CN107180704A - A kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt - Google Patents
A kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt Download PDFInfo
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- CN107180704A CN107180704A CN201710342096.3A CN201710342096A CN107180704A CN 107180704 A CN107180704 A CN 107180704A CN 201710342096 A CN201710342096 A CN 201710342096A CN 107180704 A CN107180704 A CN 107180704A
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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
- H01G11/46—Metal oxides
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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
- H01G11/48—Conductive polymers
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt, preparation process is as follows：Step 1, prepare the sour nickel nano-wire array of cobalt；Step 2, prepare the sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt；Step 3, prepare the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt.The present invention uses Hydrothermal Synthesiss technology, using good conductivity and the nickel foam with loose porous unique texture passes through two step hydro-thermals as substrate and the sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt is made, the process of cumbersome making electrode slice was so both avoided, active material utilization can also be effectively improved, increase active surface, improve the diffusion mass transfer performance of material.Polyaniline is deposited to by the sour nickel core-shell nano linear array surface of the sour nickel tungsten of cobalt by simple chemical polymerization again and obtains the sour nickel/polyaniline tri compound core-shell nano linear array of the sour nickel tungsten of cobalt.
Description
Technical field
The invention belongs to the preparation field of electrode material for super capacitor, more particularly to a kind of sour nickel/polyphenyl of the sour nickel tungsten of cobalt
The preparation method of amine tri compound nano line array electrode material.
Background technology
With continuing to develop and scientific and technical continuous progress for human society, the mankind get over to the demand of the energy and resource
Come bigger, thus in the urgent need to some efficiently, cleaning, the sustainable energy and new technology store and change energy.It is super
Level capacitor has high power density, quick charge and discharge process, the life-span of length, low cost, environment-friendly and safe
The advantages of, it has also become the new focus of research that people pay close attention in recent years.
Electrode material for super capacitor is its key components.Research finds unitary electrode material often due to some
Deficiency causes overall chemical property to decline.In recent years, with going deep into nano materials research, people are begun attempt to material
It is combined on nanoscale.Wherein core-shell nano-composite material (including nm-class core-and-shell particles and nano-array etc.) is
A kind of typical form of nano composite material, its study to the effect that by nano particle or array surface coating or
Wrap up one layer of new material to assign the characteristic that they are new, and further study its surface, interface property.Answered as a kind of orderly
Structure is closed, core-shell nano-composite material shows the incomparable performance of one-component nano material.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of sour nickel/polyaniline tri compound nano wire of the sour nickel tungsten of cobalt
The preparation method of array electrode material, by the compound of material, the synergy between the structure and material of nucleocapsid is effectively carried
The high chemical property of composite.
The present invention is achieved through the following technical solutions：
A kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt, step is as follows：
Step 1, prepare the sour nickel nano-wire array of cobalt：At room temperature, it is nickel nitrate, cobalt nitrate and urea is dense by the amount of material
The ratio between degree 1:2:8 are dissolved in deionized water and obtain precursor solution A；Precursor solution A is transferred to water after ultrasonic half an hour
In thermal response kettle and a piece of nickel foam cut is added, hydro-thermal reaction in baking oven is placed in after sealing, room is then naturally cooled to
Temperature, takes out nickel foam, washs, vacuum drying, and the sour nickel nano-wire array of cobalt is obtained after calcining；
Step 2, prepare the sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt：At room temperature, by nickel nitrate, sodium tungstate and urea
By the ratio between substance withdrawl syndrome 1:1:4 are dissolved in deionized water and obtain precursor solution B, after ultrasonic half an hour that presoma is molten
Liquid B is transferred in hydrothermal reaction kettle and added the sour nickel nano-wire array of cobalt that step 1 is obtained, and hydro-thermal in baking oven is placed in after sealing anti-
Should, room temperature is then naturally cooled to, nickel foam is taken out, washed, vacuum drying obtains the sour nickel nucleocapsid of the sour nickel tungsten of cobalt and received after calcining
Nanowire arrays；
Step 3, prepare the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt：By aniline and to toluene sulphur
Sour ultrasonic disperse obtains mixed solution in deionized water/absolute ethyl alcohol in the mixed solvent, is transferred in ice bath, and step 2 is obtained
To the sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt be put into mixed solution, ammonium persulfate solution, ice bath reaction knot is slowly added dropwise
Shu Hou, is washed, vacuum drying, obtains the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt.
In step 1,110-150 DEG C of the hydrothermal temperature, time 4-8h；Wash for respectively with absolute ethyl alcohol, go from
Alternately washing 3 times of sub- water, dry to be dried in vacuo 12h, 300-400 DEG C of calcining heat under the conditions of 60-80 DEG C.
In step 2,110-150 DEG C of the hydrothermal temperature, time 4-8h, wash for respectively with absolute ethyl alcohol, go from
Alternately washing 3 times of sub- water, dry to be dried in vacuo 12h, 300-400 DEG C of calcining heat under the conditions of 60-80 DEG C.
In step 3, the deionized water/absolute ethyl alcohol in the mixed solvent, deionized water and absolute ethyl alcohol volume ratio are 1:
1；The amount ratio of the aniline, p-methyl benzenesulfonic acid and deionized water/absolute ethyl alcohol mixed solvent is 0.20~0.40mL:0.43g:
100mL；The concentration of the ammonium persulfate solution is 19mg/mL；The volume ratio of the ammonium sulfate and the mixed solution is
1:5；The reaction time is 6-10h, is washed alternately to be washed 3 times with absolute ethyl alcohol, deionized water respectively, it is 60-80 to dry
12h is dried in vacuo under the conditions of DEG C.
The processing mode of the nickel foam is as follows：Nickel foam is cut to the wide 1cm of growth 1cm thin slice, respectively with acetone,
1mol/L hydrochloric acid, absolute ethyl alcohol, deionized water supersound washing 20min is then placed in 80 DEG C of dry 6h in vacuum drying chamber.
Beneficial effect：
The present invention use Hydrothermal Synthesiss technology, using good conductivity and with loose porous unique texture nickel foam as
The sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt is made by two step hydro-thermals in substrate, has so both avoided the mistake of cumbersome making electrode slice
Journey, can also effectively improve active material utilization, increase active surface, improve the diffusion mass transfer performance of material.Again by simple
Chemical polymerization polyaniline deposited into the sour nickel core-shell nano linear array surface of the sour nickel tungsten of cobalt obtain the sour nickel of the sour nickel tungsten of cobalt/poly-
Aniline tri compound core-shell nano linear array.
Brief description of the drawings
Fig. 1 (a) and (b) are respectively scanning electron microscope (SEM) photograph of the sour nickel of cobalt under different multiplying in embodiment 1；(c) it is embodiment 1
The scanning electron microscope (SEM) photograph of the sour nickel of the sour nickel tungsten of middle cobalt；(d) it is the scanning electron microscope (SEM) photograph of the sour nickel/polyaniline of the sour nickel tungsten of cobalt in embodiment 1.
Fig. 2 (a) is the X-ray diffraction of the sour nickel of the cobalt of embodiment 1, the sour nickel of the sour nickel tungsten of cobalt and the sour nickel/polyaniline of the sour nickel tungsten of cobalt
Collection of illustrative plates；(b) it is the sour nickel/Organic conductor figure of the sour nickel tungsten of the cobalt of embodiment 1.
Fig. 3 (a) is that the pure foam nickel of embodiment 1, the sour nickel of cobalt, the sour nickel of the sour nickel tungsten of cobalt and the sour nickel/polyaniline of the sour nickel tungsten of cobalt exist
Sweep speed is 10mV s-1When cyclic voltammetry curve figure；(b) be the sour nickel of the cobalt of embodiment 1, the sour nickel of the sour nickel tungsten of cobalt and the sour nickel of cobalt/
Nickel tungstate/polyaniline is 1A g in current density-1When constant current charge-discharge figure.
Embodiment
With reference to specific embodiment, the invention will be further described：
Embodiment 1
1mmol nickel nitrates accurately are weighed, 2mmol cobalt nitrates and 8mmol urea are dissolved in 40mL deionized waters and stirred
To clarifying, it is then transferred into 50mL hydrothermal reaction kettles, and is put into a piece of treated nickel foam, 130 DEG C of constant temperature is anti-after sealing
Answer 6h.After after natural cooling, nickel foam is taken out, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C are dried in vacuo 12h,
The last 2h that calcined at 350 DEG C obtains the sour nickel nano-wire array of cobalt.
Accurate to weigh 1mmol nickel nitrates, 1mmol sodium tungstates and 6mmol urea, which are dissolved in 40mL deionized waters, to be stirred to mixed
Close uniform, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettles, and will be previously obtained
The sour nickel nano-wire array foam nickel base of cobalt be put into wherein, 130 DEG C of isothermal reaction 6h after sealing.It is cooled to after room temperature, takes
Go out nickel foam, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C of vacuum dryings finally calcine 2h at 400 DEG C and obtain cobalt
The sour nickel core-shell nano linear array of sour nickel tungsten.
0.30mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in 100mL volume ratios 1 at room temperature:1 second alcohol and water
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after well mixed, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and 20mL 0.38g containing the ammonium persulfate aqueous solution, the polymerisation in ice-water bath is then added dropwise
6h.Take out nickel foam, with alternately washing 3 times of absolute ethyl alcohol, deionized water, obtain after 60 DEG C of vacuum dryings the sour nickel of the sour nickel tungsten of cobalt/
Polyaniline tri compound core-shell nano linear array.
Fig. 1 (a) and (b) are respectively scanning electron microscope (SEM) photograph of the sour nickel of cobalt under different multiplying.It can be seen that three-dimensional many
The sour nickel nano material of one layer of cobalt of the nickel foam superficial growth in hole.After enlargement ratio, it can be seen that a large amount of uniform nanowire-junctions
Structure, its intermediate width is about 50nm, and length is about 3 μm.Fig. 1 (c) is the scanning electron microscope (SEM) photograph of the sour nickel of the sour nickel tungsten of cobalt, it can be seen that
Cobalt acid nickel nanowire surface is wrapped in by wolframic acid nickel particle.Fig. 1 (d) is the scanning electron microscope (SEM) photograph of the sour nickel/polyaniline of the sour nickel tungsten of cobalt.
It is observed that membrane structure is presented in polyaniline, the sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt is connected and wrapped up, is formed
Good three-dimensional conductive structure, can be conducive to improving the electron transfer rate of electrode material for super capacitor.Fig. 2 (a) is cobalt
The X ray diffracting spectrum of the sour nickel of the sour nickel tungsten of sour nickel, cobalt and the sour nickel/polyaniline of the sour nickel tungsten of cobalt.It can be seen that every song
All there is very strong diffraction maximum at 44.8 °, 51.7 ° and 77.2 ° in line, and this is probably the diffraction maximum of foam nickel base
(JCPDS:04-0850), except these characteristic peaks are not found other diffraction maximums, illustrate that the foam nickel base is very pure
Only.The diffraction maximum of cobalt acid nickel nano-wire array corresponds respectively to stand at 18.6 °, 30.9 °, 36.5 °, 59.1 ° and 64.9 ° in figure
(111), (220), (331), (511) and (440) crystal face of the sour nickel of square phase cobalt, the sour nickel core-shell nano linear array of cobalt acid nickel tungsten is removed
NiCo2O4Diffraction maximum beyond also show other diffraction maximums, correspond respectively to (010) and (- 122) crystal face of nickel tungstate,
Show that nickel tungstate has been deposited on the sour nickel nano-wire array of cobalt.Fig. 2 (b) is the sour nickel/Organic conductor of the sour nickel tungsten of cobalt
Figure.In figure, 3420cm-1Place be H-O-H stretching vibrations caused by absworption peak, illustrate that material surface has physical absorption water.
1489 and 1572cm-1Place occurs in that C=C stretching vibration absworption peaks and the quinoid and the characteristic peak of benzene-type ring of polyaniline, and this is poly-
The presence of functional group in aniline.Fig. 3 (a) is pure foam nickel, the sour nickel of cobalt, the sour nickel of the sour nickel tungsten of cobalt and the sour nickel of the sour nickel tungsten of cobalt/poly-
Aniline is 10mV s in sweep speed-1When cyclic voltammetry curve figure.It is obvious that the integral area very little of nickel foam, illustrates bubble
The specific capacitance very little of foam nickel substrate, can thus ignore the influence of its specific capacitance to material.It may also be seen that three
Planting material has a pair of good redox peaks, shows the characteristic that typical fake capacitance material has.Fig. 3 (b) is cobalt
The sour nickel of the sour nickel tungsten of sour nickel, cobalt and the sour nickel/polyaniline of the sour nickel tungsten of cobalt are 1A g in current density-1When constant current charge-discharge figure.
It is 1A g to obtain the sour nickel/polyaniline of the sour nickel tungsten of cobalt in current density by calculating-1When specific capacitance be 1741F g-1, higher than cobalt acid
Nickel tungsten acid nickel (1305F g-1) and sour nickel (the 706F g of cobalt-1).This is mainly attributed to the sour nickel of cobalt, three kinds of materials of nickel tungstate and polyaniline
Synergy, and the unique appearance structure of trielement composite material are produced between material.
Embodiment 2
1mmol nickel nitrates accurately are weighed, 2mmol cobalt nitrates and 8mmol urea are dissolved in 40mL deionized waters and stirred
To clarifying, it is then transferred into 50mL hydrothermal reaction kettles, and is put into a piece of treated nickel foam, 110 DEG C of constant temperature is anti-after sealing
Answer 4h.After after natural cooling, nickel foam is taken out, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C are dried in vacuo 12h,
The last 2h that calcined at 400 DEG C obtains the sour nickel nano-wire array of cobalt.
Accurate to weigh 1mmol nickel nitrates, 1mmol sodium tungstates and 6mmol urea, which are dissolved in 40mL deionized waters, to be stirred to mixed
Close uniform, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettles, and will be previously obtained
The sour nickel nano-wire array foam nickel base of cobalt be put into wherein, 110 DEG C of isothermal reaction 4h after sealing.It is cooled to after room temperature, takes
Go out nickel foam, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C of vacuum dryings finally calcine 2h at 400 DEG C and obtain cobalt
The sour nickel core-shell nano linear array of sour nickel tungsten.
0.20mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in 100mL volume ratios 1 at room temperature:1 second alcohol and water
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after well mixed, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and 20mL 0.38g containing the ammonium persulfate aqueous solution, the polymerisation in ice-water bath is then added dropwise
8h.Take out nickel foam, with alternately washing 3 times of absolute ethyl alcohol, deionized water, obtain after 60 DEG C of vacuum dryings the sour nickel of the sour nickel tungsten of cobalt/
Polyaniline tri compound core-shell nano linear array.
Embodiment 3
1mmol nickel nitrates accurately are weighed, 2mmol cobalt nitrates and 8mmol urea are dissolved in 40mL deionized waters and stirred
To clarifying, it is then transferred into 50mL hydrothermal reaction kettles, and is put into a piece of treated nickel foam, 150 DEG C of constant temperature is anti-after sealing
Answer 8h.After after natural cooling, nickel foam is taken out, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C are dried in vacuo 12h,
The last 2h that calcined at 350 DEG C obtains the sour nickel nano-wire array of cobalt.
Accurate to weigh 1mmol nickel nitrates, 1mmol sodium tungstates and 6mmol urea, which are dissolved in 40mL deionized waters, to be stirred to mixed
Close uniform, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettles, and will be previously obtained
The sour nickel nano-wire array foam nickel base of cobalt be put into wherein, 150 DEG C of isothermal reaction 8h after sealing.It is cooled to after room temperature, takes
Go out nickel foam, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C of vacuum dryings finally calcine 2h at 350 DEG C and obtain cobalt
The sour nickel core-shell nano linear array of sour nickel tungsten.
0.31mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in 100mL volume ratios 1 at room temperature:1 second alcohol and water
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after well mixed, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and 20mL 0.380g containing the ammonium persulfate aqueous solution is then added dropwise, and is polymerize in ice-water bath anti-
Answer 8h.Nickel foam is taken out, is alternately washed 3 times with absolute ethyl alcohol, deionized water, the sour nickel tungsten acid of cobalt is obtained after 60 DEG C of vacuum dryings
Nickel/polyaniline tri compound core-shell nano linear array.
Embodiment 4
1mmol nickel nitrates accurately are weighed, 2mmol cobalt nitrates and 8mmol urea are dissolved in 40mL deionized waters and stirred
To clarifying, it is then transferred into 50mL hydrothermal reaction kettles, and is put into a piece of treated nickel foam, 130 DEG C of constant temperature is anti-after sealing
Answer 6h.After after natural cooling, nickel foam is taken out, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C are dried in vacuo 12h,
The last 2h that calcined at 350 DEG C obtains the sour nickel nano-wire array of cobalt.
Accurate to weigh 1mmol nickel nitrates, 1mmol sodium tungstates and 6mmol urea, which are dissolved in 40mL deionized waters, to be stirred to mixed
Close uniform, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettles, and will be previously obtained
The sour nickel nano-wire array foam nickel base of cobalt be put into wherein, 130 DEG C of isothermal reaction 6h after sealing.It is cooled to after room temperature, takes
Go out nickel foam, with alternately washing 3 times of absolute ethyl alcohol, deionized water, 60 DEG C of vacuum dryings finally calcine 2h at 400 DEG C and obtain cobalt
The sour nickel core-shell nano linear array of sour nickel tungsten.
0.40mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in 100mL volume ratios 1 at room temperature:1 second alcohol and water
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after well mixed, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and 20mL 0.380g containing the ammonium persulfate aqueous solution is then added dropwise, and is polymerize in ice-water bath anti-
Answer 10h.Nickel foam is taken out, is alternately washed 3 times with absolute ethyl alcohol, deionized water, the sour nickel tungsten acid of cobalt is obtained after 60 DEG C of vacuum dryings
Nickel/polyaniline tri compound core-shell nano linear array.
Claims (4)
1. a kind of preparation method of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt, it is characterised in that step
It is rapid as follows：
Step 1, at room temperature, by nickel nitrate, cobalt nitrate and urea by the ratio between substance withdrawl syndrome 1:2:8 are dissolved in deionized water
In obtain precursor solution A；Precursor solution A is transferred in hydrothermal reaction kettle after ultrasonic half an hour and a piece of cut is added
Nickel foam, hydro-thermal reaction in baking oven is placed in after sealing, room temperature is then naturally cooled to, nickel foam is taken out, washing, vacuum is done
It is dry, the sour nickel nano-wire array of cobalt is obtained after calcining；
Step 2, at room temperature, by nickel nitrate, sodium tungstate and urea by the ratio between substance withdrawl syndrome 1:1:4 are dissolved in deionized water
In obtain precursor solution B, precursor solution B be transferred in hydrothermal reaction kettle and add step 1 after ultrasonic half an hour obtain
The sour nickel nano-wire array of cobalt, hydro-thermal reaction in baking oven is placed in after sealing, room temperature is then naturally cooled to, nickel foam is taken out, washes
Wash, be dried in vacuo, the sour nickel core-shell nano linear array of the sour nickel tungsten of cobalt is obtained after calcining；
Step 3, that in deionized water/absolute ethyl alcohol in the mixed solvent aniline and p-methyl benzenesulfonic acid ultrasonic disperse are obtained into mixing is molten
Liquid, is transferred in ice bath, and the sour nickel core-shell nano linear array of the sour nickel tungsten of the cobalt that step 2 is obtained is put into mixed solution, slowly
Ammonium persulfate solution is added dropwise, after ice bath reaction terminates, washs, vacuum drying, obtains the sour nickel/polyaniline ternary of the sour nickel tungsten of cobalt and answers
Close nano line array electrode.
2. a kind of preparation of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt according to claim 1
Method, it is characterised in that in step 1,110-150 DEG C of the hydrothermal temperature, time 4-8h；Wash to use anhydrous second respectively
Alternately washing 3 times of alcohol, deionized water, dry to be dried in vacuo 12h, 300-400 DEG C of calcining heat under the conditions of 60-80 DEG C.
3. a kind of preparation of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt according to claim 1
Method, it is characterised in that in step 2,110-150 DEG C of the hydrothermal temperature, time 4-8h washs to use anhydrous second respectively
Alternately washing 3 times of alcohol, deionized water, dry to be dried in vacuo 12h, 300-400 DEG C of calcining heat under the conditions of 60-80 DEG C.
4. a kind of preparation of the sour nickel/polyaniline tri compound nano line array electrode of the sour nickel tungsten of cobalt according to claim 1
Method, it is characterised in that in step 3, the deionized water/absolute ethyl alcohol in the mixed solvent, deionized water and absolute ethyl alcohol body
Product is than being 1:1；The amount ratio of the aniline, p-methyl benzenesulfonic acid and deionized water/absolute ethyl alcohol mixed solvent be 0.20~
0.40mL:0.43g:100mL；The concentration of the ammonium persulfate solution is 19mg/mL；The ammonium sulfate mixes molten with described
The volume ratio of liquid is 1:5；The reaction time is 6-10h, is washed alternately to be washed 3 times with absolute ethyl alcohol, deionized water respectively,
Dry to be dried in vacuo 12h under the conditions of 60-80 DEG C.
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Cited By (4)
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| CN107572604A (en) * | 2017-10-31 | 2018-01-12 | 南阳理工学院 | A kind of preparation method of wolframic acid nanosized nickel rods super capacitor material |
| CN109939707A (en) * | 2019-03-06 | 2019-06-28 | 中国科学院合肥物质科学研究院 | Two cobalt@nickel tungstate nucleocapsid heterojunction material of phosphatization and the preparation method and application thereof |
| CN110354905A (en) * | 2019-08-13 | 2019-10-22 | 哈尔滨理工大学 | A kind of electrolysis water liberation of hydrogen catalyst n iCoP/NF@PANI composite material and preparation method |
| CN111009422A (en) * | 2019-12-10 | 2020-04-14 | 中北大学 | Nickel-based NiCo with core-shell structure2O4Preparation method of polyaniline nano material |
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