CN102437371A - Electrolyte of lithium iron phosphate battery and lithium iron phosphate battery containing same - Google Patents
Electrolyte of lithium iron phosphate battery and lithium iron phosphate battery containing same Download PDFInfo
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- CN102437371A CN102437371A CN2010102958021A CN201010295802A CN102437371A CN 102437371 A CN102437371 A CN 102437371A CN 2010102958021 A CN2010102958021 A CN 2010102958021A CN 201010295802 A CN201010295802 A CN 201010295802A CN 102437371 A CN102437371 A CN 102437371A
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Abstract
The invention provides an electrolyte of a lithium iron phosphate battery, which comprises lithium salt, non-aqueous solvent and additive, wherein the additive contains stabilizing additive which is phenanthroline. The invention also provides the lithium iron phosphate battery adopting the electrolyte. The electrolyte of the lithium iron phosphate battery provided by the invention contains the stabilizing additive which is phenanthroline, and forms a stable complex together with iron ions dissolved in the electrolyte, so that the iron ions can be effectively prevented from being separated out on a negative pole, and the circulation performance and the high-temperature performance of the lithium iron phosphate battery can be improved.
Description
Technical field
The invention belongs to the lithium ion battery field, relate in particular to a kind of ferric phosphate lithium cell electrolyte and contain the ferric phosphate lithium cell of this electrolyte.
Background technology
Advantages such as lithium ion battery has that operating voltage height, specific energy are big, pollution-free, memory-less effect and life-span are long; Be widely used in portable electronics devices such as mobile phone, digital camera and notebook computer, simultaneously as the alternative energy source of oil on electric motor car and hybrid electric vehicle also with large-scale application.As the positive electrode of lithium ion battery, study more have cobalt acid lithium, lithium nickelate, LiMn2O4 and LiFePO4 at present.
LiFePO4 is as positive electrode; Have low price, nontoxic, Environmental compatibility good, rich in mineral resources, higher specific capacity (theoretical capacity 170mAh/g; Thereby cause people's extensive concern energy density 550Wh/kg) and higher operating voltage (3.4V/Li), discharge and recharge to flatten and advantage such as delay, have extended cycle life, security performance is good.But ferric phosphate lithium cell is in the charge and discharge cycles process; Ferro element meeting oligodynamical in the anode active material of phosphate iron lithium is in electrolyte; On negative pole, reduce then and separate out; Especially the charge and discharge process under hot conditions is more outstanding, has therefore greatly influenced the circulation and the high-temperature behavior of battery.
CN101635378A discloses a kind of electrolyte that is applicable to ferric phosphate lithium cell, contains organic solvent and lithium salts electrolyte, also contains the component of sulfonate group class lithium salts in this electrolyte.In this electrolyte; Contain sulfonate group class lithium salts material composition through adding; Stop the dissolving of ferro element in electrolyte system in the iron phosphate lithium positive pole, and then stop iron separating out on negative pole, improve LiFePO4 power-type lithium ion battery high-temperature storage and circulation chemical property.
Summary of the invention
The invention solves that ferro element is dissolved in the electrolyte in the iron phosphate lithium positive pole that exists in the prior art, reduce the cycle performance of battery and the technical problem of high-temperature behavior.
The invention provides a kind of electrolyte of ferric phosphate lithium cell, comprise lithium salts, nonaqueous solvents and additive; Contain stabilization additives in the said additive, said stabilization additives is a phenanthroline.
The present invention also provides a kind of ferric phosphate lithium cell, comprises housing and the electric core, the nonaqueous electrolytic solution that are contained in the housing, and electric core comprises positive pole, negative pole and the barrier film between positive pole and negative pole; Wherein, said nonaqueous electrolytic solution is an electrolyte provided by the invention.
In the electrolyte of ferric phosphate lithium cell provided by the invention; Owing to contain the stabilization additives phenanthroline; Form stable complex compound with the iron ion that is dissolved in the electrolyte, thereby effectively control iron ion separating out on negative pole, improve the cycle performance and the high-temperature behavior of ferric phosphate lithium cell.
Embodiment
The invention provides a kind of electrolyte of ferric phosphate lithium cell, comprise lithium salts, nonaqueous solvents and additive; Contain stabilization additives in the said additive, said stabilization additives is a phenanthroline.
Contain ferro element in the positive electrode of ferric phosphate lithium cell, in charge and discharge process, ferro element can be dissolved in and form iron ion in the electrolyte, on negative pole, is reduced then and separates out, and reduces the cycle performance and the high-temperature behavior of battery.In order to prevent iron separating out on negative pole, mainly contain two kinds of methods: (1) suppresses the dissolving of ferro element in electrolyte in the iron phosphate lithium positive pole; (2) suppress to be dissolved in iron ion in the electrolyte in the reduction of negative pole.The CN101635378A disclosed method; Promptly be to adopt (1) kind method, promptly, stop ferro element in electrolyte, to dissolve through in electrolyte, adopting the lithium salts of sulfonate group; But the lithium salts of sulfonate group can influence the conductivity of electrolyte, reduces the cycle performance of ferric phosphate lithium cell; In addition, the lithium salts of part sulfonate group, for example two trifluoromethane sulfonic acid imines lithiums, trifluoromethyl sulfonic acid lithium are understood the corrosive aluminum foil collector, reduce the stability of ferric phosphate lithium cell.
And electrolyte of the present invention; Through in electrolyte, adopting phenanthroline, the iron ion in phenanthroline and the electrolyte forms stable complex compound, can prevent effectively that iron ion is reduced at negative pole; Promptly adopt (2) kind method, thereby guarantee the cycle performance and the high-temperature behavior of ferric phosphate lithium cell.
In the electrolyte of the present invention, the content of the stabilization additives of employing need not too high, can improve the cycle performance and the high-temperature behavior of ferric phosphate lithium cell.Particularly, be benchmark with the electrolyte of 100 weight portions, the content of phenanthroline is the 0.1-2 weight portion.
In the electrolyte of the present invention, lithium salts, nonaqueous solvents and content of additive are not had special demands, in the usual range in present technique field, get final product.Particularly, be benchmark with the lithium-ion battery electrolytes of 100 weight portions, the content of lithium salts is the 10-19.5 weight portion, the content of nonaqueous solvents is the 80-89.5 weight portion.
Said lithium salts for example can be selected from lithium hexafluoro phosphate (LiPF for the various lithium salts that those skilled in the art use always
6), LiBF4 (LiBF
4), lithium perchlorate (LiClO
4), hexafluoroarsenate lithium (LiAsF
6), hexafluorosilicic acid lithium (LiSiF
6), di-oxalate lithium borate (LiBOB), lithium chloride (LiCl), lithium bromide (LiBr), Li (CF
3SO
2)
2At least a among the N.Under the preferable case, in the electrolyte of the present invention, the concentration of lithium salts is 0.5-2mol/L, more preferably 0.8-1.5mol/L.
Among the present invention, the various nonaqueous solventss that said nonaqueous solvents adopts those skilled in the art to use always get final product.For example, said nonaqueous solvents contains at least a in first solvent, second solvent, the 3rd solvent, the 4th solvent.
Wherein, the various esters solvents used always for those skilled in the art of first solvent; Particularly, said first solvent is selected from ethylene carbonate (EC), propene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), carbonic acid first propyl ester (MPC), methyl formate, Ethyl formate, methyl acetate, ethyl acetate, propyl acetate, ethyl propionate, methyl butyrate, ethyl butyrate, ethylene sulfite, propylene sulfite, trimethyl phosphate, triethyl phosphate or tributyl phosphate.The various ether solvents that second solvent is used always for those skilled in the art; Particularly, said second solvent is selected from dimethoxymethane, 1,2-dimethoxy-ethane, 1,2-diethoxyethane, oxinane, dimethyl-tetrahydrofuran, diethylene glycol dimethyl ether or tetramethyl-1,3-dioxolane.The various ketones solvents that the 3rd solvent is used always for those skilled in the art; Particularly, said the 3rd solvent is selected from N-methyl pyrrolidone or acetone.The derivative of the various carbonic esters that said the 4th solvent is used always for those skilled in the art; Particularly, said the 4th solvent is selected from chlorocarbonic acid vinyl acetate, chlorocarbonic acid propylene ester, dichloro-propene carbonate, three chloro propene carbonates, fluorinated ethylene carbonate, fluoro propene carbonate, two fluoro propene carbonates or three fluoro propene carbonates.
Also contain film for additive in the additive of the present invention.Said film for additive is selected from vinylene carbonate, vinylethylene carbonate, 1,3-sulfonic acid propiolactone or 1, at least a in the 4-sulfonic acid butyrolactone.Electrolyte with 100 weight portions is benchmark, and the content of film for additive is the 0.2-5 weight portion, is preferably the 0.5-3 weight portion.
The present invention also provides a kind of ferric phosphate lithium cell, comprises housing and the electric core, the nonaqueous electrolytic solution that are contained in the housing, and electric core comprises positive pole, negative pole and the barrier film between positive pole and negative pole; Wherein, said nonaqueous electrolytic solution is an electrolyte provided by the invention.
Because the preparation technology of negative plate, positive plate, barrier film is a technology known in the field, and the assembling of battery is technology known in the field also, just repeats no more at this.
Below in conjunction with embodiment lithium-ion battery electrolytes of the present invention and the lithium ion battery that contains this electrolyte are described further.Adopt all in embodiment and the Comparative Examples and be commercially available.
Embodiment 1
1. the preparation of electrolyte
At room temperature; In the glove box of water content＜5ppm; Vinyl carbonate (EC), dimethyl carbonate (DMC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC) are mixed as nonaqueous solvents by weight 1:0.4:0.5:1.15, with the LiPF of 12.2 weight portions
6Be dissolved in the nonaqueous solvents of 85.8 weight portions, add the vinylene carbonate (VC) of 2 weight portions again, obtain mixed solution.Then, the phenanthroline of 1 weight portion is added in the mixed solution of 99 weight portions, obtain the electrolyte of present embodiment, be designated as S1.
2. button cell is made
Press mass ratio LiFePO
4: the mixed of acetylene black: PVDF=8:1:1 is pressed into anode pole piece after evenly, with pole piece in 120 ℃ of baking ovens more than the vacuumize 12h.Then, anode pole piece is as work electrode, and lithium metal is to electrode, and the electrolyte S1 that adopts step 1 to make is assembled into button cell A1 in the argon gas glove box.
3. the preparation of full battery
With LiFePO4 LiFePO
4For positive electrode active materials, graphite are that negative active core-shell material adds binding agent, conductive agent and solvent respectively, process positive and negative plate respectively through batching, coating, drying, roll-in, after cutting.The polypropylene diaphragm of positive and negative plate and 20 micron thick is wound into the electrode group of rectangular lithium ion battery, and this electrode is assembled in the rectangular cell aluminum hull of 5mm * 34mm * 50 mm.The electrolyte that subsequently step 1 is made is injected in the battery case for 3.2 milliliters, and 053450 type lithium ion battery is processed in sealing, then through ageing, change into, promptly get battery B1 of the present invention behind the partial volume.
Embodiment 2
Adopt with embodiment 1 identical method and prepare positive pole, negative pole, electrolyte and battery; Difference is: in the step 1; The phenanthroline of 0.1 weight portion is joined in the mixed solution of 99.9 weight portions; The quality percentage composition of phenanthroline in electrolyte is 0.1%, obtains the electrolyte S2 of present embodiment.
According to the method identical, make button cell A2 and full battery B2 respectively with embodiment 1.
Embodiment 3
Adopt with embodiment 1 identical method and prepare positive pole, negative pole, electrolyte and battery; Difference is: in the step 1; The phenanthroline of 0.5 weight portion is joined in the mixed solution of 99.5 weight portions; The quality percentage composition of phenanthroline in electrolyte is 0.5%, obtains the electrolyte S3 of present embodiment.
According to the method identical, make button cell A3 and full battery B3 respectively with embodiment 1.
Embodiment 4
Adopt with embodiment 1 identical method and prepare positive pole, negative pole, electrolyte and battery; Difference is: in the step 1; The phenanthroline of 1.5 weight portions is joined in the mixed solution of 98.5 weight portions; The quality percentage composition of phenanthroline in electrolyte is 1.5%, obtains the electrolyte S4 of present embodiment.
According to the method identical, make button cell A4 and full battery B4 respectively with embodiment 1.
Embodiment 5
Adopt with embodiment 1 identical method and prepare positive pole, negative pole, electrolyte and battery; Difference is: in the step 1; The phenanthroline of 2 weight portions is joined in the mixed solution of 98 weight portions; The quality percentage composition of phenanthroline in electrolyte is 2%, obtains the electrolyte S5 of present embodiment.
According to the method identical, make button cell A5 and full battery B5 respectively with embodiment 1.
Comparative Examples 1
1. the preparation of electrolyte
At room temperature; In the glove box of water content＜5ppm; Vinyl carbonate (EC), dimethyl carbonate (DMC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC) are mixed as nonaqueous solvents by weight 1:0.4:0.5:1.15, with the LiPF of 12.2 weight portions
6Be dissolved in the nonaqueous solvents of 85.8 weight portions, add the vinylene carbonate (VC) of 2 weight portions again, obtain the electrolyte of this Comparative Examples, be designated as SC1.
2. button cell is made
Press mass ratio LiFePO
4: acetylene black: the mixed of PVDF=8:1:1 is pressed into anode pole piece after evenly, with pole piece in 120 ℃ of baking ovens more than the vacuumize 12h.Then, anode pole piece is as work electrode, and lithium metal is to electrode, adopts the electrolyte SC1 of step 1, in the argon gas glove box, is assembled into button cell AC1.
3. the preparation of full battery
With LiFePO4 LiFePO
4For positive electrode active materials, graphite are that negative active core-shell material adds binding agent, conductive agent and solvent respectively, process positive and negative plate respectively through batching, coating, drying, roll-in, after cutting.The polypropylene diaphragm of positive and negative plate and 20 micron thick is wound into the electrode group of rectangular lithium ion battery; And this electrode is assembled in the rectangular cell aluminum hull of 5mm * 34mm * 50 mm; Electrolyte with step 1 is injected in the battery case for 3.2 milliliters subsequently; 053450 type lithium ion battery is processed in sealing, then through ageing, change into, promptly get full battery BC1 behind the partial volume.
Comparative Examples 2
Adopt with embodiment 1 identical method and prepare positive pole, negative pole, electrolyte and battery; Difference is: in the step 1; Two trifluoromethane sulfonic acid imines lithiums of 7 weight portions are joined in the mixed solution of 93 weight portions; The quality percentage composition of sulfonate group lithium salts in electrolyte is 7%, obtains the electrolyte SC2 of this Comparative Examples.
According to the method identical, make button cell AC2 and full battery BC2 respectively with embodiment 1.
Performance test:
(1) specific capacity test
A1-A5 and AC1-AC2 button cell are respectively got 20, on the strange BK-6016 secondary cell of indigo plant device for detecting performance, 25 ± 1 ℃ of following test battery capacity.Testing procedure is following: shelve 30min; 0.1mA constant current charge is to 3.8V; Constant voltage to electric current is less than 0.01mA; Shelved 10 minutes; Constant-current discharge is to 2.0V.Then, lithium-iron phosphate active material quality in the specific capacity=test battery capacity/button cell of record active material is averaged.Test result is as shown in table 1.
(2) normal temperature loop test
B1-B5 and the full battery of BC1-BC2 are respectively got 20, holding up on day BS-9300 secondary cell device for detecting performance, under 25 ± 1 ℃ of conditions, battery is carried out the charge and discharge cycles test with 0.2C.Step is following: shelve 10min; Constant voltage charge ends to 3.8V/0.05C; Shelve 10min; Constant-current discharge is 1 circulation to 2.0V.Repeat this step, the internal resistance of cell after the record cycle-index has circulated is averaged for every group.Test result is as shown in table 2.
(3) high temperature circulation test
The full battery of B1-B5 and BC1-BC2 is respectively got 20, holding up on day BS-9300 secondary cell device for detecting performance, under 60 ± 1 ℃ of conditions, battery is carried out the charge and discharge cycles test with 0.2C.Step is following: shelve 10min; Constant voltage charge ends to 3.8V/0.05C; Shelve 10min; Constant-current discharge is to 2.0V; Be 1 circulation.Repeat this step, the internal resistance of cell after the record cycle-index has circulated is averaged for every group.Test result is as shown in table 2.
Table 1
| The battery numbering | A1 | A2 | A3 | A4 | A5 | AC1 | AC2 |
| Charge ratio capacity/Ah/g | 157 | 150 | 154 | 154 | 152 | 150 | 147 |
| Specific discharge capacity/mAh/g | 156 | 148 | 152 | 150 | 146 | 144 | 142 |
| Efficient/% first | 99.2 | 98.5 | 98.6 | 97.5 | 96.3 | 96.1 | 96.6 |
Table 2
| The battery numbering | B1 | B2 | B3 | B4 | B5 | BC1 | BC2 |
| Normal temperature cycle life/inferior | 1202 | 985 | 1130 | 1253 | 1052 | 850 | 930 |
| The normal temperature circulation back internal resistance of cell/m Ω | 64 | 68 | 63 | 63 | 72 | 76 | 85 |
| 60 ℃ of cycle life/inferior | 975 | 852 | 930 | 1036 | 915 | 532 | 691 |
| The internal resistance of cell after 60 ℃ of circulations/m Ω | 153 | 182 | 165 | 189 | 208 | 220 | 236 |
Can find out from the test result of table 1 and table 2, owing to adopt the stabilization additives phenanthroline, can effectively improve specific capacity, cycle life and the high-temperature behavior of ferric phosphate lithium cell in the electrolyte provided by the invention.
Claims (8)
1. the electrolyte of a ferric phosphate lithium cell comprises lithium salts, nonaqueous solvents and additive, it is characterized in that, contains stabilization additives in the said additive, and said stabilization additives is a phenanthroline.
2. electrolyte according to claim 1 is characterized in that, is benchmark with the electrolyte of 100 weight portions, and the content of phenanthroline is the 0.1-2 weight portion.
3. electrolyte according to claim 1 is characterized in that, is benchmark with the electrolyte of 100 weight portions, and the content of lithium salts is the 10-19.5 weight portion, and the content of nonaqueous solvents is the 80-89.5 weight portion.
4. according to claim 1 or 3 described electrolyte, it is characterized in that said lithium salts is selected from LiClO
4, LiPF
6, LiBF
4, LiAsF
6, LiCl, LiBr, Li (CF
3SO
2)
2At least a among the N.
5. according to claim 1 or 3 described electrolyte, it is characterized in that said nonaqueous solvents contains at least a in first solvent, second solvent, the 3rd solvent, the 4th solvent;
Said first solvent is selected from ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, carbonic acid first propyl ester, methyl formate, Ethyl formate, methyl acetate, ethyl acetate, propyl acetate, ethyl propionate, methyl butyrate, ethyl butyrate, ethylene sulfite, propylene sulfite, trimethyl phosphate, triethyl phosphate or tributyl phosphate;
Said second solvent is selected from dimethoxymethane, 1,2-dimethoxy-ethane, 1,2-diethoxyethane, oxinane, dimethyl-tetrahydrofuran, diethylene glycol dimethyl ether or tetramethyl-1,3-dioxolane;
Said the 3rd solvent is selected from N-methyl pyrrolidone or acetone;
Said the 4th solvent is selected from chlorocarbonic acid vinyl acetate, chlorocarbonic acid propylene ester, dichloro-propene carbonate, three chloro propene carbonates, fluorinated ethylene carbonate, fluoro propene carbonate, two fluoro propene carbonates or three fluoro propene carbonates.
6. electrolyte according to claim 1 is characterized in that, contains film for additive in the additive; Said film for additive is selected from vinylene carbonate, vinylethylene carbonate, 1,3-sulfonic acid propiolactone or 1, at least a in the 4-sulfonic acid butyrolactone.
7. electrolyte according to claim 6 is characterized in that, is benchmark with the electrolyte of 100 weight portions, and the content of film for additive is the 0.2-5 weight portion.
8. a ferric phosphate lithium cell comprises housing and the electric core, the nonaqueous electrolytic solution that are contained in the housing, and electric core comprises positive pole, negative pole and the barrier film between positive pole and negative pole; It is characterized in that said nonaqueous electrolytic solution is each described electrolyte of claim 1-7.
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102983362A (en) * | 2012-12-20 | 2013-03-20 | 中国东方电气集团有限公司 | Low-temperature electrolyte for LiFePO4 (lithium iron phosphate) lithium-ion batteries |
| CN105914401A (en) * | 2016-06-27 | 2016-08-31 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery containing same |
| DE102016209588A1 (en) * | 2016-06-01 | 2017-12-07 | Robert Bosch Gmbh | Hybrid supercapacitor with increased energy density |
| CN109216766A (en) * | 2017-07-07 | 2019-01-15 | 通用汽车环球科技运作有限责任公司 | Inhibit or minimize the electrolyte system that metal pollutant and dendrite are formed in lithium ion battery |
| US10581119B2 (en) | 2017-07-07 | 2020-03-03 | GM Global Technology Operations LLC | Polymeric ion traps for suppressing or minimizing transition metal ions and dendrite formation or growth in lithium-ion batteries |
| US10581117B2 (en) | 2017-07-07 | 2020-03-03 | GM Global Technology Operations LLC | Iron ion trapping van der Waals gripper additives for electrolyte systems in lithium-ion batteries |
| CN114430039A (en) * | 2020-10-28 | 2022-05-03 | 比亚迪股份有限公司 | Lithium ion battery and power vehicle |
| CN116072971A (en) * | 2023-04-03 | 2023-05-05 | 宁德新能源科技有限公司 | Electrolyte and electrochemical device |
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| CN1320285A (en) * | 1998-08-31 | 2001-10-31 | 株式会社日立制作所 | Lithium secondary cell and device |
| CN101394008A (en) * | 2008-11-03 | 2009-03-25 | 广州天赐高新材料股份有限公司 | Lithium ion secondary battery using lithium iron phosphate as anode material with overall consideration of high and low temperature performance |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102983362A (en) * | 2012-12-20 | 2013-03-20 | 中国东方电气集团有限公司 | Low-temperature electrolyte for LiFePO4 (lithium iron phosphate) lithium-ion batteries |
| DE102016209588A1 (en) * | 2016-06-01 | 2017-12-07 | Robert Bosch Gmbh | Hybrid supercapacitor with increased energy density |
| CN105914401A (en) * | 2016-06-27 | 2016-08-31 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery containing same |
| CN109216766A (en) * | 2017-07-07 | 2019-01-15 | 通用汽车环球科技运作有限责任公司 | Inhibit or minimize the electrolyte system that metal pollutant and dendrite are formed in lithium ion battery |
| US10418668B2 (en) * | 2017-07-07 | 2019-09-17 | GM Global Technology Operations LLC | Electrolyte system including complexing agent to suppress or minimize metal contaminants and dendrite formation in lithium ion batteries |
| US10581119B2 (en) | 2017-07-07 | 2020-03-03 | GM Global Technology Operations LLC | Polymeric ion traps for suppressing or minimizing transition metal ions and dendrite formation or growth in lithium-ion batteries |
| US10581117B2 (en) | 2017-07-07 | 2020-03-03 | GM Global Technology Operations LLC | Iron ion trapping van der Waals gripper additives for electrolyte systems in lithium-ion batteries |
| CN109216766B (en) * | 2017-07-07 | 2021-11-02 | 通用汽车环球科技运作有限责任公司 | Electrolyte system for inhibiting or minimizing metal contamination and dendrite formation in lithium ion batteries |
| CN114430039A (en) * | 2020-10-28 | 2022-05-03 | 比亚迪股份有限公司 | Lithium ion battery and power vehicle |
| CN114430039B (en) * | 2020-10-28 | 2023-08-08 | 比亚迪股份有限公司 | Lithium ion battery and power vehicle |
| CN116072971A (en) * | 2023-04-03 | 2023-05-05 | 宁德新能源科技有限公司 | Electrolyte and electrochemical device |
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Application publication date: 20120502 |