CN107611428A - A kind of battery molybdenum disulfide cathode size preparation method and products thereof and application - Google Patents

A kind of battery molybdenum disulfide cathode size preparation method and products thereof and application Download PDF

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Publication number
CN107611428A
CN107611428A CN201710646997.1A CN201710646997A CN107611428A CN 107611428 A CN107611428 A CN 107611428A CN 201710646997 A CN201710646997 A CN 201710646997A CN 107611428 A CN107611428 A CN 107611428A
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molybdenum disulfide
cathode size
slurry
preparation
nmp
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CN107611428B (en
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何丹农
段磊
王艳丽
吴晓燕
李敏
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • 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 present invention provides a kind of lithium battery molybdenum disulfide cathode size preparation method and products thereof and application, and solute includes 90 95% active material molybdenum disulfide, 2.5 5% conductive agents are the binding agent polyvinylidene fluoride of electrically conductive graphite sp and ks 6,2.5 5%(PVDF), account for the 25 30% of total stock quality;Solvent is N methyl pyrrolidones(NMP), the 70 75% of total stock quality is accounted for, sp and the mass ratioes of ks 6 are 1:1‑2:1;First PVDF is poured into the NMP of 2/3 mass and stirred, add sp, ks 6 and molybdenum disulfide, the slurry after stirring is subjected to micro-nanoization processing, obtains microcosmic well dispersed molybdenum disulfide cathode size.The present invention need not refilter, and both improved the service efficiency of active material, also whole preparation process is possessed continuity;This method is simple and reliable, good process repeatability, workable, and the battery cell uniformity of preparation is high.

Description

A kind of battery molybdenum disulfide cathode size preparation method and products thereof and application
Technical field
Preparation method the present invention relates to a kind of battery with molybdenum disulfide cathode size, more particularly to a kind of battery with two Molybdenum sulfide cathode size and its preparation method and application.
Background technology
Lithium ion battery compared with conventional batteries, has discharge voltage height, self discharge as a kind of mechanism of new electrochemical power sources The advantages that small, memory-less effect, and it is widely used in the fields such as information, electronics, traffic, national defense and military.Preferable lithium ion Cell negative electrode material should have high specific capacity and structure and the performances such as Volume Changes are small during embedding lithium, de- lithium.At present, silicon Base, germanium base, tin-based material are got most of the attention due to its higher theoretical capacity, but these materials can produce during removal lithium embedded Raw very big volumetric expansion, so as to influence the cycle performance of battery.2H-MoS2Layer structure be advantageous to lithium ion in electrode body Quickly spread in system, the volumetric expansion of material is small during removal lithium embedded, and molybdenum disulfide sufficiency of natural resources, as lithium electricity With higher specific capacity during the negative pole of pond, has very much development potentiality.The cathode sizes such as general molybdenum disulfide are after carrying out stirring slurry process It is that aggregate or the undispersed siccative in slurry are removed using filtering, had both caused the waste of active material, and also have impact on Continuity prepared by whole electrode slurry.
A kind of preparation method the invention provides battery with molybdenum disulfide cathode size, it is innovative by fine point of high speed Scattered mixer is incorporated into battery pulping process, and the micro-nanoization processing of microcosmic point has been carried out to slurry, obtained negative pole slurry Expect that composition is uniform, adhesive force is preferable, without carrying out filter progress again, has both improved the service efficiency of active material, also makes whole Electrode slurry preparation process possesses continuity.And method is simple and reliable, good process repeatability is workable, the battery of assembling Uniformity is good, has wide market prospects.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at:A kind of battery molybdenum disulfide cathode size is provided.
It is still another object of the present invention to provide the product that above-mentioned preparation method obtains.
A further object of the present invention is:The application of the said goods is provided.
The object of the invention is realized by following proposal:A kind of preparation method of lithium battery molybdenum disulfide cathode size, bag Include following step:
(1)Molybdenum disulfide cathode size dispensing:Weigh in mass ratio, solute including active material is molybdenum disulfide, conductive agent is Electrically conductive graphite sp and ks-6, binding agent are polyvinylidene fluoride(PVDF), as solute, account for the 25-30% of gross mass;Solvent is 1-METHYLPYRROLIDONE(NMP), account for the 70-75% of gross mass, the quality percentage of active material, conductive agent and binding agent in solute Than being respectively;90-95%, 2.5-5% and 2.5-5%, sp and ks-6 mass ratio is 1 in conductive agent:1-2:1;
(2)PVDF is poured into the NMP of 2/3 mass, be stirred at a slow speed by magnetic agitation to clear gum thing, whipping process In to container carry out encapsulation process, prevent NMP volatilization;
(3)Electrically conductive graphite sp, ks-6 and molybdenum disulfide are divided 3-4 times and added in above-mentioned jelly, examination stirring state batch adds Enter the NMP of remaining 1/3 mass, 2000-3000 r/min, mixing time is 3-5 hour, in last of whipping process Hour carries out vacuumize process, eliminates caused bubble in whipping process;
(4)Slurry after stirring is subjected to micro-nanoization processing, obtains microcosmic well dispersed molybdenum disulfide cathode size, through place Slurry viscosity after reason is good with the aluminium foil attachment used in subsequent coated in 1500-2500mPas, can carry out effective slurry Coating.
High speed fine dispersion mixing machine is incorporated into battery pulping process by the present invention, and microcosmic point has been carried out to slurry Micro-nanoization processing, obtained cathode size composition is uniform, and adhesive force is preferable, without carrying out filter progress again, both improves work The service efficiency of property material, also makes whole electrode slurry preparation process possess continuity.
Preferably, active material, conductive agent and binding agent account for the 27% of gross mass in slurry;Solvent NMP accounts for gross mass 73%。
Preferably, the percentage that active material, conductive agent and binding agent account for solute gross mass in slurry is respectively:93%、 3.5% and 3.5%, sp and ks-6 mass ratio is 2 in conductive agent:1.
On the basis of such scheme, step(3)Middle mixing speed is 2500 r/min, and mixing time is 4 hours.
On the basis of such scheme, step(4)Micro-nanoization processing mode be to be mixed using HPCF type high speed fine dispersions Conjunction machine carries out the microcosmic scattered of electrode slurry.
The present invention provides a kind of according to the lithium battery that above-mentioned preparation method obtains molybdenum disulfide cathode size product.
The present invention provide it is a kind of according to the said goods in application of the lithium battery as cathode size.
The present invention is advantageous in that, innovative that high speed fine dispersion mixing machine is incorporated into battery pulping process, right Slurry has carried out the micro-nanoization processing of microcosmic point, and obtained cathode size composition is uniform, and adhesive force is preferable, without carrying out again Filter progress, had both improved the service efficiency of active material, whole electrode slurry preparation process is possessed continuity.And method Simple and reliable, good process repeatability is workable, and the battery consistency of assembling is good, is adapted to industrialized production.This method need not Filter progress is carried out again, has both improved the service efficiency of active material, whole electrode slurry preparation process is possessed continuity; And this method is simple and reliable, good process repeatability is workable, and the battery cell uniformity of preparation is high, can be widely popularized.
Embodiment
The present invention is described in detail by following instantiation, but protection scope of the present invention is not only restricted to these Examples of implementation.
Embodiment 1
Weigh in mass ratio, active material(Molybdenum disulfide), conductive agent(Electrically conductive graphite sp and ks-6, and mass ratio is 1:1)With And binding agent(Polyvinylidene fluoride, i.e. PVDF), account for the 25% of gross mass;Solvent is 1-METHYLPYRROLIDONE(Also known as NMP), account for The 75% of gross mass.The mass ratio of active material, conductive agent and binding agent is respectively 90%, 5% and 5% in solute.PVDF is poured into In the NMP of 2/3 mass, it is stirred at a slow speed by magnetic agitation to clear gum thing, container is sealed in whipping process Processing, prevents NMP volatilization.Sp, ks-6 and molybdenum disulfide are divided 3-4 times and added in above-mentioned jelly, examination stirring state batch The secondary NMP for adding remaining 1/3 mass, mixing speed is 2000 r/min, and mixing time is 5 hours, in whipping process Last hour carries out vacuumize process, eliminates caused bubble in whipping process.Slurry after stirring is used into HPCF types High speed fine dispersion mixing machine carries out the microcosmic scattered of electrode slurry, obtains microcosmic well dispersed molybdenum disulfide cathode size. Slurry viscosity after processing is 1500mPas, good with the aluminium foil attachment used in subsequent coated, can carry out effective slurry Coating.
Embodiment 2
Weigh in mass ratio, active material(Molybdenum disulfide), conductive agent(Electrically conductive graphite sp and ks-6, and mass ratio is 1.5:1) And binding agent(Polyvinylidene fluoride, i.e. PVDF), account for the 27% of gross mass;Solvent is 1-METHYLPYRROLIDONE(Also known as NMP), Account for the 73% of gross mass.The mass ratio of active material, conductive agent and binding agent is respectively 93%, 3.5% and 3.5% in solute.Will PVDF is poured into the NMP of 2/3 mass, is stirred at a slow speed by magnetic agitation to clear gum thing, to container in whipping process Encapsulation process is carried out, prevents NMP volatilization.Sp, ks-6 and molybdenum disulfide are divided 3-4 times and added in above-mentioned jelly, examination is stirred The NMP that situation batch adds remaining 1/3 mass is mixed, mixing speed is 2500 r/min, and mixing time is 4 hours, is being stirred Last hour for mixing process carries out vacuumize process, eliminates caused bubble in whipping process.Slurry after stirring is adopted The microcosmic scattered of electrode slurry is carried out with HPCF type high speed fine dispersion mixing machines, microcosmic well dispersed molybdenum disulfide is obtained and bears Pole slurry.Slurry viscosity after processing is good with the aluminium foil attachment used in subsequent coated in 2000mPas, can carry out effectively Slurry coating.
Embodiment 3
Weigh in mass ratio, active material(Molybdenum disulfide), conductive agent(Electrically conductive graphite sp and ks-6, and mass ratio is 2:1)With And binding agent(Polyvinylidene fluoride, i.e. PVDF), account for the 30% of gross mass;Solvent is 1-METHYLPYRROLIDONE(Also known as NMP), account for The 70% of gross mass.The mass ratio of active material, conductive agent and binding agent is respectively 95%, 2.5% and 2.5% in solute.By PVDF Pour into the NMP of 2/3 mass, be stirred at a slow speed by magnetic agitation to clear gum thing, container is carried out in whipping process Encapsulation process, prevent NMP volatilization.Sp, ks-6 and molybdenum disulfide are divided 3-4 times and added in above-mentioned jelly, examination stirring feelings Condition batch adds the NMP of remaining 1/3 mass, and mixing speed is 3000 r/min, and mixing time is 3 hours, stirred Last hour of journey carries out vacuumize process, eliminates caused bubble in whipping process.Slurry after stirring is used HPCF type high speed fine dispersion mixings machine carries out the microcosmic scattered of electrode slurry, obtains microcosmic well dispersed molybdenum disulfide negative pole Slurry.Slurry viscosity after processing is good with the aluminium foil attachment used in subsequent coated in 2500mPas, can carry out effective Slurry coats.

Claims (7)

1. a kind of lithium battery preparation method of molybdenum disulfide cathode size, comprises the steps:
(1)Molybdenum disulfide cathode size dispensing:Weigh in mass ratio, solute including active material is molybdenum disulfide, conductive agent is Electrically conductive graphite sp and ks-6, binding agent are polyvinylidene fluoride(PVDF), as solute, account for the 25-30% of gross mass;Solvent is 1-METHYLPYRROLIDONE(NMP), account for the 70-75% of gross mass, the quality percentage of active material, conductive agent and binding agent in solute Than being respectively;90-95%, 2.5-5% and 2.5-5%, sp and ks-6 mass ratio is 1 in conductive agent:1-2:1;
(2)PVDF is poured into the NMP of 2/3 mass, be stirred at a slow speed by magnetic agitation to clear gum thing, whipping process In to container carry out encapsulation process, prevent NMP volatilization;
(3)Electrically conductive graphite sp, ks-6 and molybdenum disulfide are divided 3-4 times and added in above-mentioned jelly, examination stirring state batch adds Enter the NMP of remaining 1/3 mass, 2000-3000 r/min, mixing time is 3-5 hour, in last of whipping process Hour carries out vacuumize process, eliminates caused bubble in whipping process;
(4)Slurry after stirring is subjected to micro-nanoization processing, obtains microcosmic well dispersed molybdenum disulfide cathode size, through place Slurry viscosity after reason is good with the aluminium foil attachment used in subsequent coated in 1500-2500mPas, can carry out effective slurry Coating.
A kind of 2. preparation method of lithium battery molybdenum disulfide cathode size according to claim 1, it is characterised in that slurry Active material, conductive agent and binding agent account for the 27% of gross mass in material;Solvent NMP accounts for the 73% of gross mass.
3. a kind of preparation method of lithium battery molybdenum disulfide cathode size, its feature exist according to claim 1 or 2 In the percentage that active material, conductive agent and binding agent account for solute gross mass in slurry is respectively:93%th, 3.5% and 3.5%, lead Sp and ks-6 mass ratio is 2 in electric agent:1.
A kind of 4. preparation method of lithium battery molybdenum disulfide cathode size according to claim 1, it is characterised in that step Suddenly(3)Middle mixing speed is 2500 r/min, and mixing time is 4 hours.
A kind of 5. preparation method of lithium battery molybdenum disulfide cathode size according to claim 1, it is characterised in that step Suddenly(4)Micro-nanoization processing mode be that the microcosmic scattered of electrode slurry is carried out using HPCF type high speed fine dispersion mixings machine.
A kind of 6. lithium battery molybdenum disulfide cathode size product obtained according to any preparation methods of claim 1-5.
7. a kind of product according to claim 6 is in application of the lithium battery as cathode size.
CN201710646997.1A 2017-08-01 2017-08-01 Preparation method of molybdenum disulfide cathode slurry for battery, product and application thereof Active CN107611428B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103311503A (en) * 2013-05-17 2013-09-18 贵州航天电源科技有限公司 Dispersion method of lithium-ion battery paste
CN103545487A (en) * 2013-10-28 2014-01-29 深圳格林德能源有限公司 Preparation method of high-viscosity ultra-fine dispersion anode slurry of lithium ion battery
CN106252603A (en) * 2016-08-31 2016-12-21 中航锂电(洛阳)有限公司 A kind of preparation method of pulp of lithium ion battery
US20170077546A1 (en) * 2015-09-14 2017-03-16 Aruna Zhamu Alkali metal or Alkali-Ion batteries having high volumetric and gravimetric energy densities
CN106663779A (en) * 2014-08-07 2017-05-10 中央研究院 Method of preparation a battery electrode by spray coating, an electrode and a battery made by method thereof
CN106981647A (en) * 2017-05-31 2017-07-25 青岛海澄知识产权事务有限公司 A kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103311503A (en) * 2013-05-17 2013-09-18 贵州航天电源科技有限公司 Dispersion method of lithium-ion battery paste
CN103545487A (en) * 2013-10-28 2014-01-29 深圳格林德能源有限公司 Preparation method of high-viscosity ultra-fine dispersion anode slurry of lithium ion battery
CN106663779A (en) * 2014-08-07 2017-05-10 中央研究院 Method of preparation a battery electrode by spray coating, an electrode and a battery made by method thereof
US20170077546A1 (en) * 2015-09-14 2017-03-16 Aruna Zhamu Alkali metal or Alkali-Ion batteries having high volumetric and gravimetric energy densities
CN106252603A (en) * 2016-08-31 2016-12-21 中航锂电(洛阳)有限公司 A kind of preparation method of pulp of lithium ion battery
CN106981647A (en) * 2017-05-31 2017-07-25 青岛海澄知识产权事务有限公司 A kind of nitrogen-doped carbon nanosphere/molybdenum disulfide sodium-ion battery negative plate

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