CN103346347A - High-voltage lithium ion battery - Google Patents
High-voltage lithium ion battery Download PDFInfo
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- CN103346347A CN103346347A CN201310279185XA CN201310279185A CN103346347A CN 103346347 A CN103346347 A CN 103346347A CN 201310279185X A CN201310279185X A CN 201310279185XA CN 201310279185 A CN201310279185 A CN 201310279185A CN 103346347 A CN103346347 A CN 103346347A
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Abstract
The invention provides a high-voltage lithium ion battery, and relates to a lithium ion battery, which can provide a working voltage over 4.8V 1V higher than the working voltage provided by the current lithium ion battery, realize good cycle performance and have good compatibility between a carbon cathode and an electrolyte. For the high-voltage lithium ion battery, the anode material is fluoro-phosphate with a molecule general formula of LixA(2-x)MPO4, wherein x is more than or equal to 1 and less than or equal to 2, A is Na or K, M is Co, Ni, Mn or Fe, the electrolyte is a high-voltage lithium ion battery electrolyte which is prepared from 5-20wt% of a lithium salt, 40-85wt% o a carbonic ester solvent, 5-50wt% of a bi-nitrile solvent and 0.1-5wt% of an electrolyte additive, and the total weight percent is 100%.
Description
Technical field
The present invention relates to lithium ion battery, especially relate to a kind of high-voltage lithium ion batteries.
Background technology
Along with the development of electronic products such as smart mobile phone, panel computer, more and more higher requirement has been proposed for the energy density of lithium ion battery.The lifting of energy content of battery density, except the capacity that improves constantly existing battery material system, the positive electrode that exploitation has the high potential workbench has become a kind of trend.
The fluoro phosphate material is the novel high-voltage anode material of a class, and its voltage platform is up to more than the 4.8V.In addition, owing to the introducing of fluorine ion makes lithium ion increase one, therefore be expected to pass through M
2+/ M
4+The utilization of redox couple realizes surpassing the reversible exchange of a lithium, thereby obtains higher reversible specific capacity.At present, in this series material about Li
2CoPO
4The research of F is more.Studies show that its reversible capacity is at 130mAh g
-1About, voltage platform is at 5.1V (vs.Li
+/ Li) [Journal of Power Sources, 2012,220 (0): 122-129].But since its voltage platform considerably beyond the oxidation-stabilized window of conventional carbon acid esters electrolyte (＜4.5V), under this current potential, oxidation Decomposition takes place in electrolyte easily, so its cycle performance is unsatisfactory.Such material is wanted to be used in lithium ion battery, the high voltage type electrolyte that must exploitation adapts with it.
Two nitrile organic substances are the high organic solvents of antioxidizing, patent report is arranged, this organic substance can be used as additive and is applied to lithium ion battery, be used for improving high-temperature behavior and storge quality [the Chinese patent CN201110052098 of lithium ion battery, Chinese patent CN201210007949, Chinese patent CN201110173521].Because the additive use amount is little, generally be lower than 5% even 2%, therefore this occupation mode also can't improve the non-oxidizability of carbonic ester electrolyte, can't be used for high-voltage lithium ion batteries.Patent WO138132A1, CN201080038112, CN201010291454 have tested by lithium salts LiPF
6, the redox window of electrolyte on inert electrode (platinum electrode) formed of carbonate solvent and two nitrile or the two nitrile solvents of fluoro, the result shows, two nitriles or the two nitrile organic substances of fluoro are added in the carbonate solvent in a large number as solvent, can effectively improve the electrochemical oxidation window of electrolyte.But document [Journal of the Electrochemical Society, 2009,156 (1): A60-A65] also finds, this pair of nitrile organic substance and traditional carbon negative pole material compatibility are very poor, and carbon negative pole material is by LiPF
6Can't realize normal charge and discharge cycles in the electrolyte that lithium salts is formed.Therefore to develop with LiPF
6Be the high-pressure type lithium-ion battery electrolytes solvent of lithium salts, must solve the compatibility between two nitrile solvents and the carbon negative pole.
Summary of the invention
The object of the present invention is to provide operating voltage greater than 4.8V, than the high about 1V of existing lithium ion battery, can realize the good circulation performance, simultaneously a kind of high-voltage lithium ion batteries that has favorable compatibility between carbon negative pole and the electrolyte.
Operating voltage of the present invention is greater than 4.8V, and positive electrode is fluoro phosphate, and its general molecular formula is Li
xA
2-xMPO
4F, 1≤x≤2 wherein, A is Na or K, M is Co, Ni, Mn or Fe element; Electrolyte is the high voltage type lithium-ion battery electrolytes, the raw material of described high voltage type lithium-ion battery electrolytes is formed and is comprised lithium salts, carbonate solvent, two nitrile solvents and electrolysis additive, the mass fraction of described each component of electrolyte is lithium salts 5%～20%, carbonate solvent 40%～85%, two nitrile solvents 5%～50%, electrolysis additive 0.1～5%, total amount are 100%.
Described fluoro phosphate can adopt the fluoro cobalt phosphate lithium, and the molecular formula of described fluoro cobalt phosphate lithium is Li
2CoPO
4F.
Described lithium salts can adopt lithium hexafluoro phosphate (LiPF
6) etc.
Described carbonate solvent can be selected from least a in ethyl carbonate ester (EC), dimethyl carbonate (DMC), Methylethyl carbonic ester (EMC), the diethyl carbonate (DEC) etc.
Described pair of nitrile solvents general molecular formula is R-(CN)
2, wherein the R=carbon number is organic carbochain of 4～10.
The described pair of nitrile solvents can be selected from least a in succinonitrile, adiponitrile, the hexamethylene dicyanide etc.
Described electrolysis additive can be selected from least a in dioxalic acid lithium borate (LiBOB), vinylene carbonate (VC), vinylethylene carbonate (VEC), the fluorinated ethylene carbonate (FEC) etc.
Below provide the method for evaluating performance of high-voltage lithium ion batteries of the present invention and electrolyte:
1, the oxidizing potential of electrolyte is measured
Adopt three-electrode system, the linear potential scanning technique is investigated the oxidizing potential of electrolyte, and wherein metal Pt sheet is as work electrode, and metal Li is reference electrode and auxiliary electrode, is limited to 6.5V on the cut-ff voltage, and sweep speed is 1mV/s.
2, battery charging and discharging performance evaluation
The assembled battery model is carried out the charge-discharge test of battery for the CR2025 button cell.Use Li
2CoPO
4F is as positive pole, and material with carbon element is negative pole, and Celgard2400 is assembled into Li/ carbon battery and Li/Li respectively as barrier film
2CoPO
4The F battery is to Li/Li
2CoPO
4The F battery discharges and recharges with the 143mA/g current density, and the Li/ carbon battery is carried out the constant current charge-discharge test with the 72mA/g current density.
Anodal manufacturing process is as follows:
Li
2CoPO
4F material, conductive agent acetylene black (AB), binding agent Kynoar (PVDF) are prepared burden in 80: 10: 10 ratio, place agate jar, and add a certain amount of (NMP) as dispersant, adopt planetary ball mill, speed ball milling mixing 3h with 300rpm makes the slurries with certain viscosity.Be that the circular aluminium flake of 14mm is used washed with de-ionized water after with the ultrasonic processing of 0.1M NaOH 10min to diameter, 120 ° of C convection oven dryings.The slurries that will contain electrode material with little glass rod are coated on the aluminium flake after the processing, and coated weight is about 6～7mg/cm
2Pole piece after the coating uses 20MPa pressure compression molding standby at the dry 1h of 120 ° of C convection oven at hydraulic press.
Negative pole manufacturing process is as follows:
Negative material Delanium (CAG) material, conductive agent acetylene black (AB), binding agent Kynoar (PVDF) are prepared burden in 92: 4: 4 ratio, place agate jar, and add a certain amount of (NMP) as dispersant, adopt planetary ball mill, speed ball milling mixing 3h with 300rpm makes the slurries with certain viscosity.Be that the circular copper sheet of 14mm is used washed with de-ionized water after with the ultrasonic processing of acetone 10min to diameter, 120 ° of C convection oven dryings.The slurries that will contain electrode material with little glass rod are coated on the copper sheet after the processing, and coated weight is about 3～4mg/cm
2Pole piece after the coating uses 10MPa pressure compression molding standby at the dry 1h of 120 ° of C convection oven at hydraulic press.
Compared with prior art, the present invention has following advantage and effect: high-voltage lithium ion batteries operating voltage provided by the invention is higher than the existing about 1V of lithium ion battery greater than 4.8V, has improved the lithium ion battery energy density.The high voltage type electrolyte that uses can have higher electrochemical oxidation window than existing carbonic ester electrolyte, improves the cycle performance of this battery.Simultaneously, owing to used suitable additive in this electrolyte, can obviously improve electrolyte to the compatibility of carbon negative pole, carbon negative pole material can normally discharge and recharge and circulate in this electrolyte.
Description of drawings
Fig. 1 carries out the curve chart that the linear potential sweep test obtains for the present invention to the lithium-ion battery electrolytes of the hexamethylene dicyanide (SUN) that contains different proportion.In Fig. 1, abscissa is current potential (V), and ordinate is electric current (mA); Mark ■ is reference, ● be reference+5%SUN, ▲ be reference+10%SUN, ▼ is reference+20%SUN; Reference electrolyte is not for adding the carbonic ester electrolyte of two nitriles, and component is 1M LiPF
6/ EC+DMC (1: 1, wt%).
Fig. 2 carries out the curve chart that the linear potential sweep test obtains for the present invention to the lithium-ion battery electrolytes of the adiponitrile (ADN) that contains different proportion.In Fig. 2, abscissa is current potential (V), and ordinate is electric current (mA); Mark ■ is reference, ● be reference+5%ADN, ▲ be reference+10%ADN, ▼ is reference+20%AND; Reference is not for adding the carbonic ester electrolyte of two nitriles, and component is 1M LiPF
6/ EC+DEC+EMC (1: 1: 1, wt%).
Fig. 3 is the cycle performance of positive electrode Li2CoPO4F in hexamethylene dicyanide (SUN) electrolyte, and the charging/discharging voltage interval is 3～5.4V, and current density is 143mA/g.In Fig. 3, abscissa is the circulation number of turns, and ordinate is specific capacity (mAh/g); Mark is reference, and zero is reference+5%SUN, and △ is reference+10%SUN, and ▽ is reference+20%SUN; Reference electrolyte is not for adding the carbonic ester electrolyte of two nitriles, and component is 1M LiPF
6/ EC+DMC (1: 1, wt%).
Fig. 4 is the first charge-discharge curve of artificial graphite material (CAG) in SUN electrolyte.The charging/discharging voltage interval is 0.005～2.5V, and current density is 72mA/g.In Fig. 4, abscissa is the circulation number of turns (mAh/g), and ordinate is voltage (V); Mark is reference, and zero is reference+30%SUN, and △ is reference+30%SUN+2%LiBOB; Reference electrolyte is not for adding the carbonic ester electrolyte of two nitriles, and component is 1M LiPF
6/ EC+DMC (1: 1, wt%)
Fig. 5 is the cycle performance of artificial graphite material (CAG) preceding 100 circles in SUN electrolyte, and the charging/discharging voltage interval is 0.005～2.5V, and current density is 72mA/g.In Fig. 5, abscissa is the circulation number of turns, and ordinate is specific capacity (mAh/g); Mark ■ is reference, ● be reference+30%SUN, ▲ be reference+30%SUN+2%LiBOB; Reference electrolyte is not for adding the carbonic ester electrolyte of two nitriles, and component is 1M LiPF
6/ EC+DMC (1: 1, wt%).
Embodiment
Following examples will the present invention is further illustrated by reference to the accompanying drawings.
Embodiment 1
In order to understand different content hexamethylene dicyanide (SUN) to the influence of electrolyte oxidizing potential, with linear potential scanning measuring 1M LiPF
6/ EC+DMC (1: 1, wt%) the linear potential curve of adding different content SUN electrolyte in the electrolyte.The result as shown in Figure 1.As shown in Figure 1, in adding a certain amount of SUN electrolyte system, its oxidation resistance all has enhancing in various degree, and its enhancing degree increases along with the increase of SUN solvent.When SUN content reached 20%, the oxidizing potential of this electrolyte was increased to above 5.5V, far above the electrochemical stability current potential (being lower than 5V) of benchmark electrolyte.
In order to understand different content adiponitrile (ADN) to the influence of electrolyte oxidizing potential, with linear potential scanning measuring 1M LiPF
6/ EC+DEC+EMC (1: 1: 1, wt%) the linear potential curve of adding different content ADN electrolyte in the electrolyte.The result as shown in Figure 2.The same with SUN result, the oxidation resistance of electrolyte obviously improves along with the increase of SUN solvent.
Embodiment 3
In order to understand different content succinonitrile (SN) to the influence of electrolyte oxidizing potential, with linear potential scanning measuring 1MLiPF
6/ EC+DMC (1: 1, wt%) the linear potential curve of adding different content SN electrolyte in the electrolyte, the oxidation resistance of electrolyte obviously improves along with the increase of SN solvent.
Embodiment 4
In order to understand hexamethylene dicyanide (SUN) adding to the influence of anodal material electrochemical performance, this example has been measured the Li2CoPO4F material at 1M LiPF
6/ EC+DMC (1: 1, wt%) contain battery charging and discharging performance in the different proportion SUN electrolyte in the electrolyte, the result is as shown in Figure 3.As shown in Figure 3, the adding of SUN does not have influence substantially for positive electrode Li2CoPO4F specific discharge capacity first, even the degree of SUN increased to 20% o'clock, the first discharge specific capacity of battery still is 135mAh/g, and is almost identical with the specific discharge capacity that uses benchmark electrolyte reference; Positive electrode Li2CoPO4F shows the cycle performance of non-constant in LD120 electrolyte, its 100 times circulation back capacity is 25.1mAh/g, and corresponding capability retention only is 18.4%.And in electrolyte, add 5% and 10%SUN after, the cycle performance of material is significantly improved, 100 circle circulation back capability retentions bring up to 61.6% and 64.7% respectively.
In order to understand adiponitrile (ADN) adding to the influence of anodal material electrochemical performance, this example has been measured the Li2CoPO4F material at 1M LiPF
6/ EC+DEC+EMC (1: 1: 1, wt%) contain battery charging and discharging performance in the different proportion ADN electrolyte in the electrolyte.Behind interpolation 5% and the 10%ADN, can obviously improve the cyclicity of material equally in electrolyte, 100 circle circulation back specific capacities are 72.9mAh/g and 71.4mAh/g, and corresponding capability retention is respectively 54.5% and 52.8%.
Embodiment 6
In order to understand hexamethylene dicyanide (SUN) to the influence of carbon negative pole material chemical property, this example has been measured Delanium material (CAG) at 1M LiPF
6/ EC+DMC (1: 1, wt%) contain battery charging and discharging performance in the 30%SUN electrolyte in the electrolyte, the result is shown in Figure 4 and 5.As shown in Figure 4, the adding of SUN has a significant effect to the discharge capacity of CAG material, and when adding 30%SUN, the discharge capacity first of material is down to 277mAh/g from 368mAh/g, the discharge capacity that adds the obvious reduction of affiliation negative material CAG of this explanation SUN.As shown in Figure 5, the capacity of material C AG and cycle performance all are better than and contain material in the 30%SUN electrolyte in LD120 electrolyte.After 100 circle circulations, the material discharging capacity is 250mAh/g in the LD120 electrolyte, and capability retention is 76.0%; The material discharging capacity only is 143mAh/g in the 30%SUN electrolyte and contain, and capability retention is 66.5%.
Embodiment 7
Add the effect of improving nitrile and carbon negative pole material compatibility in order to understand additive LiBOB, this example has been measured the chemical property that adds 2%LiBOB among the embodiment 6, and the result is shown in Figure 4 and 5.When at SUN be in the electrolyte when adding 2%LiBOB, material discharge capacity first obviously increases, and reaches 330mAh/g, its cycle performance obviously improves, 100 times circulation back discharge capacity is increased to 224mAh/g, capability retention is up to 86.8%.
Embodiment 8
Add the effect of improving nitrile and carbon negative pole material compatibility in order to understand additive FEC, this example has been measured the chemical property that adds 5%FEC among the embodiment 6, when at SUN be in the electrolyte when adding 2%FEC, material discharge capacity first is increased to 320mAh/g, and its 100 circulation volume conservation rates reach 85%.
Embodiment 9
Add the effect of improving nitrile and carbon negative pole material compatibility in order to understand additive VC and VEC, this example has been measured the chemical property that adds 1%VC and 0.1%VEC among the embodiment 6, when at SUN be in the electrolyte when adding 1%VC and 0.2%VEC, material discharge capacity first is increased to 325mAh/g, and its 100 circulation volume conservation rates reach 87.5%.
Claims (8)
1. high-voltage lithium ion batteries is characterized in that positive electrode is fluoro phosphate, and its general molecular formula is Li
xA
2-xMPO
4F, 1≤x≤2 wherein, A is Na or K, M is Co, Ni, Mn or Fe element; Electrolyte is the high voltage type lithium-ion battery electrolytes, the raw material of described high voltage type lithium-ion battery electrolytes is formed and is comprised lithium salts, carbonate solvent, two nitrile solvents and electrolysis additive, the mass fraction of described each component of electrolyte is lithium salts 5%～20%, carbonate solvent 40%～85%, two nitrile solvents 5%～50%, electrolysis additive 0.1～5%, total amount are 100%.
2. high-voltage lithium ion batteries according to claim 1 is characterized in that the operating voltage of described high-voltage lithium ion batteries is greater than 4.8V.
3. high-voltage lithium ion batteries according to claim 1 is characterized in that described fluoro phosphate adopts the fluoro cobalt phosphate lithium, and the molecular formula of described fluoro cobalt phosphate lithium is Li
2CoPO
4F.
4. high-voltage lithium ion batteries according to claim 1 is characterized in that described lithium salts adopts lithium hexafluoro phosphate.
5. high-voltage lithium ion batteries according to claim 1 is characterized in that described carbonate solvent is selected from least a in ethyl carbonate ester, dimethyl carbonate, Methylethyl carbonic ester, the diethyl carbonate.
6. high-voltage lithium ion batteries according to claim 1 is characterized in that described pair of nitrile solvents general molecular formula is R-(CN)
2, wherein the R=carbon number is organic carbochain of 4～10.
7. high-voltage lithium ion batteries according to claim 1 is characterized in that described pair of nitrile solvents is selected from least a in succinonitrile, adiponitrile, the hexamethylene dicyanide.
8. high-voltage lithium ion batteries according to claim 1 is characterized in that described electrolysis additive is selected from least a in dioxalic acid lithium borate, vinylene carbonate, vinylethylene carbonate, the fluorinated ethylene carbonate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779604A (en) * | 2014-02-21 | 2014-05-07 | 宁德新能源科技有限公司 | Lithium ion secondary battery and electrolyte thereof |
| CN104401957A (en) * | 2014-10-13 | 2015-03-11 | 济南大学 | Hydrothermally preparing method of lithium secondary battery anode material cobalt lithium fluorophosphate |
| WO2017215121A1 (en) * | 2016-06-15 | 2017-12-21 | 中国科学院宁波材料技术与工程研究所 | Battery paste, battery electrode plate, and preparation method therefor |
| WO2018001274A1 (en) * | 2016-06-30 | 2018-01-04 | 江苏国泰超威新材料有限公司 | Application of fluorophosphate in preparation of lithium ion battery electrode, lithium ion battery electrode and preparation method therefor and application thereof |
| CN109980221A (en) * | 2017-12-27 | 2019-07-05 | 中国科学院上海硅酸盐研究所 | A kind of anode material for high-voltage lithium ion and its preparation method and application |
| CN116799300A (en) * | 2022-03-15 | 2023-09-22 | 浙江大学 | High-voltage electrolyte suitable for quick-charging lithium battery and lithium battery |
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| CN101548425A (en) * | 2006-12-06 | 2009-09-30 | 三菱化学株式会社 | Nonaqueous electrolyte solution and nonaqueous electrolyte secondary battery |
| CN102576906A (en) * | 2009-08-28 | 2012-07-11 | 株式会社爱考斯研究 | Electrolyte for lithium-ion cell |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101548425A (en) * | 2006-12-06 | 2009-09-30 | 三菱化学株式会社 | Nonaqueous electrolyte solution and nonaqueous electrolyte secondary battery |
| CN102576906A (en) * | 2009-08-28 | 2012-07-11 | 株式会社爱考斯研究 | Electrolyte for lithium-ion cell |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779604A (en) * | 2014-02-21 | 2014-05-07 | 宁德新能源科技有限公司 | Lithium ion secondary battery and electrolyte thereof |
| CN103779604B (en) * | 2014-02-21 | 2016-10-19 | 宁德新能源科技有限公司 | Lithium rechargeable battery and electrolyte thereof |
| CN104401957A (en) * | 2014-10-13 | 2015-03-11 | 济南大学 | Hydrothermally preparing method of lithium secondary battery anode material cobalt lithium fluorophosphate |
| WO2017215121A1 (en) * | 2016-06-15 | 2017-12-21 | 中国科学院宁波材料技术与工程研究所 | Battery paste, battery electrode plate, and preparation method therefor |
| US10978693B2 (en) | 2016-06-15 | 2021-04-13 | Ningbo Institute Of Materials Technology And Engineering, Chinese Academy Of Sciences | Battery paste, battery electrode plate, and preparation method therefor |
| WO2018001274A1 (en) * | 2016-06-30 | 2018-01-04 | 江苏国泰超威新材料有限公司 | Application of fluorophosphate in preparation of lithium ion battery electrode, lithium ion battery electrode and preparation method therefor and application thereof |
| CN109980221A (en) * | 2017-12-27 | 2019-07-05 | 中国科学院上海硅酸盐研究所 | A kind of anode material for high-voltage lithium ion and its preparation method and application |
| CN116799300A (en) * | 2022-03-15 | 2023-09-22 | 浙江大学 | High-voltage electrolyte suitable for quick-charging lithium battery and lithium battery |
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Application publication date: 20131009 |