CN113193198A - Cobalt-doped vanadium disulfide micron sheet and preparation method thereof - Google Patents
Cobalt-doped vanadium disulfide micron sheet and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention discloses a cobalt-doped vanadium disulfide micron sheet and a preparation method thereof, and the preparation method comprises the steps of 1) mixing a cobalt nitrate methanol solution with the concentration of 0.04-0.08 mol/L and a di-methylimidazole methanol solution with the concentration of 0.16-0.32 mol/L according to the molar ratio of cobalt nitrate to di-methylimidazole of 1 (4-6), stirring, centrifuging, washing and drying to obtain ZIF-67; 2) adding the ZIF-67 obtained in the step 1) into water, adjusting the pH value to be alkaline, uniformly stirring, adding a vanadium source and a sulfur source, and stirring to obtain a mixed solution; the mass ratio of the added vanadium source to the ZIF-67 is (2-7): 1; the concentration of a vanadium source in the obtained mixed solution is 0.039-0.12 mol/L; the concentration of the sulfur source is 0.32-0.78 mol/L; 3) heating the mixed solution obtained in the step 2) to 160-180 ℃, preserving heat for 24 hours, naturally cooling, and then performing suction filtration, washing and freeze drying to obtain the cobalt-doped vanadium disulfide micron sheet; the preparation method is simple and easy to obtain, and the prepared cobalt-doped vanadium disulfide micron sheet has the capacity of 390mAh/g under the current density of 0.5A/g as the negative electrode material of the sodium-ion battery.
Description
Technical Field
The invention belongs to the field of battery electrode materials, and particularly relates to a cobalt-doped vanadium disulfide micron sheet and a preparation method thereof.
Background
Vanadium disulfide is taken as one of transition metal sulfides, and is regarded as a sodium ion battery cathode material with great development potential due to variable V valence, metal state characteristics, large interlayer spacing and weak interlayer bonding force. However, during the electrochemical reaction process, two problems of pulverization and charge transfer delay are easy to occur, so that the poor cycle stability and rate capability are caused. (Z.Hu, Q.Liu, S. -L.Chou, S.X.Dou, Advances and Challeges in Metal Sulfides/Selenides for Next-Generation Rechargeable Sodium-Ion Batteries [ J ]. Advanced Materials, (2017)1700606.) while Metal doping in Metal Sulfides can introduce some lattice changes (such as twisting, expansion and contraction), vacancies and electronic defects, providing a convenient route for Sodium penetration into the matrix material. (Fan Y, Luan D, Lou X W D. Recent Advances on Mixed Metal Sulfides [ J ] Advanced Materials,2020,32(42) ]) therefore, cobalt is doped in vanadium disulfide, the Sodium Ion transmission path can be shortened, and the electrochemical performance of the material can be improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the preparation method of the cobalt-doped vanadium disulfide micron sheet with simple preparation process, and the prepared cobalt-doped vanadium disulfide micron sheet has uniform and stable structure, excellent conductivity and electrochemical performance.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a cobalt-doped vanadium disulfide micron sheet specifically comprises the following steps:
step 1: mixing a cobalt nitrate methanol solution with the concentration of 0.04-0.08 mol/L and a di-methylimidazole methanol solution with the concentration of 0.16-0.32 mol/L according to the molar ratio of cobalt nitrate to di-methylimidazole of 1 (4-6), stirring, centrifuging, washing and drying to obtain ZIF-67;
step 2: adding the ZIF-67 obtained in the step 1 into water, adjusting the pH value to be alkaline, uniformly stirring, adding a vanadium source and a sulfur source, and stirring to obtain a mixed solution; the mass ratio of the added vanadium source to the ZIF-67 is (2-7): 1, a source of vanadium; the concentration of a vanadium source in the obtained mixed solution is 0.039-0.12 mol/L, and the concentration of a sulfur source in the obtained mixed solution is 0.32-0.78 mol/L;
and step 3: and (3) filling the mixed solution obtained in the step (2) into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an oven, heating to 160-180 ℃, preserving heat for 24 hours, naturally cooling a reaction product, and performing suction filtration, washing and freeze drying to obtain the cobalt-doped vanadium disulfide nanosheet.
Further, in the step 1, a magnetic stirrer of 500-700 r/min is adopted for stirring at room temperature for 12-24 hours.
Further, the centrifugation treatment in the step 1 adopts methanol treatment.
Further, the drying treatment in the step 1 is drying for 12 hours in an oven with the temperature of 60 ℃.
Further, the stirring treatment in the step 2 is to stir for 60min at room temperature by adopting a magnetic stirrer of 500-700 r/min.
Further, the washing treatment in the step 3 is suction filtration washing with water and ethanol alternately.
Further, in the step 2, the vanadium source is one or a mixture of sodium metavanadate, sodium vanadate and ammonium metavanadate.
Further, in the step 2, the sulfur source is one or a mixture of thioacetamide and thiourea.
A cobalt-doped vanadium disulfide micron sheet is in a sheet stacking structure and has a capacity of 390mAh/g under a current density of 0.5A/g.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention adopts stirring and solvothermal synthesis, and has simple and easily obtained preparation process, uniform structure and easy regulation and control.
2) The cobalt doping in the cobalt-doped vanadium disulfide micron sheet structure prepared by the invention can provide more reaction active sites, improve the carrier mobility and improve the conductivity; compared with a common cobalt source, the cobalt source ZIF-67 is adopted and can be used as a template agent, and the structural bonding is firmer.
3) The invention can cause slight lattice expansion/contraction of the structure by cobalt doping, thereby causing higher mobility and more defect structures, lowering diffusion barrier and promoting Na+And the electrochemical performance of the vanadium disulfide is improved by the diffusion of ions.
Drawings
FIG. 1 is an XRD diffraction pattern of cobalt-doped vanadium disulfide nanoplatelets prepared in example 2 of the present invention;
FIG. 2 is an SEM image of cobalt-doped vanadium disulfide nanosheets prepared in example 2 of the present invention;
FIG. 3 is a graph of rate capability of cobalt-doped vanadium disulfide nanosheets prepared in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1
The invention provides a preparation method of a cobalt-doped vanadium disulfide micron sheet, which specifically comprises the following steps:
step 1: dissolving 4mmol of cobalt nitrate in 100ml of methanol, dissolving 16mmol of di-methylimidazole in 100ml of methanol, slowly pouring the methanol solution dissolved with the di-methylimidazole into the methanol solution dissolved with the cobalt nitrate, stirring for 12 hours at room temperature by adopting a magnetic stirrer of 500-700 r/min, centrifuging for three times by using the methanol to wash the solution, collecting a centrifuged sample, and drying for 12 hours at 60 ℃ in an oven to obtain the ZIF-67.
Step 2: adding 0.1g of ZIF-67 into a mixed solution of 35ml of water and 7ml of ammonia water, uniformly stirring, adding a certain amount of sodium metavanadate to adjust the concentration of a vanadium source to be 0.039mol/L, stirring for 15min, adding a certain amount of thioacetamide to adjust the concentration of a sulfur source to be 0.32mol/L, and stirring for 60min at room temperature by adopting a magnetic stirrer of 500-700 r/min to obtain a mixed solution;
and step 3: and (3) filling the mixed solution obtained in the step (2) into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in a drying oven, heating to 160 ℃, preserving the temperature for 24 hours, after the reaction product is naturally cooled, alternately washing with water and ethanol, performing suction filtration, and performing freeze drying to obtain the cobalt-doped vanadium disulfide micron sheet.
Example 2
The invention provides a preparation method of a cobalt-doped vanadium disulfide micron sheet, which specifically comprises the following steps:
step 1: dissolving 4mmol of cobalt nitrate in 60ml of methanol, dissolving 18mmol of di-methylimidazole in 80ml of methanol, slowly pouring the methanol solution dissolved with the di-methylimidazole into the methanol solution dissolved with the cobalt nitrate, stirring for 16h at room temperature by adopting a magnetic stirrer of 500-700 r/min, centrifuging for three times by using the methanol to wash the solution, collecting a centrifuged sample, and drying for 12h at 60 ℃ in an oven to obtain the ZIF-67.
Step 2: adding 0.1g of ZIF-67 into a mixed solution of 35ml of water and 7ml of ammonia water, uniformly stirring, adding a certain amount of sodium metavanadate to adjust the concentration of a vanadium source to be 0.06mol/L, stirring for 15min, adding a certain amount of thioacetamide to adjust the concentration of a sulfur source to be 0.38mol/L, and stirring for 60min at room temperature by adopting a magnetic stirrer of 500-700 r/min to obtain a mixed solution;
and step 3: and (3) filling the mixed solution obtained in the step (2) into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in a drying oven, heating to 160 ℃, preserving the temperature for 24 hours, after the reaction product is naturally cooled, alternately washing with water and ethanol, performing suction filtration, and performing freeze drying to obtain the cobalt-doped vanadium disulfide micron sheet.
FIG. 1 is an XRD diffraction pattern of the cobalt-doped vanadium disulfide nanosheet prepared in example 2, wherein the abscissa is an angle of 2 theta and the ordinate is intensity, and as can be seen from FIG. 1, diffraction peaks point to JCPDS36-1139 PDF cards, which proves that VS is synthesized2。
Fig. 2 is an SEM image of the cobalt-doped vanadium disulfide nanosheets prepared in example 2, and it can be seen from fig. 2 that the cobalt-doped vanadium disulfide exhibits the morphology of a lamellar stack.
Fig. 3 is a graph of the rate performance of the cobalt-doped vanadium disulfide micro-scale sheet prepared in example 2, wherein the abscissa is the number of cycles and the ordinate is the capacity (mAh/g), and it can be seen from fig. 3 that the cobalt-doped vanadium disulfide micro-scale sheet still has a capacity of 390mAh/g after 100 cycles at a current density of 0.5A/g.
Example 3
The invention provides a preparation method of a cobalt-doped vanadium disulfide micron sheet, which specifically comprises the following steps:
step 1: dissolving 4mmol of cobalt nitrate in 70ml of methanol, dissolving 20mmol of di-methylimidazole in 80ml of methanol, slowly pouring the methanol solution dissolved with the di-methylimidazole into the methanol solution dissolved with the cobalt nitrate, stirring for 18 hours at room temperature by adopting a magnetic stirrer of 500-700 r/min, centrifuging for three times by using the methanol to wash the solution, collecting a centrifuged sample, and drying for 12 hours at 60 ℃ in an oven to obtain the ZIF-67.
Step 2: adding 0.1g of ZIF-67 into a mixed solution of 40ml of water and 8ml of ammonia water, uniformly stirring, adding a certain amount of sodium metavanadate to adjust the concentration of a vanadium source to be 0.1mol/L, stirring for 15min, adding a certain amount of thioacetamide to adjust the concentration of a sulfur source to be 0.5mol/L, and stirring for 60min at room temperature by adopting a magnetic stirrer of 500-700 r/min to obtain a mixed solution;
and step 3: and (3) filling the mixed solution obtained in the step (2) into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in a drying oven, heating to 180 ℃, preserving the temperature for 24 hours, after the reaction product is naturally cooled, alternately washing with water and ethanol, performing suction filtration, and performing freeze drying to obtain the cobalt-doped vanadium disulfide micron sheet.
Example 4
The invention provides a preparation method of a cobalt-doped vanadium disulfide micron sheet, which specifically comprises the following steps:
step 1: dissolving 4mmol of cobalt nitrate in 50ml of methanol, dissolving 24mmol of di-methylimidazole in 75ml of methanol, slowly pouring the methanol solution dissolved with the di-methylimidazole into the methanol solution dissolved with the cobalt nitrate, stirring at room temperature for 24 hours by adopting a magnetic stirrer of 500-700 r/min, centrifuging the solution for three times by using the methanol to wash the solution, collecting the centrifuged sample, and drying the centrifuged sample in an oven at 60 ℃ for 12 hours to obtain the ZIF-67.
Step 2: adding 0.1g of ZIF-67 into a mixed solution of 35ml of water and 7ml of ammonia water, uniformly stirring, adding a certain amount of sodium metavanadate to adjust the concentration of a vanadium source to be 0.12mol/L, stirring for 15min, adding a certain amount of thioacetamide to adjust the concentration of a sulfur source to be 0.78mol/L, and stirring for 60min at room temperature by adopting a magnetic stirrer of 500-700 r/min to obtain a mixed solution.
And step 3: and (3) filling the mixed solution obtained in the step (2) into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in a drying oven, heating to 180 ℃, preserving the temperature for 24 hours, after the reaction product is naturally cooled, alternately washing with water and ethanol, performing suction filtration, and performing freeze drying to obtain the cobalt-doped vanadium disulfide micron sheet.
Claims (9)
1. A preparation method of a cobalt-doped vanadium disulfide micron sheet is characterized by comprising the following steps:
step 1: mixing a cobalt nitrate methanol solution with the concentration of 0.04-0.08 mol/L and a di-methylimidazole methanol solution with the concentration of 0.16-0.32 mol/L according to the molar ratio of cobalt nitrate to di-methylimidazole of 1 (4-6), stirring, centrifuging, washing and drying to obtain ZIF-67;
step 2: adding the ZIF-67 obtained in the step 1 into water, adjusting the pH value to be alkaline, uniformly stirring, adding a vanadium source and a sulfur source, and stirring to obtain a mixed solution; the mass ratio of the added vanadium source to the ZIF-67 is (2-7): 1, a source of vanadium; the concentration of a vanadium source in the obtained mixed solution is 0.039-0.12 mol/L, and the concentration of a sulfur source in the obtained mixed solution is 0.32-0.78 mol/L;
and step 3: and (3) filling the mixed solution obtained in the step (2) into a polytetrafluoroethylene lining, placing the polytetrafluoroethylene lining in an oven, heating to 160-180 ℃, preserving heat for 24 hours, naturally cooling a reaction product, and performing suction filtration, washing and freeze drying to obtain the cobalt-doped vanadium disulfide nanosheet.
2. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps: in the step 1, a magnetic stirrer of 500-700 r/min is adopted for stirring at room temperature for 12-24 h.
3. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps: the centrifugation treatment in the step 1 adopts methanol treatment.
4. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps: the drying treatment in the step 1 is drying for 12 hours in an oven with the temperature of 60 ℃.
5. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps: and the stirring treatment in the step 2 is to stir for 60min at room temperature by adopting a magnetic stirrer of 500-700 r/min.
6. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps: and the washing treatment in the step 3 is suction filtration washing with water and ethanol alternately.
7. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps:
and in the step 2, the vanadium source is one or a mixture of sodium metavanadate, sodium vanadate and ammonium metavanadate.
8. The method for preparing the cobalt-doped vanadium disulfide micron sheet according to claim 1, wherein the method comprises the following steps: in the step 2, the sulfur source is one or a mixture of thioacetamide and thiourea.
9. The cobalt-doped vanadium disulfide micron sheet prepared by the preparation method of any one of claims 1 to 8, wherein: the micron sheet is in a sheet stack structure and has a capacity of 390mAh/g at a current density of 0.5A/g.
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CN114975963A (en) * | 2022-06-28 | 2022-08-30 | 陕西科技大学 | VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof |
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CN114975963A (en) * | 2022-06-28 | 2022-08-30 | 陕西科技大学 | VS for synergistically promoting high-capacity high-pseudocapacitance sodium storage 2 /S composite material and preparation method and application thereof |
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