CN105449272A - A salt additive for an electrolyte of a lithium ion battery - Google Patents

A salt additive for an electrolyte of a lithium ion battery Download PDF

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Publication number
CN105449272A
CN105449272A CN201410427343.6A CN201410427343A CN105449272A CN 105449272 A CN105449272 A CN 105449272A CN 201410427343 A CN201410427343 A CN 201410427343A CN 105449272 A CN105449272 A CN 105449272A
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Prior art keywords
ion battery
lithium
battery electrolytes
electrolyte
salt additives
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CN201410427343.6A
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Inventor
贠娇娇
郑洪河
沈鸣
张先林
沈锦良
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JIANGSU HUASHENG CHEMICALS CO Ltd
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JIANGSU HUASHENG CHEMICALS CO Ltd
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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

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Abstract

The invention relates to a salt additive for an electrolyte of a lithium ion battery. The salt additive comprises nickel cations. The salt additive greatly improves the specific capacity of a graphite anode in the lithium ion battery, and improves rate capability of a cathode material. The invention also relates to the electrolyte system using the salt additive. The salt additive is simple in process and technique, and is suitable for popularization and application in lithium ion batteries, electrolytes, and other related fields.

Description

The salt additives of lithium-ion battery electrolytes
Technical field
The present invention relates to the salt additives of lithium-ion battery electrolytes and use the electrolyte system of this salt additives.This salt additives add the high rate performance that can improve graphite negative electrode of lithium ion battery first charge-discharge capacity and cell positive material.
Background technology
Lithium ion battery has the features such as high-energy-density, high voltage and long-life due to it and is widely used in the portable electronics market such as cell phone, digital camera, PC, also become the important selection in current power and energy storage field simultaneously, development " low-carbon economy " and enforcement China " 12 " new forms of energy strategy are had great importance.
Lithium-ion battery electrolytes, primarily of lithium salts and organic carbonate composition, is called as the blood of battery.Electrolyte is the bridge connecting positive and negative electrode, plays a part transmission ion and conduction current at inside battery.Therefore, electrolyte properties affects highly significant to battery performance, and the performance of optimization to raising lithium ion battery of electrolyte composition and performance has very important significance.
In lithium ion battery first charge-discharge process, can there is irreversible reduction reaction on Carbon anode surface in lithium salts, solvent and additive, form the solid electrolyte interface film (SEI film) that one deck electronic isolation ion can be led.The formation of SEI is an irreversible reaction, can consume the lithium ion that the part in battery can circulate, and causes the reversible capacity of battery to reduce.Add additive can when do not increase or substantially do not increase battery cost, do not change production technology improve cell integrated chemical property, it has consumption feature little, with strong points.Additive is in the past that organic solvent is as vinylene carbonate (VC), fluorinated ethylene carbonate (FEC) etc. mostly.These additives not only prepare and purification difficulty large, and itself also has higher combustibility, to reducing the cost of battery and to improve the fail safe of battery unfavorable.
Therefore, prior art is badly in need of a kind of additive that can improve graphite negative electrode of lithium ion battery discharge capacity and improve iron phosphate lithium positive pole high rate performance.
Summary of the invention
The present invention aims to provide a kind of salt additives that can improve graphite negative electrode of lithium ion battery discharge capacity and improve lithium ion cell positive high rate performance.This salt additives has aboundresources, price is low, use amount is little, performance is good and without advantages such as combustibility, and in lithium-ion battery electrolytes, have use value widely.
For achieving the above object, the invention provides a kind of salt additives of lithium-ion battery electrolytes, wherein, this salt additives comprises nickel metal cation.
In one embodiment of the present invention, in described lithium-ion battery electrolytes, solvent is carbonic ester; Electrolyte is selected from LiPF 6, LiBF 4, LiClO 4, one or more in LiTFSI, LiBOB and LiDOFB.
In one embodiment of the present invention, described lithium-ion battery electrolytes is battery electrolyte that is liquid or gel state.
In one embodiment of the present invention, described electrolytical concentration is 0.8 ~ 2.0M.
In one embodiment of the present invention, this salt additives comprises and is selected from Cl -, NO 3 -, C 2o 4 2-, acetate (Ac -) and sulfonate radical in one or more anion.
In one embodiment of the present invention, in described lithium-ion battery electrolytes, the content of described salt additives is between 50 to 10000ppm.
On the other hand, the invention provides a kind of lithium ion battery comprising lithium-ion battery electrolytes, wherein, described lithium-ion battery electrolytes comprises salt additives of the present invention.
Another aspect, the invention provides described salt additives and is improving the purposes in the electrode specific energy of lithium ion battery, specific power and cyclical stability.
Finally, the invention provides a kind of preparation method of lithium-ion battery electrolytes of nickeliferous salt additives, said method comprising the steps of:
(1) nickel salt is fully dry under vacuum;
(2) obtain anhydrous nickel salt after cooling, enclosed package is for subsequent use;
(3) under argon shield, anhydrous nickel salt is added in lithium-ion battery electrolytes as electrolyte, stirs;
(4) described lithium-ion battery electrolytes encapsulates preservation under argon shield, obtains the lithium-ion battery electrolytes of nickeliferous salt additives.
Specifically, the technical solution used in the present invention is: use the salt additives based on metallic nickel ions.
In the execution mode that the present invention is concrete, the anion of described nickel salt additive can be Cl -, ClO 4 -, NO 3 -, C 2o 4 2-, acetate (Ac -) and sulfonate radical in one or more.
On the other hand, the invention provides the method utilizing nickel salt additive to prepare high performance lithium ion battery electrolyte, described method comprises the steps:
(1) nickel salt is fully dry under vacuum;
(2) obtain anhydrous nickel salt after cooling, enclosed package is for subsequent use;
(3) under argon shield, anhydrous nickel salt is added in (such as, industrial) lithium-ion battery electrolytes as electrolyte, stirs;
(4) described lithium-ion battery electrolytes encapsulates preservation under argon shield, obtains the lithium-ion battery electrolytes containing nickel salt additive.
In described step (1), the anion of nickel salt is selected from Cl -, ClO 4 -, NO 3 -, C 2o 4 2-, acetate (Ac -) and sulfonate radical in one or more.In described step (1), baking temperature is between 80-180 DEG C, drying time 2-24 hour.
In described step (3), lithium-ion battery electrolytes is the battery electrolyte that lithium ion battery industry is commonly used, and wherein, carbonic ester is solvent; LiPF 6, LiBF 4, LiClO 4, LiTFSI, LiBOB or LiDOFB be liquid state or the gel state electrolyte system of electrolyte (solute).In the present invention, the electrolytical concentration of lithium salts is 0.5 ~ 2.0M.
In described step (3), in electrolyte, the concentration of nickel salt additive controls between 50-10000ppm.
In a further aspect, the invention provides the high performance lithium ion battery using above-mentioned obtained lithium-ion battery electrolytes to manufacture.
Relative to existing lithium-ion battery electrolytes, the electrolyte adopting the present invention to prepare and lithium ion battery have the following advantages:
(1) electrode specific energy is high: the battery using the electrolyte containing described nickel salt additive to prepare can improve the specific capacity of Carbon anode;
(2) specific power of battery is large: for traditional electrolyte, uses the anode high rate performance of the electrolyte manufacture containing nickel salt additive to significantly improve; With
(3) good cycling stability: in battery electrochemical process, electrode/electrolyte boundary is stablized, and the side reaction between electrode and electrolyte is little, is conducive to the cycle life extending battery.
Owing to employing nickel salt additive provided by the invention, the present invention compared with prior art has following advantages:
1. the present invention has excavated new industrial use to known nickel salt electrolyte, has opened up a new application;
2. nickel salt electrolyte is prepared high performance lithium ion battery electrolyte as additive by the present invention, and battery specific capacity prepared therefrom is high, and good rate capability, has extended cycle life.
3. to development long-life energy storage and power lithium-ion battery, there is using value and prospect significantly by the lithium ion battery of high performance lithium ion battery electrolyte of the present invention manufacture.
In the present invention, manufacture and the test of lithium ion battery is carried out in the following manner:
1. the manufacture of cathode pole piece
Adopt the Carbon anode sheet of Kynoar (PVDF) binding agent:
(1) getting 8 grams of PVDF is dissolved in 100 grams of 1-METHYLPYRROLIDONE (NMP) organic solvents;
(2) 3.2 grams of acetylene black conductors are added after fully stirring;
(3) 10000 revs/min of lower high-speed stirred, obtained binding agent-conductive agent compound;
(4) 88.8 grams of spherical graphite electrode materials, mixed pulps are added;
(5) fully stir 4 hours under the speed of 4000 revs/min, slurry is fully mixed;
(6) obtained slurry even spread and drying on coating machine, use after pole drying roll squeezer, under 10 ~ 20 atmospheric pressures, obtained electrode slice is pressed into porosity is 30%.
2. the manufacture of anode pole piece
In the present invention, with such as LiFePO 4positive electrode is research object:
(1) 10g Kynoar (PVDF) binding agent and 10g acetylene black conductor are dispersed in 100gN-methyl pyrrolidone (NMP) solvent, obtained binding agent-conductive agent mixture;
(2) described binding agent-conductive agent compound and 80gLiFePO 4mixed pulp, with the rotating speed high-speed stirred of 4000 turns per minute, mixing time is no less than 2 hours, is fully mixed by whole slurry;
(3) be coated with on coating machine and drying by obtained slurry, the dry thickness of control electrode sheet, between 70 ~ 80 microns, then uses and is pressed between 55 ~ 65 microns by the thickness of obtained electrode slice roll squeezer.
3. the manufacture of button cell
In the present invention, above-mentioned anode pole piece, cathode pole piece, Celgard2400 barrier film (purchased from American Celgard company) and 1mol/LLiPF is used 6/ ethylene carbonate (EC)+dimethyl carbonate or diethyl carbonate (DMC or DEC) (volume ratio is 1:1) electrolyte or containing 500ppmNiC 2o 4the 1mol/LLiPF of additive 6the electrolyte of/EC+DMC or DEC (volume ratio is 1:1) assembles button cell in glove box.According to the conventional process that button cell manufactures, after cutting, drying sheet, assembling, fluid injection and sealing compacting, the battery of gained changes into.
4. the changing into of battery
Use 0.1mA/cm 2the constant current of current density carries out charge and discharge cycle 3 times; The charge cutoff voltage of graphite cathode lithium ion battery is 2.0V, and discharge cut-off voltage is 0.01V; The charge cutoff voltage of iron phosphate lithium positive pole lithium ion battery is 2.5V, and discharge cut-off voltage is 4.2V.Complete after changing into, cycle performance test is carried out to battery.
The system of cycle performance of battery test is: with 2mA/cm 2the constant current of current density carries out charge and discharge circulation to graphite cathode and iron phosphate lithium positive pole lithium ion battery.The charge cutoff voltage of graphite cathode lithium ion battery is 2.0V, and discharge cut-off voltage is 0.01V; The charge cutoff voltage of iron phosphate lithium positive pole lithium ion battery is 2.5V, and discharge cut-off voltage is 4.2V; Circular gap 10 minutes, circulates 200 times with such system.
Test result shows: the lithium ion batteries anodes specific capacity using the electrolyte containing nickel salt additive to manufacture improves more than 5% (see Fig. 1); The high rate performance of iron phosphate lithium positive pole have also been obtained and significantly improves (see Fig. 2).Moreover, the lithium ion battery life-span using electrolyte of the present invention to prepare is significantly improved (Fig. 3).
In sum, the lithium ion battery adopting the electrolyte of nickel salt additive to prepare has higher capacity and longer cycle life, has good meaning to development long-life power and energy storage lithium ion battery.
Accompanying drawing explanation
Fig. 1 be in one embodiment of the present invention 1 graphite cathode containing nickel salt additive NiC 2o 4with the first charge-discharge curve do not had in the electrolyte of nickel salt additive.
Fig. 2 be in one embodiment of the present invention 1 iron phosphate lithium positive pole containing nickel salt additive NiC 2o 4with the high rate performance do not had in the electrolyte of nickel salt additive.
Fig. 3 be in one embodiment of the present invention 1 graphite cathode containing nickel salt additive NiC 2o 4with the long-term cycle performance do not had in the electrolyte of nickel salt additive.
Embodiment
The present invention is further detailed by following examples, but should be noted that protection scope of the present invention is not limited to following embodiment.In the scope not departing from object described herein and aim, change wherein and amendment are included within technical scope of the present invention.
Embodiment 1:
Get high purity N iC 2o 4(99.9%) 5g, is placed in vacuum drying chamber, and under 120 DEG C of conditions, vacuumize 8 hours, takes out for subsequent use.
Under high-purity argon gas protection, by LITHIUM BATTERY 2500ml ethylene carbonate (EC) and 2500ml diethyl carbonate (DEC) 1:1 ratio mixing by volume, dissolve in 760gLiPF 6salt, is prepared into 1mol/LLiPF 6the electrolyte of/(EC+DEC) (1:1).
Get the NiC of 1g bone dry 2o 4, join 5000ml1mol/LLiPF 6in the electrolyte of/(EC+DEC) (1:1), stir, obtain containing 200ppmNiC 2o 4the 1mol/LLiPF of additive 6the electrolyte of/(EC+DEC) (1:1).
Test embodiment 1 as described herein, test result shows: the lithium ion batteries anodes specific capacity using the electrolyte containing nickel salt additive to manufacture improves more than 5% (see Fig. 1); The high rate performance of iron phosphate lithium positive pole have also been obtained and significantly improves (see Fig. 2).Moreover, the lithium ion battery life-span using electrolyte of the present invention to prepare is significantly improved (Fig. 3).
Embodiment 2:
Get high-purity acetic acid nickel (Ac) 2(99.9%) 5g, is placed in vacuum drying chamber, and under 100 DEG C of conditions, vacuumize 10 hours, takes out for subsequent use.
Under high-purity argon gas protection, by LITHIUM BATTERY 2500ml ethylene carbonate (EC) and 2500ml dimethyl carbonate (DMC) 1:1 ratio mixing by volume, dissolve in 760gLiPF 6salt, is prepared into 1mol/LLiPF 6the electrolyte of/(EC+DMC) (1:1).
Get the Ni (Ac) of 2g bone dry 2, join 5000ml1mol/LLiPF 6in the electrolyte of/(EC+DMC) (1:1), stir, obtain containing 400ppmNi (Ac) 2the 1mol/LLiPF of additive 6the electrolyte of/(EC+DMC) (1:1).
Test embodiment 2 as described herein, test result is similar to the test result of embodiment 1: the lithium ion batteries anodes specific capacity using the electrolyte containing nickel salt additive to manufacture improves more than 5%; The high rate performance of iron phosphate lithium positive pole have also been obtained and significantly improves; Be significantly improved with the lithium ion battery life-span using electrolyte of the present invention to prepare.
Embodiment 3:
Get high purity N i (ClO 4) 2(99.9%) 5g, is placed in vacuum drying chamber, and under 150 DEG C of conditions, vacuumize 12 hours, takes out for subsequent use.
Under high-purity argon gas protection, by LITHIUM BATTERY 2000ml ethylene carbonate (EC), the 2:2:1 mixing by volume of 2000ml methyl ethyl carbonate (EMC) and 1000ml dimethyl carbonate (DMC), dissolves in 760gLiPF 6salt, is prepared into 1mol/LLiPF 6the electrolyte of/(EC+EMC+DMC) (2:2:1).
Get the Ni (ClO of 1g bone dry 4) 2, join 5000ml1mol/LLiPF 6in the electrolyte of/(EC+EMC+DMC) (2:2:1), stir, obtain containing 200ppmNi (ClO 4) 2the 1mol/LLiPF of additive 6the electrolyte of/(EC+EMC+DMC) (2:2:1).
Test embodiment 3 as described herein, test result is similar to the test result of embodiment 1: the lithium ion batteries anodes specific capacity using the electrolyte containing nickel salt additive to manufacture improves more than 5%; The high rate performance of iron phosphate lithium positive pole have also been obtained and significantly improves; Be significantly improved with the lithium ion battery life-span using electrolyte of the present invention to prepare.
Embodiment 4:
Get high-purity trifluoromethyl sulphonic acid nickel C 2f 6niO 6s 2(99.5%) 5g, is placed in vacuum drying chamber, and under 80 DEG C of conditions, vacuumize 12 hours, takes out for subsequent use.
Under high-purity argon gas protection, by LITHIUM BATTERY 2000ml ethylene carbonate (EC), the 2:1:2 mixing by volume of 1000ml second methyl carbonic (EMC) and 2000ml dimethyl carbonate (DEC), dissolves in 760gLiPF 6salt, is prepared into 1mol/LLiPF 6the electrolyte of/(EC+EMC+DEC) (2:1:2).
Get the C of 3g bone dry 2f 6niO 6s 2join 5000ml1mol/LLiPF 6in the electrolyte of/(EC+EMC+DEC) (2:1:2), stir, obtain containing 600ppmC 2f 6niO 6s 2the 1mol/LLiPF of additive 6the electrolyte of/(EC+EMC+DEC) (2:1:2).
Test embodiment 4 as described herein, test result is similar to the test result of embodiment 1: the lithium ion batteries anodes specific capacity using the electrolyte containing nickel salt additive to manufacture improves more than 5%; The high rate performance of iron phosphate lithium positive pole have also been obtained and significantly improves; Be significantly improved with the lithium ion battery life-span using electrolyte of the present invention to prepare.
In sum, the lithium ion battery adopting the electrolyte of nickel salt additive to prepare has higher capacity and longer cycle life, has good meaning to development long-life power and energy storage lithium ion battery.

Claims (9)

1. a salt additives for lithium-ion battery electrolytes, is characterized in that, this salt additives comprises nickel metal cation.
2. the salt additives of lithium-ion battery electrolytes according to claim 1, is characterized in that, in described lithium-ion battery electrolytes, solvent is carbonic ester; Electrolyte is selected from LiPF 6, LiBF 4, LiClO 4, one or more in LiTFSI, LiBOB and LiDOFB.
3. the salt additives of lithium-ion battery electrolytes according to claim 1, is characterized in that, described lithium-ion battery electrolytes is battery electrolyte that is liquid or gel state.
4. the salt additives of lithium-ion battery electrolytes according to claim 2, is characterized in that, described electrolytical concentration is 0.8 ~ 2.0M.
5. the salt additives of lithium-ion battery electrolytes according to claim 1, is characterized in that, this salt additives comprises and is selected from Cl -, NO 3 -, C 2o 4 2-, one or more anion in acetate and sulfonate radical.
6. the salt additives of lithium-ion battery electrolytes according to claim 1, it is characterized in that, in described lithium-ion battery electrolytes, the content of described salt additives is between 50 to 10000ppm.
7. comprise a lithium ion battery for lithium-ion battery electrolytes, wherein, described lithium-ion battery electrolytes comprises the salt additives described in any one of claim 1-6.
8. salt additives described in any one of claim 1-6 is improving the purposes in the electrode specific energy of lithium ion battery, specific power and cyclical stability.
9. a preparation method for the lithium-ion battery electrolytes of nickeliferous salt additives, said method comprising the steps of:
(1) nickel salt is fully dry under vacuum;
(2) obtain anhydrous nickel salt after cooling, enclosed package is for subsequent use;
(3) under argon shield, anhydrous nickel salt is added in lithium-ion battery electrolytes as electrolyte, stirs;
(4) described lithium-ion battery electrolytes encapsulates preservation under argon shield, obtains the lithium-ion battery electrolytes of nickeliferous salt additives.
CN201410427343.6A 2014-08-27 2014-08-27 A salt additive for an electrolyte of a lithium ion battery Pending CN105449272A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106450460A (en) * 2016-12-09 2017-02-22 中国科学院物理研究所 Lithium ion battery electrolyte additive, electrolyte thereof, preparation method and battery
JP7258205B1 (en) 2022-06-01 2023-04-14 住友精化株式会社 Electrodes for lithium ion batteries and lithium ion batteries
WO2023236031A1 (en) * 2022-06-07 2023-12-14 宁德时代新能源科技股份有限公司 Non-aqueous electrolyte and preparation method therefor, secondary battery comprising same, and electric device

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106450460A (en) * 2016-12-09 2017-02-22 中国科学院物理研究所 Lithium ion battery electrolyte additive, electrolyte thereof, preparation method and battery
JP7258205B1 (en) 2022-06-01 2023-04-14 住友精化株式会社 Electrodes for lithium ion batteries and lithium ion batteries
WO2023234016A1 (en) * 2022-06-01 2023-12-07 住友精化株式会社 Electrode for lithium ion batteries, and lithium ion battery
JP2023176984A (en) * 2022-06-01 2023-12-13 住友精化株式会社 Electrode for lithium ion battery, and lithium ion battery
WO2023236031A1 (en) * 2022-06-07 2023-12-14 宁德时代新能源科技股份有限公司 Non-aqueous electrolyte and preparation method therefor, secondary battery comprising same, and electric device

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