CN104993170A - Preparation method of lithium sulfur secondary battery cathode material - Google Patents

Preparation method of lithium sulfur secondary battery cathode material Download PDF

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Publication number
CN104993170A
CN104993170A CN201510268449.0A CN201510268449A CN104993170A CN 104993170 A CN104993170 A CN 104993170A CN 201510268449 A CN201510268449 A CN 201510268449A CN 104993170 A CN104993170 A CN 104993170A
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Prior art keywords
preparation
solvent
precursor pulp
sulfur
adhesive
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CN201510268449.0A
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CN104993170B (en
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徐宁
靳佳
吴孟涛
杨晓亮
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Tianjin B&M Science and Technology Co Ltd
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Tianjin B&M Science and Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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

Abstract

The invention discloses a preparation method of a lithium sulfur secondary battery cathode material. The method includes the steps of: 1) in an inert atmosphere, adding elemental sulfur, a coating material and a solvent I into a ball mill together to conduct coarse grinding to obtain a precursor slurry I; 2) drying the precursor slurry I, then adding the dried precursor slurry I, a solvent II and an adhesive into a sand mill to perform fine grinding, thus obtaining a precursor slurry II; 3) drying the precursor slurry II with a spray dryer to obtain coated precursor powder; and 4) heating the coated precursor powder in the inert atmosphere till carbonization of the adhesive, thus obtaining the lithium sulfur secondary battery cathode material. The product prepared by the method has uniform particle size and two coating layers, can improve the electron conduction between particles, and also can inhibit the loss of sulfur active substances in a circulation process.

Description

The preparation method of lithium-sulfur rechargeable battery anode material
Technical field
The present invention relates to electrode material of secondary lithium ion battery preparation field, particularly relate to a kind of preparation method of lithium-sulfur rechargeable battery anode material.
Background technology
Spray drying technology originates from people to be attempted to control the pattern of particle and particle size distribution range, has now been widely used in the preparation field of pharmacy, catalysis, coating, transducer, photoelectric material and lithium rechargeable battery positive and negative pole material.In lithium rechargeable battery positive and negative pole material preparation field, spray drying technology has realized the preparation of industry size to LiFePO4 and lithium titanate; And laboratory scale preparation is realized to ternary material, LiMn2O4, high-nickel material, graphite cathode material and silicon based anode material etc., but not yet complete industrialization preparation.Patent CN103682280A provides a kind of method utilizing spray drying technology to prepare the sulphur positive electrode of lithium-sulfur cell, but the hybrid mode of conductive additive and sulfur granules and heat treatment method are not described in detail in patent, and the molecule of sulfur granules is hydrophobic grouping, dispersed very poor in water, the conductive additive obtained and the dispersing uniformity of sulfur compound poor.The most frequently used solvent of spraying dry is water, and sulphur is dispersed in water not goodly also counteracts that its application in the art.
Elemental sulfur or sublimed sulfur are due to its poorly conductive, the active material feature such as easy loss in charge and discharge cycles process, and normal and clad material is combined with each other as the positive electrode of lithium-sulfur rechargeable battery.The method of clad material and elemental sulfur compound has a variety of.Such as: patent CN103219493A utilizes organic solvent by after ultrasonic to sublimed sulfur and conductive oxide mixing, utilizes ball-milling method to obtain sulphur conductive oxide composite material; The method CS used 2extremely inflammable, use dangerous high.Patent CN102832379A utilizes organic solvent elemental sulfur, material with carbon element to be combined with each other, but its organic solvent used is carbon disulfide, toluene etc., and toxicity is comparatively large, and environmental pollution is more serious.Biomass active carbon powder and sulphur powder are obtained composite powder by mixed grinding method by patent CN104157852A, carbon dust and sulphur powder cannot be made to combine closely for the method and each powder distribution is uneven, in cyclic process, active material therefore still cannot be avoided seriously to run off.Patent CN103794768A simulate supercritical extracting equipment carry out carry sulphur, but due to porous carbon materials and sulphur be simple mixing, therefore material with carbon element carry a sulfur content should not reach industrialized requirement.Patent CN103840143A obtains elemental sulfur by chemical reaction, then with mesoporous TiO 2s/TiO is obtained through heat treated 2composite material, the wherein more difficult control of chemical reaction gained simple substance sulphur granule particle diameter.In sum, prior art still effectively can not solve elemental sulfur or sublimed sulfur poorly conductive, active material easy technical problem run off in charge and discharge cycles process.
Summary of the invention
In order to above-mentioned technical problem, the invention provides a kind of preparation method of lithium-sulfur rechargeable battery anode material, obtained product cut size is homogeneous and have two-layer coating layer, can improve electrical conductivity between particle, sulphur active material can be suppressed again to run off in cyclic process.
For this reason, technical scheme of the present invention is as follows:
A preparation method for lithium-sulfur rechargeable battery anode material, comprises the following steps:
1) in an inert atmosphere, elemental sulfur, clad material are added in ball mill together with solvent I and roughly grinds, obtain precursor pulp I;
2) add fine grinding in sand mill with solvent II together with adhesive after being dried by described precursor pulp I, obtain precursor pulp II;
3) utilized by described precursor pulp II spray dryer dry, obtain coated after presoma powder;
4) by described coated after presoma powder heat in an inert atmosphere, namely obtain described lithium-sulfur rechargeable battery anode material after to be bonded dose of carbonization.
Step 3) utilize spray dryer, it is spherical for can making to obtain product, and particle diameter is comparatively homogeneous, and namely domain size distribution is narrower.
Described solvent I and solvent II are non-polar solven, preferred acetone or ether.The addition of described solvent I is 40 ~ 80% of elemental sulfur, clad material and solvent I three gross mass.The addition of described solvent II is 40 ~ 80% of precursor pulp I, solvent II and adhesive three gross mass after drying.
Step 1) in elemental sulfur, clad material mass ratio be 1 ~ 5:1.
Step 2) described in adhesive have loose particle adherence character together, and belong to lipophile adhesive; Any one or both in preferred PVDF and PTFE with arbitrarily than mixture; The quality of adhesive be precursor pulp I after drying and solvent II quality and 1 ~ 3%.
Described clad material is electric conducting material, in preferred carbon black, porous activated carbon, regular porous template material with carbon element, single-layer graphene, graphene oxide, Single Walled Carbon Nanotube, multi-walled carbon nano-tubes and porous SnO 2 any one or arbitrarily several with arbitrarily than mixture.
Step 1) in the corase grind time be 2 ~ 5h; Step 2) in the bake out temperature of precursor pulp I be 80 ~ 100 DEG C, the fine grinding time is 3 ~ 10h.
Step 3) to utilize spray dryer to carry out dry air inlet temperature be 250 ~ 350 DEG C, outlet temperature is 50 ~ 90 DEG C, and air inlet is inert gas, preferred argon gas or nitrogen.Select dissimilar spray dryer can obtain the product of different-grain diameter size, the grain size that General Requirements obtains is less than 100 μm.As utilized the controlled spherical particle size range obtaining product of centrifugal atomizing disc-type atomiser at 20 ~ 100 μm, and select ultra-fine atomization spray nozzle can control the spherical particle size range of obtained product at 1 ~ 20 μm.
Step 4) in heating-up temperature be 300 ~ 800 DEG C.
Step 1) and step 4) described in inert atmosphere all refer to Ar or N 2.
The present invention has the following advantages:
1) by lithium-sulfur rechargeable battery anode material prepared by spray drying process, compared with simple polishing, ball-milling method, solvent-thermal method, heat treated method, hydro thermal method, can narrow diameter distribution be prepared and coated uniform spherical lithium-sulfur rechargeable battery anode material, improve electron mobility.
2) coating layer is two-layer: nexine is by DIC or oxide is coated improves electrical conductivity between particle; Outer coated by organic carbon, two-coat can suppress the loss of sulphur active material in cyclic process effectively, improves the electrochemistry cycle performance of battery.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A preparation method for lithium-sulfur rechargeable battery anode material, comprises the following steps:
1) in argon gas atmosphere, be that 2:1 adds in ball mill and roughly grinds 2 hours together with ether with weight ratio by elemental sulfur and porous activated carbon, obtain precursor pulp I, during corase grind, the addition of ether requires to make the solid content in slurry be 20wt.%;
2) described precursor pulp I is dried under 80 DEG C of conditions, then to add in sand mill fine grinding 5 hours together with ether, PVDF, obtain precursor pulp II; Wherein, during fine grinding the addition of ether require to make the solid content in slurry be the addition of 30wt.%, PVDF be the precursor pulp I and ether quality of drying and 3%;
3) the dry precursor pulp II of centrifugal atomizing pan spray drier is utilized; Condition is: pass into inert atmosphere Ar, and air inlet temperature is adjusted to 250 DEG C, and outlet temperature is 60 DEG C, obtains out that average grain diameter is 50 μm, the spherical and presoma powder of coated porous active carbon and organic PVDF carbon source;
4) by step 3) the presoma powder that finally obtains puts into the kiln that the closed container being full of Ar maybe can pass into inert gas, make the carbonization of organic PVDF carbon source finally form spherical coated sulphur composite positive pole at 700 DEG C, be described lithium-sulfur rechargeable battery anode material.
Embodiment 2
A preparation method for lithium-sulfur rechargeable battery anode material, comprises the following steps:
1) in argon gas atmosphere, be that 3:1 adds in ball mill and roughly grinds 3 hours together with acetone with weight ratio by elemental sulfur and Single Walled Carbon Nanotube, obtain precursor pulp I, during corase grind, the addition of acetone requires to make the solid content in slurry be 30wt.%;
2) described precursor pulp I is dried under 90 DEG C of conditions, then to add in sand mill fine grinding 7 hours together with acetone, PTFE, obtain precursor pulp II; Wherein, during fine grinding the addition of acetone require to make the solid content in slurry be the addition of 40wt.%, PTFE be the precursor pulp I and acetone quality of drying and 2%;
3) the dry precursor pulp II of centrifugal atomizing pan spray drier is utilized; Condition is: pass into inert atmosphere Ar, and air inlet temperature is adjusted to 300 DEG C, and outlet temperature is 70 DEG C, obtains out that average grain diameter is 30 μm, spherical and coated single-walled carbon nano tube and organic PTFE carbon source presoma powder;
4) by step 3) the presoma powder that finally obtains puts into the kiln that the closed container being full of Ar maybe can pass into inert gas, make the carbonization of organic PTFE carbon source finally form spherical coated sulphur composite positive pole at 600 DEG C, be described lithium-sulfur rechargeable battery anode material.
Embodiment 3
A preparation method for lithium-sulfur rechargeable battery anode material, comprises the following steps:
1) in nitrogen atmosphere, by elemental sulfur and porous SnO 2with weight ratio be 5:1 add together with acetone in ball mill roughly grind 5 hours, obtain precursor pulp I, during corase grind acetone addition require make the solid content in slurry be 50wt.%;
2) described precursor pulp I is dried under 90 DEG C of conditions, then to add in sand mill fine grinding 10 hours together with acetone, PVDF, obtain precursor pulp II; Wherein, during fine grinding the addition of acetone require to make the solid content in slurry be the addition of 60wt.%, PVDF be the precursor pulp I and acetone quality of drying and 1%;
3) the dry precursor pulp II of ultra-fine atomization spray nozzle formula spray dryer is utilized; Condition is: pass into inert atmosphere nitrogen, and air inlet temperature is adjusted to 330 DEG C, and outlet temperature is 90 DEG C, obtains that average grain diameter is 15 μm, spherical and coated porous SnO 2with the presoma powder of organic PVDF carbon source;
4) by step 3) the presoma powder that finally obtains puts into the kiln that the closed container being full of nitrogen maybe can pass into inert gas, make the carbonization of organic PVDF carbon source finally form spherical coated sulphur composite positive pole at 700 DEG C, be described lithium-sulfur rechargeable battery anode material.
With the battery that the positive electrode that the inventive method obtains is made, discharge and recharge cut-ff voltage is 1.5-3.0V.Each embodiment is obtained material be assembled into 2032 type lithium sulphur button cells and test, obtains data and see the following form:
Embodiment 0.1C is discharge capacity (mAh/g) first 50 weeks circulation conservation rates (%)
1 830 85
2 862 87
3 910 82
As can be seen from the table, with the battery that the positive electrode that the method for the invention provides obtains is made, discharge capacity is greater than 800mAh/g first, within 50 weeks, circulating battery still can reach the capability retention of more than 80%, shows sulphur active material in charge and discharge process because double-layer carbon clad structure is suppressed preferably.

Claims (10)

1. a preparation method for lithium-sulfur rechargeable battery anode material, is characterized in that comprising the following steps:
1) in an inert atmosphere, elemental sulfur, clad material are added in ball mill together with solvent I and roughly grinds, obtain precursor pulp I;
2) add fine grinding in sand mill with solvent II together with adhesive after being dried by described precursor pulp I, obtain precursor pulp II;
3) utilized by described precursor pulp II spray dryer dry, obtain coated after presoma powder;
4) by described coated after presoma powder heat in an inert atmosphere, namely obtain described lithium-sulfur rechargeable battery anode material after to be bonded dose of carbonization.
2. preparation method as claimed in claim 1, it is characterized in that: described solvent I and solvent II are non-polar solven, the addition of described solvent I is 40 ~ 80% of elemental sulfur, clad material and solvent I three gross mass; The addition of described solvent II is 40 ~ 80% of precursor pulp I, solvent II and adhesive three gross mass after drying.
3. preparation method as claimed in claim 1, is characterized in that: described clad material be in carbon black, porous activated carbon, regular porous template material with carbon element, single-layer graphene, graphene oxide, Single Walled Carbon Nanotube, multi-walled carbon nano-tubes and porous SnO 2 any one or arbitrarily several with arbitrarily than mixture.
4. preparation method as claimed in claim 1, is characterized in that: described adhesive be PVDF or PTFE or both with arbitrarily than mixture; The quality of described adhesive be precursor pulp I after drying and solvent II quality and 1 ~ 3%.
5. preparation method as claimed in claim 1, is characterized in that: step 1) in elemental sulfur, clad material mass ratio be 1 ~ 5:1.
6. preparation method as claimed in claim 1, it is characterized in that: described solvent I is acetone or ether, described solvent II is acetone or ether.
7. preparation method as claimed in claim 1, is characterized in that: step 1) in the corase grind time be 2 ~ 5h; Step 2) in the bake out temperature of precursor pulp I be 80 ~ 100 DEG C, the fine grinding time is 3 ~ 10h.
8. preparation method as claimed in claim 1, is characterized in that: step 3) to utilize spray dryer to carry out dry air inlet temperature be 250 ~ 350 DEG C, outlet temperature is 50 ~ 90 DEG C, and air inlet is inert gas.
9. preparation method as claimed in claim 1, is characterized in that: step 4) in heating-up temperature be 300 ~ 800 DEG C.
10. preparation method as claimed in claim 8, is characterized in that: described inert atmosphere or inert gas all refer to argon gas or nitrogen.
CN201510268449.0A 2015-05-25 2015-05-25 The preparation method of lithium-sulfur rechargeable battery anode material Active CN104993170B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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CN109546103A (en) * 2018-10-25 2019-03-29 北京化工大学 A kind of electrode material and its preparation method and application of binder as carbon precursor
CN110073458A (en) * 2016-12-12 2019-07-30 韩国地质资源研究院 The preparation method of accordion graphene complex, the complex thus prepared and the supercapacitor comprising complex

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CN104766957A (en) * 2014-01-02 2015-07-08 奇瑞汽车股份有限公司 Lithium sulfur battery cathode material, preparation method thereof, and lithium sulfur batteries

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN110073458A (en) * 2016-12-12 2019-07-30 韩国地质资源研究院 The preparation method of accordion graphene complex, the complex thus prepared and the supercapacitor comprising complex
CN110073458B (en) * 2016-12-12 2022-07-08 韩国地质资源研究院 Preparation method of corrugated graphene composite, composite prepared by preparation method and supercapacitor containing composite
CN109546103A (en) * 2018-10-25 2019-03-29 北京化工大学 A kind of electrode material and its preparation method and application of binder as carbon precursor

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