CN107017094A - A kind of graphene@NiMn LDH combination electrode materials of polyaniline-coated and preparation method thereof - Google Patents
A kind of graphene@NiMn LDH combination electrode materials of polyaniline-coated and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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Abstract
The invention belongs to electrode material technical field, the graphene@NiMn LDH combination electrode materials of specially a kind of polyaniline-coated and preparation method thereof.Preparation process of the present invention includes：Graphene oxide is dissolved in deionized water and carries out ultrasound；Aniline is added to dispersant for ultrasonic and prepares aniline dispersion liquid；Graphene oxide solution mixes ultrasound with aniline dispersion liquid；Graphene oxide/aniline mixed liquor carries out polymerisation and obtains graphene oxide/polyaniline crude product；Nickel source, manganese source and conditioning agent are added into graphene oxide/polyaniline crude product and carries out hydro-thermal reaction；Filtration washing and drying, that is, obtain the graphene NiMn LDH composites of polyaniline-coated.The composite has played the electrochemistry feature of polyaniline, graphene and nickel manganese layered double hydroxide, big with specific surface area, conducts electricity very well, the features such as specific capacitance is high.
Description
Technical field
Present invention relates particularly to a kind of graphene@NiMn-LDH combination electrode materials of polyaniline-coated and its preparation side
Method, belongs to electrode composite material technical field.
Background technology
Ultracapacitor, the electrochemistry advantage with better than traditional capacitor and secondary cell, with than traditional capacitor
High energy density, the power density higher than secondary cell and long cycle life.Electrode material as ultracapacitor core
Center portion part, decides the quality of ultracapacitor chemical property.The focus electrode material studied at present mainly includes graphene
Deng carbon material, transition metal oxide, conducting polymer materials.
Polyaniline has conjugated system as a kind of intrinsic conducting polymer on its main chain, can be conductive by doping.
The features such as polyaniline is by low cost, green non-pollution, ability of adulterating by force, high porosity, wide potential range, good reversibility,
There is preferably application, theoretical specific capacitance is up to 2000Fg in terms of preparing electrode of super capacitor-1, as in super capacitor electrode
One of conducting polymer of greatest concern in the material of pole.Polyaniline is by occurring Faraday pseudo-capacitance effect storage energy, in electricity
Redox reaction storage electric charge occurs in the intrinsic material of pole.High-energy-density and high specific capacitance that transition metal oxide has
Also received much concern in ultracapacitor field.Such as MnO2、Co3O4、Fe3O4、CoFe2O4Deng transition metal oxide, but its compared with
Low conductance and not high power density limit the further raising of its chemical property.
Graphene is as the two-dimensional material of ultra-thin and ultra-light, specific surface area and high-strength electrical conductivity by superelevation, as super
Favorite in level capacitor material.Conjugation group on polyaniline backbone can interact with graphene, and such as π-π are common
Yoke, electrostatic interaction, are adsorbed in graphenic surface, can regulate and control the functional group's number and species of graphenic surface, improve electrode material
The specific capacitance of material；Polyaniline can also be by wrapping up the specific capacitance of the further composite of transition metal oxide.
The content of the invention
In order to improve the chemical property of electrode material for super capacitor, it is an object of the invention to provide a kind of polyaniline bag
Graphene@NiMn-LDH combination electrode materials covered and preparation method thereof.The present invention can solve existing laminated type bimetal hydroxide
The problem of thing electrode material specific capacitance is not high enough, and strengthen its cycle performance.
A kind of preparation method of the graphene@NiMn-LDH combination electrode materials of polyaniline-coated provided by the present invention,
Its preparing raw material includes：Graphene oxide, aniline, neopelex, ammonium persulfate, concentrated hydrochloric acid, nickel nitrate, nitric acid
Manganese, urea and ammonium fluoride.
The present invention provides a kind of preparation method of the graphene@NiMn-LDH combination electrode materials of polyaniline-coated, specifically
Step is as follows：
(1) initiator and inorganic acid are added in graphene oxide/aniline mixed liquor, polymerisation is carried out, after reaction terminates,
Centrifugation, filter cake is washed with deionized to the pH of efflux untill neutral, obtains graphene oxide/polyaniline crude product；
(2) nickel nitrate, manganese nitrate, ammonium fluoride and urea or hexa-methylene are added into graphene oxide/polyaniline crude product
Tetramine, carries out ultrasound；
(3) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron and carries out hydro-thermal reaction, reaction terminates
Afterwards, filter, wash, being dried to obtain the graphene@NiMn-LDH combination electrode materials of polyaniline-coated.
In above-mentioned steps (1), graphene oxide/aniline mixed liquor is mixed by graphene oxide water solution and aniline dispersion liquid
Obtain；In graphene oxide water solution, the mass ratio of graphene oxide and deionized water is 1:2~3:2；Aniline dispersion liquid is by benzene
Amine and dispersant are 1 in mass ratio:5~10:1 is mixed to get, and dispersant is neopelex.
In above-mentioned steps (1), the mass ratio of graphene oxide and aniline in graphene oxide/aniline mixed liquor is 1:10
~5:1；Initiator is ammonium persulfate；Hydrochloric acid is concentrated hydrochloric acid.
In above-mentioned steps (2), the mass ratio of graphene oxide/polyaniline crude product and nickel nitrate is 1:2~1:10；Nickel nitrate
Mass ratio with manganese nitrate is 2:1~6:1；The mass ratio of nickel nitrate and urea or hexa is 1:1~5:1；Nitric acid
The mass ratio of nickel and ammonium fluoride is 10:1~20:1；Ultrasonic time is 1~2h.
In above-mentioned steps (3), hydrothermal temperature is 160~180 DEG C；The hydro-thermal reaction time is 12~24h.
In above-mentioned steps (3), drying temperature is 30~60 DEG C；Drying time is 12~18h.
The present invention also provides a kind of graphene@NiMn-LDH combination electrodes of polyaniline-coated made from above-mentioned preparation method
Material.
Compared to the prior art, the beneficial effects of the present invention are：
The graphene@NiMn-LDH composites of polyaniline-coated prepared by the present invention, polyaniline successfully wraps up graphene@
NiMn, parcel is uniform, with higher specific surface area.
The graphene@NiMn-LDH composites of polyaniline-coated prepared by the present invention, are used as electrode of super capacitor material
Material, shows excellent chemical property.
Brief description of the drawings
Fig. 1 be the graphene@NiMn-LDH composites of the polyaniline-coated of the gained of embodiment 1 at 10000 times and
Scanning electron microscope (SEM) photograph under 1000000 times.
Fig. 2 is graphene@NiMn-LDH composites the sweeping under 10000 times of the polyaniline-coated of the gained of embodiment 2
Retouch electron microscope.
Fig. 3 is the XRD diffraction patterns of the graphene@NiMn-LDH composites of the polyaniline-coated of the gained of embodiment 3.
Fig. 4 is that the graphene@NiMn-LDH composites of the polyaniline-coated of the gained of embodiment 4 pass through electro-chemical test institute
The cyclic voltammogram obtained.
Embodiment
In order to more specifically illustrate the present invention, the present invention is further explained below by specific embodiment and with reference to accompanying drawing
State, but do not limit the scope of the invention.
Embodiment 1
(1) 10mg graphene oxides are added in 20mg deionized waters, and carry out ultrasonic mixing 1h；
(2) 100mg aniline monomers are weighed to be added in 100mg dispersant neopelexes, aniline is obtained and disperses
Liquid；
(3) graphene dispersing solution for obtaining step (1) mixes ultrasound 1h with the aniline dispersion liquid that step (2) is obtained；
(4) initiator ammonium persulfate 50mg is sequentially added in the graphene oxide obtained to step (3)/aniline mixed liquor,
Concentrated hydrochloric acid 90mg, then at 0 DEG C, rotating speed is that 300r/min stirring 12h progress polymerisations obtain mixed liquor, is centrifuged, gained
The pH to efflux is washed with deionized untill neutrality in filter cake, obtains graphene oxide/polyaniline crude product；
(5) 20mg graphene oxides/polyaniline crude product is taken, 180mg nickel nitrates, 90mg manganese nitrates, 60mg urine is sequentially added
Plain (or hexa), 18mg ammonium fluorides carry out ultrasound 1h；
(6) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 160 DEG C
24h；
(7) graphite that oven drying 12h at filtration washing, 40 DEG C obtains polyaniline-coated is carried out with ethanol and deionized water
Alkene@NiMn-LDH composites.
According to the graphene@NiMn-LDH composites of the polyaniline-coated obtained by this embodiment method, it is 10000
See Fig. 1 with the ESEM under 1000000 times again, product performance multi-layer flower laminated structure, polyaniline-graphite alkene is wrapped up
NiMn-LDH surface.Electrode of super capacitor is prepared into, with 2molL-1KOH solution is used as ginseng as electrolyte, Ag electrodes
Than electrode, nickel foam is as reference electrode, and specimen material determines its chemical property, be in current density as working electrode
0.5Ag-1When, its specific capacitance is 1699.3F g-1, obvious redox peaks are showed in cyclic voltammetry, counterfeit electricity is represented
Hold effect；Specific capacitance after the circle of circulation 2000 is 1609.23F g-1, cycle efficieny is up to 94.7%.
Embodiment 2
(1) 20mg graphene oxides are added in 20mg deionized waters, and carry out ultrasonic mixing 2h；
(2) 140mg aniline monomers are weighed to be added in 500mg dispersant neopelexes, aniline is obtained and disperses
Liquid；
(3) graphene dispersing solution for obtaining step (1) mixes ultrasound 2h with the aniline dispersion liquid that step (2) is obtained；
(4) initiator ammonium persulfate 50mg is sequentially added in the graphene oxide obtained to step (3)/aniline mixed liquor,
Concentrated hydrochloric acid 100mg, then at 0 DEG C, rotating speed is that 200r/min stirring 24h progress polymerisations obtain mixed liquor, is centrifuged, gained
The pH to efflux is washed with deionized untill neutrality in filter cake, obtains graphene oxide/polyaniline crude product；
(5) 150mg graphene oxides/polyaniline crude product is taken, 260mg nickel nitrates, 130mg manganese nitrates, 100mg is sequentially added
Urea (or hexa), 30mg ammonium fluorides carry out ultrasound 1h；
(6) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 180 DEG C
18h；
(7) graphite that oven drying 16h at filtration washing, 40 DEG C obtains polyaniline-coated is carried out with ethanol and deionized water
Alkene@NiMn-LDH composites.
According to the graphene@NiMn-LDH composites of the polyaniline-coated obtained by this embodiment method, it is 10000
ESEM under times is shown in Fig. 2, and graphene-polyaniline has wrapped up NiMn-LDH.Electrode of super capacitor is prepared into, with 2mol
L-1KOH solution is as electrolyte, and Ag electrodes are as reference electrode, and nickel foam is used as work electricity as reference electrode, specimen material
Pole, determines its chemical property, is 0.5A g in current density-1When, its specific capacitance is 1257.8F g-1；After the circle of circulation 2000
Specific capacitance be 1142.1F g-1, cycle efficieny is 90.8%.
Embodiment 3
(1) 20mg graphene oxides are added in 20mg deionized waters, and carry out ultrasonic mixing 2h；
(2) 160mg aniline monomers are weighed to be added in 200mg dispersant neopelexes, aniline is obtained and disperses
Liquid；
(3) graphene dispersing solution for obtaining step (1) mixes ultrasound 2h with the aniline dispersion liquid that step (2) is obtained；
(4) initiator ammonium persulfate 30mg is sequentially added in the graphene oxide obtained to step (3)/aniline mixed liquor,
Concentrated hydrochloric acid 60mg, then at 0 DEG C, rotating speed is that 300r/min stirring 15h progress polymerisations obtain mixed liquor, is centrifuged, gained
The pH to efflux is washed with deionized untill neutrality in filter cake, obtains graphene oxide/polyaniline crude product；
(5) 100mg graphene oxides/polyaniline crude product is taken, 350mg nickel nitrates, 180mg manganese nitrates, 150mg is sequentially added
Urea (or hexa), 60mg ammonium fluorides carry out ultrasound 1h；
(6) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 180 DEG C
18h；
(7) graphite that oven drying 16h at filtration washing, 40 DEG C obtains polyaniline-coated is carried out with ethanol and deionized water
Alkene@NiMn-LDH composites.
According to the graphene@NiMn-LDH composites of the polyaniline-coated obtained by this embodiment method, its XRD diffraction
Figure is shown in Fig. 3, the angle of diffraction 11.07 °, 19.25 °, 23.64 °, 32.72 °, 33.71 °, 36.49 °, 37.37 °, 43.16 °,
46.94 °, 51.87 °, 53.22 °, 59.00 °, 60.82 ° respectively correspond to crystal face (110), (211), (221), (322), (330),
(421), (332), (440), (530), (621), (533), (640), (113), show NiMn-LDH successful synthesis；It is prepared into
Electrode of super capacitor, with 2molL-1KOH solution is as electrolyte, and Ag electrodes are used as control as reference electrode, nickel foam
Electrode, specimen material determines its chemical property as working electrode, is 0.5A g in current density-1When, its specific capacitance is
1096.3F g-1, obvious faraday's redox peaks are showed in cyclic voltammetry；Circulating the specific capacitance after 2000 circles is
972.4F g-1, cycle efficieny is 88.7%.
Embodiment 4
(1) 20mg graphene oxides are added in 20mg deionized waters, and carry out ultrasonic mixing 2h；
(2) 220mg aniline monomers are weighed to be added in 500mg dispersant neopelexes, aniline is obtained and disperses
Liquid；
(3) graphene dispersing solution for obtaining step (1) mixes ultrasound 1.5h with the aniline dispersion liquid that step (2) is obtained；
(4) initiator ammonium persulfate 30mg is sequentially added in the graphene oxide obtained to step (3)/aniline mixed liquor,
Concentrated hydrochloric acid 100mg, then at 0 DEG C, rotating speed is that 200r/min stirring 12h progress polymerisations obtain mixed liquor, is centrifuged, gained
The pH to efflux is washed with deionized untill neutrality in filter cake, obtains graphene oxide/polyaniline crude product；
(5) 100mg graphene oxides/polyaniline crude product is taken, 500mg nickel nitrates, 300mg manganese nitrates, 200mg is sequentially added
Urea (or hexa), 80mg ammonium fluorides carry out ultrasound 1h；
(6) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 160 DEG C
12h；
(7) graphite that oven drying 16h at filtration washing, 40 DEG C obtains polyaniline-coated is carried out with ethanol and deionized water
Alkene@NiMn-LDH composites.
According to the graphene@NiMn-LDH composites of the polyaniline-coated obtained by this embodiment method, it is prepared into super
Level electrode for capacitors, with 2molL-1KOH solution is as electrolyte, and Ag electrodes are used as control electricity as reference electrode, nickel foam
Pole, specimen material determines its chemical property as working electrode, and obvious redox is showed in cyclic voltammetry
Peak, its cyclic voltammogram is shown in Fig. 4；It is 0.5A g in current density-1When, its specific capacitance is 1381.6F g-1；After the circle of circulation 2000
Specific capacitance be 1242.1F g-1, cycle efficieny is 89.9%.
Embodiment 5
(1) 20mg graphene oxides are added in 20mg deionized waters, and carry out ultrasonic mixing 2h；
(2) 200mg aniline monomers are weighed to be added in 400mg dispersant neopelexes, aniline is obtained and disperses
Liquid；
(3) graphene dispersing solution for obtaining step (1) mixes ultrasound 2h with the aniline dispersion liquid that step (2) is obtained；
(4) initiator ammonium persulfate 30mg is sequentially added in the graphene oxide obtained to step (3)/aniline mixed liquor,
Concentrated hydrochloric acid 120mg, then at 0 DEG C, rotating speed is that 300r/min stirring 12h progress polymerisations obtain mixed liquor, is centrifuged, gained
The pH to efflux is washed with deionized untill neutrality in filter cake, obtains graphene oxide/polyaniline crude product；
(5) 100mg graphene oxides/polyaniline crude product is taken, 700mg nickel nitrates, 300mg manganese nitrates, 200mg is sequentially added
Urea (or hexa), 80mg ammonium fluorides carry out ultrasound 1h；
(6) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 160 DEG C
24h；
(7) graphite that oven drying 18h at filtration washing, 40 DEG C obtains polyaniline-coated is carried out with ethanol and deionized water
Alkene@NiMn-LDH composites.
According to the graphene@NiMn-LDH composites of the polyaniline-coated obtained by this embodiment method, it is prepared into super
Level electrode for capacitors, with 2molL-1KOH solution is as electrolyte, and Ag electrodes are used as control electricity as reference electrode, nickel foam
Pole, specimen material determines its chemical property as working electrode, is 0.5Ag in current density-1When, its specific capacitance is
1512.7F g-1, when current density is 10Ag-1When, its specific capacitance is 1266F g-1, with good high rate performance；In circulation
Obvious redox peaks are showed in volt-ampere test, fake capacitance effect is represented；Specific capacitance after the circle of circulation 2000 is 1408.3F
g-1, cycle efficieny is 93.1%.
Embodiment 6
(1) 20mg graphene oxides are added in 20mg deionized waters, and carry out ultrasonic mixing 2h；
(2) 500mg aniline monomers are weighed to be added in 1000mg dispersant neopelexes, aniline is obtained and disperses
Liquid；
(3) graphene dispersing solution for obtaining step (1) mixes ultrasound 2h with the aniline dispersion liquid that step (2) is obtained；
(4) initiator ammonium persulfate 80mg is sequentially added in the graphene oxide obtained to step (3)/aniline mixed liquor,
Concentrated hydrochloric acid 200mg, then at 0 DEG C, rotating speed is that 200r/min stirring 24h progress polymerisations obtain mixed liquor, is centrifuged, gained
The pH to efflux is washed with deionized untill neutrality in filter cake, obtains graphene oxide/polyaniline crude product；
(5) 200mg graphene oxides/polyaniline crude product is taken, 1000mg nickel nitrates are sequentially added, 600mg manganese nitrates,
500mg urea (or hexa), 200mg ammonium fluorides carry out ultrasound 1h；
(6) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 180 DEG C
12h；
(7) graphite that oven drying 18h at filtration washing, 40 DEG C obtains polyaniline-coated is carried out with ethanol and deionized water
Alkene@NiMn-LDH composites.
According to the graphene@NiMn-LDH composites of the polyaniline-coated obtained by this embodiment method, it is prepared into super
Level electrode for capacitors, with 2molL-1KOH solution is as electrolyte, and Ag electrodes are used as control electricity as reference electrode, nickel foam
Pole, specimen material determines its chemical property as working electrode, is 0.5Ag in current density-1When, its specific capacitance is
1294.8F g-1；Specific capacitance after the circle of circulation 2000 is 1145.9F g-1, cycle efficieny is 88.5%.
Embodiment 7
This embodiment compared with Example 1, does not add graphene and polyaniline, and other steps are consistent with embodiment, system
Standby NiMn-LDH, is comprised the following steps that：
(1) 180mg nickel nitrates are taken, 90mg manganese nitrates, 60mg urea (or hexa), 18mg ammonium fluorides are surpassed
The scattered 1h of sound mixing；
(2) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron, in carrying out hydro-thermal reaction at 160 DEG C
24h；
(3) oven drying 12h at filtration washing, 40 DEG C is carried out with ethanol and deionized water and obtains NiMn-LDH materials.
According to the NiMn-LDH materials obtained by this embodiment method, electrode of super capacitor is prepared into, with 2molL- 1KOH solution is as electrolyte, and Ag electrodes are as reference electrode, and nickel foam is used as work electricity as reference electrode, specimen material
Pole, determines its chemical property, is 0.5A g in current density-1When, its specific capacitance is 756.3F g-1；After the circle of circulation 2000
Specific capacitance is 677.6F g-1, cycle efficieny is up to 89.6%.
Claims (7)
1. a kind of preparation method of the graphene@NiMn-LDH combination electrode materials of polyaniline-coated, it is characterised in that specific step
It is rapid as follows：
(1) initiator and inorganic acid are added in graphene oxide/aniline mixed liquor, polymerisation is carried out, after reaction terminates, from
The heart, filter cake is washed with deionized to the pH of efflux untill neutral, obtains graphene oxide/polyaniline crude product；
(2) nickel nitrate, manganese nitrate, ammonium fluoride and urea or hexa are added into graphene oxide/polyaniline crude product,
Carry out ultrasound；
(3) mixed liquor after ultrasound is transferred to polytetrafluoroethylene (PTFE) stainless steel cauldron and carries out hydro-thermal reaction, after reaction terminates, mistake
Filter, wash, being dried to obtain the graphene@NiMn-LDH combination electrode materials of polyaniline-coated.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), graphene oxide/aniline mixed liquor by
Graphene oxide water solution and aniline dispersion liquid are mixed to get；In graphene oxide water solution, graphene oxide and deionized water
Mass ratio be 1:2~3:2；Aniline dispersion liquid is 1 in mass ratio by aniline and dispersant:5~10:1 is mixed to get, dispersant
For neopelex.
3. preparation method as claimed in claim 1, it is characterised in that in step (1), in graphene oxide/aniline mixed liquor
Graphene oxide and aniline mass ratio be 1:10~5:1；Initiator is ammonium persulfate；Hydrochloric acid is concentrated hydrochloric acid.
4. preparation method as claimed in claim 1, it is characterised in that in step (2), graphene oxide/polyaniline crude product with
The mass ratio of nickel nitrate is 1:2~1:10；The mass ratio of nickel nitrate and manganese nitrate is 2:1~6:1；Nickel nitrate and urea or six are sub-
The mass ratio of tetramine is 1:1~5:1；The mass ratio of nickel nitrate and ammonium fluoride is 10:1~20:1；Ultrasonic time be 1~
2h。
5. preparation method as claimed in claim 1, it is characterised in that in step (3), hydrothermal temperature is 160~180
℃；The hydro-thermal reaction time is 12~24h.
6. preparation method as claimed in claim 1, it is characterised in that in step (3), drying temperature is 30~60 DEG C；Dry
Time is 12~18h.
7. a kind of graphene@NiMn-LDH combination electrodes of polyaniline-coated made from preparation method as described in claim 1~6
Material.
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| CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
| CN110517898A (en) * | 2019-08-14 | 2019-11-29 | 上海应用技术大学 | The preparation method of the graphene@CoAl-LDH combination electrode material of polyaniline-coated |
| CN110676067A (en) * | 2019-10-24 | 2020-01-10 | 陈丰 | Polyaniline-double metal hydroxide supercapacitor material and preparation method thereof |
| CN110880424A (en) * | 2019-11-28 | 2020-03-13 | 朱旭烈 | Polybenzazole coated nickel-cobalt compound supercapacitor material and preparation method thereof |
| CN111118908A (en) * | 2019-12-31 | 2020-05-08 | 浙江大学 | Layered double-metal hydroxide-polyaniline modified porous conductive composite material and preparation method and application thereof |
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| CN108766785B (en) * | 2018-07-02 | 2020-05-22 | 桂林电子科技大学 | Graphene-polypyrrole-cobalt-nickel double-metal hydroxide composite material and preparation method and application thereof |
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| CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
| CN111974429A (en) * | 2019-05-21 | 2020-11-24 | 南京大学 | Preparation method of multilayer pie-shaped NiMn-LDHs catalyst |
| CN111974429B (en) * | 2019-05-21 | 2022-04-19 | 南京大学 | Preparation method of multilayer pie-shaped NiMn-LDHs catalyst |
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| CN110676067A (en) * | 2019-10-24 | 2020-01-10 | 陈丰 | Polyaniline-double metal hydroxide supercapacitor material and preparation method thereof |
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| CN112375415A (en) * | 2020-11-12 | 2021-02-19 | 厦门大学 | Preparation method and application of graphene-based composite material anti-corrosion auxiliary agent |
| CN112542328A (en) * | 2020-12-02 | 2021-03-23 | 浙江大学 | Ternary layered metal hydroxide @ polyaniline composite electrode material and preparation method and application thereof |
| CN113345723A (en) * | 2021-04-30 | 2021-09-03 | 上海交通大学 | Porous graphene/polyaniline composite film and preparation method and application thereof |
| CN113813945A (en) * | 2021-09-30 | 2021-12-21 | 宁德师范学院 | Three-dimensional space network graphene-based polyaniline/PtAg composite catalyst and preparation method thereof |
| CN113813945B (en) * | 2021-09-30 | 2023-08-18 | 宁德师范学院 | Three-dimensional space network graphene-based polyaniline/PtAg composite catalyst and preparation method thereof |
| CN115172065A (en) * | 2022-06-16 | 2022-10-11 | 宁德师范学院 | Three-dimensional capacitance electrode material with graphene surface grafted with polyaniline/titanium dioxide |
| CN115172065B (en) * | 2022-06-16 | 2023-04-25 | 宁德师范学院 | Three-dimensional capacitance electrode material with polyaniline/titanium dioxide grafted on graphene surface |
| CN115798946A (en) * | 2023-01-30 | 2023-03-14 | 昆山美淼新材料科技有限公司 | Production process of metal graphene multi-element composite electrode |
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