CN102055017A - Carbonic ester electrolyte with annular sultone and oxalyl lithium tetraborate composition added - Google Patents
Carbonic ester electrolyte with annular sultone and oxalyl lithium tetraborate composition added Download PDFInfo
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- CN102055017A CN102055017A CN2010102364540A CN201010236454A CN102055017A CN 102055017 A CN102055017 A CN 102055017A CN 2010102364540 A CN2010102364540 A CN 2010102364540A CN 201010236454 A CN201010236454 A CN 201010236454A CN 102055017 A CN102055017 A CN 102055017A
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Abstract
The invention discloses a carbonic ester electrolyte with an annular sultone and oxalyl lithium tetraborate composition added. The electrolyte adopts a carbonate as solvent, and adopts the following formulation proportion by weight portion: 1 solvent, 0.068-0.2 lithium carbonate, and 0.005-0.2 additive; and the additive is an annular sultone and oxalyl lithium tetraborate composition which adopts the component proportion by weight portion: 1: 0.1-12, preferably, 1:0.5-5, and further preferably, 1:1-3. The carbonic ester electrolyte with the annular sultone and oxalyl lithium tetraborate composition added adopts the annular sultone and oxalyl lithium tetraborate composition as the additive, the annular sultone is provided with good film forming property; the oxalyl lithium tetraborate improves the stability and the circulative performance of the electrolyte system, the safety performance is greatly improved, meanwhile electric conductivity can not be affected; and the manufacturing technology is simple, the cost is low, the circulative performance is improved by more than 50% and the electrolyte is suitable for various lithium ion batteries.
Description
Technical field
The present invention relates to lithium ion battery, particularly a kind of lithium ion battery carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition.
Background technology
Lithium ion battery has advantages such as specific energy height, in light weight, memory-less effect, be widely used in the powerful electronic installation, for example on notebook computer, digital camera, DV, electric automobile and the electric tool, occupation rate of market is higher than similar NI-G, Ni-MH battery far away.But the lithium ion battery performance of domestic production at present generally is inferior to external product, especially cycle performance.
Lithium ion battery is a secondary cell, can repeated charge-discharge cycles use, and in charge and discharge process, between the volume of its internal electrode and the structure reversible variation can take place.Lithium ion battery uses the anode pole piece of the activating substance that contains lithium and the cathode pole piece of special molecular structure carbon usually.In charging process, applying electrical potential forces anodal compound to discharge lithium ion, embeds the negative pole molecules align and is in the carbon of lamellar structure; During discharge, lithium ion is separated out from negative pole, again with the compound combination of positive pole, and this mobile electric current that produced of lithium ion.In general, require battery that charge-discharge performance, cycle life characteristics, high-temperature standing properties are preferably arranged.For the battery of cathode pole piece use carbonaceous material, along with the variation of electrolyte kind, the performance of battery has a great difference.Existing ethylene carbonate, dimethyl carbonate and ethylene carbonate are the electrolyte of solvent, and solvent can be accompanied by the generation of gas in the electrode process and decompose, and so, along with the increase of charge and discharge cycles number of times, battery capacity can reduce gradually.
Using ethylene carbonate, dimethyl carbonate and ethylene carbonate to be nonaqueous electrolytic solution as the electrolyte of solvent, is the critical material of lithium ion battery, determines the performance of battery to a great extent, to the influence of the cycle performance of battery more so.This be because, when lithium ion battery changed into, electrolyte can form one deck solid electrolytic liquid film (SEI film) on both positive and negative polarity, this layer solid electrolyte film is lower to the conductivity of lithium ion, can cause the charge-discharge performance of battery significantly to reduce.The cycle performance of battery and high rate performance depend on this layer SEI film, and electrolyte is formed the quality that influences SEI film component, structure and performance.
Summary of the invention
For improving charge-discharge performance, cycle performance and the high-temperature behavior of lithium ion battery, the invention provides a kind of lithium ion battery with being the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition.
The present invention adds the carbonic ester electrolyte of ring-type sultones and oxalyl lithium borate composition, and selecting carbonic ester for use is solvent, and its configuration proportion is: solvent 1 weight portion; Lithium salts 0.068-0.2 weight portion; Additive 0.005-0.2 weight portion;
Described additive is ring-type sultones and oxalyl lithium borate composition, and its composition weight ratio is 1: 0.1-12; Be preferably 1: 0.5-5; More preferably 1: 1-3.
The preferred value of the preparation part by weight of described electrolyte is: solvent 1 weight portion; Lithium salts 0.1-0.164 weight portion; Additive 0.01-0.1 weight portion.
The further preferred value of the preparation part by weight of described electrolyte is: solvent 1 weight portion; Lithium salts 0.123-0.164 weight portion; Additive 0.06-0.08 weight portion.
Described carbonic ester is selected from one or more in ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate and the gamma-butyrolacton, is preferably ethylene carbonate or propene carbonate.
The purity of described carbonic ester is greater than 99.98%, and moisture content is less than 0.0005%.
Described lithium salts is selected from one or more in lithium hexafluoro phosphate, LiBF4, diacetyl lithium borate and the arsenic hexafluoride lithium.
Described ring-type sultones is selected from 1,3-propane sultone, 1, and 4-butane sultones, 1,3-butane sultones and 1, one or more in the 3-propene sulfonic acid lactone are preferably 1, the 3-propane sultone.
The compound method of described electrolyte is as follows:
4) in solubilizer such as the reactor;
5) add lithium salts, be heated to 40-55 ℃, stir, form basic non-aqueous eletrolyte;
6) with the basic electrolyte cool to room temperature, add additive, i.e. ring-type sultones and oxalyl difluoro lithium borate composition, ultrasonic agitation forms water white electrolyte.
The present invention adds the carbonic ester electrolyte of ring-type sultones and oxalyl lithium borate composition, and adopting ring-type sultones and oxalyl difluoro lithium borate composition is additive, and the ring-type sultones has good filming performance, oxalyl difluoro lithium borate and PF
6Form the compound of stinging, organized LiPF
6Catabolite PF
6And the chemical reaction between the electrolyte, improved the stability of electrolyte system, and the formation that can improve diaphragm when once charging, protection is based on negative pole in the electrolyte of carbonic ester, reduced the irreversible capacity that electrolyte interface consumed, improved cycle performance, security performance is greatly improved, simultaneously can not influence conductivity, conductivity reaches 11.0mS/cm; And production technology is simple, and is with low cost, and cycle performance improves more than 50%, is applicable to various lithium ion batteries.
Description of drawings
Fig. 1 is that the present invention adds the carbonic ester electrolyte of ring-type sultones and oxalyl lithium borate composition and the cycle performance correlation curve figure of Comparative Examples electrolyte.
Embodiment
Below in conjunction with embodiment the carbonic ester electrolyte that the present invention adds ring-type sultones and oxalyl lithium borate composition is done more detailed explanation.
Embodiment one:
1) ethylene carbonate that refines (EC), gamma-butyrolacton (GBL), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 880g carbonate solution;
2) slowly add the LiPF of 1M
6120g makes it to dissolve fully, forms basic electrolyte;
3) add 2.0% 1,3-propane sultone and 0.5% oxalyl difluoro lithium borate composition additive, ultrasonic agitation is even, obtains water white electrolyte, water white electrolyte is by 100%.
The electrolyte property test: for the moisture and the acidity of strictness control electrolyte, gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.In the time spent hand ion battery electro-chemical test instrument change into, cycle performance test, test condition is: at first with constant current 0.2C with 18650 type lithium ion cell chargings to 4.2V, change the 4.2V constant voltage charge immediately over to, cut-off current is 40mA, stops when being discharged to voltage 2.75 with constant current 0.2C then.So circulation is 3 times, and the electric current of using 0.5C instead carries out charge and discharge cycles between 2.75-4.2V, and with this cycle performance of determining battery, the circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Comparative Examples one:
1) ethylene carbonate that refines (EC), gamma-butyrolacton (GBL), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 880g carbonate solution;
2) slowly add the LiPF of 1M
6120g makes it to dissolve fully, forms basic electrolyte.
The electrolyte of the Comparative Examples one that obtains is tested by the method for testing of embodiment one, and test result is seen Fig. 1 and table 1.
As can be seen, the cycle performance of embodiment one obviously is better than Comparative Examples one, and embodiment one cycle-index (80% capacity) can surpass 600 times, and the cycle-index of Comparative Examples one same situation is less than 400 times.
Comparative Examples two:
1) ethylene carbonate that refines (EC), gamma-butyrolacton (GBL), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 880g carbonate solution;
2) slowly add the LiPF of 1M
6120g makes it to dissolve fully, forms basic electrolyte;
3) add 1 of 2.0g, the 3-propane sultone, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Comparative Examples three
1) ethylene carbonate that refines (EC), gamma-butyrolacton (GBL), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 880g carbonate solution;
2) slowly add the LiPF of 1M
6120g makes it to dissolve fully, forms basic electrolyte;
3) the oxalyl difluoro lithium borate of adding 5g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment two
1) ethylene carbonate that refines (EC), DMC, methyl ethyl carbonate (EMC) and propene carbonate were by weight 0.8: 1: 1: 0.2 mixes, and obtains the 880g carbonate solution;
2) slowly add the LiPF of 1.1M
6120g makes it to dissolve fully, forms basic electrolyte;
3) add 1.0% 1,3-propane sultone and 1.0% oxalyl difluoro lithium borate composition additive, ultrasonic agitation is even, obtains water white electrolyte, water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.Do the heavy impact test according to the box hat battery of present embodiment making and the box hat battery of embodiment one and Comparative Examples one, its security performance contrast sees Table 2.
Embodiment three:
1) ethylene carbonate that refines (EC), DMC, methyl ethyl carbonate (EMC) and diethyl carbonate (DEC) were by weight 0.8: 1: 1: 0.2 mixes, and obtains the 880g carbonate solution;
2) slowly add the LiPF of 1.2M
6144g makes it to dissolve fully, forms basic electrolyte;
3) be sequentially added into 1.6% vinylene carbonate, 1.5% 1,3-propane sultone and 1.5% oxalyl difluoro lithium borate composition additive, ultrasonic agitation is even, obtains water white electrolyte, water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment four:
1) ethylene carbonate that refines (EC), DMC mixed by weight 1: 1, obtained the 880g carbonate solution;
2) slowly add the LiPF of 1.1M
666g makes it to dissolve fully, forms basic electrolyte;
3) be sequentially added into 1.0% 1,3-propane sultone and 1.0% oxalyl difluoro lithium borate composition additive, ultrasonic agitation is even, obtains water white electrolyte, water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment five:
1) ethylene carbonate that refines (EC) 587g, DMC93g mix;
2) slowly add the LiPF of 1.1M
6132g makes it to dissolve fully, forms basic electrolyte;
3) be sequentially added into 1.0% 1,3-propane sultone and 1.0% oxalyl difluoro lithium borate composition additive, ultrasonic agitation is even, obtains water white electrolyte, water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment six:
1) ethylene carbonate that refines (EC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 1000g carbonate solution;
2) slowly add 68g LiPF
6, make it to dissolve fully, form basic electrolyte;
3) be sequentially added into 1 of 4.5g, the oxalyl difluoro lithium borate composition additive of 3-propane sultone and 0.5g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment seven:
1) ethylene carbonate that refines (EC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 1000g carbonate solution;
2) slowly add the LiPF of 100g
6, make it to dissolve fully, form basic electrolyte;
3) be sequentially added into 1 of 9.1g, the oxalyl difluoro lithium borate composition additive of 3-propane sultone and 0.9g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment eight:
1) ethylene carbonate that refines (EC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 1000g carbonate solution;
2) slowly add the LiPF of 100g
6, make it to dissolve fully, form basic electrolyte;
3) be sequentially added into 1 of 66.7g, the oxalyl difluoro lithium borate composition additive of 3-propane sultone and 33.3g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment nine:
1) ethylene carbonate that refines (EC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 1000g carbonate solution;
2) slowly add the LiPF of 160g
6, make it to dissolve fully, form basic electrolyte;
3) be sequentially added into 1 of 45g, the oxalyl difluoro lithium borate composition additive of 3-propane sultone and 15g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment ten:
1) ethylene carbonate that refines (EC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 1000g carbonate solution;
2) slowly add the LiPF of 160g
6, make it to dissolve fully, form basic electrolyte;
3) be sequentially added into 1 of 50g, the oxalyl difluoro lithium borate composition additive of 3-propane sultone and 10g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Embodiment 11:
1) ethylene carbonate that refines (EC), dimethyl carbonate (DMC), methyl ethyl carbonate (EMC) mixed by weight 1: 1: 1, obtained the 1000g carbonate solution;
2) slowly add the LiPF of 100g
6, make it to dissolve fully, form basic electrolyte;
3) be sequentially added into 1 of 9g, the oxalyl difluoro lithium borate composition additive of 3-propane sultone and 1g, ultrasonic agitation is even, obtains water white electrolyte, and water white electrolyte is by 100%.
Gained electrolyte is injected 18650 type cylindrical lithium ion batteries in the Braun glove box, positive pole is a spinelle manganic acid lithium material, and negative pole is a graphite material.The circulate electrolyte performance curve that obtains is seen Fig. 1, and data see Table 1.
Table 1 cycle performance of battery
Table 2 box hat battery (18650 type) security performance contrast test
Claims (9)
1. carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition, selecting carbonic ester for use is solvent, it is characterized in that: described electrolyte quota ratio is: solvent 1 weight portion; Lithium salts 0.068-0.2 weight portion; Additive 0.005-0.2 weight portion; Described additive is ring-type sultones and oxalyl lithium borate composition, and its composition weight ratio is 1: 0.1-12.
2. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 1, it is characterized in that: described additive is the part by weight of ring-type sultones and oxalyl lithium borate composition, is preferably 1: 0.5-5; More preferably 1: 1-3.
3. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 1 and 2, it is characterized in that: the preferred value of the preparation part by weight of described electrolyte is: solvent 1 weight portion; Lithium salts 0.1-0.164 weight portion; Additive 0.01-0.1 weight portion.
4. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 3, it is characterized in that: the further preferred value of the preparation part by weight of described electrolyte is: solvent 1 weight portion; Lithium salts 0.123-0.164 weight portion; Additive 0.06-0.08 weight portion.
5. according to the described carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition of one of claim 1-4, it is characterized in that: described carbonic ester is selected from one or more in ethylene carbonate, propene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate and the gamma-butyrolacton, is preferably ethylene carbonate or propene carbonate.
6. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 5, it is characterized in that: the purity of described carbonic ester is greater than 99.98%, and moisture content is less than 0.0005%.
7. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 6, it is characterized in that: described lithium salts is selected from one or more in lithium hexafluoro phosphate, LiBF4, diacetyl lithium borate and the arsenic hexafluoride lithium.
8. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 7, it is characterized in that: described ring-type sultones is selected from 1,3-propane sultone, 1,4-butane sultones, 1,3-butane sultones and 1, in the 3-propene sulfonic acid lactone one or more are preferably 1, the 3-propane sultone.
9. the carbonic ester electrolyte that adds ring-type sultones and oxalyl lithium borate composition according to claim 8, it is characterized in that: the compound method of described electrolyte is as follows:
1) in solubilizer such as the reactor;
2) add lithium salts, be heated to 40-55 ℃, stir, form basic non-aqueous eletrolyte;
3) with the basic electrolyte cool to room temperature, add additive, i.e. ring-type sultones and oxalyl difluoro lithium borate composition, ultrasonic agitation forms water white electrolyte.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102593520A (en) * | 2012-02-20 | 2012-07-18 | 宁德新能源科技有限公司 | Method for improving hardness of lithium ion cell |
| TWI472083B (en) * | 2011-10-28 | 2015-02-01 | Asahi Chemical Ind | Non-aqueous system secondary cell |
| CN106410282A (en) * | 2016-10-19 | 2017-02-15 | 广州天赐高新材料股份有限公司 | Pretreatment agent and pretreatment method for high-nickel positive electrode of power lithium ion battery |
| CN112830498A (en) * | 2020-11-13 | 2021-05-25 | 厦门永力鑫新能源科技有限公司 | Lithium salt and preparation method thereof, lithium ion battery electrolyte additive, lithium ion battery electrolyte and lithium ion battery |
| CN114094181A (en) * | 2020-08-25 | 2022-02-25 | 深圳市比亚迪锂电池有限公司 | Lithium ion electrolyte, preparation method and lithium ion battery |
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| CN101572331A (en) * | 2009-06-09 | 2009-11-04 | 东莞市杉杉电池材料有限公司 | Lithium ion battery electrolyte applicable to high-temperature environment and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI472083B (en) * | 2011-10-28 | 2015-02-01 | Asahi Chemical Ind | Non-aqueous system secondary cell |
| US10644353B2 (en) | 2011-10-28 | 2020-05-05 | Asahi Kasei Kabushiki Kaisha | Non-aqueous secondary battery |
| CN102593520A (en) * | 2012-02-20 | 2012-07-18 | 宁德新能源科技有限公司 | Method for improving hardness of lithium ion cell |
| CN106410282A (en) * | 2016-10-19 | 2017-02-15 | 广州天赐高新材料股份有限公司 | Pretreatment agent and pretreatment method for high-nickel positive electrode of power lithium ion battery |
| CN114094181A (en) * | 2020-08-25 | 2022-02-25 | 深圳市比亚迪锂电池有限公司 | Lithium ion electrolyte, preparation method and lithium ion battery |
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| CN112830498A (en) * | 2020-11-13 | 2021-05-25 | 厦门永力鑫新能源科技有限公司 | Lithium salt and preparation method thereof, lithium ion battery electrolyte additive, lithium ion battery electrolyte and lithium ion battery |
| CN112830498B (en) * | 2020-11-13 | 2022-08-30 | 厦门永力鑫新能源科技有限公司 | Lithium salt and preparation method thereof, lithium ion battery electrolyte additive, lithium ion battery electrolyte and lithium ion battery |
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Application publication date: 20110511 |