CN106898498B - A kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode and preparation method thereof - Google Patents
A kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode and preparation method thereof Download PDFInfo
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Abstract
Disclosed herein is a kind of polypyrrole/nickel hydroxide/nickel foam integrated electrodes and preparation method thereof, it is supported in nickel foam and is constituted by polypyrrole and nickel hydroxide, wherein, the total load amount of polypyrrole and nickel hydroxide in nickel foam is 0.9% ~ 1.4%, and the mass ratio of polypyrrole and nickel hydroxide is 1：3~2：1.Electro-chemical test is carried out to the integrated electrode, show that the electrode has excellent chemical property, and with the increase of polypyrrole amount, material specific capacitance first increases to be reduced afterwards, is 1 in nickel nitrate and hexa molar ratio：1, a concentration of 0.05mol L of pyrrole monomer‑1When the electrode in 2A g‑1Specific capacitance is up to 2174F g under current density‑1, and there is highest specific capacitance conservation rate.
Description
Technical field
The invention belongs to electric chemical super capacitor new energy fields, and in particular to arrive a kind of polypyrrole/nickel hydroxide/bubble
The preparation of foam nickel integrated electrode simultaneously tests its chemical property.
Background technology
Today's society is increasingly sharpened with the production of fossil energy and using caused environmental problem, is developed novel
Energy storage with using device be the key that renewable new energy utilizes, ultracapacitor is one of them.Carbon material, metal
Oxide/hydroxide and conducting polymer are the important electrode material for super capacitor of three classes.Specific surface area is super capacitor
One critically important performance indicator of device electrode material, big specific surface area can provide more active sites in charge and discharge
And then accelerate the migration of charge, reach higher electric double layer capacitance, therefore material nanoization can be significantly improved to the storage of material
Deposit charge capability and utilization ratio.For nickel hydroxide as transistion metal compound, it has higher theoretical capacitance, unique shape
Looks structure, the advantage that at low cost and synthesis is convenient.But two intrinsic defects：Poor circulation and poorly conductive result in
Performance is not fully up to expectations when it is separately as electrode material for super capacitor.By Ni (OH)2Compound acquisition is carried out with other materials
The composite material haveing excellent performance is one of improvement alternative.For example, document (Zhang J, Kong L B, Cai J J, et
al.Hierarchically porous nickel hydroxide/mesoporous carbon composite
materials for electrochemical capacitors[J].Microporous and Mesoporous
Materials,2010,132(1):In 154-162.) in nickel hydroxide introduce mesoporous carbon can prepare nickel hydroxide/
Mesoporous carbon composite material, charge migration resistance are obviously reduced, cause material current density be 5mA cm-2When specific capacitance pole
It is high.Polypyrrole not only has certain fake capacitance, but also have good electric conductivity as a kind of conducting polymer.By poly- pyrrole
It coughs up and carries out compound the shortcomings that preparing the good composite material of electric conductivity, homogenous material itself can either be overcome with other materials
Also two kinds of materials can be made to generate synergistic effect, promoted to obtain outstanding chemical property mutually.For example, document (Sharma
R K,Rastogi A C,Desu S B.Manganese oxide embedded polypyrrole nanocomposites
for electrochemical supercapacitor[J].Electrochimica Acta,2008,53(26):7690-
7695.) then manganese dioxide is embedded into formation manganese dioxide/polypyrrole material in polypyrrole by leading strand shape polypyrrole in,
This composite material has the specific capacitance much larger than homogenous material.Therefore, it is that a new generation is super to prepare high-performance combination electrode material
One trend of grade capacitor development.
Invention content
The purpose of the present invention is prepare a kind of polypyrrole/nickel hydroxide/nickel foam by easy environmentally protective method
Integrated electrode, and it is used for ultracapacitor.
Realizing the technical solution of the object of the invention is：A kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode,
The total load amount of polypyrrole and nickel hydroxide in nickel foam is 0.9%~1.4%, and the mass ratio of polypyrrole and nickel hydroxide is
1：3~2：1.
A kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode preparation method, includes the following steps：
Step 1, it under water bath with thermostatic control, will be immersed in the ethanol solution of nickel acetate by pretreated foam nickel base；
Step 2, step 1 gained substrate is calcined；
Step 3, step 1 is repeated to more times of step 2；
Step 4, the mixed aqueous solution of nickel nitrate and hexa is prepared, and step 3 gained substrate is immersed into solution,
Hydro-thermal reaction takes out substrate washing drying after having reacted cooling；
Step 5, p-methyl benzenesulfonic acid is dissolved in absolute ethyl alcohol, pyrrole monomer is then added and stirs to form solution A, incited somebody to action
Ammonium sulfate is added dissolving in deionized water and forms solution B；
Step 6, step 4 gained substrate is kept flat with surface plate, takes equivalent solution A and solution B equal successively with liquid-transfering gun
It is even to be added drop-wise in substrate；
Step 7, step 6 gained substrate is reacted under dark condition, washs drying after having reacted, obtains polypyrrole/hydrogen
Nickel oxide/nickel foam integrated electrode.
Further, in step 1, a concentration of 18mmol L of the ethanol solution of nickel acetate-1。
Further, in step 1, water bath with thermostatic control temperature is 60 ± 10 DEG C, and the time is 45min or more.
Further, in step 2, calcination temperature is 275 ± 10 DEG C, and the time is 30~40min, and heating rate is 2 DEG C
min-1。
Further, in step 3, number of repetition is not less than 2 times.
Further, in step 4, the molar ratio of nickel nitrate and hexa is 1：2~2：1；Hydrothermal temperature
Be 120 ± 10 DEG C, the reaction time be 18~20h, drying temperature be 60 ± 10 DEG C, drying time be for 24 hours more than.
Further, in step 5, a concentration of 0.04mol L of p-methyl benzenesulfonic acid in solution A-1, pyrrole monomer it is a concentration of
0.025~0.15mol L-1；A concentration of 0.0263mol L of ammonium persulfate in solution B-1。
Further, in step 6, the solution A of 0.11ml~0.13ml equivalent and solution B is taken uniformly to drip successively with liquid-transfering gun
It is added in substrate.
Further, in step 7, the reaction time be 18~20h, drying temperature be 60 ± 10 DEG C, drying time be for 24 hours with
On.
Compared with prior art, the present invention its remarkable advantage is：(1) polypyrrole/nickel hydroxide/foam has successfully been prepared
This integrated electrode of nickel；(2) synthetic method is convenient and efficient, environmentally protective；(3) electrode material pattern is well controllable, hydroxide
Nickel is nano-sheet and polypyrrole is Nanoparticulate；(4) this integrated electrode has excellent chemical property.
Description of the drawings
Attached drawing 1 is that the X- of polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment 3 of the present invention is penetrated
Ray diffraction diagram is composed；
Attached drawing 2 is the infrared of polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment 3 of the present invention
Abosrption spectrogram；
Attached drawing 3 is the scanning of polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment 3 of the present invention
Electron microscope；
Attached drawing 4 is polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment 2-4,6,7 of the present invention
Electrochemical property test figure：Sweep speed is 10mV s-1When Cyclic voltamogram curve (a), current density be 4A g-1
Under constant current charge-discharge curve (b), ac impedance measurement curve (c) and material specific capacitance comparison diagram (d).
Specific implementation mode
It is further illustrated the present invention below by embodiment.This embodiment can make those skilled in the art more comprehensively
Understanding the present invention, but do not limit the invention in any way.With reference to embodiment and attached drawing to a kind of polypyrrole/hydrogen-oxygen
Change nickel/nickel foam integrated electrode and preparation method thereof to be described further, the present invention is prepared by following steps：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Nickelous nitrate hexahydrate and hexa are added in 50ml deionized waters and form mixed solution by the 5th step, and
Substrate obtained by 4th step is immersed into the solution；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added pyrrole monomer magnetic agitation
10min forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B, the wherein pyrroles of solution A
Monomer concentration is 0.025mol L-1~0.15mol L-1；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Finally obtain polypyrrole/nickel hydroxide/nickel foam integrated electrode.
The electrochemical property test of electrode be directly using CHI760C types electrochemical workstation to polypyrrole/nickel hydroxide/
This integrated electrode of nickel foam is tested.Wherein working electrode is the polypyrrole/nickel hydroxide/nickel foam integration prepared
Electrode, be to electrode platinized platinum, reference electrode be saturated calomel electrode, test electrolyte is 6mol L-1KOH solution.Test hand
Section is cyclic voltammetry, constant current charge-discharge test and ac impedance measurement.
Embodiment 1：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.0873g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.053ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.025M-1。
Embodiment 2：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.1745g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.053ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.025M。
Electrochemical property test, as shown in Fig. 4, the integration are carried out to the integrated electrode prepared by embodiment 2
Electrode is in 2A g-1Specific capacitance is 938F g under current density-1, current density is 32A g-1When specific capacitance conservation rate be 13.6%.
Embodiment 3：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.1745g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.105ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.05M。
Attached drawing 1 and attached drawing 2 are that the X- of polypyrrole/nickel hydroxide/nickel foam integrated electrode prepared by embodiment 3 is penetrated
Line diffraction spectrogram and infrared absorpting light spectra show that foam nickel base surface grown nickel hydroxide and by chemical method in substrate
On polymerize polypyrrole.
Integrated electrode pattern prepared by embodiment 3 is characterized, such as attached drawing 3, is shown in nickel foam and grows
Nickel hydroxide be nano-sheet, and polypyrrole is grown in nickel hydroxide nano piece surface in the form of nano particle.
Electrochemical property test, as shown in Fig. 4, the integration are carried out to the integrated electrode prepared by embodiment 3
Electrode is in 2A g-1Specific capacitance is 2174F g under current density-1, current density is 32A g-1When specific capacitance conservation rate be
34.2%.
Embodiment 4：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.1745g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.158ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.075M。
Electrochemical property test, as shown in Fig. 4, the integration are carried out to the integrated electrode prepared by embodiment 4
Electrode is in 2A g-1Specific capacitance is 1715F g under current density-1, current density is 32A g-1When specific capacitance conservation rate be
16.8%.
Embodiment 5：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.3490g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.158ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.075M-1。
Embodiment 6：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.1745g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.210ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.10M。
Electrochemical property test, as shown in Fig. 4, the integration are carried out to the integrated electrode prepared by embodiment 6
Electrode is in 2A g-1Specific capacitance is 1665F g under current density-1, current density is 32A g-1When specific capacitance conservation rate be
11.5%.
Embodiment 7：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.1745g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.315ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.15M。
Electrochemical property test, as shown in Fig. 4, the integration are carried out to the integrated electrode prepared by embodiment 7
Electrode is in 2A g-1Specific capacitance is 694F g under current density-1, current density is 32A g-1When specific capacitance conservation rate be 20.7%.
Embodiment 8：
The first step weighs six hydrated Ni acetates of 0.1792g and is added in 40ml ethyl alcohol, stirring and dissolving；
Second step will be immersed by pretreated clean foam nickel base in step 2 acquired solution, the constant temperature at 60 DEG C
Water-bath 45min；
Third walks, and will be calcined in tube furnace obtained by second step, and calcination temperature is 275 DEG C, time 30min, heat up speed
Rate is 2 DEG C of min-1；
4th step repeats the first step to third and walks 2 times；
Shape in 50ml deionized waters is added in 0.3490g Nickelous nitrate hexahydrates and 0.0845g hexas by the 5th step
The solution is immersed at mixed solution, and by substrate obtained by the 4th step；
5th step solution is transferred in hydrothermal reaction kettle by the 6th step, reacts 18h at 120 DEG C, is taken after having reacted cooling
Go out substrate washing, is dried for 24 hours in 60 DEG C of baking ovens；
7th step, then 0.228g p-methyl benzenesulfonic acid, which is dissolved in 30ml absolute ethyl alcohols, is added 0.315ml pyrrole monomer magnetic
Power stirs 10min and forms solution A, and dissolving in 20ml deionized waters, which is added, in 0.12g ammonium persulfates forms solution B；
8th step lies against substrate obtained by the 6th step in surface plate, successively taken with liquid-transfering gun equivalent 0.12ml solution As and
Solution B drops evenly in substrate；
Substrate obtained by 8th step under dark condition is reacted 18h, is washed with deionized water and ethyl alcohol after having reacted by the 9th step
It washs multiple and is dried for 24 hours in 60 DEG C of baking ovens.Polypyrrole/nickel hydroxide/nickel foam integrated electrode is finally obtained, is abbreviated as
0.15M-1。
Claims (10)
1. a kind of polypyrrole/nickel hydroxide/nickel foam integrated electrode, structure in nickel foam is supported on by polypyrrole and nickel hydroxide
At, which is characterized in that the total load amount of polypyrrole and nickel hydroxide in nickel foam is 0.9% ~ 1.4%, polypyrrole and hydrogen-oxygen
The mass ratio for changing nickel is 1：3~2：1, the electrode is made by the steps：
Step 1, it under water bath with thermostatic control, will be immersed in the ethanol solution of nickel acetate by pretreated foam nickel base；
Step 2, step 1 gained substrate is calcined；
Step 3, step 1 is repeated to more times of step 2；
Step 4, the mixed aqueous solution of nickel nitrate and hexa is prepared, and step 3 gained substrate is immersed into solution, hydro-thermal
Reaction takes out substrate washing drying after having reacted cooling；
Step 5, p-methyl benzenesulfonic acid is dissolved in absolute ethyl alcohol, pyrrole monomer is then added and stirs to form solution A, by persulfuric acid
Ammonium is added dissolving in deionized water and forms solution B；
Step 6, step 4 gained substrate is kept flat with surface plate, takes equivalent solution A and solution B uniformly to drip successively with liquid-transfering gun
It is added in substrate；
Step 7, step 6 gained substrate is reacted under dark condition, washs drying after having reacted, obtains polypyrrole/hydroxide
Nickel/nickel foam integrated electrode.
2. the preparation method of polypyrrole/nickel hydroxide/nickel foam integrated electrode as described in claim 1, which is characterized in that
Include the following steps：
Step 1, it under water bath with thermostatic control, will be immersed in the ethanol solution of nickel acetate by pretreated foam nickel base；
Step 2, step 1 gained substrate is calcined；
Step 3, step 1 is repeated to more times of step 2；
Step 4, the mixed aqueous solution of nickel nitrate and hexa is prepared, and step 3 gained substrate is immersed into solution, hydro-thermal
Reaction takes out substrate washing drying after having reacted cooling；
Step 5, p-methyl benzenesulfonic acid is dissolved in absolute ethyl alcohol, pyrrole monomer is then added and stirs to form solution A, by persulfuric acid
Ammonium is added dissolving in deionized water and forms solution B；
Step 6, step 4 gained substrate is kept flat with surface plate, takes equivalent solution A and solution B uniformly to drip successively with liquid-transfering gun
It is added in substrate；
Step 7, step 6 gained substrate is reacted under dark condition, washs drying after having reacted, obtains polypyrrole/hydroxide
Nickel/nickel foam integrated electrode.
3. method as claimed in claim 2, which is characterized in that in step 1, the ethanol solution of nickel acetate it is a concentration of
18mmol L-1。
4. method as claimed in claim 2, which is characterized in that in step 1, water bath with thermostatic control temperature is 60 ± 10 DEG C, when immersion
Between be 45min or more.
5. method as claimed in claim 2, which is characterized in that in step 2, calcination temperature be 275 ± 10 DEG C, the time be 30 ~
40min, heating rate are 2 DEG C of min-1。
6. method as claimed in claim 2, which is characterized in that in step 3, number of repetition is not less than 2 times.
7. method as claimed in claim 2, which is characterized in that in step 4, the molar ratio of nickel nitrate and hexa is
1：2~2：1；Hydrothermal temperature is 120 ± 10 DEG C, and the reaction time is 18 ~ 20h, and drying temperature is 60 ± 10 DEG C, drying time
More than for 24 hours.
8. method as claimed in claim 2, which is characterized in that in step 5, p-methyl benzenesulfonic acid is a concentration of in solution A
0.04mol L-1, a concentration of 0.025 ~ 0.15mol L of pyrrole monomer-1；A concentration of 0.0263mol of ammonium persulfate in solution B
L-1。
9. method as claimed in claim 2, which is characterized in that in step 6, take 0.11ml ~ 0.13ml etc. successively with liquid-transfering gun
The solution A and solution B of amount drop evenly in substrate.
10. method as claimed in claim 2, which is characterized in that in step 7, the reaction time is 18 ~ 20h, drying temperature 60
± 10 DEG C, drying time be for 24 hours more than.
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| CN108010736B (en) * | 2018-01-12 | 2020-03-31 | 西安交通大学 | NiCo construction based on foamed nickel template2S4@Ni(OH)2Method for applying @ PPy material to supercapacitor |
| CN114132973A (en) * | 2020-09-03 | 2022-03-04 | 南京安捷驰新能源科技有限公司 | Preparation method of modified nickel hydroxide cathode material |
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