CN107180704B - A kind of preparation method of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode - Google Patents
A kind of preparation method of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode Download PDFInfo
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- CN107180704B CN107180704B CN201710342096.3A CN201710342096A CN107180704B CN 107180704 B CN107180704 B CN 107180704B CN 201710342096 A CN201710342096 A CN 201710342096A CN 107180704 B CN107180704 B CN 107180704B
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Abstract
The present invention provides a kind of preparation method of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode, preparation step is as follows: step 1 prepares cobalt acid nickel nano-wire array；Step 2 prepares cobalt acid nickel tungsten acid nickel core-shell nano linear array；Step 3 prepares cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode.The present invention uses hydrothermal synthesis technology, using good conductivity and the nickel foam with loose porous unique texture passes through two step hydro-thermals as substrate and cobalt acid nickel tungsten acid nickel core-shell nano linear array is made, the process of cumbersome production electrode slice had both been avoided in this way, active material utilization can also be effectively improved, increase active surface, improves the diffusion mass transfer performance of material.Polyaniline is deposited to by cobalt acid nickel tungsten acid nickel core-shell nano linear array surface by simple chemical polymerization again and obtains cobalt acid nickel tungsten acid nickel/polyaniline tri compound core-shell nano linear array.
Description
Technical field
The invention belongs to the preparation field of electrode material for super capacitor more particularly to a kind of cobalt acid nickel tungsten acid nickel/polyphenyl
The preparation method of amine tri compound nano line array electrode material.
Background technique
With the continuous development of human society and being constantly progressive for science and technology, the mankind get over the demand of the energy and resource
Come it is bigger, so there is an urgent need to it is some efficiently, cleaning, the sustainable energy and new technology store and convert energy.It is super
Grade capacitor has high power density, quick charge and discharge process, the service life of length, low cost, environmental-friendly and safe
The advantages that, it has also become the new hot spot 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 certain
Deficiency causes overall chemical property to decline.In recent years, with going deep into nano materials research, people are begun trying to material
It is carried out on nanoscale compound.Wherein core-shell nano-composite material (including nm-class core-and-shell particles and nano-array etc.) is
A kind of typical form of nanocomposite, research to the effect that by nano particle or array surface coating or
One layer of new material is wrapped up to assign their new characteristics, and further studies its surface, interface property.It is answered as a kind of orderly
Structure is closed, core-shell nano-composite material shows the incomparable performance of one-component nano material.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano wires
The preparation method of array electrode material, by the compound of material, the synergistic effect between the structure and material of nucleocapsid is effectively mentioned
The high chemical property of composite material.
The present invention is achieved through the following technical solutions:
A kind of preparation method of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode, steps are as follows:
Step 1 prepares cobalt acid nickel nano-wire array: at room temperature, nickel nitrate, cobalt nitrate and urea is dense by the amount of substance
The ratio between degree 1:2:8, which is dissolved in deionized water, obtains 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, sealing is placed on hydro-thermal reaction in baking oven, then naturally cools to room
Temperature takes out nickel foam, washs, and vacuum drying obtains cobalt acid nickel nano-wire array after calcining；
Step 2 prepares cobalt acid nickel tungsten acid nickel core-shell nano linear array: at room temperature, by nickel nitrate, sodium tungstate and urea
It is dissolved in deionized water by the ratio between substance withdrawl syndrome 1:1:4 and obtains precursor solution B, it is after ultrasonic half an hour that presoma is molten
Liquid B is transferred in hydrothermal reaction kettle and is added the cobalt acid nickel nano-wire array that step 1 obtains, and it is anti-that sealing is placed on hydro-thermal in baking oven
It answers, then cooled to room temperature, takes out nickel foam, wash, vacuum drying obtains cobalt acid nickel tungsten acid nickel nucleocapsid and receives after calcining
Nanowire arrays；
Step 3 prepares cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode: by aniline and to toluene sulphur
Sour ultrasonic disperse obtains mixed solution in deionized water/dehydrated alcohol in the mixed solvent, is transferred in ice bath, and step 2 is obtained
To cobalt acid nickel tungsten acid nickel core-shell nano linear array be put into mixed solution, be slowly added dropwise ammonium persulfate solution, ice bath reaction knot
Shu Hou is washed, and vacuum drying obtains cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode.
In step 1,110-150 DEG C of the hydrothermal temperature, time 4-8h；Washing for respectively with dehydrated alcohol, go from
Alternately washing 3 times of sub- water, it is dry be 60-80 DEG C under the conditions of be dried in vacuo 12h, 300-400 DEG C of calcination temperature.
In step 2,110-150 DEG C of the hydrothermal temperature, time 4-8h, wash for respectively with dehydrated alcohol, go from
Alternately washing 3 times of sub- water, it is dry be 60-80 DEG C under the conditions of be dried in vacuo 12h, 300-400 DEG C of calcination temperature.
In step 3, the deionized water/dehydrated alcohol in the mixed solvent, deionized water and dehydrated alcohol volume ratio are 1:
1；The aniline, p-methyl benzenesulfonic acid and deionized water/dehydrated alcohol mixed solvent amount ratio are 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 to use alternately washing 3 times of dehydrated alcohol, deionized water respectively, dry is 60-80
12h is dried in vacuo under the conditions of DEG C.
The processing mode of the nickel foam is as follows: nickel foam cut to the thin slice of growth 1cm wide 1cm, uses acetone respectively,
1mol/L hydrochloric acid, dehydrated alcohol, deionized water supersound washing 20min are then placed in 80 DEG C of dry 6h in vacuum oven.
The utility model has the advantages that
The present invention use hydrothermal synthesis technology, using good conductivity and with loose porous unique texture nickel foam as
Cobalt acid nickel tungsten acid nickel core-shell nano linear array is made by two step hydro-thermals in substrate, has both avoided the mistake of cumbersome production electrode slice in this way
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 cobalt acid nickel tungsten acid nickel core-shell nano linear array surface obtain cobalt acid nickel tungsten acid nickel/poly-
Aniline tri compound core-shell nano linear array.
Detailed description of the invention
Fig. 1 (a) and (b) are respectively scanning electron microscope (SEM) photograph of the cobalt acid nickel under different multiplying in embodiment 1；It (c) is embodiment 1
The scanning electron microscope (SEM) photograph of middle cobalt acid nickel tungsten acid nickel；It (d) is cobalt acid nickel tungsten acid nickel/polyaniline scanning electron microscope (SEM) photograph in embodiment 1.
Fig. 2 (a) is 1 cobalt acid nickel of embodiment, cobalt acid nickel tungsten acid nickel and cobalt acid nickel tungsten acid nickel/polyaniline X-ray diffraction
Map；It (b) is 1 cobalt acid nickel tungsten acid nickel of embodiment/Organic conductor figure.
Fig. 3 (a) is that 1 pure foam nickel of embodiment, cobalt acid nickel, cobalt acid nickel tungsten acid nickel and cobalt acid nickel tungsten acid nickel/polyaniline exist
Sweep speed is 10mV s-1When cyclic voltammetry curve figure；(b) for 1 cobalt acid nickel of embodiment, cobalt acid nickel tungsten acid nickel and cobalt acid nickel/
Nickel tungstate/polyaniline is 1A g in current density-1When constant current charge-discharge figure.
Specific embodiment
The invention will be further described combined with specific embodiments below:
Embodiment 1
1mmol nickel nitrate is accurately weighed, 2mmol cobalt nitrate and 8mmol urea are dissolved in 40mL deionized water and stir
It to clarification, is then transferred into 50mL hydrothermal reaction kettle, and is put into a piece of processed nickel foam, 130 DEG C of constant temperature are anti-after sealing
Answer 6h.After natural cooling, nickel foam is taken out, is alternately washed 3 times, 60 DEG C of vacuum drying 12h with dehydrated alcohol, deionized water,
Finally cobalt acid nickel nano-wire array is obtained in 350 DEG C of calcining 2h.
1mmol nickel nitrate is accurately weighed, 1mmol sodium tungstate and 6mmol urea, which are dissolved in 40mL deionized water, to be stirred to mixed
It closes uniformly, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettle, and will be previously obtained
Cobalt acid nickel nano-wire array foam nickel base be put into wherein, 130 DEG C of isothermal reaction 6h after sealing.After being cooled to room temperature, take
Nickel foam out, with alternately washing 3 times of dehydrated alcohol, deionized water, 60 DEG C of vacuum dryings finally obtain cobalt in 400 DEG C of calcining 2h
Sour nickel tungsten acid nickel core-shell nano linear array.
0.30mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in the second alcohol and water of 100mL volume ratio 1:1 at room temperature
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after mixing, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and the aqueous solution of 20mL 0.38g containing ammonium persulfate, the polymerization reaction in ice-water bath is then added dropwise
6h.Take out nickel foam, with alternately washing 3 times of dehydrated alcohol, deionized water, obtain after 60 DEG C of vacuum dryings cobalt acid nickel tungsten acid nickel/
Polyaniline tri compound core-shell nano linear array.
Fig. 1 (a) and (b) are respectively scanning electron microscope (SEM) photograph of the cobalt acid nickel under different multiplying.It can be seen from the figure that three-dimensional more
The foam nickel surface in hole grown one layer of cobalt acid nickel nano material.After enlargement ratio, it can be seen that a large amount of uniform nanowire-junctions
Structure, in-between width are about 50nm, and length is about 3 μm.Fig. 1 (c) is the scanning electron microscope (SEM) photograph of cobalt acid nickel tungsten acid nickel, it can be seen that
Cobalt acid nickel nanowire surface is wrapped in by wolframic acid nickel particle.Fig. 1 (d) is cobalt acid nickel tungsten acid nickel/polyaniline scanning electron microscope (SEM) photograph.
It can be observed that membrane structure is presented in polyaniline, cobalt acid nickel tungsten acid nickel core-shell nano linear array is connected and wrapped up, is formed
Good three-dimensional conductive structure can be conducive to the electron transfer rate for improving electrode material for super capacitor.Fig. 2 (a) is cobalt
Sour nickel, cobalt acid nickel tungsten acid nickel and cobalt acid nickel tungsten acid nickel/polyaniline X ray diffracting spectrum.It can be seen from the figure that every song
All there is very strong diffraction maximum at 44.8 °, 51.7 ° and 77.2 ° in line, this may be the diffraction maximum of foam nickel base
(JCPDS:04-0850), in addition to 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 square phase cobalt acid nickel, cobalt acid nickel tungsten acid nickel core-shell nano linear array are removed
NiCo2O4Diffraction maximum other than also show other diffraction maximums, correspond respectively to (010) and (- 122) crystal face of nickel tungstate,
Show that nickel tungstate has deposited on cobalt acid nickel nano-wire array.Fig. 2 (b) is cobalt acid nickel tungsten acid nickel/Organic conductor
Figure.3420cm in the figure-1Place is absorption peak caused by H-O-H stretching vibration, illustrates that material surface has physical absorption water.?
1489 and 1572cm-1There is the characteristic peak of the quinoid of C=C stretching vibration absworption peak and polyaniline and benzene-type ring in place, this is poly-
The presence of functional group in aniline.Fig. 3 (a) is pure foam nickel, cobalt acid nickel, cobalt acid nickel tungsten acid nickel and cobalt acid nickel tungsten acid nickel/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 to steep
The specific capacitance very little of foam nickel substrate can thus ignore its influence to the specific capacitance of material.It may also be seen that three
Kind material has a pair of good redox peaks, shows characteristic possessed by typical fake capacitance material.Fig. 3 (b) is cobalt
Sour nickel, cobalt acid nickel tungsten acid nickel and cobalt acid nickel tungsten acid nickel/polyaniline are 1A g in current density-1When constant current charge-discharge figure.
It is 1A g that cobalt acid nickel tungsten acid nickel/polyaniline, which is obtained by calculation, in current density-1When specific capacitance be 1741F g-1, it is higher than cobalt acid
Nickel tungsten acid nickel (1305F g-1) and cobalt acid nickel (706F g-1).This is mainly attributed to three kinds of cobalt acid nickel, nickel tungstate and polyaniline materials
Synergistic effect and the unique appearance structure of trielement composite material are generated between material.
Embodiment 2
1mmol nickel nitrate is accurately weighed, 2mmol cobalt nitrate and 8mmol urea are dissolved in 40mL deionized water and stir
It to clarification, is then transferred into 50mL hydrothermal reaction kettle, and is put into a piece of processed nickel foam, 110 DEG C of constant temperature are anti-after sealing
Answer 4h.After natural cooling, nickel foam is taken out, is alternately washed 3 times, 60 DEG C of vacuum drying 12h with dehydrated alcohol, deionized water,
Finally cobalt acid nickel nano-wire array is obtained in 400 DEG C of calcining 2h.
1mmol nickel nitrate is accurately weighed, 1mmol sodium tungstate and 6mmol urea, which are dissolved in 40mL deionized water, to be stirred to mixed
It closes uniformly, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettle, and will be previously obtained
Cobalt acid nickel nano-wire array foam nickel base be put into wherein, 110 DEG C of isothermal reaction 4h after sealing.After being cooled to room temperature, take
Nickel foam out, with alternately washing 3 times of dehydrated alcohol, deionized water, 60 DEG C of vacuum dryings finally obtain cobalt in 400 DEG C of calcining 2h
Sour nickel tungsten acid nickel core-shell nano linear array.
0.20mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in the second alcohol and water of 100mL volume ratio 1:1 at room temperature
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after mixing, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and the aqueous solution of 20mL 0.38g containing ammonium persulfate, the polymerization reaction in ice-water bath is then added dropwise
8h.Take out nickel foam, with alternately washing 3 times of dehydrated alcohol, deionized water, obtain after 60 DEG C of vacuum dryings cobalt acid nickel tungsten acid nickel/
Polyaniline tri compound core-shell nano linear array.
Embodiment 3
1mmol nickel nitrate is accurately weighed, 2mmol cobalt nitrate and 8mmol urea are dissolved in 40mL deionized water and stir
It to clarification, is then transferred into 50mL hydrothermal reaction kettle, and is put into a piece of processed nickel foam, 150 DEG C of constant temperature are anti-after sealing
Answer 8h.After natural cooling, nickel foam is taken out, is alternately washed 3 times, 60 DEG C of vacuum drying 12h with dehydrated alcohol, deionized water,
Finally cobalt acid nickel nano-wire array is obtained in 350 DEG C of calcining 2h.
1mmol nickel nitrate is accurately weighed, 1mmol sodium tungstate and 6mmol urea, which are dissolved in 40mL deionized water, to be stirred to mixed
It closes uniformly, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettle, and will be previously obtained
Cobalt acid nickel nano-wire array foam nickel base be put into wherein, 150 DEG C of isothermal reaction 8h after sealing.After being cooled to room temperature, take
Nickel foam out, with alternately washing 3 times of dehydrated alcohol, deionized water, 60 DEG C of vacuum dryings finally obtain cobalt in 350 DEG C of calcining 2h
Sour nickel tungsten acid nickel core-shell nano linear array.
0.31mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in the second alcohol and water of 100mL volume ratio 1:1 at room temperature
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after mixing, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and the aqueous solution of 20mL 0.380g containing ammonium persulfate 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 dehydrated alcohol, deionized water, cobalt acid nickel tungsten acid is obtained after 60 DEG C of vacuum dryings
Nickel/polyaniline tri compound core-shell nano linear array.
Embodiment 4
1mmol nickel nitrate is accurately weighed, 2mmol cobalt nitrate and 8mmol urea are dissolved in 40mL deionized water and stir
It to clarification, is then transferred into 50mL hydrothermal reaction kettle, and is put into a piece of processed nickel foam, 130 DEG C of constant temperature are anti-after sealing
Answer 6h.After natural cooling, nickel foam is taken out, is alternately washed 3 times, 60 DEG C of vacuum drying 12h with dehydrated alcohol, deionized water,
Finally cobalt acid nickel nano-wire array is obtained in 350 DEG C of calcining 2h.
1mmol nickel nitrate is accurately weighed, 1mmol sodium tungstate and 6mmol urea, which are dissolved in 40mL deionized water, to be stirred to mixed
It closes uniformly, then mixed solution is transferred in 50mL inner liner polytetrafluoroethylene stainless steel hydrothermal reaction kettle, and will be previously obtained
Cobalt acid nickel nano-wire array foam nickel base be put into wherein, 130 DEG C of isothermal reaction 6h after sealing.After being cooled to room temperature, take
Nickel foam out, with alternately washing 3 times of dehydrated alcohol, deionized water, 60 DEG C of vacuum dryings finally obtain cobalt in 400 DEG C of calcining 2h
Sour nickel tungsten acid nickel core-shell nano linear array.
0.40mL aniline and 0.43g p-methyl benzenesulfonic acid are dissolved in the second alcohol and water of 100mL volume ratio 1:1 at room temperature
In the mixed solvent is simultaneously stirred to being transferred in ice-water bath (0-5 DEG C) after mixing, and the nickel foam that above-mentioned second step is obtained
Substrate is put into mixed solution, and the aqueous solution of 20mL 0.380g containing ammonium persulfate 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 dehydrated alcohol, deionized water, cobalt acid nickel tungsten acid 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 cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode, which is characterized in that step
It is rapid as follows:
Step 1, at room temperature, is dissolved in deionized water by the ratio between substance withdrawl syndrome 1:2:8 for nickel nitrate, cobalt nitrate and urea
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, sealing is placed on hydro-thermal reaction in baking oven, then cooled to room temperature, takes out nickel foam, and washing, vacuum is dry
It is dry, cobalt acid nickel nano-wire array is obtained after calcining；
Step 2, at room temperature, is dissolved in deionized water by the ratio between substance withdrawl syndrome 1:1:4 for nickel nitrate, sodium tungstate and urea
In obtain precursor solution B, precursor solution B be transferred in hydrothermal reaction kettle after ultrasonic half an hour and step 1 is added obtain
Cobalt acid nickel nano-wire array, sealing is placed on hydro-thermal reaction in baking oven, and then cooled to room temperature is taken out nickel foam, washed
It washs, is dried in vacuo, cobalt acid nickel tungsten acid nickel core-shell nano linear array is obtained after calcining；
Step 3, aniline and p-methyl benzenesulfonic acid ultrasonic disperse in deionized water/dehydrated alcohol in the mixed solvent are obtained mixing it is molten
Liquid, the aniline, p-methyl benzenesulfonic acid and deionized water/dehydrated alcohol mixed solvent amount ratio are 0.20~0.40mL:
0.43g:100mL is transferred in ice bath, and by the cobalt acid nickel tungsten acid nickel core-shell nano linear array that step 2 obtains be put into mixing it is molten
In liquid, ammonium persulfate solution is slowly added dropwise, ice bath after reaction, washs, and vacuum drying obtains cobalt acid nickel tungsten acid nickel/polyphenyl
Amine tri compound nano line array electrode.
2. a kind of preparation of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode according to claim 1
Method, which is characterized in that in step 1,110-150 DEG C of the hydrothermal temperature, time 4-8h；Washing is respectively with anhydrous second
Alternately washing 3 times of alcohol, deionized water, it is dry be 60-80 DEG C under the conditions of be dried in vacuo 12h, 300-400 DEG C of calcination temperature.
3. a kind of preparation of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode according to claim 1
Method, which is characterized in that in step 2,110-150 DEG C of the hydrothermal temperature, time 4-8h is washed as respectively with anhydrous second
Alternately washing 3 times of alcohol, deionized water, it is dry be 60-80 DEG C under the conditions of be dried in vacuo 12h, 300-400 DEG C of calcination temperature.
4. a kind of preparation of cobalt acid nickel tungsten acid nickel/polyaniline tri compound nano line array electrode according to claim 1
Method, which is characterized in that in step 3, the deionized water/dehydrated alcohol in the mixed solvent, deionized water and dehydrated alcohol body
Product is than being 1:1；The concentration of the ammonium persulfate solution is 19mg/mL；The volume of the ammonium sulfate and the mixed solution
Than for 1:5；The reaction time is 6-10h, is washed to use dehydrated alcohol, deionized water alternately to wash 3 times respectively, drying is
12h is dried in vacuo under the conditions of 60-80 DEG C.
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| CN109939707B (en) * | 2019-03-06 | 2021-08-24 | 中国科学院合肥物质科学研究院 | Cobaltous phosphide @ nickel tungstate core-shell heterojunction material and 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 |
| CN111009422B (en) * | 2019-12-10 | 2021-10-08 | 中北大学 | Nickel-based NiCo with core-shell structure2O4Preparation method of polyaniline nano material |
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| CN102891016B (en) * | 2012-10-19 | 2016-08-10 | 常州大学 | A kind of cobalt acid nickel graphene composite material and application thereof and preparation method |
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| Title |
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| Nawishta Jabeen.Unique Core−Shell Nanorod Arrays with Polyaniline Deposited into Mesoporous NiCo2O4 Support for High-Performance Supercapacitor Electrodes.《ACS Appl. Mater. Interfaces》.2016,第75卷 * |
| Three-dimensional NiCo2O4@NiWO4 core–shell nanowire arrays for high performance supercapacitors;Sanming Chen等;《J. Mater. Chem》;20170121;第5卷;摘要，experimental部分 * |
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