CN113299910A - Iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet and preparation method and application thereof - Google Patents
Iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet and preparation method and application thereof Download PDFInfo
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- 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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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet and a preparation method and application thereof, and belongs to the technical field of energy storage materials. Dissolving nickel nitrate hexahydrate, cobalt nitrate hexahydrate and iron nitrate nonahydrate in methanol to obtain a methanol solution of mixed polymetallic, dissolving 2-methylimidazole in methanol to obtain a methanol solution of 2-methylimidazole, quickly pouring the methanol solution of 2-methylimidazole into the methanol solution of mixed polymetallic, transferring the obtained mixed solution into a high-pressure reaction kettle containing foamed nickel, carrying out solvothermal reaction, washing and drying to obtain the iron-doped nickelThe nickel/cobalt-based metal organic framework nanosheet and an aqueous solution of a vulcanizing agent are subjected to hydrothermal vulcanization reaction, and after cooling, washing and drying are carried out, so that the iron-doped nickel/cobalt-based multi-metal sulfide nanosheet is obtained on foamed nickel and used as an energy storage electrode material with a single electrode and the specific capacity of 1919.6F.g‑1The composite material has good cycle stability and rate capability, and is used for a hybrid super capacitor or a battery.
Description
Technical Field
The invention belongs to the technical field of energy storage materials, relates to an energy storage electrode material, and particularly relates to an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet and a preparation method and application thereof.
Background
Super capacitors, also called electrochemical capacitors, are receiving increasing attention as a new type of energy storage device. Compared with other energy storage devices, the super capacitor has many advantages, such as rapid charging and discharging, long service life, higher power density than a battery, lower internal resistance, higher energy density than a traditional capacitor and the like, is applied to the fields of portable electronic devices and hybrid electric vehicles, and the energy storage demand is gradually increased along with the continuous expansion of the application field.
Electrode materials are important factors influencing the electrochemical performance of energy storage devices, metal organic framework materials are receiving more and more attention due to higher porosity, larger specific surface area, and diversity of structures and functions, but the application of the metal organic framework materials is limited by lower conductivity. The metal organic framework derived sulfide can effectively improve the conductivity of the material, such as nickel-based sulfide, nickel-cobalt-based sulfide, iron-doped nickel/cobalt-based sulfide and the like, and compared with unitary and binary metal sulfides, the multi-metal sulfide with the doped components can provide more abundant redox active sites and better conductivity. However, the production of the polysulfide is complicated, the number of elements involved is large, and the parameters to be controlled are also complicated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet which is high in specific capacitance and good in rate capability.
The second purpose of the invention is to provide the preparation method of the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet, which is accurate and reliable, simple to operate and easy to produce.
The third purpose of the invention is to provide the application of the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet as an energy storage electrode material in a hybrid supercapacitor or battery, and the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet has an efficient energy storage effect.
In order to achieve the purpose, the invention adopts the technical scheme that:
the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet provided by the invention is obtained by directly growing an iron-doped nickel/cobalt metal organic framework precursor on foamed nickel through a solvothermal method and then performing a hydrothermal vulcanization method on the foamed nickel.
The invention provides a preparation method of the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet, which comprises the following steps:
(1) dissolving nickel nitrate hexahydrate, cobalt nitrate hexahydrate and ferric nitrate nonahydrate in methanol to obtain a mixed polymetallic methanol solution, dissolving 2-methylimidazole in methanol to obtain a 2-methylimidazole methanol solution, quickly pouring the 2-methylimidazole methanol solution into the mixed polymetallic methanol solution, transferring the obtained mixed solution into a high-pressure reaction kettle containing foamed nickel, carrying out thermal reaction on the mixed solution, washing and drying to obtain the iron-doped nickel/cobalt-based metal organic framework nanosheet;
(2) and (2) carrying out hydrothermal vulcanization reaction on the iron-doped nickel/cobalt-based metal organic framework nanosheet obtained in the step (1) and an aqueous solution of a vulcanizing agent, cooling, washing and drying to obtain the iron-doped nickel/cobalt-based polymetallic sulfide nanosheet on foamed nickel.
Further, in the step (1), the concentration of nickel nitrate hexahydrate in the mixed multi-metal methanol solution is 0.02-0.1 mol.L-1The concentration of the cobalt nitrate hexahydrate is 0.01-0.05 mol.L-1The concentration of ferric nitrate nonahydrate is 0.002-0.01 mol.L-1。
Further, in the step (1), the concentration of the 2-methylimidazole in the methanol solution of the 2-methylimidazole is 0.1 to 0.5mol-1。
Further, in the step (1), the high-pressure reaction kettle is a stainless steel reaction kettle with a polytetrafluoroethylene lining.
Further, in the step (1), the solvothermal reaction temperature is 160-.
Further, in the step (1), washing is carried out by using deionized water and ethanol; the drying temperature is 60-70 deg.C, and the drying time is 2-4 h.
Further, in the step (1), the size of the foamed nickel is 0.5 multiplied by 0.5cm2Or 1X 1cm2。
Further, in the step (2), the vulcanizing agent is selected from thioacetamide or sodium sulfide.
Further, in the step (2), the concentration of the vulcanizing agent in the aqueous solution of the vulcanizing agent is 0.005-0.02 mol-1。
Further, in the step (2), the hydrothermal reaction temperature is 120-.
Further, in the step (2), washing is carried out by using deionized water; the drying temperature is 60-70 deg.C, and the drying time is 12-14 h.
The invention also provides application of the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet as an energy storage electrode material in a hybrid supercapacitor or battery.
Compared with the prior art, the invention has the beneficial effects that: the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet prepared by the method has the advantages of wide raw material source, low cost, accurate and reliable preparation method, simple operation and easy production; the obtained iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet as an energy storage electrode material has high specific capacitance, good cycle stability and rate capability, and has an efficient energy storage effect when being used for a hybrid super capacitor or a battery.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
fig. 1 is a flow chart of the preparation of iron-doped nickel/cobalt metal organic framework derivatized sulfide nanosheets of the present invention;
FIG. 2 is an SEM photograph of Fe-doped Ni/Co MOFs derivatized sulfide (FIG. 2a) and binary Ni/Co MOFs derivatized sulfide nanosheets (FIG. 2b) in a preferred embodiment;
FIG. 3 is a low magnification TEM image of Fe-doped Ni/Co MOFs derivatized sulfide (FIG. 3a) and binary Ni/Co MOFs derivatized sulfide nanosheets (FIG. 3b) in a preferred embodiment;
FIG. 4 is a high magnification TEM image of Fe-doped Ni/Co MOFs derivatized sulfide (FIG. 4a) and binary Ni/Co MOFs derivatized sulfide nanosheets (FIG. 4b) in a preferred embodiment;
FIG. 5 is a graph of the rate capability of iron-doped nickel/cobalt metal organic framework derivatized sulfide nanoplates in a preferred embodiment;
fig. 6 is a graph of the cycling stability of iron-doped nickel/cobalt metal organic framework derivatized sulfide nanoplates in a preferred embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
As shown in fig. 1, a preparation method of an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is exemplarily described, and the iron-doped nickel/cobalt metal organic framework precursor is directly grown on foamed nickel through a solvothermal method and then obtained on the foamed nickel through a hydrothermal vulcanization method, and the preparation method comprises the following steps:
(1) dissolving nickel nitrate hexahydrate, cobalt nitrate hexahydrate and ferric nitrate nonahydrate in methanol to obtain a mixed polymetallic methanol solution, dissolving 2-methylimidazole in methanol to obtain a 2-methylimidazole methanol solution, quickly pouring the 2-methylimidazole methanol solution into the mixed polymetallic methanol solution, transferring the obtained mixed solution into a high-pressure reaction kettle containing foamed nickel, carrying out solvothermal reaction, washing and drying to obtain the iron-doped nickel/cobalt-based metal organic framework nanosheet;
(2) and (2) carrying out hydrothermal vulcanization reaction on the iron-doped nickel/cobalt-based metal organic framework nanosheet obtained in the step (1) and an aqueous solution of a vulcanizing agent, cooling, washing and drying to obtain the iron-doped nickel/cobalt-based polymetallic sulfide nanosheet on foamed nickel.
In some embodiments, the concentration of nickel nitrate hexahydrate in the mixed multimetal methanol solution is from 0.02 to 0.1mol-1The concentration of the cobalt nitrate hexahydrate is 0.01-0.05 mol.L-1The concentration of ferric nitrate nonahydrate is 0.002-0.01 mol.L-1。
In some examples, the concentration of 2-methylimidazole in the methanol solution of 2-methylimidazole is 0.1 to 0.5mol.L-1。
In some embodiments, in step (1), the autoclave is a stainless steel autoclave with a teflon liner.
In some embodiments, in step (1), the solvothermal reaction temperature is 160-.
In some embodiments, in step (1), the washing is performed by washing with deionized water and ethanol; the drying temperature is 60-70 deg.C, and the drying time is 2-4 h.
In some embodiments, in step (1), the nickel foam has a size of 0.5X 0.5cm2Or 1X 1cm2。
In some embodiments, in step (2), the sulfurizing agent is selected from thioacetamide or sodium sulfide.
In some examples, in step (2), the concentration of the sulfiding agent in the aqueous solution of sulfiding agent is 0.005-0.02 mol-1。
In some embodiments, in the step (2), the hydrothermal reaction temperature is 120-.
In some embodiments, in the step (2), the washing is performed by using deionized water; the drying temperature is 60-70 deg.C, and the drying time is 12-14 h.
The above technical solution of the present invention is further explained in detail by examples below.
Example 1
In this embodiment, an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is prepared by the following steps:
the method comprises the following steps: dissolving 0.1mmol nickel nitrate hexahydrate, 0.05mmol cobalt nitrate hexahydrate and 0.01mmol iron nitrate nonahydrate in 17.5mL methanol solution, dissolving 4mmol 2-methylimidazole in 17.5mL methanol, rapidly pouring the methanol solution of 2-methylimidazole into mixed metal salt solution, and transferring the obtained mixed solution to a solution containing 1 × 1cm2Reacting for 6 hours at 180 ℃ in a high-pressure reaction kettle for foamed nickel, cooling to room temperature, washing with deionized water and ethanol for three times respectively, drying for 2 hours at 60 ℃, and obtaining an iron-doped nickel/cobalt metal organic framework precursor on the foamed nickel;
step two: dissolving 0.4mmol of thioacetamide in 30mL of deionized water, magnetically stirring for 30min, transferring the mixed solution to a high-pressure reaction kettle containing an iron-doped nickel/cobalt metal organic framework nanosheet precursor, reacting for 3h at 120 ℃, cooling to room temperature, washing with the deionized water for three times, drying for 12h at 60 ℃, and obtaining the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet on foamed nickel.
Example 2
In this embodiment, an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is prepared by the following steps:
the method comprises the following steps: dissolving 0.1mmol nickel nitrate hexahydrate, 0.05mmol cobalt nitrate hexahydrate and 0.01mmol iron nitrate nonahydrate in 17.5mL methanol solution, dissolving 4mmol 2-methylimidazole in 17.5mL methanol, rapidly pouring the methanol solution of 2-methylimidazole into mixed metal salt solution, and transferring the obtained mixed solution to a solution containing 0.5 × 0.5cm2Reacting for 6 hours at 180 ℃ in a high-pressure reaction kettle for foamed nickel, cooling to room temperature, washing with deionized water and ethanol for three times respectively, drying for 2 hours at 60 ℃, and obtaining an iron-doped nickel/cobalt metal organic framework precursor on the foamed nickel;
step two: dissolving 0.04mmol of thioacetamide in 30mL of deionized water, magnetically stirring for 30min, transferring the mixed solution to a high-pressure reaction kettle containing an iron-doped nickel/cobalt metal organic framework nanosheet precursor, reacting for 1h at 120 ℃, cooling to room temperature, washing with the deionized water for three times, drying for 12h at 60 ℃, and obtaining the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet on foamed nickel.
Example 3
In this embodiment, an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is prepared by the following steps:
the method comprises the following steps: dissolving 0.2mmol nickel nitrate hexahydrate, 0.1mmol cobalt nitrate hexahydrate and 0.02mmol iron nitrate nonahydrate in 17.5mL methanol solution, dissolving 4mmol 2-methylimidazole in 17.5mL methanol, rapidly pouring the methanol solution of 2-methylimidazole into mixed metal salt solution, and transferring the obtained mixed solution to a solution containing 1 × 1cm2Reacting for 6 hours at 180 ℃ in a high-pressure reaction kettle for foamed nickel, cooling to room temperature, washing with deionized water and ethanol for three times respectively, drying for 2 hours at 60 ℃, and obtaining an iron-doped nickel/cobalt metal organic framework precursor on the foamed nickel;
step two: dissolving 0.4mmol of sodium sulfide in 30mL of deionized water, magnetically stirring for 30min, transferring the mixed solution to a high-pressure reaction kettle containing an iron-doped nickel/cobalt metal organic framework nanosheet precursor, reacting for 12h at 120 ℃, cooling to room temperature, washing with the deionized water for three times, drying for 12h at 60 ℃, and obtaining the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet on foamed nickel.
Example 4
In this embodiment, an iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is prepared by the following steps:
the method comprises the following steps: dissolving 0.5mmol nickel nitrate hexahydrate, 0.25mmol cobalt nitrate hexahydrate and 0.05mmol iron nitrate nonahydrate in 17.5mL methanol solution, dissolving 4mmol 2-methylimidazole in 17.5mL methanol, rapidly pouring the methanol solution of 2-methylimidazole into mixed metal salt solution, and transferring the obtained mixed solution to a solution containing 0.5 × 0.5cm2Reacting for 6 hours at 180 ℃ in a high-pressure reaction kettle for foamed nickel, cooling to room temperature, washing with deionized water and ethanol for three times respectively, drying for 2 hours at 60 ℃, and obtaining an iron-doped nickel/cobalt metal organic framework precursor on the foamed nickel;
step two: dissolving 0.04mmol of sodium sulfide in 30mL of deionized water, magnetically stirring for 30min, transferring the mixed solution to a high-pressure reaction kettle containing an iron-doped nickel/cobalt metal organic framework nanosheet precursor, reacting for 3h at 120 ℃, cooling to room temperature, washing with the deionized water for three times, drying for 12h at 60 ℃, and obtaining the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet on foamed nickel.
The iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet prepared in the embodiment is used as a working electrode, mercury/mercury oxide is used as a reference electrode, a platinum electrode with the same area is used as an auxiliary electrode, and 1mol.L of the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is used as a working electrode-1The potassium hydroxide solution is used as electrolyte to form a three-electrode system. Constant current charge and discharge tests were carried out in CHI660E electrochemical workstation over a potential range of 0-0.6V (vs. mercury/mercury oxide). When the current density is 1Ag-1The specific capacitance of the material is 1919.6F.g-1(ii) a When the current density reaches 10Ag-1When the specific capacitance of the material is still 1122.0F.g-1The result shows that the iron-doped nickel/cobalt metal organic framework derived sulfide nanosheet as the energy storage electrode material has high stability and good rate.
Claims (10)
1. The preparation method of the iron-doped nickel/cobalt metal organic framework derivative sulfide nanosheet is characterized by comprising the following steps of:
(1) dissolving nickel nitrate hexahydrate, cobalt nitrate hexahydrate and ferric nitrate nonahydrate in methanol to obtain a mixed polymetallic methanol solution, dissolving 2-methylimidazole in methanol to obtain a 2-methylimidazole methanol solution, quickly pouring the 2-methylimidazole methanol solution into the mixed polymetallic methanol solution, transferring the obtained mixed solution into a high-pressure reaction kettle containing foamed nickel, carrying out thermal reaction on the mixed solution, washing and drying to obtain the iron-doped nickel/cobalt-based metal organic framework nanosheet;
(2) and (2) carrying out hydrothermal vulcanization reaction on the iron-doped nickel/cobalt-based metal organic framework nanosheet obtained in the step (1) and an aqueous solution of a vulcanizing agent, cooling, washing and drying to obtain the iron-doped nickel/cobalt-based polymetallic sulfide nanosheet on foamed nickel.
2. The method of claim 1, wherein the mixed multi-metal in methanol solution is hexa-valentThe concentration of the aqueous nickel nitrate is 0.02-0.1 mol.L-1The concentration of the cobalt nitrate hexahydrate is 0.01-0.05 mol.L-1The concentration of ferric nitrate nonahydrate is 0.002-0.01 mol.L-1。
3. The method for preparing iron-doped nickel/cobalt metal organic framework-derived sulfide nanosheets according to claim 1, wherein the concentration of 2-methylimidazole in the methanol solution of 2-methylimidazole is 0.1-0.5 mol.L-1。
4. The method for preparing iron-doped nickel/cobalt metal organic framework-derived sulfide nanosheets according to claim 1, wherein in step (1), the high-pressure reaction vessel is a stainless steel reaction vessel with a polytetrafluoroethylene lining; the size of the foamed nickel is 0.5 multiplied by 0.5cm2Or 1X 1cm2。
5. The method for preparing Fe-doped Ni/Co metal-organic framework derivative sulfide nanosheets as claimed in claim 1, wherein in step (1), the solvothermal reaction temperature is 160-180 ℃ and the solvothermal reaction time is 6-8 h; washing with deionized water and ethanol; the drying temperature is 60-70 deg.C, and the drying time is 2-4 h.
6. The method for preparing iron-doped nickel/cobalt metal organic framework derivatized sulfide nanosheets according to claim 1, wherein in step (2), the vulcanizing agent is selected from thioacetamide or sodium sulfide.
7. The method of preparing iron-doped nickel/cobalt metal organic framework-derived sulfide nanosheets of claim 6, wherein the concentration of sulfidizing agent in the aqueous solution of sulfidizing agent is from 0.005 to 0.02mol.L-1。
8. The method for preparing Fe-doped Ni/Co metal organic framework-derived sulfide nanosheets as claimed in claim 1, wherein in step (2), the hydrothermal reaction temperature is 120-; washing with deionized water; the drying temperature is 60-70 deg.C, and the drying time is 12-14 h.
9. Iron-doped nickel/cobalt metal organic framework derivatized sulfide nanosheets, obtainable by the method of making iron-doped nickel/cobalt metal organic framework derivatized sulfide nanosheets of any one of claims 1 to 8.
10. Use of the iron-doped nickel/cobalt metal organic framework derivatized sulfide nanosheets of claim 9 as an energy storage electrode material in a hybrid supercapacitor or battery.
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