 宁德时代新能源科技股份有限公司 | Electrolyte and secondary battery using same |
| WO2017020431A1 (en) * | 2015-08-03 | 2017-02-09 | 深圳新宙邦科技股份有限公司 | Non-aqueous electrolyte of lithium-ion battery and lithium-ion battery |
| CN107710490A (en) * | 2015-07-02 | 2018-02-16 | 麦克赛尔控股株式会社 | Nonaqueous electrolyte battery and its manufacture method |
| CN109004273A (en) * | 2017-06-07 | 2018-12-14 | 宁德时代新能源科技股份有限公司 | Electrolyte solution and secondary battery |
| CN109148942A (en) * | 2017-06-28 | 2019-01-04 | 福建省辉锐材料科技有限公司 | A kind of preparation method of novel aluminum Dual-ion cell |
| CN110676513A (en) * | 2019-11-20 | 2020-01-10 | 凌帕新能源科技(上海)有限公司 | Lithium battery electrolyte and lithium battery |
| CN111864262A (en) * | 2019-04-29 | 2020-10-30 | 诺莱特电池材料(苏州)有限公司 | Lithium ion battery non-aqueous electrolyte and lithium ion battery |
| CN111934014A (en) * | 2020-08-27 | 2020-11-13 | 珠海市赛纬电子材料股份有限公司 | Electrolyte and lithium ion battery containing same |
| CN112331917A (en) * | 2020-11-04 | 2021-02-05 | 泰州纳新新能源科技有限公司 | Wide-temperature-range lithium ion battery electrolyte and preparation method and application thereof |
| CN113054258A (en) * | 2021-04-21 | 2021-06-29 | 广州天赐高新材料股份有限公司 | Novel application of substituted silicon-based phosphate compound, electrolyte and lithium ion battery |
| CN113937361A (en) * | 2021-11-16 | 2022-01-14 | 远景动力技术(江苏)有限公司 | Preparation method and application of long-circulating non-aqueous electrolyte of energy storage battery cell |
| CN114094185A (en) * | 2020-03-20 | 2022-02-25 | 宁德新能源科技有限公司 | Electrolyte solution, electrochemical device, and electronic device |
| US11735771B2 (en) | 2019-01-25 | 2023-08-22 | Ningde Amperex Technology Limited | Electrolyte solution and electrochemical device using the same |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103597647B (en) * | 2012-04-30 | 2016-09-14 | 株式会社Lg化学 | Electrolyte solution additive, the non-aqueous electrolytic solution comprising this additive and lithium secondary battery |
| US9666901B2 (en) | 2012-04-30 | 2017-05-30 | Lg Chem, Ltd. | Additive for electrolyte solution, non-aqueous electrolyte solution including the additive and lithium secondary battery including the electrolyte solution |
| CN103597647A (en) * | 2012-04-30 | 2014-02-19 | 株式会社Lg化学 | Electrolyte additive, lithium secondary battery and non-aqueous electrolyte comprising additive |
| CN106328993A (en) * | 2015-06-17 | 2017-01-11 | 深圳市沃特玛电池有限公司 | Electrolyte used for lithium iron phosphate high-magnification lithium ion battery |
| CN107710490A (en) * | 2015-07-02 | 2018-02-16 | 麦克赛尔控股株式会社 | Nonaqueous electrolyte battery and its manufacture method |
| WO2017020431A1 (en) * | 2015-08-03 | 2017-02-09 | 深圳新宙邦科技股份有限公司 | Non-aqueous electrolyte of lithium-ion battery and lithium-ion battery |
| CN105789698B (en) * | 2016-03-04 | 2019-01-25 | 深圳新宙邦科技股份有限公司 | A kind of non-aqueous electrolyte for lithium ion cell and lithium ion battery |
| CN105789698A (en) * | 2016-03-04 | 2016-07-20 | 深圳新宙邦科技股份有限公司 | Non-aqueous electrolyte of lithium ion battery and lithium ion battery |
| CN106099186A (en) * | 2016-07-12 | 2016-11-09 | 华南师范大学 | A kind of high pressure corrosion resistant erosion electrolyte and preparation method and application |
| CN106356559A (en) * | 2016-10-11 | 2017-01-25 | 宁德时代新能源科技股份有限公司 | Electrolyte and secondary battery using same |
| CN109004273A (en) * | 2017-06-07 | 2018-12-14 | 宁德时代新能源科技股份有限公司 | Electrolyte solution and secondary battery |
| CN109148942A (en) * | 2017-06-28 | 2019-01-04 | 福建省辉锐材料科技有限公司 | A kind of preparation method of novel aluminum Dual-ion cell |
| US11735771B2 (en) | 2019-01-25 | 2023-08-22 | Ningde Amperex Technology Limited | Electrolyte solution and electrochemical device using the same |
| CN111864262A (en) * | 2019-04-29 | 2020-10-30 | 诺莱特电池材料(苏州)有限公司 | Lithium ion battery non-aqueous electrolyte and lithium ion battery |
| CN110676513A (en) * | 2019-11-20 | 2020-01-10 | 凌帕新能源科技(上海)有限公司 | Lithium battery electrolyte and lithium battery |
| CN114094185A (en) * | 2020-03-20 | 2022-02-25 | 宁德新能源科技有限公司 | Electrolyte solution, electrochemical device, and electronic device |
| CN111934014A (en) * | 2020-08-27 | 2020-11-13 | 珠海市赛纬电子材料股份有限公司 | Electrolyte and lithium ion battery containing same |
| CN112331917A (en) * | 2020-11-04 | 2021-02-05 | 泰州纳新新能源科技有限公司 | Wide-temperature-range lithium ion battery electrolyte and preparation method and application thereof |
| CN113054258A (en) * | 2021-04-21 | 2021-06-29 | 广州天赐高新材料股份有限公司 | Novel application of substituted silicon-based phosphate compound, electrolyte and lithium ion battery |
| CN113054258B (en) * | 2021-04-21 | 2023-07-04 | 广州天赐高新材料股份有限公司 | New application of substituted silicon-based phosphate compound, electrolyte and lithium ion battery |
| CN113937361A (en) * | 2021-11-16 | 2022-01-14 | 远景动力技术(江苏)有限公司 | Preparation method and application of long-circulating non-aqueous electrolyte of energy storage battery cell |
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Application publication date: 20120328 |