CN109326780B - A kind of preparation method of tungsten disulfide negative electrode material-coated sulfur composite material - Google Patents
A kind of preparation method of tungsten disulfide negative electrode material-coated sulfur composite material Download PDFInfo
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- CN109326780B CN109326780B CN201811085617.2A CN201811085617A CN109326780B CN 109326780 B CN109326780 B CN 109326780B CN 201811085617 A CN201811085617 A CN 201811085617A CN 109326780 B CN109326780 B CN 109326780B
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 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
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 30
- 239000011593 sulfur Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 5
- 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
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 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 5
- 238000001035 drying Methods 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 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
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-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
- 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
- 239000010406 cathode material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000002156 mixing Methods 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
- 238000004321 preservation Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
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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
- 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
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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
- H01M4/38—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
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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
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
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Abstract
本发明涉及一种二硫化钨负极材料包覆硫复合材料制备方法，属于锂离子电池技术领域。将硫粉与四硫代钨酸铵按照质量比为1:1.5~1:4加入到去离子水中，超声搅拌至硫粉在溶液中分散均匀，然后加入盐酸溶液调节pH值至1~3，反应4~6h，产生沉淀，经过滤、洗涤、干燥得到沉淀物；将得到沉淀物在保护气氛下，在温度为200~300℃保温1~4h，自然冷却后得到二硫化钨负极材料包覆硫复合材料。本方法工艺简单、环境污染小，得到的产物粒度均匀且电化学性能优异，可以达到目前市场所需求的标准。The invention relates to a preparation method of a tungsten disulfide negative electrode material-coated sulfur composite material, and belongs to the technical field of lithium ion batteries. Add sulfur powder and ammonium tetrathiotungstate into deionized water according to the mass ratio of 1:1.5~1:4, stir ultrasonically until the sulfur powder is evenly dispersed in the solution, and then add hydrochloric acid solution to adjust the pH value to 1~3, The reaction is carried out for 4-6 hours to produce a precipitate, which is filtered, washed and dried to obtain a precipitate; the obtained precipitate is kept at a temperature of 200-300 °C for 1-4 hours under a protective atmosphere, and then naturally cooled to obtain a coating of tungsten disulfide negative electrode material. Sulfur composite. The method has the advantages of simple process and little environmental pollution, and the obtained product has uniform particle size and excellent electrochemical performance, and can meet the standards required by the current market.
Description
Technical Field
The invention relates to a preparation method of a tungsten disulfide negative electrode material coated sulfur composite material, and belongs to the technical field of lithium ion batteries.
Background
The tungsten disulfide is used as a material with a larger prospect, has a wide application field, can be used in aerospace, automobiles, carbon anti-friction materials and the like, and can also replace graphite to be used as a lithium ion battery cathode material. Although tungsten disulfide has a graphite-like lamellar structure, there are still many problems to be solved in order to completely replace graphite as a negative electrode of a lithium battery. On the one hand, the production of tungsten disulfide is mainly prepared by a vapor deposition method at present, the yield is low, and the highly toxic gas hydrogen sulfide pollutes the air. On the other hand, the actual specific capacity of the tungsten disulfide is influenced by a plurality of factors and can not meet the quality requirement of industrial production.
The invention adopts a precipitation method to prepare the tungsten disulfide negative electrode material coated sulfur composite material, not only solves the problem of environmental pollution, but also improves the actual specific capacity of the material by compounding with sulfur, so that the actual specific capacity of the material completely reaches the standard required by the current market.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides a preparation method of a tungsten disulfide negative electrode material coated sulfur composite material. The method has simple process and little environmental pollution, and the obtained product has uniform granularity and excellent electrochemical performance and can reach the standard required by the current market. The invention is realized by the following technical scheme.
A preparation method of a sulfur composite material coated by a tungsten disulfide negative electrode material comprises the following specific steps:
step 1, adding sulfur powder and ammonium tetrathiotungstate into deionized water according to the mass ratio of 1: 1.5-1: 4, ultrasonically stirring until the sulfur powder is uniformly dispersed in the solution, then adding a hydrochloric acid solution to adjust the pH value to 1-3, reacting for 4-6 h to generate a precipitate, and filtering, washing and drying to obtain the precipitate;
and 2, preserving the heat of the precipitate obtained in the step 1 at the temperature of 200-300 ℃ for 1-4 h in a protective atmosphere, and naturally cooling to obtain the tungsten disulfide negative electrode material coated sulfur composite material.
In the step 1, the particle size of the sulfur powder is 2-5 mu m.
The concentration of the ammonium tetrathiotungstate in the solution obtained in the step 1 is 0.2-0.6 mol/L.
The concentration of the hydrochloric acid solution in the step 1 is 4-8 mol/L.
The invention has the beneficial effects that:
(1) the tungsten disulfide negative electrode material coated sulfur composite material prepared by the invention has higher specific capacity, and can provide a reliable negative electrode material for the production of large-capacity lithium ion batteries.
(2) The preparation process is easy to control, the granularity of the material in the reaction process can be controlled by controlling the pH value and the annealing heat preservation time, the requirements of various products are met, and the pollution in the whole production process is small.
Drawings
FIG. 1 is an XRD pattern of a tungsten disulfide negative electrode material coated sulfur composite obtained in example 1 of the present invention;
FIG. 2 is a charge/discharge curve diagram of a lithium ion battery prepared from a sulfur composite coated with a tungsten disulfide negative electrode material obtained in example 1 of the present invention at a current density of 100 mA/g;
fig. 3 is a cycle curve diagram of a lithium ion battery prepared by coating a sulfur composite material with a tungsten disulfide negative electrode material obtained in example 1 of the present invention at different rates.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
The preparation method of the tungsten disulfide negative electrode material coated sulfur composite material comprises the following specific steps:
step 1, adding 1g of sulfur powder and 1.5g of ammonium tetrathiotungstate into deionized water according to the mass ratio of 1:1.5, ultrasonically stirring until the sulfur powder is uniformly dispersed in the solution, then adding a hydrochloric acid solution (the concentration of the hydrochloric acid solution is 4mol/L) to adjust the pH value to 1.5, reacting for 5 hours to generate a precipitate, and filtering, washing and drying to obtain the precipitate; wherein the particle size of the sulfur powder is 2-5 mu m, and the concentration of the ammonium tetrathiotungstate is 0.2 mol/L;
and 2, keeping the precipitate obtained in the step 1 at the temperature of 280 ℃ for 2h under a protective atmosphere (nitrogen, the flow is 2L/min), naturally cooling to obtain the tungsten disulfide negative electrode material coated sulfur composite material, wherein the XRD (X-ray diffraction) diagram of the obtained tungsten disulfide negative electrode material coated sulfur composite material is shown in figure 1, and the main crystal phase of the outer layer coating material can be seen as tungsten disulfide in figure 1.
The tungsten disulfide negative electrode material prepared in this example was coated with a sulfur composite material to perform electrochemical performance testing: mixing and grinding the composite material powder, acetylene black and polyvinylidene fluoride (PVDF) according to the mass ratio of 8:1:1 to assemble the CR2025 button cell; and (3) testing the charge and discharge performance after standing for 24 hours, wherein the specific process is as follows:
weighing the obtained tungsten disulfide negative electrode material coated sulfur composite material powder, acetylene black and polyvinylidene fluoride (PVDF) according to the mass ratio of 8:1:1, placing the materials in an agate mortar, and dropwise adding a proper amount of N-methyl-2-pyrrolidone (NMP) for uniform grinding; coating the copper foil on a Cu foil with the thickness of 0.15mm, drying the copper foil in a vacuum drying oven at 90 ℃ for 24h, and taking out the pole piece to serve as a negative electrode.
② metal lithium sheets are used as negative electrode and reference electrode, polypropylene microporous membrane is used as diaphragm, 1mol/L LiPF6The + EC/DMC/EMC is electrolyte, and is assembled into a CR2025 stainless steel button cell in a glove box filled with argon and with the moisture content lower than 2 ppm; and testing the charge and discharge performance after standing for 24 hours.
The charge-discharge curve of the lithium ion battery prepared by the tungsten disulfide negative electrode material coated sulfur composite material prepared in the embodiment under the current density of 100mA/g is shown in fig. 2, and it can be seen from fig. 2 that the first specific discharge capacity is 1078.5mA hg-1The capacity can still be 996.4mA hg after 50 cycles-1The capacity retention rate reaches 92.4%. The cycle curve of the lithium ion battery prepared by the tungsten disulfide negative electrode material coated sulfur composite material obtained in the embodiment under different multiplying factors is shown in fig. 3, and it can be seen from fig. 3 that the multiplying factor performance of the material is excellent, and the cycle is still stable when the multiplying factor is increased.
Example 2
The preparation method of the tungsten disulfide negative electrode material coated sulfur composite material comprises the following specific steps:
step 1, adding 1g of sulfur powder and 4g of ammonium tetrathiotungstate into deionized water according to the mass ratio of 1:4, ultrasonically stirring until the sulfur powder is uniformly dispersed in the solution, then adding a hydrochloric acid solution (the concentration of the hydrochloric acid solution is 8mol/L) to adjust the pH value to 1, reacting for 4 hours to generate a precipitate, and filtering, washing and drying to obtain the precipitate; wherein the particle size of the sulfur powder is 2-5 mu m, and the concentration of the ammonium tetrathiotungstate is 0.6 mol/L;
and 2, keeping the precipitate obtained in the step 1 at the temperature of 200 ℃ for 4h under a protective atmosphere (nitrogen, with the flow rate of 2L/min), and naturally cooling to obtain the tungsten disulfide negative electrode material coated sulfur composite material.
Example 3
The preparation method of the tungsten disulfide negative electrode material coated sulfur composite material comprises the following specific steps:
step 1, adding 1g of sulfur powder and 2.5g of ammonium tetrathiotungstate into deionized water according to the mass ratio of 1:2.5, ultrasonically stirring until the sulfur powder is uniformly dispersed in the solution, then adding a hydrochloric acid solution (the concentration of the hydrochloric acid solution is 6mol/L) to adjust the pH value to 3, reacting for 6 hours to generate a precipitate, and filtering, washing and drying to obtain the precipitate; wherein the particle size of the sulfur powder is 2-5 mu m, and the concentration of the ammonium tetrathiotungstate is 0.4 mol/L;
and 2, keeping the precipitate obtained in the step 1 at the temperature of 300 ℃ for 1h under a protective atmosphere (nitrogen, with the flow rate of 2L/min), and naturally cooling to obtain the tungsten disulfide negative electrode material coated sulfur composite material.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (4)
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