CN109326780A - A kind of tungsten disulfide negative electrode material cladding sulphur composite material and preparation method thereof - Google Patents
A kind of tungsten disulfide negative electrode material cladding sulphur composite material and preparation method thereof Download PDFInfo
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- CN109326780A CN109326780A CN201811085617.2A CN201811085617A CN109326780A CN 109326780 A CN109326780 A CN 109326780A CN 201811085617 A CN201811085617 A CN 201811085617A CN 109326780 A CN109326780 A CN 109326780A
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- negative electrode
- tungsten disulfide
- composite material
- electrode material
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000005864 Sulphur Substances 0.000 title claims abstract description 47
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 30
- 238000005253 cladding Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000013049 sediment Substances 0.000 claims abstract description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 230000001376 precipitating effect Effects 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 8
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 238000013019 agitation Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000003831 antifriction material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- 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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 present invention relates to a kind of tungsten disulfide negative electrode materials to coat sulphur composite material and preparation method thereof, belongs to technical field of lithium ion.Sulphur powder is add to deionized water with tetrathio ammonium tungstate according to mass ratio for 1:1.5 ~ 1:4, ultrasonic agitation is uniformly dispersed in the solution to sulphur powder, and hydrochloric acid solution is then added and adjusts pH value to 1 ~ 3, reacts 4 ~ 6h, precipitating is generated, is filtered, washed, is dried to obtain sediment;Sediment will be obtained under protective atmosphere, be 200 ~ 300 DEG C of 1 ~ 4h of heat preservation in temperature, tungsten disulfide negative electrode material cladding sulphur composite material is obtained after natural cooling.This method simple process, environmental pollution are small, obtained product particle size uniformly and electrochemical performance, can achieve the required standard of existing market.
Description
Technical field
The present invention relates to a kind of tungsten disulfide negative electrode materials to coat sulphur composite material and preparation method thereof, belongs to lithium ion battery skill
Art field.
Background technique
For tungsten disulfide as a kind of material with larger prospect, application field is very wide, in addition to being used in space flight and aviation, vapour
Vehicle and carbon antifriction material etc. are outer, graphite can also be replaced as lithium ion battery negative material.Although tungsten disulfide has class
Graphite it is laminar structured, but graphite to be replaced still to need to solve there are many problem as cathode of lithium battery completely.On the one hand,
The production of tungsten disulfide is mainly prepared at present with vapour deposition process, and yield is lower and extremely toxic gas cure hydrogen contamination air.
On the other hand, the actual specific capacity of tungsten disulfide is influenced the quality requirement that industrialization production is not achieved by factors.
The present invention prepares tungsten disulfide negative electrode material cladding sulphur composite material using the precipitation method, not only solves environment dirt
Dye problem also by with the compound actual specific capacity for improving material of sulphur, so that the actual specific capacity of material is fully meet current city
The standard that place needs.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of tungsten disulfide negative electrode material cladding sulphur
Composite material and preparation method thereof.This method simple process, environmental pollution are small, and obtained product particle size is uniform and chemical property is excellent
It is different, it can achieve the required standard of existing market.The invention is realized by the following technical scheme.
A kind of tungsten disulfide negative electrode material cladding sulphur composite material and preparation method thereof, the specific steps of which are as follows:
Sulphur powder and tetrathio ammonium tungstate are add to deionized water according to mass ratio for 1:1.5 ~ 1:4 by step 1, are stirred by ultrasonic
It is uniformly dispersed in the solution to sulphur powder, hydrochloric acid solution is then added and adjusts pH value to 1 ~ 3, reacts 4 ~ 6h, generates precipitating, pass through
It filters, wash, be dried to obtain sediment;
Step 1 is obtained sediment under protective atmosphere by step 2, is 200 ~ 300 DEG C of 1 ~ 4h of heat preservation in temperature, after natural cooling
Obtain tungsten disulfide negative electrode material cladding sulphur composite material.
The step 1 sulphur powder particle size is 2 ~ 5 μm.
The concentration of tetrathio ammonium tungstate is 0.2 ~ 0.6mol/L in step 1 solution.
Concentration of hydrochloric acid solution is 4 ~ 8mol/L in the step 1.
The beneficial effects of the present invention are:
(1) the tungsten disulfide negative electrode material cladding sulphur composite material specific capacity that the present invention is prepared is higher, can be large capacity
Lithium ion battery production a kind of reliable negative electrode material is provided.
(2) preparation process of the invention is relatively easy to control, and the granularity of material can be by controlling pH value during the reaction
With annealing soaking time control, meet various products demand, and entire production process less pollution.
Detailed description of the invention
Fig. 1 is the tungsten disulfide negative electrode material cladding sulphur composite material XRD diagram that present example 1 obtains;
Fig. 2 is the lithium ion battery for the tungsten disulfide negative electrode material cladding sulphur composite material preparation that invention example 1 of the present invention obtains
Charging and discharging curve figure under 100mA/g current density;
Fig. 3 is the lithium ion battery for the tungsten disulfide negative electrode material cladding sulphur composite material preparation that invention example 1 of the present invention obtains
Cyclic curve figure under different multiplying.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The tungsten disulfide negative electrode material coats sulphur composite material and preparation method thereof, the specific steps of which are as follows:
1g sulphur powder and 1.5g tetrathio ammonium tungstate are add to deionized water according to mass ratio for 1:1.5 by step 1, and ultrasound is stirred
It mixes to sulphur powder and is uniformly dispersed in the solution, then addition hydrochloric acid solution (concentration of hydrochloric acid solution 4mol/L) adjusting pH value to 1.5,
5h is reacted, precipitating is generated, is filtered, washed, is dried to obtain sediment;Wherein sulphur powder particle size is 2 ~ 5 μm, tetrathio wolframic acid
The concentration of ammonium is 0.2mol/L;
Step 1 is obtained sediment (nitrogen, flow 2L/min) under protective atmosphere by step 2, is 280 DEG C of heat preservations in temperature
2h obtains tungsten disulfide negative electrode material cladding sulphur composite material after natural cooling, obtained tungsten disulfide negative electrode material cladding sulphur
Composite material XRD diagram is as shown in Figure 1, as can be seen from Figure 1 external sheath material principal crystalline phase is tungsten disulfide.
The tungsten disulfide negative electrode material cladding sulphur composite material that the present embodiment is prepared carries out electrochemical property test:
Composite powder, acetylene black, Kynoar (PVDF) are assembled into mass ratio for the ratio mixed grinding of 8:1:1
CR2025 button cell;Standing tests its charge-discharge performance, detailed process afterwards for 24 hours are as follows:
1. obtained tungsten disulfide negative electrode material is coated sulphur composite powder and acetylene black, Kynoar (PVDF) by matter
Amount is weighed than the ratio for 8:1:1 and is placed in agate mortar, and it is uniform that appropriate n-methyl-2-pyrrolidone (NMP) grinding is added dropwise;
It is coated on Cu foil, coated in, with a thickness of 0.15mm, then 90 DEG C of dryings are placed in a vacuum drying oven for 24 hours on Cu foil, so
Pole piece is taken out afterwards, as cathode.
2. metal lithium sheet, as cathode and reference electrode, microporous polypropylene membrane is diaphragm, with 1mol/LiPF6 +EC/DMC/
EMC is electrolyte, in full of the glove box of argon gas, moisture content lower than 2ppm, is assembled into CR2025 stainless steel button cell;
Standing tests its charge-discharge performance afterwards for 24 hours.
The lithium ion battery for the tungsten disulfide negative electrode material cladding sulphur composite material preparation that the present embodiment is prepared exists
Charging and discharging curve under 100mA/g current density is as shown in Fig. 2, as can be seen from Figure 2 first discharge specific capacity is
1078.5mA hg-1, 50 times circulation after capacity still can be with 996.4mA hg-1Capacity retention ratio reaches 92.4%.The present embodiment obtains
The cladding sulphur composite material preparation of tungsten disulfide negative electrode material cyclic curve figure such as Fig. 3 under different multiplying of lithium ion battery
Shown, the high rate performance of material is also more excellent as can be seen from Figure 3, when multiplying power becomes larger, recycles still sufficiently stable.
Embodiment 2
The tungsten disulfide negative electrode material coats sulphur composite material and preparation method thereof, the specific steps of which are as follows:
1g sulphur powder and 4g tetrathio ammonium tungstate are add to deionized water according to mass ratio for 1:4 by step 1, and ultrasonic agitation is extremely
Sulphur powder is uniformly dispersed in the solution, and hydrochloric acid solution (concentration of hydrochloric acid solution 8mol/L) is then added and adjusts pH value to 1, reacts
4h generates precipitating, is filtered, washed, is dried to obtain sediment;Wherein sulphur powder particle size is 2 ~ 5 μm, tetrathio ammonium tungstate
Concentration is 0.6mol/L;
Step 1 is obtained sediment (nitrogen, flow 2L/min) under protective atmosphere by step 2, is 200 DEG C of heat preservations in temperature
4h obtains tungsten disulfide negative electrode material cladding sulphur composite material after natural cooling.
Embodiment 3
The tungsten disulfide negative electrode material coats sulphur composite material and preparation method thereof, the specific steps of which are as follows:
1g sulphur powder and 2.5g tetrathio ammonium tungstate are add to deionized water according to mass ratio for 1:2.5 by step 1, and ultrasound is stirred
It mixes to sulphur powder and is uniformly dispersed in the solution, then addition hydrochloric acid solution (concentration of hydrochloric acid solution 6mol/L) adjusting pH value to 3, instead
6h is answered, precipitating is generated, is filtered, washed, is dried to obtain sediment;Wherein sulphur powder particle size is 2 ~ 5 μm, tetrathio ammonium tungstate
Concentration be 0.4mol/L;
Step 1 is obtained sediment (nitrogen, flow 2L/min) under protective atmosphere by step 2, is 300 DEG C of heat preservations in temperature
1h obtains tungsten disulfide negative electrode material cladding sulphur composite material after natural cooling.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (4)
1. a kind of tungsten disulfide negative electrode material coats sulphur composite material and preparation method thereof, it is characterised in that specific step is as follows:
Sulphur powder and tetrathio ammonium tungstate are add to deionized water according to mass ratio for 1:1.5 ~ 1:4 by step 1, are stirred by ultrasonic
It is uniformly dispersed in the solution to sulphur powder, hydrochloric acid solution is then added and adjusts pH value to 1 ~ 3, reacts 4 ~ 6h, generates precipitating, pass through
It filters, wash, be dried to obtain sediment;
Step 1 is obtained sediment under protective atmosphere by step 2, is 200 ~ 300 DEG C of 1 ~ 4h of heat preservation in temperature, after natural cooling
Obtain tungsten disulfide negative electrode material cladding sulphur composite material.
2. tungsten disulfide negative electrode material according to claim 1 coats sulphur composite material and preparation method thereof, it is characterised in that: institute
Stating step 1 sulphur powder particle size is 2 ~ 5 μm.
3. tungsten disulfide negative electrode material according to claim 1 coats sulphur composite material and preparation method thereof, it is characterised in that: institute
The concentration for stating tetrathio ammonium tungstate in step 1 solution is 0.2 ~ 0.6mol/L.
4. tungsten disulfide negative electrode material according to claim 1 coats sulphur composite material and preparation method thereof, it is characterised in that: institute
Stating concentration of hydrochloric acid solution in step 1 is 4 ~ 8mol/L.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114628673A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Three-dimensional macroporous tungsten disulfide/carbon composite material and preparation method and application thereof |
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CN114628673A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Three-dimensional macroporous tungsten disulfide/carbon composite material and preparation method and application thereof |
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