CN106898498A - A kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode and preparation method thereof - Google Patents

Abstract

This paper discloses a polypyrrole/nickel hydroxide/nickel foam integrated electrode and its preparation method. The loading is 0.9%~1.4%, and the mass ratio of polypyrrole to nickel hydroxide is 1:3~2:1. The electrochemical test of the integrated electrode shows that the electrode has excellent electrochemical performance, and with the increase of the amount of polypyrrole, the specific capacitance of the material increases first and then decreases. When the concentration of pyrrole monomer is 1:1 and the concentration of pyrrole monomer is 0.05mol L ^‑1 , the specific capacitance of the electrode is as high as 2174F g ^{‑1 at a current density of 2A g ‑1 ,} and has the highest specific capacitance retention rate.

Description

A polypyrrole/nickel hydroxide/nickel foam integrated electrode and its preparation method

technical field

The invention belongs to the field of new energy sources of electrochemical supercapacitors, and in particular relates to the preparation of a polypyrrole/nickel hydroxide/nickel foam integrated electrode and the testing of its electrochemical performance.

Background technique

In today's society, with the increasing environmental problems caused by the production and utilization of fossil energy, the development of new energy storage and utilization devices is the key to the utilization of renewable new energy, and supercapacitors are one of them. Carbon materials, metal oxides/hydroxides, and conductive polymers are three important types of supercapacitor electrode materials. The specific surface area is a very important performance index of supercapacitor electrode materials. A large specific surface area can provide more active sites during charge and discharge, thereby accelerating charge migration and achieving higher electric double layer capacitance. Therefore, the material nano Chemicalization can significantly improve the charge storage capacity and utilization efficiency of materials. As a transition metal compound, nickel hydroxide has the advantages of high theoretical capacitance, unique morphology, low cost and convenient synthesis. However, two inherent defects: poor cycle performance and poor conductivity lead to unsatisfactory performance when used alone as a supercapacitor electrode material. Combining Ni(OH) ₂ with other materials to obtain composite materials with excellent performance is one of the improvement strategies. For example, in the literature (Zhang J, Kong LB, Cai JJ, et al. Hierarchically porous nickel hydroxide/mesoporous carbon composite materials for electrochemical capacitors [J]. Microporous and Mesoporous Materials, 2010, 132 (1): 154-162.) in Ni-MH Nickel hydroxide/mesoporous carbon composites can be prepared by introducing mesoporous carbon into the oxide, and its charge transfer resistance is significantly reduced, resulting in extremely high specific capacitance of the material at a current density of 5mA cm ^-2 . As a conductive polymer, polypyrrole not only has a certain pseudocapacitance, but also has good conductivity. Combining polypyrrole with other materials to prepare a composite material with good electrical conductivity can not only overcome the shortcomings of the single material itself but also enable the two materials to have a synergistic effect and promote each other to obtain outstanding electrochemical performance. For example, in the literature (SharmaR K, Rastogi AC, Desu S B. Manganese oxide embedded polypyrrole nanocomposites for electrochemical supercapacitor [J]. Electrochimica Acta, 2008, 53 (26): 7690-7695.) first synthesize chain polypyrrole, and then Manganese dioxide is embedded in polypyrrole to form a manganese dioxide/polypyrrole material, and this composite material has a specific capacitance much greater than that of a single material. Therefore, the preparation of high-performance composite electrode materials is a trend in the development of a new generation of supercapacitors.

Contents of the invention

The purpose of the present invention is to prepare a polypyrrole/nickel hydroxide/foam nickel integrated electrode through a simple and green method, and use it for a supercapacitor.

The technical solution for realizing the object of the present invention is: a polypyrrole/nickel hydroxide/nickel foam integrated electrode, the total load of polypyrrole and nickel hydroxide on the foam nickel is 0.9%～1.4%, polypyrrole and hydrogen The mass ratio of nickel oxide is 1:3-2:1.

A method for preparing polypyrrole/nickel hydroxide/foam nickel integrated electrode, comprising the steps of:

Step 1, under a constant temperature water bath, immerse the pretreated foamed nickel substrate in an ethanol solution of nickel acetate;

Step 2, calcining the substrate obtained in step 1;

Step 3, repeat steps 1 to 2 multiple times;

Step 4, preparing a mixed aqueous solution of nickel nitrate and hexamethylenetetramine, immersing the substrate obtained in step 3 into the solution, performing a hydrothermal reaction, taking out the substrate after cooling after the reaction, washing and drying;

Step 5, dissolving p-toluenesulfonic acid in absolute ethanol, then adding pyrrole monomer and stirring to form solution A, and adding ammonium persulfate into deionized water to dissolve to form solution B;

Step 6, place the substrate obtained in step 4 flat on a watch glass, and use a pipette gun to sequentially take equal amounts of solution A and solution B and evenly drop them onto the substrate;

In step 7, the substrate obtained in step 6 is reacted under dark conditions, washed and dried after the reaction, to obtain a polypyrrole/nickel hydroxide/nickel foam integrated electrode.

Further, in step 1, the concentration of the ethanol solution of nickel acetate is 18 mmol L ^-1 .

Further, in step 1, the temperature of the constant temperature water bath is 60±10° C., and the time is more than 45 minutes.

Further, in step 2, the calcination temperature is 275±10°C, the time is 30-40min, and the heating rate is 2°C min ^-1 .

Further, in step 3, the number of repetitions is not less than 2 times.

Further, in step 4, the molar ratio of nickel nitrate to hexamethylenetetramine is 1:2-2:1; the hydrothermal reaction temperature is 120±10°C, the reaction time is 18-20h, and the drying temperature is 60±10°C 10°C, the drying time is more than 24h.

Further, in step 5, the concentration of p-toluenesulfonic acid in solution A is 0.04mol L ^-1 , the concentration of pyrrole monomer is 0.025-0.15mol L -1 ; the concentration of ammonium persulfate in solution B is ^0.0263mol L ^{-1 1} .

Further, in step 6, use a pipette gun to sequentially take 0.11ml-0.13ml equal amounts of solution A and solution B and evenly drop them onto the substrate.

Further, in step 7, the reaction time is 18-20 hours, the drying temperature is 60±10° C., and the drying time is more than 24 hours.

Compared with the prior art, the present invention has the remarkable advantages of: (1) the integrated electrode of polypyrrole/nickel hydroxide/foam nickel has been successfully prepared; (2) the synthesis method is convenient, quick and green; (3) The morphology of the electrode material is good and controllable, the nickel hydroxide is in the shape of nano flakes and the polypyrrole is in the shape of nanoparticles; (4) this integrated electrode has excellent electrochemical performance.

Description of drawings

Accompanying drawing 1 is the X-ray diffraction pattern of polypyrrole/nickel hydroxide/foam nickel integrated electrode prepared by embodiment example 3 of the present invention;

Accompanying drawing 2 is the infrared absorption spectrogram of the prepared polypyrrole/nickel hydroxide/foam nickel integrated electrode of embodiment example 3 of the present invention;

Accompanying drawing 3 is the scanning electron micrograph of polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment example 3 of the present invention;

Accompanying drawing 4 is the electrochemical performance test figure of the polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment example 2-4, 6, 7 of the present invention: the cyclic voltammetry characteristic when the scan rate is 10mV s ^-1 Curve (a), constant current charge and discharge curve (b) at a current density of 4A g ^-1 , AC impedance test curve (c), and specific capacitance comparison chart (d) of the material.

detailed description

The present invention is further illustrated below by implementing examples. This implementation example can enable those skilled in the art to understand the present invention more comprehensively, but does not limit the present invention in any way. A polypyrrole/nickel hydroxide/nickel foam integrated electrode and its preparation method are further described below in conjunction with the implementation examples and accompanying drawings. The present invention is prepared by the following steps:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, nickel nitrate hexahydrate and hexamethylenetetramine are added to 50 ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B, wherein the pyrrole monomer in solution A The monomer concentration is 0.025mol L ^-1 ~0.15mol L ^-1 ;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained.

The electrochemical performance test of the electrode is to directly use the CHI760C electrochemical workstation to test the integrated electrode of polypyrrole/nickel hydroxide/nickel foam. The working electrode is the prepared polypyrrole/nickel hydroxide/nickel foam integrated electrode, the counter electrode is a platinum sheet, the reference electrode is a saturated calomel electrode, and the test electrolyte is 6mol L ^-1 KOH solution. The test methods are cyclic voltammetry, constant current charge and discharge test and AC impedance test.

Implementation example 1:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.0873g of nickel nitrate hexahydrate and 0.0845g of hexamethylenetetramine are added to 50ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.053ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.025M-1.

Implementation example 2:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.1745g of nickel nitrate hexahydrate and 0.0845g of hexamethylenetetramine are added to 50ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.053ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.025M.

The electrochemical performance test was carried out on the integrated electrode prepared in Example 2, as shown in Figure 4, the specific capacitance of the integrated electrode was 938F g ^-1 at a current density of 2A g ^-1 , and the current density was 32A g ^-1 The specific capacitance retention rate was 13.6%.

Implementation example 3:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.1745g of nickel nitrate hexahydrate and 0.0845g of hexamethylenetetramine are added to 50ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.105ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.05M.

Accompanying drawing 1 and accompanying drawing 2 are the X-ray diffraction spectrogram and the infrared absorption spectrogram of the prepared polypyrrole/nickel hydroxide/nickel foam integrated electrode of embodiment 3, show that nickel hydroxide has been grown on the nickel foam substrate surface and Polypyrrole is chemically polymerized on the substrate.

The morphology of the integrated electrode prepared in Example 3 is characterized, as shown in Figure 3, showing that the nickel hydroxide grown on the nickel foam is in the form of nanosheets, and polypyrrole is grown on the nickel hydroxide nanosheets in the form of nanoparticles. surface.

The electrochemical performance test was carried out on the integrated electrode prepared in Example 3, as shown in Figure 4, the specific capacitance of the integrated electrode was 2174F g ^-1 at a current density of 2A g ^-1 , and the current density was 32A g ^-1 The specific capacitance retention rate was 34.2%.

Implementation example 4:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.1745g of nickel nitrate hexahydrate and 0.0845g of hexamethylenetetramine are added to 50ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.158ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.075M.

The electrochemical performance test was carried out on the integrated electrode prepared in Example 4, as shown in Figure 4, the specific capacitance of the integrated electrode was 1715F g ^-1 at a current density of 2A g ^-1 , and the current density was 32A g ^-1 The specific capacitance retention rate was 16.8%.

Implementation example 5:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.3490 g of nickel nitrate hexahydrate and 0.0845 g of hexamethylenetetramine are added to 50 ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.158ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.075M-1.

Implementation example 6:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.1745g of nickel nitrate hexahydrate and 0.0845g of hexamethylenetetramine are added to 50ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.210ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.10M.

The electrochemical performance test was carried out on the integrated electrode prepared in Example 6, as shown in Figure 4, the specific capacitance of the integrated electrode was 1665F g ^-1 at a current density of 2A g ^-1 , and the current density was 32A g ^-1 The specific capacitance retention rate was 11.5%.

Implementation example 7:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.1745g of nickel nitrate hexahydrate and 0.0845g of hexamethylenetetramine are added to 50ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.315ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.15M.

The electrochemical performance test was carried out on the integrated electrode prepared in Example 7, as shown in Figure 4, the specific capacitance of the integrated electrode was 694F g ^-1 at a current density of 2A g ^-1 , and the current density was 32A g ^-1 The specific capacitance retention rate was 20.7%.

Implementation example 8:

In the first step, weigh 0.1792g of nickel acetate hexahydrate and add it to 40ml of ethanol, stir to dissolve;

In the second step, immerse the pretreated clean nickel foam substrate in the solution obtained in step 2, and place it in a constant temperature water bath at 60°C for 45 minutes;

In the third step, calcining the obtained product in the second step in a tube furnace, the calcining temperature is 275°C, the time is 30min, and the heating rate is 2°C min ^-1 ;

The fourth step, repeat the first step to the third step 2 times;

In the fifth step, 0.3490 g of nickel nitrate hexahydrate and 0.0845 g of hexamethylenetetramine are added to 50 ml of deionized water to form a mixed solution, and the substrate obtained in the fourth step is immersed in the solution;

In the sixth step, transfer the solution in the fifth step to a hydrothermal reaction kettle and react at 120°C for 18 hours. After the reaction is completed and cooled, take out the substrate for washing, and dry it in an oven at 60°C for 24 hours;

Step 7: Dissolve 0.228g of p-toluenesulfonic acid in 30ml of absolute ethanol, then add 0.315ml of pyrrole monomer and magnetically stir for 10min to form solution A, add 0.12g of ammonium persulfate to 20ml of deionized water and dissolve to form solution B;

In the eighth step, place the substrate obtained in the sixth step flat on a watch glass, and use a pipette gun to take an equal amount of 0.12ml solution A and solution B and drop them evenly on the substrate;

In the ninth step, the substrate obtained in the eighth step was reacted in the dark for 18 hours. After the reaction, it was washed with deionized water and ethanol several times and dried in an oven at 60°C for 24 hours. Finally, a polypyrrole/nickel hydroxide/nickel foam integrated electrode is obtained, abbreviated as 0.15M-1.

Claims (10)

1. a kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode, be loaded on foamed nickel by polypyrrole and nickel hydroxide, it is characterized in that, the total load capacity of polypyrrole and nickel hydroxide on foamed nickel is 0.9%-1.4%, the mass ratio of polypyrrole to nickel hydroxide is 1:3-2:1. 2. the preparation method of polypyrrole/nickel hydroxide/nickel foam integrated electrode as claimed in claim 1, is characterized in that, comprises the steps: Step 1, under a constant temperature water bath, immerse the pretreated foamed nickel substrate in an ethanol solution of nickel acetate; Step 2, calcining the substrate obtained in step 1; Step 3, repeat steps 1 to 2 multiple times; Step 4, preparing a mixed aqueous solution of nickel nitrate and hexamethylenetetramine, immersing the substrate obtained in step 3 into the solution, performing a hydrothermal reaction, taking out the substrate after cooling after the reaction, washing and drying; Step 5, dissolving p-toluenesulfonic acid in absolute ethanol, then adding pyrrole monomer and stirring to form solution A, and adding ammonium persulfate into deionized water to dissolve to form solution B; Step 6, place the substrate obtained in step 4 flat on a watch glass, and use a pipette gun to sequentially take equal amounts of solution A and solution B and evenly drop them onto the substrate; In step 7, the substrate obtained in step 6 is reacted under dark conditions, washed and dried after the reaction, to obtain a polypyrrole/nickel hydroxide/nickel foam integrated electrode. 3. The method according to claim 2, characterized in that, in step 1, the concentration of nickel acetate in ethanol solution is 18 mmolL ^-1 . 4. The method according to claim 2, characterized in that, in step 1, the temperature of the constant temperature water bath is 60±10° C., and the immersion time is more than 45 minutes. 5. The method according to claim 2, characterized in that in step 2, the calcination temperature is 275±10°C, the time is 30-40min, and the heating rate is 2°Cmin ^-1 . 6. The method according to claim 2, characterized in that, in step 3, the number of repetitions is not less than 2. 7. The method according to claim 2, characterized in that, in step 4, the molar ratio of nickel nitrate to hexamethylenetetramine is 1:2 to 2:1; the hydrothermal reaction temperature is 120±10°C, The reaction time is 18-20 hours, the drying temperature is 60±10°C, and the drying time is more than 24 hours. 8. The method according to claim 2, wherein in step 5, the concentration of p-toluenesulfonic acid in solution A is 0.04 mol L ^-1 , and the concentration of pyrrole monomer is 0.025-0.15 mol L ^-1 ; the solution The concentration of ammonium persulfate in B is 0.0263 mol L ^-1 . 9. The method according to claim 2, characterized in that, in step 6, 0.11ml-0.13ml equal amounts of solution A and solution B are sequentially taken with a pipette gun and evenly dropped onto the substrate. 10. The method according to claim 2, wherein in step 7, the reaction time is 18-20 hours, the drying temperature is 60±10°C, and the drying time is more than 24 hours.