CN115785464A - Preparation method and application of electrode material Ln(s) -Co compound of super capacitor - Google Patents
Preparation method and application of electrode material Ln(s) -Co compound of super capacitor Download PDFInfo
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Abstract
The invention belongs to the field of functional material preparation, and particularly relates to a preparation method and application of a supercapacitor electrode material Ln(s) -Co compound, which are implemented according to the following steps: (1) Putting pyridine 2,5-dicarboxylic acid, rare earth nitrate and cobalt nitrate into a reaction kettle, adding deionized water, and stirring at room temperature; (2) Transferring the product obtained in the step (1) to an oven for constant temperature treatment; (3) Naturally cooling the product obtained in the step (2) to room temperature, washing with deionized water and ultrasonically cleaning, and then filtering to obtain mauve acicular crystals; drying under natural conditions to obtain the Ln(s) -Co-MOF material. (4) And (4) calcining the product obtained in the step (3) under the protection of inert gas to obtain the Ln(s) -Co compound which can be used for the electrode of the super capacitor. The method has good reproducibility, the target product has ideal shape and structure, and the performance of the electrode active material used as the super capacitor is excellent.
Description
Technical Field
The invention belongs to the field of functional material preparation, and particularly relates to a preparation method and application of an electrode material Ln(s) -Co compound of a super capacitor.
Background
The super capacitor has the advantages of long cycle life, high power density, short charging and discharging time, wide working temperature range and the like, promotes the development of new energy industry, and obtains relatively rapid development in the field of energy storage, particularly the field of electric vehicles. At present, the electrode materials of supercapacitors are mainly based on carbon materials, transition metal oxides and conductive polymers. However, many reported materials have disadvantages in terms of size, microstructure, stability, etc. Making conventional materials limited in application.
Metal Organic Frameworks (MOFs) draw attention of researchers due to their advantages such as specific two-dimensional and three-dimensional morphologies, adjustable framework structures, large specific surface areas, active sites which are beneficial to electrolyte transportation and ion transmission, and the like, and complex-derived materials which can maintain the original framework of complexes or undergo phase transition in situ. The complex and the derivative material thereof are used as one of candidate substances applied to sustainable energy, and are developed rapidly. The method is applied to the aspect of the super capacitor at present.
In recent years, MOF materials have been widely used as supercapacitor electrode materials due to their high specific surface area, adjustable pore size distribution, and adjustable composition and morphology. However, MOF materials suffer from more problems in practical applications, such as: (1) The MOF framework is easy to collapse and has obvious volume effect in the charging and discharging processes; (2) The MOF material has poor conductivity, so that the transmission performance of electrons is restricted; (3) The morphology of the derivative prepared from the MOF material is not controllable, or the specific surface is reduced after sintering. This has somewhat hindered their use in the field of electrochemistry.
Disclosure of Invention
In order to solve the problems of the prior MOF materials mentioned above, the invention mainly aims to invent an electrode material which has high specific capacity, good cycling stability and stable structure and can be used for a super capacitor. The product of the invention also highlights a technical highlight, namely the product structure at the conventional calcination temperature (450-600 ℃) is found to keep the original framework structure in the process of preparing the derivative. But the phase change occurs in a high-temperature narrow region (750-800 ℃), and the phase change product has excellent electrochemical performance and can be applied as an ideal electrode material of a super capacitor. The product from continued heating thereafter is still understood to be a collapsed fouling zone of the conventional framework.
In order to solve the technical problem, the invention is realized as follows:
a preparation method of a supercapacitor electrode material Ln(s) -Co compound is implemented according to the following steps:
(1) Putting pyridine 2,5-dicarboxylic acid, rare earth nitrate and cobalt nitrate into a reaction kettle, adding deionized water, and stirring at room temperature;
(2) Transferring the product obtained in the step (1) to an oven for constant temperature treatment;
(3) Naturally cooling the product obtained in the step (2) to room temperature, washing with deionized water and ultrasonically cleaning, and then filtering to obtain mauve acicular crystals; drying under natural conditions to obtain an Ln(s) -Co-MOF material;
(4) And (4) calcining the product obtained in the step (3) under the protection of inert gas to obtain the target product, namely the electrode material Ln(s) -Co compound of the super capacitor.
Further, the rare earth nitrate is cerium nitrate, praseodymium nitrate, neodymium nitrate, samarium nitrate, europium nitrate, gadolinium nitrate or holmium nitrate.
Further, in the step (1) of the present invention, the pyridine 2,5-dicarboxylic acid, the rare earth nitrate, the cobalt nitrate and the deionized water are sequentially in a mass ratio of: 0.3 to 0.4:0.25 to 0.3:0.15 to 0.2:10 to 12.
Further, in the step (2), the preheating temperature of the oven is 180-190 ℃; the constant temperature is 180-190 ℃; the constant temperature time is 55-60 h.
Further, in the step (3), the product obtained in the step (2) is washed with deionized water for 2-3 times, and dried for 10-12 hours under natural conditions, so that the preparation method of the Ln(s) -Co-MOF is obtained.
Further, in the step (4) of the invention, the calcination temperature is 750-800 ℃; the constant temperature time is 1.5-2 h.
The application of the product obtained by the preparation method of the electrode material Ln(s) -Co composite of the super capacitor in the aspect of the electrode of the super capacitor is implemented according to the following steps: fully grinding the Ln(s) -Co compound, polyvinylidene fluoride, conductive acetylene black and N-methyl pyrrolidone to obtain electrode slurry of the super capacitor; and uniformly coating the electrode slurry of the super capacitor on foamed nickel to obtain an electrode plate, and drying, cooling and slicing to obtain the test electrode of the super capacitor.
Further, the mass ratio of the Ln(s) -Co compound, the conductive acetylene black and the polyvinylidene fluoride is as follows in sequence: 5 to 8:1 to 3:0.5 to 2.
Further, the electrode slice is dried for 10 to 13 hours in a vacuum drying oven of 0.1Mpa at the temperature of between 80 and 110 ℃.
Furthermore, in the test of the super capacitor, the adopted electrolyte is a KOH solution with the concentration of 3-6M.
The rare earth lanthanide (Ln (s)) has the characteristic of performance gradient, and when the rare earth lanthanide is used in the electrode material of the super capacitor, the volume effect in the charge-discharge process can be reduced, and the performance of the super capacitor can be effectively improved. The rare earth-transition metal bimetal MOF material derivative not only has more active sites, but also can make full use of the respective characteristics of the bimetal, thereby improving the performance of the super capacitor. Rare earth-transition metal bimetallic MOF materials (Ln(s) -Co-MOF) are less reported, while derivatives prepared on this basis (Ln(s) -Co complexes) are rare.
The invention adopts pyridine 2,5-diThe synthesized material Ln(s) -Co-MOF is stable in structure and is a precursor of the electrode material of the super capacitor with a novel structure. The Ln(s) -Co compound prepared by taking Ln(s) -Co-MOF as a precursor has multiple active sites and a special structure, and the material is made into a super capacitor electrode material for electrochemical test, so that excellent electrochemical performance is shown. When the current density is 2 A.g -1 1440F. G was shown -1 The specific capacity of (A). At 20A. G -1 After 2000 cycles of current density, the capacitance is more than 88.5% of the initial capacitance.
Drawings
The invention is further described with reference to the following figures and detailed description. The scope of the invention is not limited to the following expressions.
FIG. 1 is a crystal morphology diagram of Ln(s) -Co-MOF under an optical microscope of the invention;
FIG. 2 is a graph of the pyrolysis of Ln(s) -Co-MOF according to the invention;
FIG. 3 is an SEM representation of Ln(s) -Co composite of the present invention;
FIG. 4 is a diagram of constant current charge and discharge of the Ln(s) -Co complex of the present invention;
FIG. 5 is a graph showing the cycle profile of Ln(s) -Co composite of the present invention.
Detailed Description
As shown, the electrode active material Ln(s) -Co composite, conductive acetylene black, and polyvinylidene fluoride (PVDF) were mixed at a ratio of 7:2:1, and then adding a proper amount of solvent N-methyl pyrrolidone (NMP). The mixture was thoroughly ground to form a uniform paste. The paste slurry was then coated on nickel foam and dried in a vacuum (0.1 MPa) oven at 80 ℃ for 12 hours from the nickel foam coated with the active material. After cooling to room temperature, the nickel foam coated with active material was removed from the oven. During electrochemical testing, the nickel foam coated with active material was cut to 1 x 2cm 2 Then accurately weighing the electrode using a one-ten-thousandth balance. The reaction was then carried out on an electrochemical workstation of the model CHI660, using a platinum plate as counter electrode, a reference electrode as Hg/HgO electrode, and 6M as KOH as electrolyte. Interval of charging and discharging voltage0-0.5V, room temperature, charge and discharge test of 2000 circles, initial discharge capacity of 1232F g -1 When the current density is 20A · g -1 After 2000 cycles of the experiment, the capacitance of the Ln(s) -Co composite remained well at 88.5% of the initial capacitance (the experimental results are shown in FIG. 5).
Example 1
The preparation method of the Ln(s) -Co compound is implemented according to the following steps:
the method comprises the following steps: 0.2g of Co (NO) 3 ) 2 ·6H 2 O, 0.250g Ce (NO) 3 ) 3 ·6H 2 O, 2,5-Pda of 0.3g and 11.0g H 2 O is added into a stainless steel reaction kettle with a polytetrafluoroethylene lining. Stirring for 3h at room temperature, sealing the reaction kettle, transferring to an oven preheated to 180 ℃, and keeping the temperature of 180 ℃ for 55h. Naturally cooling the oven to room temperature, washing the solid product with deionized water (100 mL) for 3 times, ultrasonically cleaning, filtering to obtain mauve acicular crystals, and drying under natural environment conditions to obtain the Ln(s) -Co-MOF material.
Step two: taking Ln(s) -Co-MOF material as a precursor, and in a vacuum tube furnace at 3 ℃ for min under the atmosphere of nitrogen -1 The temperature rise rate of (2) was adjusted from the internal temperature to 750 ℃ and 2h was maintained at this temperature, and a sample was collected to obtain an Ln(s) -Co composite.
Step three: the application of the Ln(s) -Co compound in the super capacitor is implemented according to the following steps: electrode active material Ln(s) -Co composite, conductive acetylene black and polyvinylidene fluoride (PVDF) were mixed at a ratio of 7:2:1, and then adding a proper amount of solvent N-methyl pyrrolidone (NMP). The mixture was thoroughly ground to form a uniform paste. The paste slurry was then coated on nickel foam and dried in a vacuum (0.1 MPa) oven at 80 ℃ for 12 hours from the nickel foam coated with the active material. After cooling to room temperature, the nickel foam coated with active material was removed from the oven. Cutting foamed nickel coated with active material into 1X 2cm 2 Then accurately weigh the electrode using a one-ten-thousandth balance.
Step four: electrochemical performance tests were performed on a CHI660 electrochemical workstation using a platinum sheet as the counter electrode, a Hg/HgO electrode as the reference electrode, and 6M KOH as the electrolyte.
Example 2
The preparation method of the Ln(s) -Co compound is implemented according to the following steps:
the method comprises the following steps: 0.2g of Co (NO) 3 ) 2 ·6H 2 O, 0.250g Ce (NO) 3 ) 3 ·6H 2 O, 2,5-Pda of 0.3g and 11.0g H 2 O is added into a stainless steel reaction kettle with a polytetrafluoroethylene lining. Stirring for 3h at room temperature, sealing the reaction kettle, transferring to an oven preheated to 180 ℃, and keeping the temperature of 180 ℃ for 55h. Naturally cooling the oven to room temperature, washing the solid product with deionized water (100 mL) for 3 times, ultrasonically cleaning, filtering to obtain mauve needle crystals, and drying under natural environment to obtain the Ln(s) -Co-MOF material.
Step two: taking Ln(s) -Co-MOF material as a precursor, and in a vacuum tube furnace at 3 ℃ for min under the atmosphere of nitrogen -1 The temperature rise rate of (2) was from the internal temperature to 800 ℃ and maintained at this temperature for 1.5 hours, and a sample was collected to obtain an Ln(s) -Co complex.
Step three: the application of the Ln(s) -Co compound in the super capacitor is implemented according to the following steps: electrode active material Ln(s) -Co composite, conductive acetylene black and polyvinylidene fluoride (PVDF) were mixed at a ratio of 7:2:1, and then adding a proper amount of solvent N-methyl pyrrolidone (NMP). The mixture was thoroughly ground to form a uniform paste. The paste slurry was then coated on nickel foam and dried in a vacuum (0.1 MPa) oven at 80 ℃ for 12 hours from the nickel foam coated with the active material. After cooling to room temperature, the nickel foam coated with active material was removed from the oven. Cutting foamed nickel coated with active material into 1X 2cm 2 Then accurately weighing the electrode using a one-ten-thousandth balance.
Step four: electrochemical performance tests were performed on a CHI660 type electrochemical workstation using a platinum sheet as the counter electrode, a Hg/HgO electrode as the reference electrode, and 6M KOH as the electrolyte.
Example 3
The preparation method of the Ln(s) -Co compound is implemented according to the following steps:
the method comprises the following steps: 0.2g of Co (NO) 3 ) 2 ·6H 2 O, 0.3g of Pr (NO) 3 ) 3 ·6H 2 O, 2,5-Pda at 0.350 g and H at 12.0g 2 O is added into a stainless steel reaction kettle with a polytetrafluoroethylene lining. Stirring for 3h at room temperature, sealing the reaction kettle, transferring to an oven preheated to 180 ℃, and keeping the temperature at 180 ℃ for 60h. Naturally cooling the oven to room temperature, washing the solid product with deionized water (100 mL) for 3 times, ultrasonically cleaning, filtering to obtain mauve acicular crystals, and drying under natural environment conditions to obtain the Ln(s) -Co-MOF material.
Step two: taking Ln(s) -Co-MOF material as a precursor, and in a vacuum tube furnace at 3 ℃ for min under the atmosphere of nitrogen -1 The temperature rise rate of (2) was increased from the internal temperature to 800 ℃ and maintained at the internal temperature for 2 hours, and a sample was collected to obtain an Ln(s) -Co complex.
Step three: the application of the Ln(s) -Co compound in the super capacitor is implemented according to the following steps: electrode active material Ln(s) -Co composite, conductive acetylene black and polyvinylidene fluoride (PVDF) were mixed at a ratio of 7:2:1, and then adding a proper amount of solvent N-methyl pyrrolidone (NMP). The mixture was thoroughly ground to form a uniform paste. The paste slurry was then coated on nickel foam and dried in a vacuum (0.1 MPa) oven at 80 ℃ for 12 hours from the nickel foam coated with the active material. After cooling to room temperature, the nickel foam coated with active material was removed from the oven. The nickel foam coated with active material was cut into 1 x 2cm 2 pieces and the electrodes were accurately weighed using a one-ten-thousandth balance.
Step four: a platinum sheet is used as a counter electrode, an Hg/HgO electrode is used as a reference electrode, 6M KOH is used as electrolyte, and electrochemical performance test is carried out on a CHI660 type electrochemical workstation.
The test result is that when the current density is 2 A.g -1 1440F. G was shown -1 The specific capacity of (A). At 20A. G -1 After 2000 cycles of current density, the capacitance is initialAnd the capacitance is more than 88.5 percent.
It will be apparent to those skilled in the art that other various modifications and variations can be made in the technical spirit of the present invention, and all such modifications and variations are intended to fall within the scope of the appended claims.
Claims (10)
1. A preparation method of an electrode material Ln(s) -Co compound of a super capacitor is characterized by comprising the following steps:
(1) Putting pyridine 2,5-dicarboxylic acid, rare earth nitrate and cobalt nitrate into a reaction kettle, adding deionized water, and stirring at room temperature;
(2) Transferring the product obtained in the step (1) to an oven for constant temperature treatment;
(3) Naturally cooling the product obtained in the step (2) to room temperature, washing with deionized water and ultrasonically cleaning, and then filtering to obtain mauve acicular crystals; drying under natural conditions to obtain an Ln(s) -Co-MOF material;
(4) And (4) calcining the product obtained in the step (3) under the protection of inert gas to obtain the target product, namely the electrode material Ln(s) -Co compound of the super capacitor.
2. The method for preparing the electrode material Ln(s) -Co composite of the supercapacitor as claimed in claim 1, wherein: the rare earth nitrate is cerium nitrate, praseodymium nitrate, neodymium nitrate, samarium nitrate, europium nitrate, gadolinium nitrate or holmium nitrate.
3. The method for preparing the electrode material Ln(s) -Co composite of the supercapacitor as claimed in claim 2, wherein: in the step (1), the pyridine 2,5-dicarboxylic acid, the rare earth nitrate, the cobalt nitrate and the deionized water are sequentially in the mass ratio: 0.3 to 0.4:0.25 to 0.3:0.15 to 0.2:10 to 12.
4. The method for preparing the electrode material Ln(s) -Co composite of the supercapacitor as claimed in claim 3, wherein: in the step (2), the preheating temperature of the oven is 180-190 ℃; the constant temperature is 180-190 ℃; the constant temperature time is 55-60 h.
5. The method for preparing the electrode material Ln(s) -Co composite of the supercapacitor as claimed in claim 4, wherein: and (3) washing the product obtained in the step (2) with deionized water for 2-3 times, and drying for 10-12 h under natural conditions to obtain the preparation method of the Ln(s) -Co-MOF.
6. The method for preparing the electrode material Ln(s) -Co composite of the supercapacitor as claimed in claim 5, wherein: in the step (4), the calcining temperature is 750-800 ℃; the constant temperature time is 1.5-2 h.
7. The application of the product obtained by the preparation method of the Ln(s) -Co composite of the electrode material of the super capacitor as claimed in the claims 1-6 in the aspect of the electrode of the super capacitor is characterized by comprising the following steps: fully grinding the Ln(s) -Co compound, polyvinylidene fluoride, conductive acetylene black and N-methyl pyrrolidone to obtain electrode slurry of the super capacitor; and uniformly coating the electrode slurry of the super capacitor on foamed nickel to obtain an electrode plate, and drying, cooling and slicing to obtain the test electrode of the super capacitor.
8. The application of the product obtained by the preparation method of the electrode material Ln(s) -Co compound of the supercapacitor according to claim 7 in the aspect of electrodes of the supercapacitor is characterized in that: the mass ratio of the Ln(s) -Co compound to the conductive acetylene black to the polyvinylidene fluoride is as follows in sequence: 5 to 8:1 to 3:0.5 to 2.
9. The application of the product obtained by the preparation method of the electrode material Ln(s) -Co compound of the supercapacitor according to claim 8 in the aspect of electrodes of the supercapacitor is characterized in that: drying the electrode slice in a vacuum drying oven of 0.1Mpa at 80-110 ℃ for 10-13 h.
10. The application of the product obtained by the preparation method of the electrode material Ln(s) -Co compound of the supercapacitor in the aspect of electrodes of the supercapacitor is characterized in that: in the test of the super capacitor, the adopted electrolyte is a KOH solution with the concentration of 3-6M.
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