CN112837943A - Ultrathin two-dimensional nanosheet layer NiCo-MOF material, and preparation method and application thereof - Google Patents
Ultrathin two-dimensional nanosheet layer NiCo-MOF material, and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of an ultrathin two-dimensional nano flaky material Ni-Co-MOF for a super capacitor. The metal salt and the imidazole compound are used as raw materials, the reaction is carried out at a certain temperature after the metal salt and the imidazole compound are dissolved in water, and the ultrathin two-dimensional nano metal organic framework material is prepared by regulating and controlling the proportion of reactants and reaction conditions. The method is environment-friendly, the process is simple, and the obtained electrode material has good electrochemical performance.
Description
Technical Field
The invention belongs to the field of supercapacitors, and relates to an ultrathin two-dimensional nanosheet layer NiCo-MOF material, and a preparation method and application thereof.
Background
The super capacitor is used as a novel energy storage device, has power density far higher than that of a lithium ion battery, has considerable energy density at the same time, and fills up the defects of high-power energy storage equipment. In addition, the super capacitor has the advantages of high charging and discharging speed, long cycle life, environmental protection and the like, so that the super capacitor is widely applied to the fields of industrial large UPS power systems, electric automobiles, aerospace and the like. In recent years, with the development of new energy technology, the application scene of the super capacitor is mature, the market scale is rapidly expanded, the downstream application puts higher requirements on the performance of the super capacitor, and the improvement of the energy density while maintaining the high power density is an urgent demand and target for the future development of the super capacitor. The electrode material is the core of the super capacitor and directly determines the overall performance of the super capacitor, so that the development of the electrode material with high capacity and high stability is critical.
Research shows that MOF and derivatives thereof are potential electrochemical energy storage materials (adv. Mater., 2017, 29, 1703614; ACS Nano, 2017, 11, 5293-5308.). For example, Lee et al synthesized Co-MOF films with terephthalic acid as the organic ligand, and the electrode materials of the films showed good pseudo-capacitance behavior with a maximum specific capacitance of 206.76F g-1(Microporous Mesoporous mater, 2012, 153, 163-165.). For another example, CN110828193A discloses a nanoflower Ni-MOF material and a preparation method thereof, which is prepared by in-situ growth of nickel acetate, terephthalic acid, Sodium Dodecyl Sulfate (SDS), a solvent DMF, deionized water, and absolute ethanol by a solvothermal method. The electrode material is used as an electrode material of a super capacitor, the electrode material can be charged and discharged within the range of 0-0.5V, and the specific capacitance is 802-990F/g when the discharge current density is 1A/g. However, the specific capacitance and the cycling stability of the MOF material applied to the supercapacitor need to be further improved to meet the requirements of practical application.
Therefore, a preparation method of the MOF material for the supercapacitor, which is simple and easy to implement and strong in controllability, is needed to be provided, and the high performance requirement of the electrode material of the supercapacitor is met.
Disclosure of Invention
In view of the above problems in the prior art, the present invention aims to provide an ultrathin two-dimensional nanosheet layer NiCo-MOF material for supercapacitor electrodes, a preparation method and applications thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an ultra-thin two-dimensional nanosheet layer NiCo-MOF material for use in a supercapacitor electrode, the method comprising the steps of:
(1) dissolving nickel salt, cobalt salt and imidazole compound in water to obtain a mixed solution; the molar ratio of the nickel salt to the cobalt salt is 1: 0.2-5, the molar ratio of the total amount of the metal salt to the imidazole compound is 1: 2-15, and the total concentration of metal elements in the mixed solution is 5 mmol/L-60 mmol/L;
(2) and carrying out hydrothermal reaction on the mixed solution, separating a reaction product, and drying to obtain the NiCo-MOF material.
In the method of the present invention, the molar ratio of the nickel element to the cobalt element is 1:0.2 to 5, for example, 1:0.2, 1:0.5, 1:0.8, 1:1, 1:1.5, 1:2, 1:3, 1:4, or 1: 5.
In the method of the present invention, the molar ratio of the total amount of the metal salt to the imidazole compound is 1:2 to 15, for example, 1:3, 1:5, 1:7, 1:10, 1:12, 1:14, or 1: 15. The total amount of the metal salt herein means the total amount of the nickel salt and the cobalt salt.
In the method of the present invention, the total concentration of the metal elements in the mixed solution is 5mmol/L to 60 mmol/L, for example, 5mmol/L, 10mmol/L, 20mmol/L, 30 mmol/L, 40 mmol/L, 50 mmol/L or 60 mmol/L. The total concentration of the metal element herein means the total concentration of the nickel element and the cobalt element.
The invention provides a preparation method of an ultrathin two-dimensional nanosheet layer NiCo-MOF material, which is characterized in that by regulating the addition amounts of nickel salt and cobalt salt and the molar ratio of the nickel salt and the cobalt salt, metal salt and an imidazole compound are subjected to coordination to form two-dimensional flaky MOF. The material is used as an electrode material of a super capacitor, and shows good conductivity, cycling stability and high specific capacitance.
The method is simple, has strong controllability and is suitable for industrial production.
As a preferable technical scheme of the method, the molar ratio of the nickel element to the cobalt element is 1: 0.5-3, the molar ratio of the total amount of the metal salt and the imidazole compound in the step (1) is 1: 3-10, and the total concentration of the metal element in the mixed solution in the step (1) is 10 mmol/L-20 mmol/L.
In the present invention, the kind of the nickel salt and the cobalt salt is not particularly limited, and for example, the nickel salt may be selected from any one of nickel nitrate, nickel chloride, nickel oxalate or nickel sulfate or a combination of at least two thereof. The cobalt salt may be selected from any one of cobalt nitrate, cobalt chloride, cobalt oxalate or cobalt sulfate or a combination of at least two thereof.
Preferably, the imidazole compound in step (1) is selected from any one or a combination of at least two of 2-methylimidazole, 2-butylimidazole, 1-ethylimidazole, 1-methylimidazole and 1-imidazoleacetic acid.
As a preferred technical scheme of the method of the invention, the mixed solution in the step (1) is prepared according to the following method:
(a) dissolving nickel salt and cobalt salt in water, and performing ultrasonic dispersion to obtain a metal salt solution; dissolving an imidazole compound in water, and performing ultrasonic dispersion to obtain an imidazole solution;
(b) and adding the imidazole solution into the metal salt solution, and continuing to perform ultrasonic dispersion until the mixture is uniformly mixed.
It should be noted that the preparation of the metal salt solution and the preparation of the imidazole solution in step (a) are not in sequence.
In order to achieve a better mixing effect, preferably, in the preparation process of the metal salt solution and the imidazole solution in the step (a), the ultrasonic dispersion time is independently 10min to 30min, for example, 10min, 12min, 15min, 20min, 25min or 30 min; the ultrasonic dispersion time in the step (b) is 10 min-30 min, such as 10min, 15min, 20min, 25min or 30 min.
Preferably, the temperature of the hydrothermal reaction in the step (2) is 70 ℃ to 170 ℃, such as 70 ℃, 80 ℃, 100 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃ or 170 ℃, and the like, and preferably 110 ℃ to 150 ℃.
Preferably, the hydrothermal reaction time in the step (2) is 4h to 12h, such as 4h, 5h, 6h, 7h, 8h, 9h, 10h, 11h or 12 h.
In the method, the composition, the morphology and the like of the prepared metal organic framework material can be regulated and controlled by regulating the proportion and the reaction conditions among reactants, so that the ultrathin two-dimensional nano flaky NiCo-MOF is obtained.
Preferably, the drying of step (2) is vacuum drying or freeze drying. The temperature of the vacuum drying is 60-100 ℃, such as 60 ℃, 65 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃ and the like. The drying time is 12 h-24 h, such as 12h, 13h, 14h, 16h, 18h, 20h, 21h, 22h or 24 h.
In the method of the present invention, optionally, the reaction product is washed before drying in step (2).
Preferably, the washing employs a detergent comprising water and/or ethanol.
As a further preferred technical solution of the method of the present invention, the method comprises the steps of:
(1) dissolving nickel salt and cobalt salt in water, and performing ultrasonic dispersion to obtain a metal salt solution; dissolving an imidazole compound in water, and performing ultrasonic dispersion to obtain an imidazole solution;
(2) quickly pouring the dissolved imidazole into a metal salt solution, and continuously performing ultrasonic dispersion for 10-30 min until the imidazole is uniformly mixed to obtain a mixed solution;
(3) transferring the uniform mixed solution obtained in the step (2) into a polytetrafluoroethylene lined reaction kettle, reacting at the high temperature of 70-170 ℃ for 4-12 h, separating, washing and drying to obtain NiCo-MOF;
the drying is vacuum drying or freeze drying, the temperature of the vacuum drying is 60-100 ℃, the time is 12-24 hours, and the freeze drying time is 12-24 hours.
In a second aspect, the invention provides the ultrathin two-dimensional nano flaky NiCo-MOF prepared by the method in the first aspect, the flaky structure is a hexagonal structure with a sheet diameter of 50 nm-200 nm (sheet diameter such as 50nm, 60nm, 80nm, 100nm, 110nm, 120nm, 135nm, 150nm, 160nm, 180nm or 200nm and the like) formed by bonding Ni and Co with 2-methylimidazole, and the thickness is less than 10nm (thickness such as 9.5nm, 8nm, 7nm, 6nm or 5nm and the like), and the plane has an expanded two-dimensional pi-conjugation and graphene-like structure, so that the ultrathin two-dimensional nano flaky NiCo-MOF is more favorable for electron transmission.
In a third aspect, the invention provides a use of the ultra-thin two-dimensional nano-platelet NiCo-MOF of the second aspect for a supercapacitor electrode material.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of an ultrathin two-dimensional nanosheet layer NiCo-MOF material, which is characterized in that by regulating the addition amounts of nickel salt and cobalt salt and the molar ratio of the nickel salt and the cobalt salt, metal salt and an imidazole compound are subjected to coordination to form two-dimensional flaky MOF. The material is used as an electrode material of a super capacitor, and has good conductivity, cycling stability and high specific capacitance.
Drawings
FIGS. 1 and 2 are the scanning and transmission electron microscope images of the ultrathin two-dimensional nano flaky NiCo-MOF obtained in example 1, respectively.
FIG. 3 shows the result of constant current charge and discharge test, wherein the lines in the figure are sequentially the charge and discharge changes under the condition that the current density is 0.5-5A/g.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Example 1
The embodiment provides a preparation method of an ultrathin two-dimensional nanosheet layer NiCo-MOF material, which comprises the following steps:
(1) mixing Ni (NO)3)2•6H2O and Co (NO)3)2•6H2Dissolving O in 35ml of water to obtain a mixed metal salt solution; dissolving 2-methylimidazole in 35ml of water to obtain an imidazole solution;
and respectively putting the mixed metal salt solution and the imidazole solution into an ultrasonic cleaner, and performing ultrasonic dispersion for 15min until the mixed metal salt solution and the imidazole solution are completely dissolved.
(2) And quickly pouring the dissolved 2-methylimidazole into the mixed metal salt solution, and continuously performing ultrasonic dispersion for 15min until the mixture is uniformly mixed.
(3) And transferring the mixed solution into a 100 ml polytetrafluoroethylene-lined reaction kettle, reacting for 4h at the temperature of 150 ℃, separating, washing and drying in vacuum at the temperature of 80 ℃ for 12h to obtain NiCo-MOF.
In this example, Ni (NO)3)2•6H2O and Co (NO)3)2•6H2The molar ratio of O to trimesic acid is 2:1, the molar ratio of the total amount of the metal salt to trimesic acid is 1:3.5, and the mixed solution obtained in the step (2)The concentration of Ni + Co element in the alloy is 15.7 mmol/L.
FIGS. 1 and 2 are scanning and transmission electron microscope images of the ultrathin two-dimensional nano flaky NiCo-MOF obtained in example 1, and it can be seen from the images that the ultrathin two-dimensional nano flaky NiCo-MOF is obtained, the flaky structure is a hexagonal structure with a sheet diameter of 50 nm-200 nm formed by bonding Ni, Co and 2-methylimidazole, the thickness is less than 10nm, and the plane has an expanded two-dimensional pi-conjugation and graphene-like structure, so that electron transmission is facilitated.
Example 2
The embodiment provides a preparation method of an ultrathin two-dimensional nanosheet layer NiCo-MOF material, which comprises the following steps:
(1) mixing Ni (NO)3)2•6H2O and Co (NO)3)2•6H2Dissolving O in 35ml of water to obtain a mixed metal salt solution; dissolving 2-methylimidazole in 35ml of water to obtain an imidazole solution;
and respectively putting the mixed metal salt solution and the imidazole solution into an ultrasonic cleaner, and performing ultrasonic dispersion for 30min until the mixed metal salt solution and the imidazole solution are completely dissolved.
(2) And quickly pouring the dissolved 2-methylimidazole into the mixed metal salt solution, and continuously performing ultrasonic dispersion for 30min until the mixture is uniformly mixed.
(3) And transferring the mixed solution into a 100 ml polytetrafluoroethylene-lined reaction kettle, reacting for 10h at the temperature of 100 ℃, separating, washing and drying in vacuum at the temperature of 80 ℃ for 12h to obtain NiCo-MOF.
In this example, Ni (NO)3)2•6H2O and Co (NO)3)2•6H2The molar ratio of O is 1:1, the molar ratio of the total amount of the metal salt to the trimesic acid is 1:7, and the concentration of the Ni + Co element in the mixed solution obtained in the step (2) is 15.7 mmol/L.
Example 3
This example differs from example 1 only in that the reaction temperature is 70 ℃ and the other conditions and parameters are exactly the same as in example 1.
Example 4
This example differs from example 1 only in that the reaction temperature is 170 ℃ and the other conditions and parameters are exactly the same as in example 1.
Example 5
This example is different from example 1 only in that the concentration of Ni + Co element in the mixed solution obtained in step (2) was 5 mmol/L.
Example 6
This example is different from example 1 only in that the concentration of Ni + Co element in the mixed solution obtained in step (2) was 20 mmol/L.
Comparative example 1
This comparative example differs from example 1 only in that the addition of Ni (NO) is not included in step (1)3)2•6H2O, other conditions and parameters were exactly the same as those in example 1.
Comparative example 2
This comparative example differs from example 1 only in that the amount of imidazole added was changed so that the molar ratio of the total amount of metal salt and imidazole was 1: 0.3.
Comparative example 3
This comparative example differs from example 1 only in that the amount of imidazole added was changed so that the molar ratio of the total amount of metal salt and imidazole was 1: 20.
And (3) performance testing:
and mixing the obtained ultrathin two-dimensional nano flaky NiCo-MOF, Polytetrafluoroethylene (PTFE) and acetylene black according to the mass ratio of 8:1:1, and pressing and forming an electrode on a foamed nickel current collector. A three-electrode system with a Pt sheet as a counter electrode and Hg/HgO as a reference electrode is adopted, Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and alternating current impedance (EIS) tests are respectively carried out on an electrochemical workstation, and the specific capacitance retention rate after 1000 cycles under the current density of 1A/g are calculated according to the test results (the results are shown in Table 1).
FIG. 3 shows the result of constant current charge and discharge test, wherein the lines in the figure are sequentially the charge and discharge changes under the condition that the current density is 0.5-5A/g. TABLE 1
| Specific capacitance (F/g) | Specific capacity retention (%) | |
| Example 1 | 1002 | 95.2 |
| Example 2 | 860 | 94.7 |
| Example 3 | 560 | 93.0 |
| Example 4 | 820 | 93.8 |
| Example 5 | 883 | 91.5 |
| Example 6 | 791 | 92.6 |
| Comparative example 1 | 62 | 92.2 |
| Comparative example 2 | 100 | 63.7 |
| Comparative example 3 | 330 | 85.9 |
As can be seen from the comparison between example 1 and examples 3-4, the temperature of the hydrothermal reaction affects the performance of the product, the reaction temperature affects the formation and growth of MOF crystal nuclei, and further affects the formation of ordered lamellar NiCo-MOF structures, and the ordered lamellar NiCo-MOF structures affect the storage and transfer of charges in the electrochemical process and the stability of the structures, resulting in differences in specific capacitance and cycling performance.
From the comparison between example 1 and examples 5-6, the concentration of Ni + Co element in the mixed solution obtained in step (2) affects the composition and morphology of the product obtained by the reaction, thereby causing differences in specific capacitance and cycle performance.
As can be seen from the comparison between example 1 and comparative example 1, in the electrochemical reaction, compared with Co-MOF containing no metal Ni, the electrochemical performance of the ultrathin two-dimensional nano flaky NiCo-MOF is obviously enhanced, and is mainly attributed to the synergistic transfer among NiCo ions.
As can be seen from the comparison of example 1 and comparative examples 2-3, the amount of imidazole added should be controlled within a suitable range to ensure stable MOF precursor formation.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of an ultrathin two-dimensional nanosheet layer NiCo-MOF material for a supercapacitor electrode, the method comprising the steps of:
(1) dissolving nickel salt, cobalt salt and imidazole compound in water to obtain a mixed solution; the molar ratio of the nickel element to the cobalt element is 1: 0.2-5, the molar ratio of the total amount of the metal salt to the imidazole compound is 1: 2-15, and the total concentration of the metal elements in the mixed solution is 5 mmol/L-60 mmol/L;
(2) and carrying out hydrothermal reaction on the mixed solution, separating a reaction product, and drying to obtain the NiCo-MOF material.
2. The method according to claim 1, wherein the molar ratio of nickel element to cobalt element is 1: 0.5-3, the molar ratio of the total amount of the metal salt to the imidazole compound in step (1) is 1: 3-10, and the total concentration of the metal elements in the mixed solution in step (1) is 10 mmol/L-20 mmol/L.
3. The method according to claim 1, wherein the imidazole compound in step (1) is selected from any one or a combination of at least two of 2-methylimidazole, 2-butylimidazole, 1-ethylimidazole, 1-methylimidazole and 1-imidazoleacetic acid.
4. The method according to claim 1, wherein the mixed solution of step (1) is prepared by the following method:
(a) dissolving nickel salt and cobalt salt in water, and performing ultrasonic dispersion to obtain a metal salt solution; dissolving an imidazole compound in water, and performing ultrasonic dispersion to obtain an imidazole solution;
(b) and adding the imidazole solution into the metal salt solution, and continuing to perform ultrasonic dispersion until the mixture is uniformly mixed.
5. The method according to claim 1, wherein the temperature of the hydrothermal reaction in the step (2) is 70 ℃ to 170 ℃, and the time of the hydrothermal reaction in the step (2) is 4h to 12 h.
6. The method according to claim 5, wherein the temperature of the hydrothermal reaction in the step (2) is 110-150 ℃.
7. The method according to claim 1, wherein the drying in the step (2) is vacuum drying or freeze drying, the temperature of the vacuum drying is 60 ℃ to 100 ℃, and the drying time is 12h to 24 h.
8. Method according to claim 1, characterized in that it comprises the following steps:
(1) dissolving nickel salt and cobalt salt in water, and performing ultrasonic dispersion to obtain a metal salt solution; dissolving an imidazole compound in water, and performing ultrasonic dispersion to obtain an imidazole solution;
(2) quickly pouring the dissolved imidazole into a metal salt solution, and continuously performing ultrasonic dispersion for 10-30 min until the imidazole is uniformly mixed to obtain a mixed solution;
(3) transferring the uniform mixed solution obtained in the step (2) into a polytetrafluoroethylene lined reaction kettle, reacting at the high temperature of 70-170 ℃ for 4-12 h, separating, washing and drying to obtain NiCo-MOF;
the drying is vacuum drying or freeze drying, the temperature of the vacuum drying is 60-100 ℃, the time is 12-24 hours, and the freeze drying time is 12-24 hours.
9. An ultrathin two-dimensional nano flaky NiCo-MOF prepared by the method of any one of claims 1 to 8, wherein the flaky structure is a hexagonal structure with a sheet diameter of 50-200nm and a thickness of less than 10nm, and is formed by bonding Ni and Co with 2-methylimidazole.
10. Use of the ultra-thin two-dimensional, nano-platelet NiCo-MOF of claim 9, for a supercapacitor electrode material.
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| CN114743802A (en) * | 2022-05-19 | 2022-07-12 | 江苏大学 | Wide-temperature-zone supercapacitor electrode material, wide-temperature-zone supercapacitor electrode device and preparation method of wide-temperature-zone supercapacitor electrode material |
| CN114907574A (en) * | 2022-06-14 | 2022-08-16 | 浙江理工大学 | Shape-controllable metal-organic framework material and preparation method and application thereof |
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