CN112723425A - Ultrathin nanometer flower-structure hydrotalcite supercapacitor electrode material and preparation method thereof - Google Patents

Ultrathin nanometer flower-structure hydrotalcite supercapacitor electrode material and preparation method thereof Download PDF

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CN112723425A
CN112723425A CN202011587837.2A CN202011587837A CN112723425A CN 112723425 A CN112723425 A CN 112723425A CN 202011587837 A CN202011587837 A CN 202011587837A CN 112723425 A CN112723425 A CN 112723425A
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hydrotalcite
aqueous solution
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flower
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CN112723425B (en
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江伟
曹静静
周天鹏
徐云龙
周东山
齐运彪
孙平
张全兴
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Nanjing University
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Abstract

The invention discloses an ultrathin nanometer flower-structure hydrotalcite supercapacitor electrode material and a preparation method thereof, wherein a cobalt chloride aqueous solution and a nickel chloride aqueous solution are mixed to obtain a mixed solution; dropwise adding a morphology regulator amino acid aqueous solution under a stirring state, and stirring and reacting for 1-2 h; slowly dropwise adding precipitator NH3·H2Stirring and reacting the O aqueous solution for 3-5 hours; then placing the reaction system in an oil bath at the temperature of 80-100 ℃, and carrying out reflux stirring at constant temperature for 10-15 h; and finally, filtering the precipitate obtained by the reaction, alternately cleaning the precipitate by deionized water and ethanol, and filtering the precipitate in vacuum to obtain the catalyst. The ultrathin nanometer flower-structure hydrotalcite supercapacitor electrode material prepared by the method has a high specific surface areaAnd more active sites, the interlayer gaps of the nano-sheets can promote the oxidation-reduction process, the ultrathin nano-sheets provide more active sites for electrochemical reaction, and the three-dimensional nano-flower structure is stable.

Description

Ultrathin nanometer flower-structure hydrotalcite supercapacitor electrode material and preparation method thereof
Technical Field
The invention belongs to the technical field of electrode materials of super capacitors, and particularly relates to an ultrathin nanometer flower-structured hydrotalcite electrode material for a super capacitor and a preparation method thereof.
Background
Current energy structures are attracting high social attention. Advances in energy production and storage have driven the shift in energy structure to sustainable and renewable energy sources. Among the high-efficiency energy storage devices, the Super Capacitor (SC) has applications in many fields such as a backup power system, an electric vehicle, a portable electronic device, and the like due to its high power density and long cycle life. SCs are generally classified into two types according to charge storage mechanism. Class I are Electric Double Layer Capacitors (EDLCs) that are composed primarily of carbon-based materials, such as carbon nanotubes, graphene hydrogels, graphene nanoribbons, carbon foams, and the like. Type I supercapacitors have exceptional cycle/rate stability, however, low specific capacitance. Type II Pseudocapacitors (PCs) consisting essentially of metal oxide/hydroxyl and a conductive polymer, such as Nb2O5、Co3O4、MnO2、Co(OH)2And polyaniline. Type II supercapacitors typically have a high specific capacitance, but poor cycling stability. Bimetallic hydrotalcite (LDHs) is a novel two-dimensional (2D) nanosheet structure and has excellent energy storage characteristics. Bimetallic LDHs generally exhibit better electrochemical performance than monometallic hydroxides due to the stable structure and synergy of the bimetallic. The LDH hasA two-dimensional inorganic layered structure of the general formula [ M1-xM'x(OH)2]x +[(An-x/n)·mH2O]Wherein M and M' represent divalent and trivalent metal cations forming an octahedral hydrotalcite-like positively charged layer, An-Denotes charge-balancing anions (e.g. Cl between LDHs layers)-，NO3 2-，CO3 2-)。
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of the prior art, provides a hydrotalcite supercapacitor electrode material with a three-dimensional nanometer flower structure, and has the advantages of stable structure and high specific capacity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of an ultrathin nanometer flower-structured hydrotalcite supercapacitor electrode material comprises the following steps:
(1) mixing a cobalt chloride aqueous solution and a nickel chloride aqueous solution to obtain a mixed solution;
(2) dropwise adding a morphology regulator amino acid aqueous solution under a stirring state, and stirring and reacting for 1-2 h;
(3) slowly dripping a precipitator NH into the reaction system in the step (2)3·H2Stirring and reacting the O aqueous solution for 3-5 hours;
(4) placing the reaction system in the step (3) in an oil bath at the temperature of 80-100 ℃, and carrying out constant-temperature reflux stirring for 10-15 h;
(5) and (4) filtering the precipitate obtained in the step (4), alternately cleaning with deionized water and ethanol, and performing vacuum filtration to obtain the catalyst.
Specifically, in the step (1), the concentration range of the cobalt chloride aqueous solution is 0.1-0.5 mol/L; the concentration range of the nickel chloride aqueous solution is 0.1 mol/L-0.5 mol/L.
Preferably, in the step (1), the molar ratio of cobalt chloride to nickel chloride in the mixed solution is (1-2): 2-1.
Specifically, in the step (2), the amino acid in the amino acid aqueous solution is any one of aspartic acid, glutamic acid, lysine, arginine, histidine, methionine, serine, phenylalanine, asparagine and glutamate. During the synthesis process, amino acid and metal ion are coordinated.
Preferably, in the step (2), the concentration of the amino acid aqueous solution is 0.02-0.05 mol/L.
Preferably, in the step (2), the dropwise adding amount of the amino acid aqueous solution is 1: 2-1: 10 of the molar ratio of the amino acid to the total amount of the cobalt ions and the nickel ions in the step (1).
Preferably, in step (3), the NH is3·H2The concentration of the O aqueous solution is 2-4 wt.%. After the ammonia water is added, the ultra-thin hydrotalcite nanometer flower is obtained due to complexation.
Preferably, in step (3), the NH is3·H2The volume ratio of the addition amount of the O aqueous solution to the reaction system in the step (2) is 1: (5-8).
Preferably, in step (3), the NH is3·H2And slowly dripping the O aqueous solution within 2-3 h.
Further, the ultrathin electrode material of the nano flower-structured hydrotalcite supercapacitor prepared by the method is also in the protection scope of the invention.
In the one-step hydrothermal reflux synthesis process, the metal complex is formed by controlling the addition amount of amino acid and preferentially coordinating with metal ions, and then hydroxide with stronger complexing ability and the metal complex generate anion exchange action and slowly crystallize under a hydrothermal condition to form an ultrathin nanoflower structure.
Has the advantages that:
1. the invention adopts L-amino acid (LAs) as a morphology guiding agent of an electrode material for the first time to grow the 3D CoNi-OH nanosheet in situ.
2. The preparation method takes metal chloride as chloride intercalation ions, amino acid as a morphology regulating agent and ammonia water as a precipitator, and adopts a one-step hydrothermal reflux method to synthesize the ultrathin hydrotalcite nanoflower by regulating the use amounts of the metal chloride, the amino acid and the ammonia water within a proper concentration range. Compared with the traditional methods of ion exchange, calcination rehydration and the like for interlayer spacing regulation, the method has the advantages of no need of protective atmosphere, simple synthesis steps, low energy consumption, short time, high efficiency, accurate structure adjustment and the like.
3. The ultrathin nanometer flower-structured hydrotalcite supercapacitor electrode material prepared by the method has a high specific surface area and more active sites, the interlayer gaps can promote the oxidation-reduction process, the ultrathin nanosheets provide more active sites for electrochemical reaction, the three-dimensional nanometer flower structure can ensure the stability of the structure, and compared with the traditional hydrotalcite, the ultrathin nanometer flower-structured hydrotalcite supercapacitor electrode material has a higher capacitance performance; compared with the traditional hydrotalcite and the monolithic layered hydrotalcite, the material has a more stable structure and is a supercapacitor electrode material with the advantages of both stable structure and high specific capacity.
Drawings
The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
FIG. 1 is an XRD (X-ray diffraction) spectrum of a supercapacitor electrode material prepared from L-histidine, L-arginine, L-lysine, L-phenylalanine, L-serine, L-methionine, L-glutamic acid, L-aspartic acid and L-asparagine.
FIG. 2 is a scanning electron microscope image of a supercapacitor electrode material prepared from L-histidine, L-arginine, L-lysine, L-phenylalanine, L-serine, L-methionine, L-glutamic acid, L-aspartic acid and L-asparagine.
FIG. 3 is a diagram of capacitance performance of a supercapacitor electrode material prepared from L-histidine, L-arginine, L-lysine, L-phenylalanine, L-serine, L-methionine, L-glutamic acid, L-aspartic acid and L-asparagine.
Detailed Description
The invention will be better understood from the following examples.
The structures, proportions, and dimensions shown in the drawings and described in the specification are for understanding and reading the present disclosure, and are not intended to limit the scope of the present disclosure, which is defined in the claims, and are not essential to the skilled in the art. In addition, the terms "upper", "lower", "front", "rear" and "middle" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the relative positions may be changed or adjusted without substantial technical changes.
Example 1
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-histidine was weighed out and dissolved in 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in fig. 1, XRD analysis results showed that the main diffraction peaks of L-histidine/cobalt-nickel hydrotalcite were located at 19.1 °,33.4 °,38.5 ° and 51.8 ° respectively, corresponding to (001), (100), (011) and (012) planes, respectively, indicating that hydrotalcite of β phase was formed. As shown in FIG. 2, SEM results show that the L-histidine/cobalt-nickel hydrotalcite has a layered structure. FIG. 3 shows current density 1A g-1Specific time capacitance of 191.8mAh g-1Current density 10A g-1The specific time capacitance is 106.2mAh g-1The retention ratio was 55.3%.
Example 2
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-arginine was weighed into 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in fig. 1, XRD analysis results showed that the main diffraction peaks of L-arginine/cobalt-nickel hydrotalcite were located at 19.1 °,33.4 °,38.5 ° and 51.8 ° respectively, corresponding to (001), (100), (011) and (012) planes, respectively, indicating that hydrotalcite of β phase was formed. As shown in fig. 2, SEM results showed that L-arginine/cobalt nickel hydrotalcite was layered and multilayered. FIG. 3 shows current density 1A g-1The specific time capacitance is 208.8mAh g-1Current density 10A g-1The specific time capacitance is 106.8mAh g-1The retention rate was 51.1%.
Example 3
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-lysine was weighed out and dissolved in 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in fig. 1, XRD analysis results showed that the main diffraction peaks of L-lysine/cobalt-nickel hydrotalcite were located at 19.1 °,33.4 °,38.5 ° and 51.8 °, respectively, corresponding to (001), (100), (011) and (012) planes, respectively, indicating that a hydrotalcite structure of β phase was formed. As shown in FIG. 2, SEM results show that the L-lysine/cobalt-nickel hydrotalcite has a layered porous structure. FIG. 3 shows current density 1A g-1The specific time capacitance is 214.5mAh g-1Current density 10A g-1The specific time capacitance is 85.3mAh g-1The retention rate was 39.7%.
Example 4
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-phenylalanine was weighed out and dissolved in 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in FIG. 1, XRD analysis results showed that the main diffraction peaks of L-phenylalanine/cobalt-nickel hydrotalcite were located at 11.2 °,19.1 °,22.6 °,33.4 °,38.5 °,51.8 °,58.7 °,62.4 °,70.6 °, and 72.2 °, respectively, corresponding to ((003), (001), (006), (100), (011), (012), (110), (111), (103), and (112) planes, respectively, indicating that hydrotalcite structures of α, β phases were formed, as shown in FIG. 2As shown in the SEM result, the L-phenylalanine/cobalt-nickel hydrotalcite is in a bundle-like nano-block structure. FIG. 3 shows current density 1A g-1The specific time capacitance is 170.5mAh g-1Current density 10A g-1Specific time capacitance of 137mAh g-1The retention rate was 80.3%.
Example 5
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-serine was weighed out and dissolved in 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in FIG. 1, XRD analysis results showed that the main diffraction peaks of L-serine/cobalt-nickel hydrotalcite were located at 11.2 °,19.1 °,22.6 °,33.4 °,38.5 °,51.8 °,58.7 °,62.4 °,70.6 °, and 72.2 °, respectively, corresponding to ((003), (001), (006), (100), (011), (012), (110), (111), (103), and (112) planes, respectively, indicating that hydrotalcite structures of α, β phases were formed, SEM results showed that L-serine/cobalt-nickel hydrotalcite was a bundle-like structure, as shown in FIG. 2, FIG. 3 shows that the current density was 1A g-1The specific time capacitance is 226.3mAh g-1Current density 10A g-1Specific time capacitance of 58.2mAh g-1The retention rate was 25.6%.
Example 6
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-methionine was weighed out and dissolved in 40mL of water, and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in FIG. 1, XRD analysis results showed that the main diffraction peaks of L-methionine/cobalt-nickel hydrotalcite were located at 11.2 °,19.1 °,22.6 °,33.4 °,38.5 °,51.8 °,58.7 °,62.4 °,70.6 °, and 72.2 °, respectively, corresponding to ((003), (001), (006), (100), (011), (012), (110), (111), (103), and (112) planes, respectively, indicating that hydrotalcite structures of α, β phases were formed, SEM results showed that L-methionine/cobalt-nickel hydrotalcite was a bundle-like nanoblock structure, FIG. 3 showed that the current density was 1A g-1Specific time capacitance of 259.3mAh g-1Current density 10A g-1The specific time capacitance is 111.3mAh g-1The retention rate was 42.9%.
Example 7
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-aspartic acid was weighed out and dissolved in 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in FIG. 1, XRD analysis results showed that the main diffraction peaks of L-aspartic acid/cobalt-nickel hydrotalcite were located at 11.2 °,22.6 °,34.5 °, and 62.4 °, respectively, corresponding to ((003), (006), (012), and (113) planes, respectively, indicating that hydrotalcite structures of alpha phase were formed, SEM results showed that L-aspartic acid/cobalt-nickel hydrotalcite was of irregular layered structure, FIG. 3 showed that current density was 1A g-1The specific time capacitance is 205.2mAh g-1Current density 10A g-1Specific time capacitance of 70.1mAh g-1The retention rate was 34.1%.
Example 8
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-glutamic acid was weighed out and dissolved in 40mL of water, and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in FIG. 1, XRD analysis results showed that the main diffraction peaks of L-glutamic acid/cobalt-nickel hydrotalcite were located at 11.2 °,22.6 °,34.5 °, and 62.4 °, respectively, corresponding to ((003), (006), (012), and (113) planes, respectively, indicating that a hydrotalcite structure of alpha phase was formed, as shown in FIG. 2, SEM results showed that L-glutamic acid/cobalt-nickel hydrotalcite was in irregular layered structure, FIG. 3 shows that the current density was 1A g-1Specific time capacitance of 208.4mAh g-1Current density 10A g-1Specific time capacitance of 94.7mAh g-1The retention ratio was 45.4%.
Example 9
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: 1mmol of L-asparagine was weighed out and dissolved in 40mL of water and stirred well.
And step 3: the mixed solution obtained in step 2 was added to the mixed solution obtained in step 1, and stirred for 1 h.
And 4, step 4: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 3 within 3 hours3·H2O(3.5wt.％)。
And 5: the mixed solution obtained in step 4 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
Step 6: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
As shown in FIG. 1, XRD analysis results showed that the main diffraction peaks of L-asparagine/cobalt-nickel hydrotalcite were located at 11.2 °,22.6 °,34.5 °, and 62.4 °, respectively, and correspond to ((003), (006), (012), and (113) planes, respectively, indicating that hydrotalcite structures of alpha phase were formed, as shown in FIG. 2, SEM results showed that L-asparagine/cobalt-nickel hydrotalcite was in a nano-flower structure, FIG. 3 shows that the current density was 1A g-1Specific time capacitance of 405.4mAh g-1Current density 10A g-1The specific time capacitance is 256.3mAh g-1The retention rate was 63.2%.
Comparative example
Step 1: weigh 4mmol of NiCl2·6H2O and 2mmol of CoCl2·6H2O was dissolved in 20mL of water and stirred for 1 h.
Step 2: slowly dropwise adding 20mL of NH into the mixed solution obtained in the step 1 within 3 hours3·H2O(3.5wt.％)。
And step 3: the mixed solution obtained in step 2 was charged into a round-bottom flask and stirred under reflux at an oil bath temperature of 95 ℃ for 12 hours.
And 4, step 4: and (3) after the reaction, the obtained precipitate is separated from deionized water and ethanol for three times, put into a vacuum drying oven and dried overnight, and taken out to obtain the required material.
XRD analysis showed that the main diffraction peaks of cobalt-nickel hydrotalcite were located at 11.2 °,19.1 °,22.6 °,33.4 °,38.5 °,51.8 °,58.7 °,62.4 °,70.6 °, and 72.2 ° respectively, corresponding to ((003), (001), (006), (100), (011), (012), (110), (111), (103), and (112) planes, respectively, indicating formation of hydrotalcite structures of α, β phases, current density 1A g-1Specific time capacitance of 65.8mAh g-1Current density 10A g-1Specific time capacitance of 40.3mAh g-1The retention ratio was 61.2%.
The hydrotalcite of the invention takes amino acid as a structure guiding agent and ammonia water as a precipitator to obtain a hydrotalcite compound with a blocky, layered and nanoflower structure, and is a supercapacitor electrode material with adjustable structure and high specific capacity. The preparation method of the invention is characterized in that the ratio of amino acid to metal ions and the dosage of ammonia water as a precipitator are regulated within a proper concentration range. Adopting one-step hydrothermal reflux synthesis to obtain 9 kinds of hydrotalcite with block, layer and nanometer flower structure. Compared with the traditional methods of hydrotalcite ion intercalation, ion exchange and the like, the preparation method of the invention has the advantages of no need of protective atmosphere, simple synthesis steps, low energy consumption, short time, high efficiency, accurate structure adjustment and the like, and has wide application prospect.
The invention provides an ultra-thin nanometer flower structure hydrotalcite supercapacitor electrode material and a preparation method thereof, and a method and a way for realizing the technical scheme are numerous, the above description is only a preferred embodiment of the invention, and it should be noted that, for a person skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the invention, and the improvements and decorations should also be regarded as the protection scope of the invention. All the components not specified in the present embodiment can be realized by the prior art.

Claims (10)

1. A preparation method of an ultrathin nanometer flower-structured hydrotalcite supercapacitor electrode material is characterized by comprising the following steps:
(1) mixing a cobalt chloride aqueous solution and a nickel chloride aqueous solution to obtain a mixed solution;
(2) dropwise adding a morphology regulator amino acid aqueous solution under a stirring state, and stirring and reacting for 1-2 h;
(3) slowly dripping a precipitator NH into the reaction system in the step (2)3·H2Stirring and reacting the O aqueous solution for 3-5 hours;
(4) placing the reaction system in the step (3) in an oil bath at the temperature of 80-100 ℃, and carrying out constant-temperature reflux stirring for 10-15 h;
(5) and (4) filtering the precipitate obtained in the step (4), alternately cleaning with deionized water and ethanol, and performing vacuum filtration to obtain the catalyst.
2. The method for preparing the ultrathin electrode material of the nano flower-structured hydrotalcite supercapacitor, according to claim 1, wherein in the step (1), the concentration of the cobalt chloride aqueous solution is in the range of 0.1mol/L to 0.5 mol/L; the concentration range of the nickel chloride aqueous solution is 0.1 mol/L-0.5 mol/L.
3. The method for preparing the ultrathin electrode material of the nano-flower-structured hydrotalcite supercapacitor is characterized in that in the step (1), the molar ratio of cobalt chloride to nickel chloride in the mixed solution is (1-2) to (2-1).
4. The method for preparing the ultrathin electrode material of the nano-flower-structured hydrotalcite supercapacitor, according to claim 1, wherein in the step (2), the amino acid in the amino acid aqueous solution is any one of aspartic acid, glutamic acid, lysine, arginine, histidine, methionine, serine, phenylalanine, and asparagine.
5. The preparation method of the ultrathin electrode material of the nano-flower-structured hydrotalcite supercapacitor, according to claim 4, wherein in the step (2), the concentration of the amino acid aqueous solution is 0.02-0.05 mol/L.
6. The preparation method of the ultrathin nanometer flower-structured hydrotalcite supercapacitor electrode material according to claim 5, wherein in the step (2), the dropwise addition amount of the amino acid aqueous solution is added according to a molar ratio of 1: 2-1: 10 of amino acid to the total amount of cobalt ions and nickel ions in the step (1).
7. The method for preparing the ultrathin electrode material of the nano flower-structured hydrotalcite supercapacitor according to claim 1, wherein in the step (3), NH is added3·H2The concentration of the O aqueous solution is 2-4 wt.%.
8. The method for preparing the ultrathin electrode material of the nano flower-structured hydrotalcite supercapacitor according to claim 7, wherein in the step (3), NH is added3·H2The volume ratio of the addition amount of the O aqueous solution to the reaction system in the step (2) is 1: (5-8).
9. The method for preparing the ultrathin electrode material of the nano flower-structured hydrotalcite supercapacitor according to claim 8, wherein in the step (3), NH is added3·H2And slowly dripping the O aqueous solution within 2-3 h.
10. The ultrathin electrode material of the nano-flower-structure hydrotalcite supercapacitor, which is prepared by the preparation method of any one of claims 1 to 9.
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