CN114284082B - Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano-sheet - Google Patents
Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano-sheet Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet, and belongs to the field of preparation of super capacitor electrode materials. The preparation method of the rare earth doped cobaltosic oxide nano-sheet comprises the following steps: weighing a certain amount of cobalt nitrate hexahydrate and rare earth soluble salt, and dissolving the cobalt nitrate hexahydrate and the rare earth soluble salt in a mixed solvent of water and glycol to obtain a mixed solution A; weighing urea, dissolving the urea in the mixed solution A, and uniformly stirring to obtain a solution B; reacting the obtained solution B at 80-90 ℃ for 8-12h, naturally cooling to room temperature, centrifugally separating the obtained product, washing and drying to obtain a rare earth doped tricobalt tetraoxide precursor; and (3) placing the obtained precursor into a muffle furnace for calcination, and obtaining the final product rare earth doped cobaltosic oxide nano-sheet after the calcination is finished. The material obtained by the method has excellent capacitance performance and can be used for super capacitor electrode materials.
Description
Technical Field
The invention relates to the field of preparation of supercapacitor electrode materials, in particular to a preparation method and application of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet.
Background
The advantages of rapid charge and discharge, very long service life and the like of the super capacitor are brought into the attention of extensive scientific researchers. High performance supercapacitor electrode materials are primarily concerned with carbonaceous materials, metal oxides, conductive polymers and composites related thereto. Among these active materials, transition metal oxides exhibit excellent capacitive properties due to their unique crystal structure, multiple metal ion valence states, rapid redox reactions or ion insertion reactions, and are considered to be very promising pseudocapacitive materials. However, transition metal oxides have extremely poor intrinsic conductivity and slow reaction kinetics, which greatly limit research and application of transition metal oxides as electrode materials in the field of high-efficiency energy storage.
Co 3 O 4 The electrode material has the characteristics of high theoretical specific capacitance, low cost, no pollution and the like, and becomes a popular choice for electrode materials. However, the advantage of the capacitive properties is hardly exerted due to its extremely poor electrical conductivity. Rare earth doping is a way to effectively improve the capacitive performance of transition metal oxides, and its main role is to influence the crystallization behavior and conductivity of transition metal oxides. At present, rare earth doped transition metal oxides are mainly zero-dimensional nano particles, one-dimensional nano wires, nano rods and nano tubes, and the preparation of two-dimensional nano sheets and capacitance research thereof have not been reported.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method and application of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides a preparation method of rare earth doped cobaltosic oxide nano-sheets, which is characterized by comprising the following steps:
step 1: a certain amount of cobalt nitrate hexahydrate Co (NO) is weighed 3 ) 2 ·6H 2 O and rare earth soluble salt are dissolved in 120mL of mixed solvent of water and glycol to obtain mixed solution A;
step 2: weighing urea, dissolving the urea in the mixed solution A, and uniformly stirring to obtain a solution B;
step 3: reacting the solution B obtained in the step 2 at 80-90 ℃ for 8-12h, naturally cooling to room temperature, centrifugally separating the obtained product, washing and drying to obtain a rare earth doped tricobalt tetraoxide precursor;
step 4: and (3) placing the precursor obtained in the step (3) in a muffle furnace for calcination, and obtaining the final product rare earth doped cobaltosic oxide nano-sheet after the calcination is finished.
Further, in the step 1, the rare earth soluble salt is a nitrate or chloride salt of lanthanum, cerium, neodymium, holmium, erbium, ytterbium or yttrium.
Preferably, the molar ratio of the cobalt nitrate hexahydrate to the rare earth soluble salt is 100:0.5-7.
Preferably, the volume ratio of the water to the glycol in the mixed solvent of the water and the glycol is 1:7.
Further, the molar ratio of cobalt nitrate hexahydrate to urea is 1:6.
Preferably, in the step 3, the drying temperature is 60 ℃ and the drying time is 6-12h.
Preferably, in the step 4, the calcination temperature is 300 ℃ and the calcination time is 2 hours; the programmed temperature rise rate of the muffle furnace is 10 ℃/min.
On the other hand, the invention also provides a rare earth doped cobaltosic oxide nano-sheet prepared by the method.
In still another aspect, the invention further provides an application of the rare earth doped cobaltosic oxide nano-sheet in an electrode material of a super capacitor.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts cobalt nitrate hexahydrate, urea and rare earth salts as raw materials and prepares the rare earth cobalt nitrate hexahydrate and the urea in a water-glycol mixed solvent system. The method has the advantages of easily available raw materials, low preparation cost, simple process and less pollution. The rare earth doped cobaltosic oxide nano-sheet with excellent capacitance performance prepared by rare earth ion doping has good application prospect of super capacitors.
Drawings
FIG. 1 is a surface topography of rare earth lanthanum doped tricobalt tetraoxide prepared in example 1;
FIG. 2 is a surface topography of rare earth cerium doped tricobalt tetraoxide prepared in example 2 (a); in a 6mol/LKOH solution, the sample of example 2 has a charge-discharge curve (b), a specific capacitance (c) and a charge-discharge curve at 32A g at different current densities -1 A cycling stability graph (d) at current density;
FIG. 3 is a surface topography of rare earth neodymium doped tricobalt tetraoxide prepared in example 3;
fig. 4 is a surface morphology diagram of rare earth holmium doped cobaltosic oxide prepared in example 4;
FIG. 5 is a surface topography of rare earth erbium-doped tricobalt tetraoxide prepared in example 5;
FIG. 6 is a surface topography of the rare earth ytterbium doped tricobalt tetraoxide prepared in example 6;
fig. 7 is a surface topography of rare earth yttrium doped tricobalt tetraoxide prepared in example 7.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
The materials and reagents used in the present invention are not specifically described and are commercially available.
The invention provides a preparation method and application of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet, and specific embodiments are as follows.
Example 1
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.2mmol of lanthanum nitrate hexahydrate are weighed and dissolved in 120mL of a mixed solvent of water and ethylene glycol (the ratio of water to ethylene glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth lanthanum doped cobaltosic oxide.
FIG. 1 is a surface topography of rare earth lanthanum doped tricobalt tetraoxide; from the figure, it can be seen that the sample has a good nanoplatelet morphology.
Example 2
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.2mmol of cerium nitrate hexahydrate are weighed and dissolved in 120mL of a mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the mixture is stirred uniformly to obtain a solution A. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product of rare earth cerium doped cobaltosic oxide.
As shown in figure 2a, the rare earth cerium doped cobaltosic oxide material has a nano-sheet structure on the surface, the thickness of the nano-sheet structure is 15-20nm, and the appearance is good. As shown in fig. 2b and c, electricityThe electrode material exhibits typical pseudocapacitive behavior at a current density of 2A.g -1 The capacitance value is 626 F.g -1 When the current density increases to 20 A.g -1 The specific capacitance was 256 F.g -1 As shown in fig. 2d, the capacity of the material is not attenuated under 4000 charge-discharge cycles.
Example 3
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.2mmol of neodymium nitrate hexahydrate are weighed and dissolved in 120mL of a mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth neodymium doped cobaltosic oxide.
FIG. 3 is a surface topography of rare earth neodymium doped tricobalt tetraoxide; from the figure, it can be seen that the sample has a good nanoplatelet morphology.
Example 4
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.15mmol of holmium nitrate pentahydrate are weighed and dissolved in 120mL of mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth holmium doped cobaltosic oxide.
Fig. 4 shows a surface topography of rare earth holmium doped cobaltosic oxide; from the figure it can be seen that the sample has a nanoplatelet morphology.
Example 5
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.15mmol of erbium nitrate pentahydrate are weighed and dissolved in 120mL of mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth erbium-doped cobaltosic oxide.
FIG. 5 is a surface topography of rare earth erbium doped tricobalt tetraoxide; from the figure, the sample has high refinement degree, and the nanometer scale is 50-100nm.
Example 6
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.15mmol of ytterbium nitrate pentahydrate are weighed and dissolved in 120mL of mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth ytterbium doped cobaltosic oxide.
FIG. 6 shows a surface topography of rare earth ytterbium doped tricobalt tetraoxide; from the figure, it can be seen that the sample has a good nanoplatelet morphology.
Example 7
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.2mmol of yttrium nitrate hexahydrate are weighed and dissolved in 120mL of a mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 20mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 12 hours at the temperature of 90 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth yttrium doped cobaltosic oxide.
FIG. 7 is a surface topography of rare earth yttrium doped tricobalt tetraoxide; the sample can be seen from the figure to be in a nano sheet shape, and has the characteristics of porosity and porosity.
Example 8
A preparation method of a high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano sheet comprises the following steps: 5mmol of cobalt nitrate hexahydrate and 0.25mmol of erbium nitrate pentahydrate are weighed and dissolved in 120mL of mixed solvent of water and glycol (the ratio of water to glycol is 1:7), and the solution A is obtained after uniform stirring. Weighing 30mmol of urea, dissolving in the solution A, and uniformly stirring to obtain a solution B; reacting the solution B for 10 hours at the temperature of 85 ℃ under the magnetic stirring condition, naturally cooling to room temperature, centrifugally separating the obtained product, washing the product with water and absolute ethyl alcohol for 3 times respectively, and drying the separated and washed solid at the temperature of 60 ℃ for 12 hours; and then carrying out heat treatment on the obtained solid for 2 hours at the temperature of 300 ℃, and heating a muffle furnace at the temperature of 10 ℃ per minute to obtain the final product rare earth erbium-doped cobaltosic oxide.
To further illustrate the beneficial effects of the present invention, the following comparative examples were constructed with limited space using example 2 only.
Comparative example 1
Cerium nitrate hexahydrate was omitted in this comparative example, and the other conditions were the same as in example 2.
Comparative example 2
In this comparative example, ethylene glycol was replaced with an equal amount of water, and the other conditions were the same as in example 2.
Comparative example 3
In this comparative example, water was replaced with an equal amount of ethylene glycol, and the other conditions were the same as in example 2.
Comparative example 4
In this comparative example urea was replaced with an equal amount of sodium hydroxide, the rest of the conditions being the same as in example 2.
The rare earth doped tricobalt tetraoxide nanosheet materials prepared in examples 1-9 and comparative examples 1-4 above were used as electrode materials for capacitive performance testing. The specific test method comprises the following steps:
1. pretreatment of nickel foam:
ultrasonic cleaning the nickel foam with 1M HCl for 3min once and then H 2 O and C 2 H 5 And respectively ultrasonically cleaning OH for 5min for several times, and drying in a vacuum oven at the constant temperature of 60 ℃ for 4-5h for standby.
2. Preparation of working electrode:
the samples (rare earth doped cobaltosic oxide), carbon powder (super.P) and binder (PVDF) prepared in examples 1-9 and comparative examples 1-4 are respectively weighed according to the mass ratio of 70-15% and 15%, mixed and ground, and then a little ethanol solution is added dropwise to stir into slurry, and the slurry is coated on the treated foam nickel. Carrying out nickel foam tabletting treatment under the conditions of 10MPa and 5min, and drying at the normal temperature of 60 ℃ for 5min.
3. Electrochemical performance test:
the test is carried out by adopting a one-chamber three-electrode electrochemical device with nickel foam coated with electrode materials as a working electrode, a platinum wire as a counter electrode and a saturated calomel electrode as a reference electrode, and the electrolyte is 6M KOH solution.
The rare earth doped cobaltosic oxide nanosheet materials prepared in the above examples 1 to 9 were used as electrode materials for capacitive performance testing, and the results are shown in table 1.
TABLE 1
As can be seen from Table 1, the rare earth doped cobaltosic oxide nano-sheet prepared by the invention has excellent capacitance performance under different current densities, and the capacity is almost not attenuated under the charge-discharge cycle condition of more than 4000 times. The method is simple, low in cost and less in pollution, and is suitable for industrial production.
The rare earth doped cobaltosic oxide nanosheet materials prepared in comparative examples 1 to 4 were used as electrode materials for capacitive performance testing, and the results are shown in table 2.
TABLE 2
As can be seen from table 2, the capacitance value of the pure tricobalt tetraoxide as an electrode material (comparative example 1) is significantly reduced compared with the present invention; this is because the rare earth is adopted to carry out doping modification on the cobaltosic oxide, so that the oxygen vacancy concentration and the specific surface area of the material can be greatly improved. The high-concentration oxygen vacancies can promote the transportation of electrons/ions, and accelerate the oxidation-reduction reaction process; the high specific surface area enables the material to expose more reactive sites, which is beneficial to the full contact between the material and electrolyte, improves the reaction rate and improves the capacitance performance of the material; in addition, the doped rare earth ions can also be used as reactive sites for Faraday reaction, so that the capacitance performance of the rare earth ions is further improved.
Meanwhile, the capacitance performance of rare earth doped cobaltosic oxide (comparative examples 2-3) prepared by different solvents is also greatly different from that of example 2. This is because in the preparation of the material using the single solvent system of comparative examples 2 to 3, it is difficult to obtain uniform and regular morphology of flaky tricobalt tetraoxide, resulting in a small specific surface area of the prepared material, which is unfavorable for contact of the electrode material with the electrolyte, and slows down the faraday reaction to some extent, so that high capacitance performance cannot be achieved.
In the process of preparing rare earth doped cobaltosic oxide (comparative example 4) by using sodium hydroxide as a precipitator, the strong alkaline condition causes the generation speed of cobalt hydroxide to be too high, the crystal growth process of the cobalt hydroxide is seriously influenced, serious agglomeration and stacking phenomena are caused, even the particle size of the final product is far beyond the nano level, and the reactive sites of the electrode are greatly reduced, so that the high capacitance performance cannot be achieved.
And the materials prepared in comparative examples 1-4 are used as electrodes, and the capacitance performance of the materials is greatly reduced when the cycle times are about 3000 times.
In conclusion, the invention adopts cobalt nitrate hexahydrate, urea and rare earth salts as raw materials, and the raw materials are prepared in a water-glycol mixed solvent system, so that the obtained rare earth doped cobaltosic oxide nano-sheet has excellent capacitance performance and has good application prospect in the field of super capacitors.
While the foregoing is directed to the preferred embodiments of the present invention, it will be apparent to those skilled in the art that various modifications and variations can be made without departing from the principles of the invention.
Claims (7)
1. The preparation method of the rare earth doped cobaltosic oxide nano sheet is characterized by comprising the following steps of:
step 1: weighing a certain amount of cobalt nitrate hexahydrate and rare earth soluble salt, and dissolving the cobalt nitrate hexahydrate and the rare earth soluble salt in a mixed solvent of water and glycol to obtain a mixed solution A; the rare earth soluble salt is nitrate of lanthanum, cerium, neodymium, holmium, erbium, ytterbium and yttrium; the mol ratio of the cobalt nitrate hexahydrate to the rare earth soluble salt is 100:0.5-7;
step 2: weighing urea, dissolving the urea in the mixed solution A, and uniformly stirring to obtain a solution B;
step 3: reacting the solution B obtained in the step 2 at 80-90 ℃ for 8-12h, naturally cooling to room temperature, centrifugally separating the obtained product, washing and drying to obtain a rare earth doped tricobalt tetraoxide precursor;
step 4: and (3) placing the precursor obtained in the step (3) in a muffle furnace for calcination, and obtaining the final product rare earth doped cobaltosic oxide nano-sheet after the calcination is finished.
2. The method for preparing rare earth doped cobaltosic oxide nano-sheets according to claim 1, wherein the volume ratio of water to glycol in the mixed solvent of water and glycol is 1:7.
3. The method for preparing rare earth doped cobaltosic oxide nano-platelets according to claim 1, wherein the molar ratio of cobalt nitrate hexahydrate to urea is 1:6.
4. The method for preparing rare earth doped cobaltosic oxide nano-sheets according to claim 1, wherein in the step 3, the drying temperature is 60 ℃ and the drying time is 6-12h.
5. The method for preparing rare earth doped cobaltosic oxide nano-sheets according to claim 1, wherein in the step 4, the calcination temperature is 300 ℃ and the calcination time is 2 hours; the programmed temperature rise rate of the muffle furnace is 10 ℃/min.
6. A rare earth doped tricobalt tetroxide nanosheet, characterized in that it is prepared by the method of any of claims 1-5.
7. Use of rare earth doped tricobalt tetraoxide nanoplatelets according to claim 6 for supercapacitor electrode materials.
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