CN107039652A - A kind of preparation method of high security trielement composite material - Google Patents

A kind of preparation method of high security trielement composite material Download PDF

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Publication number
CN107039652A
CN107039652A CN201710181782.7A CN201710181782A CN107039652A CN 107039652 A CN107039652 A CN 107039652A CN 201710181782 A CN201710181782 A CN 201710181782A CN 107039652 A CN107039652 A CN 107039652A
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lithium
security
trielement composite
composite
compound
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丁建民
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JIANGSU LENENG BATTERY CO Ltd
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JIANGSU LENENG BATTERY CO Ltd
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention belongs to field of lithium ion battery material preparation, specifically a kind of preparation method of high security trielement composite material, its preparation process is:Porous metals lithiated compound and lithium compound are mixed to form solution first, ternary material is added, and is uniformly dispersed at a high speed, mixed slurry is obtained, afterwards by sintering, carbonization and its electrochemistry lithium up process prepare trielement composite material.It prepares composite using lithium ion and porous metals lithiated compound anion binding, in battery charge and discharge process, the lithium ion of porous metals lithiated compound can be exchanged constantly with lithium ion in electrolyte, both the security of ternary material had been maintained, the transmission rate of lithium ion is improved again;Improve its security performance and high rate performance using the characteristics of lithium ion conducting rate is high in lithium compound and being coated on ternary material surface and reducing the probability of happening of its side reaction again simultaneously.

Description

A kind of preparation method of high security trielement composite material
Technical field
The invention belongs to field of lithium ion battery material preparation, specifically a kind of high security trielement composite material and Its preparation method.
Background technology
Ternary material with its energy density it is high the advantages of and be widely used in lithium ion battery, and applied to pure electronic vapour The fields such as car, energy storage.But, the cyclical stability and heat endurance of nickel-cobalt-manganese ternary material are all poor, and it is wide that this governs it General application.Traditional improvement electrochemical stability of ternary material used in lithium ion battery and the method for heat endurance are exactly surface Modified, such as surface clad oxide, fluoride, metal phosphate etc., these clads can improve active material Interface stability between electrolyte, prevents the generation of hydrogen fluoride in charge and discharge process.But these clads are all insulation Coating, it has relatively low ion and electron conduction, adds surface impedance so that circulation volume decreases.Material list Bread covers lithium compound, can improve the three-dimensional channel of lithium ion diffusion, secondly, when with ion doping, its ionic conductivity Also it can increase.Therefore, organo-lithium compound or inorganic lithium compound lithium doping nickle cobalt lithium manganate, can improve nickel-cobalt lithium manganate material Rate capability and cyclical stability.
In the patent document for being CN105789615 A such as China Patent Publication No., a kind of modified nickle cobalt lithium manganate positive pole is disclosed Material and preparation method thereof.The invention has synthesized metatitanic acid lithium nano material using sol-gal process first, afterwards using dry method Cladding process is evenly coated on nickel-cobalt-manganese ternary material so that nickel-cobalt-manganese ternary material have good high rate performance and compared with High cyclicity, but the quantity of its lithium ion and its passage are less, cause its high rate performance general and its security performance not Improved, while the imbibition ability deviation of its clad, influences its cycle performance.Therefore develop a kind of high rate performance it is good, Cycle performance is high and its high ternary material composite of security performance seems very necessary, and applied to high-energy-density density lithium Ion battery.
The content of the invention
For current ternary material security performance is good, high rate performance it is poor in terms of presence deficiency, the invention provides A kind of security performance is high, the preparation method for the trielement composite material that cycle performance is good and its high rate performance is high, and applied to lithium from Sub- battery.
The technical scheme is that be accomplished by the following way:A kind of preparation side of high security trielement composite material Core shell structure is presented in method, the trielement composite material, and kernel is ternary material, and shell is that porous metals lithiated compound is closed with lithiumation Thing complex, it is 0.5~2 μm that it, which coats thickness,;By weight percentage, preparation method comprises the following steps:1)Mixed slurry Preparation:2)Sintering and its carbonization;3)Electrochemistry mends lithium;It is characterized in that:
1), mixed slurry preparation:10~20g binding agents are added in 500ml ionic liquid first, after being uniformly dispersed, Addition 10~30g porous metals lithiated compound, the inorganic lithium compounds of 10~3g, after stirring, then add 100g tri- successively First material, and by high speed dispersor, obtain being coated with the trielement composite material A of lithium compound;
2), sintering and its be carbonized:Trielement composite material A is transferred in tube furnace, in an inert atmosphere, using heating rate as 1 ~10 DEG C/min is warming up to 200~300 DEG C, and is incubated 1~3h, it is warming up to 600 by 1~10 DEG C/min of heating rate afterwards~ 900 DEG C, and 1~3h is incubated, Temperature fall obtains trielement composite material B to room temperature afterwards;
3), electrochemistry mend lithium:Organic lithium salt is added to the solvent that 0.1mol/L is configured in methyl ethyl carbonate, with composite B is as working electrode, and platinum electrode is as to electrode, and saturation calomel is answered as reference electrode, and using electrochemical deposition method at it Condensation material B surface deposits lithium salts, finally obtains the combination electrode C containing lithium salts, i.e. high security trielement composite material.
The step 1)Middle binding agent is one kind in Kynoar, polyvinyl alcohol, poly- methyl esters acrylate.
The step 1)Middle porous metals lithiated compound is Li3PMo12O40、Li3PW12O40、Li4SiW12O40、 Li4SiMo12O40In one kind.
The step 1)In inorganic lithium compound be:Li5La3Ta2O12、Li5La3Nb2O12、Li6BaLa2Ta2O12、 Li6MgLa2Ta2O12、LiAlO2、Li2ZrO3In one kind.
The step 1)Middle organic solvent is:Trimethyl two(Trimethyl fluoride sulfonyl)Imines, N- Methyl-N-propyl piperazines One kind in pyridine two (trimethyl fluoride sulfonyl) imines (PP13TFSI).
The step 1)Middle ternary material is LiNixCoyMn1-x-yO2(X >=0.3, y≤0.3),LiNixCoyAL1-x-yO2(x >=0.3, y≤0.3)In one kind.
The step 2)Middle organic lithium salt is one kind in difluorine oxalic acid boracic acid lithium, LiBF4.
The present invention, has a three dimensional skeletal structure in ternary material Surface coating porous metals lithium compound, lithium ion with it is many Mesoporous metal oxygen hydrochlorate anion binding, in battery charge and discharge process, the lithium ion of polyoxometallate can constantly and electrolyte Middle lithium ion is exchanged, and has both maintained the security of ternary material, and the transmission rate of lithium ion is improved again.While inorganic lithium Compound has the advantages that lithium ion conducting rate is high, high with compatibility of electrolyte, during high rate charge-discharge, raising lithium from The transmission rate of son, reduces its internal resistance, and therefore improve its security performance and its high rate performance;By electrochemical deposition method many Mesoporous metal lithium compound deposits organo-lithium compound, improves the content of its lithium ion and its compatibility with electrolyte, and play Synergy between the inorganic lithium compound of its internal layer, outer layer organo-lithium compound, improves its cycle performance and its security performance.
Brief description of the drawings
The SEM pictures for the trielement composite material that Fig. 1, embodiment 1 are prepared.
Embodiment
Core shell structure is presented in a kind of preparation method of high security trielement composite material, the trielement composite material, and kernel is Ternary material, shell is porous metals lithiated compound and lithium compound complex, and it is 0.5~2 μm that it, which coats thickness,.
Embodiment 1:
Know that a kind of preparation method of high security trielement composite material by weight percentage, comprises the following steps by Fig. 1:
1st, the preparation of mixed slurry:
15g Kynoar is added to 500ml trimethyls two first(Trimethyl fluoride sulfonyl)In imines ion liquid, point After dissipating uniformly, 20gLi is added successively3PMo12O40Porous metals lithiated compound, 20gLi5La3Ta2O12Inorganic lithium compound, is stirred After mixing uniformly, then add 100gLiNi0.3Co0.5Mn0.2O2Ternary material, and by high speed dispersor, obtain being coated with lithiumation conjunction The LiNi of thing0.3Co0.5Mn0.2O2Trielement composite material A;
2nd, sinter and its be carbonized:
Afterwards by LiNi0.3Co0.5Mn0.2O2Trielement composite material A is transferred in tube furnace, in an inert atmosphere, with heating rate 250 DEG C are warming up to for 5 DEG C/min, and is incubated 2h, 800 DEG C are warming up to by 5 DEG C/min of heating rate afterwards, and is incubated 2h, it Temperature fall obtains LiNi to room temperature afterwards0.3Co0.5Mn0.2O2Trielement composite material B;
3rd, electrochemistry mends lithium:
14.4g difluorine oxalic acid boracic acid lithiums are added to the solvent that 0.1mol/L is configured in 1000ml methyl ethyl carbonate, afterwards Using composite B as working electrode, platinum electrode is as to electrode, and saturation calomel uses cyclic voltammetric as reference electrode Method(Voltage range -2V-2V, sweep speed, 1mV/s is deposited 10 weeks)Lithium salts is deposited in its composite B surface, is finally obtained Combination electrode C containing lithium salts, i.e. high security trielement composite material.
Embodiment 2:
1st, the preparation of mixed slurry:
10g polyvinyl alcohol is added to 500ml N- Methyl-N-propyls piperidines two (trimethyl fluoride sulfonyl) imines first (PP13TFSI) in ionic liquid, after being uniformly dispersed, 10g Li are added successively3PW12O40Porous metals lithiated compound, 10gLi5La3Nb2O12Inorganic lithium compound, after stirring, then adds 100gLiNi0.3Co0.5Mn0.2O2Ternary material, and lead to High speed dispersor is crossed, obtains being coated with the LiNi of lithium compound0.3Co0.5Mn0.2O2Trielement composite material A;
2nd, sinter and its be carbonized:
Afterwards by LiNi0.3Co0.5Mn0.2O2Trielement composite material A is transferred in tube furnace, in an inert atmosphere, with heating rate 200 DEG C are warming up to for 1.0 DEG C/min, and is incubated 3h, 600 DEG C are warming up to by 1.0 DEG C/min of heating rate afterwards, and be incubated 3h, afterwards Temperature fall obtain trielement composite material B to room temperature;
3rd, electrochemistry mends lithium:
9.4g LiBF4s are added into the solvent that 1000ml is configured to 0.1mol/L into methyl ethyl carbonate, afterwards with composite wood B is expected as working electrode, and platinum electrode is as to electrode, and saturation calomel uses constant-voltage method as reference electrode(Voltage 1.5V, Time 30min)Lithium salts is deposited in its composite B surface, the combination electrode C containing lithium salts is finally obtained.
Embodiment 3:
1st, the preparation of mixed slurry:
The poly- methyl esters acrylate adhesives of 20g are added to 500ml trimethyl two first(Trimethyl fluoride sulfonyl)Imines In ionic liquid, after being uniformly dispersed, 30g Li are added successively4SiW12O40Porous metals lithiated compound, 30gLiAlO2, stirring After uniform, then add 100gLiNi0.3Co0.5Mn0.2O2Ternary material, and by high speed dispersor, obtain being coated with lithium compound LiNi0.3Co0.5Mn0.2O2Trielement composite material A;
2nd, sinter and its be carbonized:
Afterwards by LiNi0.3Co0.5Mn0.2O2Trielement composite material A is transferred in tube furnace, in an inert atmosphere, with heating rate 300 DEG C are warming up to for 10 DEG C/min, and is incubated 1h, 900 DEG C are warming up to by 10 DEG C/min of heating rate afterwards, and is incubated 1h, Temperature fall obtains LiNi to room temperature afterwards0.3Co0.5Mn0.2O2Trielement composite material B;
3rd, electrochemistry mends lithium:
14.4g difluorine oxalic acid boracic acid lithiums are added to the solvent that 0.1mol/L is configured in 1000ml methyl ethyl carbonate, afterwards Using composite B as working electrode, platinum electrode is as to electrode, and saturation calomel uses constant flow method as reference electrode (20mA/cm2, time 10min)Lithium salts is deposited in its composite B surface, the combination electrode C containing lithium salts is finally obtained.
Comparative example:
With the LiNi in embodiment0.3Co0.5Mn0.2O2Ternary material is as a comparison case;Material producer:Xinxiang Cologne new energy section Skill Co., Ltd, model:KL203L.
Surface sweeping Electronic Speculum is tested:
As seen from Figure 1, graininess is presented in the ternary material that embodiment 1 is prepared, and interparticle contact is close, and hole is small, divide Rationally, the material of its surface deposition is lithium salt compound to cloth.
Soft Roll is tested:
Respectively with embodiment 1, embodiment 2, the ternary material that embodiment 3 and comparative example are prepared is as positive electrode, with artificial Graphite is negative material, using LiPF6/EC+DEC(Volume ratio 1: 1)For electrolyte, the films of Celgard 2400 are barrier film, are prepared Go out 5Ah soft-package battery A1, A2, A3 and B1, and test the high rate performance and security performance of its soft-package battery.
High rate performance:
Afterwards and test soft-package battery A1, A2, A3 and B1 high rate performance(Rate of charge is 0.3C, discharge-rate be 0.5C, 1.0C、2.0C、4.0C、8.0C), 2.7V~4.25V, 25 ± 3.0 DEG C.Test result is as shown in table 1 below.
Table 1, embodiment can be compared with the rate of comparative example
As can be seen from Table 1, embodiment is compared with comparative example, and comparative example is substantially better than in high rate performance, and its reason is, embodiment The lithium salts for having densification is deposited in composite using electrochemical process, so that the transmission speed of the lithium ion under the conditions of improving its big multiplying power Rate, and intermediate layer of material doping porous metals lithium compound have accommodate lithium ion ability, can accommodate more lithiums from Son, further improves the big high rate performance of lithium ion, so as to improve its high rate performance.
Security performance is tested:
Striking experiment:
Example 1-3 and each 10 of comparative example battery, it is fully charged after, by the hard rod traverse of a 16.0mm diameter in On battery, fallen down and pounded on hard rod from 610mm height with one 20 pounds of weight, observe cell condition.
The embodiment of table 2 is compared with the striking experiment of comparative example
Example Whether leakage Whether catch fire
Embodiment 1 It is no It is no
Embodiment 2 It is no It is no
Embodiment 3 It is no It is no
Comparative example It is It is
As can be seen from Table 2, embodiment prepares lithium ion battery in terms of striking experiment substantially due to comparative example, and its reason is The lithium ion of porous metals lithiated compound can be exchanged constantly with lithium ion in electrolyte, both maintain the peace of ternary material Quan Xing, therefore security performance of the lithium ion battery in terms of striking experiment be improved.

Claims (7)

1. core shell structure is presented in a kind of preparation method of high security trielement composite material, the trielement composite material, kernel is three First material, shell is porous metals lithiated compound and lithium compound complex, and it is 0.5~2 μm that it, which coats thickness,;With weight hundred Divide than meter, preparation method comprises the following steps:1)The preparation of mixed slurry:2)Sintering and its carbonization;3)Electrochemistry mends lithium;It is special Levy and be:
1), mixed slurry preparation:10~20g binding agents are added in 500ml ionic liquid first, after being uniformly dispersed, Addition 10~30g porous metals lithiated compound, the inorganic lithium compounds of 10~3g, after stirring, then add 100g tri- successively First material, and by high speed dispersor, obtain being coated with the trielement composite material A of lithium compound;
2), sintering and its be carbonized:Trielement composite material A is transferred in tube furnace, in an inert atmosphere, using heating rate as 1 ~10 DEG C/min is warming up to 200~300 DEG C, and is incubated 1~3h, it is warming up to 600 by 1~10 DEG C/min of heating rate afterwards~ 900 DEG C, and 1~3h is incubated, Temperature fall obtains trielement composite material B to room temperature afterwards;
3), electrochemistry mend lithium:Organic lithium salt is added to the solvent that 0.1mol/L is configured in methyl ethyl carbonate, with composite B is as working electrode, and platinum electrode is as to electrode, and saturation calomel is answered as reference electrode, and using electrochemical deposition method at it Condensation material B surface deposits lithium salts, finally obtains the combination electrode C containing lithium salts, as high security trielement composite material.
2. a kind of preparation method of high security trielement composite material according to claim 1, it is characterised in that:The step Rapid 1)Middle binding agent is one kind in Kynoar, polyvinyl alcohol, poly- methyl esters acrylate.
3. a kind of preparation method of high security trielement composite material according to claim 1, it is characterised in that:The step Rapid 1)Middle porous metals lithiated compound is Li3PMo12O40、Li3PW12O40、Li4SiW12O40、Li4SiMo12O40In one kind.
4. a kind of preparation method of high security trielement composite material according to claim 1, it is characterised in that:, it is described Step 1)In inorganic lithium compound be:Li5La3Ta2O12、Li5La3Nb2O12、Li6BaLa2Ta2O12、Li6MgLa2Ta2O12、 LiAlO2、Li2ZrO3In one kind.
5. a kind of preparation method of high security trielement composite material according to claim 1, it is characterised in that:The step Rapid 1)Middle organic solvent is:Trimethyl two(Trimethyl fluoride sulfonyl)The imines, (trifluoromethyl of N- Methyl-N-propyls piperidines two Sulphonyl) one kind in imines (PP13TFSI).
6. a kind of preparation method of high security trielement composite material according to claim 1, it is characterised in that:The step Rapid 1)Middle ternary material is LiNixCoyMn1-x-yO2(X >=0.3, y≤0.3),LiNixCoyAL1-x-yO2(X >=0.3, y≤0.3) In one kind.
7. a kind of preparation method of high security trielement composite material according to claim 1, it is characterised in that:The step Rapid 2)Middle organic lithium salt is one kind in difluorine oxalic acid boracic acid lithium, LiBF4.
CN201710181782.7A 2017-03-24 2017-03-24 A kind of preparation method of high security trielement composite material Pending CN107039652A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107785559A (en) * 2017-11-02 2018-03-09 徐军红 A kind of graphene lithium titanate composite material and preparation method thereof, mend lithium graphene lithium titanate thin film, lithium battery
CN108417773A (en) * 2018-02-05 2018-08-17 山东丰元化学股份有限公司 A kind of LiFePO4 combination electrode and its preparation method and application
CN112164803A (en) * 2020-11-03 2021-01-01 天目湖先进储能技术研究院有限公司 Three-dimensional dielectric polyacrylonitrile/nano silver-lithium composite material and preparation method thereof

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CN103700827A (en) * 2012-09-27 2014-04-02 清华大学 Lithium ion battery positive-electrode composite material and lithium ion battery
CN105932236A (en) * 2016-05-09 2016-09-07 河海大学 Coating and modifying method for electrode material of lithium ion battery
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107785559A (en) * 2017-11-02 2018-03-09 徐军红 A kind of graphene lithium titanate composite material and preparation method thereof, mend lithium graphene lithium titanate thin film, lithium battery
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CN108417773A (en) * 2018-02-05 2018-08-17 山东丰元化学股份有限公司 A kind of LiFePO4 combination electrode and its preparation method and application
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Application publication date: 20170811