CN114975963A - VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof - Google Patents
VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof Download PDFInfo
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- CN114975963A CN114975963A CN202210740412.3A CN202210740412A CN114975963A CN 114975963 A CN114975963 A CN 114975963A CN 202210740412 A CN202210740412 A CN 202210740412A CN 114975963 A CN114975963 A CN 114975963A
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000011734 sodium Substances 0.000 title claims abstract description 25
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 24
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 24
- 238000003860 storage Methods 0.000 title claims abstract description 23
- 230000001737 promoting effect Effects 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 18
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000006210 lotion Substances 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000002195 synergetic effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 3
- 239000007773 negative electrode material Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract description 2
- NGTSQWJVGHUNSS-UHFFFAOYSA-N bis(sulfanylidene)vanadium Chemical compound S=[V]=S NGTSQWJVGHUNSS-UHFFFAOYSA-N 0.000 description 37
- 229910052717 sulfur Inorganic materials 0.000 description 11
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 10
- 239000011593 sulfur Substances 0.000 description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 9
- 239000007772 electrode material Substances 0.000 description 4
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 238000003775 Density Functional Theory Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
-
- 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
- H01M4/364—Composites as mixtures
-
- 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
-
- 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 VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 The preparation method of the/S composite material comprises the following steps: step one, weighing 1.6-3 g of ammonium metavanadate, slowly adding the ammonium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, and magnetically stirring at room temperature until the ammonium metavanadate is dissolved to obtain a solution A; step two, adding 6-9.6 g of thioacetamide into the solution A, uniformly stirring, transferring into 75ml of polytetrafluoroethylene lining, and placing into an oven for hydrothermal reaction at 160-180 ℃ for 24 hours; step three, naturally cooling the hydrothermal product to room temperature, filtering the lotion, and freeze-drying the product obtained by filtering to obtain VS 2 (ii) a/S composite; VS prepared by the invention 2 the/S composite micron flower-shaped structure has even distribution and uniform size, large space for assembling monomers and the VS 2 the/S composite structure has fast reaction kinetics and ultrahigh capacity, and realizes high-capacity and high-pseudocapacitance sodium electric cathode storage.
Description
Technical Field
The invention belongs to the technical field of functional materials, relates to an electrode material, and particularly relates to VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 An S electrode material, a preparation method and application thereof.
Background
With the increasing development of various portable electronic products and green electric vehicles, it is very urgent to develop advanced energy storage devices with fast charge and discharge capability, long service life and high energy density. Two-dimensional Transition Metal Sulfides (TMDs) allow Na due to their unique layered structure + Rapid deintercalation, is a very promising electrode material (Goikolea E, Palomares V, Wang S, et al. Na-Ion Batteries-apparatus Old and New Challenges [ J. ]]Advanced Energy Materials,2020,10(44): 2002005). With other TMDs having poor intrinsic conductivity (e.g., MoS) 2 、SnS 2 、WS 2 ) In contrast, vanadium disulfide (VS) 2 ) The conductivity is good. Density Functional Theory (DFT) also indicates VS 2 And MoS 2 Compared with the conventional diffusion barrier (Yang J, Wang J, Dong X, et al. the potential application of VS2 as an electrode material for Mg ion battery: ADFT battery [ J]Applied Surface Science,2021,544: 148775.). The current research shows that the vanadium disulfide has low capacity and poor multiplying power when applied to sodium electricity storage. (Li W, Kheimeh S, Li X. EmergingLayered Metallic variable sodium nanoparticles for Rechargeable Metallic-Ion Batteries: Progress and Opportunities [ J].ChemSusChem,2020,13(6):1172-1202.)。
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a cooperationVS to promote high capacity high pseudocapacitance sodium storage 2 /S composite material, preparation method and application thereof, and prepared VS 2 the/S composite micrometer flower-shaped structure has a uniform and stable structure, the structure synergistic effect between vanadium disulfide and sulfur improves the sodium storage performance, and the high-capacity high-pseudocapacitance sodium electric cathode storage is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 The preparation method of the/S composite material comprises the following steps:
step one, weighing 1.6-3 g of ammonium metavanadate, slowly adding the ammonium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, and magnetically stirring at room temperature until the ammonium metavanadate is dissolved to obtain a solution A;
step two, adding 6-9.6 g of thioacetamide into the solution A, uniformly stirring, transferring into 75ml of polytetrafluoroethylene lining, and placing into an oven for hydrothermal reaction at 160-180 ℃ for 24 hours;
step three, naturally cooling the hydrothermal product to room temperature, filtering the lotion, and freeze-drying the product obtained by filtering to obtain VS 2 a/S composite material.
The invention also has the following technical characteristics:
preferably, the stirring in the step one is performed for 10-30 min by adopting a magnetic stirrer at a rotating speed of 400-700 r/min.
Preferably, the stirring in the second step is performed by using a magnetic stirrer at a rotating speed of 400-700 r/min for 60-80 min.
Preferably, the suction filtration in the third step is suction filtration washing with water and ethanol alternately for three times.
The invention also protects VS prepared by the method for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 The material is in a uniformly distributed micrometer flower-shaped structure.
Compared with the prior art, the invention has the following technical effects:
the invention is carried out by a one-step hydrothermal methodVS with synthesized nano-sulfur particles distributed on vanadium disulfide micron sheet 2 the/S composite micron flower-shaped structure has even distribution and uniform size, large space for assembling monomers and the VS 2 the/S composite structure has rapid reaction kinetics and ultrahigh capacity, and is mainly attributed to the structural synergistic effect between vanadium disulfide and sulfur formed by a vanadium disulfide and sulfur composite micrometer flower-shaped structure, so that the storage of sodium ions in the reaction process of vanadium disulfide and sulfur is enhanced, the reaction kinetics is accelerated, the desorption of sodium ions is promoted, meanwhile, the shuttle effect of sulfur in the reaction process is inhibited by vanadium disulfide, the capacity of the composite structure is promoted by sulfur, the sodium storage performance is promoted by the synergistic effect, and the storage of a high-capacity and high-pseudocapacitance sodium electric cathode is realized;
the invention adopts stirring and hydrothermal method for synthesis, and the process is simple and stable;
VS prepared by the invention 2 The capacity of the/S composite structure is 780mAh/g when the current density is 1A/g and 450 circles circulate, the capacity of 376mAh/g when the current density is 20A/g and 800 circles circulate, the pseudocapacitance accounts for 94.2 percent at the sweeping speed of 0.4mV/S, the sodium storage performance with high capacity and long cycle life is shown, and the sodium storage mechanism with high pseudocapacitance is provided.
Drawings
FIG. 1 is VS prepared in example 2 2 XRD diffraction pattern of the/S composite structure;
FIG. 2 is VS prepared in example 2 2 SEM image of/S composite structure;
FIG. 3 is VS prepared in example 2 2 Cycle performance plot of the/S composite structure (1A/g);
FIG. 4 is VS prepared in example 2 2 (ii) cycle performance plot of the/S composite structure (20A/g);
FIG. 5 is VS prepared in example 2 2 A pseudo capacitance performance diagram of the/S composite structure.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1:
adding 1.6g ammonium metavanadate into the mixed solution of 45ml water and 9ml ammonia water, stirring for 20min at the normal temperature by adopting a magnetic stirrer at the rotating speed of 700r/min,adding 6g thioacetamide, stirring with a magnetic stirrer at 700r/min for 70min, transferring to 75ml polytetrafluoroethylene lining, performing hydrothermal reaction at 165 deg.C for 24h, alternately suction-filtering and washing the product with water and ethanol for three times, and freeze-drying to obtain VS 2 a/S composite material.
Example 2:
adding 2.1g of ammonium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 10min at the rotation speed of 600r/min by using a magnetic stirrer at normal temperature, adding 7.2g of thioacetamide, stirring for 60min at the rotation speed of 600r/min by using the magnetic stirrer, transferring into a 75ml of polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at 160 ℃, alternately carrying out suction filtration and washing on a product for three times by using water and ethanol until the product is washed, and carrying out freeze drying to obtain VS 2 (ii) an/S composite;
VS prepared in example 2 2 The XRD diffraction spectrogram of the/S composite material is shown in figure 1, and as can be seen from figure 1, diffraction peaks respectively correspond to a vanadium disulfide 89-1640PDF card and a sulfur 08-0247PDF card, so that the synthesis of a vanadium disulfide and sulfur composite structure is proved;
FIG. 2 is VS prepared in example 2 2 SEM image of/S composite material; as can be seen from FIG. 2, the morphology presents a uniformly distributed micron flower structure, and sulfur is distributed on the surface of the vanadium disulfide micron sheet;
FIGS. 3 and 4 are VS prepared in example 2 2 A cycle performance graph of the/S composite; VS can be seen from FIG. 3 2 The capacity of 780mAh/g of the/S composite structure is still remained after the circulation for 450 circles under the current density of 1A/g, and the VS can be seen from figure 3 2 the/S composite structure still has the capacity of 376mAh/g after circulating for 800 circles under the current density of 20A/g;
FIG. 5 is VS prepared in example 2 2 A pseudo capacitance performance diagram of the/S composite material; VS can be seen from FIG. 5 2 the/S composite structure has ultrahigh pseudocapacitance sodium storage contribution.
Example 3:
adding 1.9g ammonium metavanadate into the mixed solution of 45ml water and 9ml ammonia water, stirring for 15min at normal temperature by using a magnetic stirrer at the rotating speed of 500r/min, adding 8g thioacetamide, and rotating at 500r/min by using a magnetic stirrerStirring at high speed for 60min, transferring into 75ml polytetrafluoroethylene lining, performing hydrothermal reaction at 180 deg.C for 24h, alternately filtering and washing the product with water and ethanol for three times, and freeze drying to obtain VS 2 a/S composite material.
Example 4:
adding 3g of ammonium metavanadate mixture into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 30min at the normal temperature by using a magnetic stirrer at the rotating speed of 400r/min, adding 9.6g of thioacetamide mixture, stirring for 80min at the rotating speed of 400r/min by using the magnetic stirrer, transferring into a 75ml of polytetrafluoroethylene lining, carrying out hydrothermal reaction for 24h at the temperature of 170 ℃, alternately filtering and washing a product for three times by using water and ethanol until the product is washed, and carrying out freeze drying to obtain VS 2 a/S composite material.
The present invention is described in detail with reference to the above embodiments, and those skilled in the art will understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which should be construed broadly as set forth in the claims.
Claims (6)
1. VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 The preparation method of the/S composite material is characterized by comprising the following steps:
step one, weighing 1.6-3 g of ammonium metavanadate, slowly adding the ammonium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, and magnetically stirring at room temperature until the ammonium metavanadate is dissolved to obtain a solution A;
step two, adding 6-9.6 g of thioacetamide into the solution A, uniformly stirring, transferring into 75ml of polytetrafluoroethylene lining, and placing into an oven for hydrothermal reaction at 160-180 ℃ for 24 hours;
step three, naturally cooling the hydrothermal product to room temperature, filtering the lotion, and freeze-drying the product obtained by filtering to obtain VS 2 a/S composite material.
2. The synergistic VS for promoting high capacity high pseudocapacitance sodium storage of claim 1 2 The preparation method of the/S composite material is characterized in that the stirring in the step one is performed for 10-30 min by adopting a magnetic stirrer at the rotating speed of 400-700 r/min.
3. The synergistic VS for promoting high capacity high pseudocapacitance sodium storage of claim 1 2 The preparation method of the/S composite material is characterized in that the stirring in the step two is performed by adopting a magnetic stirrer at the rotating speed of 400-700 r/min for 60-80 min.
4. The synergistic VS for promoting high capacity high pseudocapacitance sodium storage of claim 1 2 The preparation method of the/S composite material is characterized in that the suction filtration in the third step is suction filtration washing three times by alternately using water and ethanol.
5. VS for synergistically promoting high capacity high pseudocapacitance sodium storage prepared by the method of any of claims 1-4 2 the/S composite material is characterized by being in a uniformly distributed micrometer flower-shaped structure.
6. VS for synergistically promoting high capacity high pseudocapacitance sodium storage according to claim 5 2 The application of the/S composite material in the negative electrode material of the sodium battery.
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| CN202210740412.3A CN114975963A (en) | 2022-06-28 | 2022-06-28 | VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof |
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| CN202210740412.3A CN114975963A (en) | 2022-06-28 | 2022-06-28 | VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof |
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|---|---|---|---|---|
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2022
- 2022-06-28 CN CN202210740412.3A patent/CN114975963A/en active Pending
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