CN106847547A - Three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor and its preparation - Google Patents
Three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor and its preparation Download PDFInfo
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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
- H01G11/22—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
- H01G11/84—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
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- 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
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Abstract
The present invention relates to a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor and its preparation, described molybdenum bisuphide/Pt/Polypyrrole composite material is made by the following method：(1) 3D MoS are taken2Add into solvent, and carry out ultrasonic disperse；(2) again toward the MoS of step (1)2CTAB is added in solution, stirring forms uniform and stable 3D MoS2Dispersion liquid；(3) again by 3D MoS obtained in step (2)2Dispersion liquid is placed in low temperature environment, adds pyrrole monomer, stirring；(4) continue to instill ammonium persulfate solution toward the solution of step (3), react, separate, wash, dry, that is, obtain purpose product 3D MoS2/ PPy ultracapacitor composites.Compared with prior art, the obtained molybdenum bisuphide/Pt/Polypyrrole composite material electric conductivity of the present invention is excellent, and preparation method is simple, and repeatability is high.
Description
Technical field
The present invention relates to organic/inorganic composite material field, more particularly, to a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole
Composite electrode material for super capacitor and its preparation.
Background technology
With the fast development of global economy, the challenge and the problem of urgent need to resolve that the mankind run into are also more and more.This its
Include the petroleum fuel of increasingly depleted and its problem of environmental pollution being derived.
The appearance of ultracapacitor is undoubtedly a revolutionary development in energy storage field, and ultracapacitor is provided simultaneously with
Power density and energy density higher, is the novel energy storage apparatus between secondary cell and traditional capacitor.Super electricity
Container have have extended cycle life, energy density is high, power density is big, low production cost, operating temperature range wide and safety, pollution
Small the advantages of, by the extensive concern of researcher in the past few decades, in portable type electronic product, mobile communication and electronic
It is used widely in the fields such as automobile.
Ultracapacitor can be divided into symmetric form ultracapacitor and asymmetric type supercapacitor, to obtain energy higher
Density, compared to symmetric form ultracapacitor, asymmetric type supercapacitor has broader practice prospect.At present, mostly
Number research all concentrates on the positive electrode for developing new excellent performance, and the research and development of negative material are little.Ultracapacitor is total
Capacity can be according to formula：1/C=1/C++ 1/C_ is calculated.According to formula, the overall performance of capacitor depends on negative material.Mesh
Before, conventional negative material-carbon-based material, because of its relatively low specific capacity (about 300F/g), limit ultracapacitor enters one
Step application.Thus, the exploitation to negative material is significant.
Stratiform MoS2Due to reasons such as two dimension (2D) layer structure of its uniqueness and larger specific surface areas so that MoS2Tool
There are electric transmission speed faster and theoretical specific capacitance higher, these superior performances are MoS2As a kind of outstanding electrode
Material provides precondition.Meanwhile, MoS2As a kind of important inorganic material, with excellent chemical stability, make
It can be used as a kind of excellent electrode material for super capacitor.However, the MoS of brand-new2During drying is post-processed, easily
Easily reunite, so as to reduce MoS2Itself there is the characteristic of active reaction sites high as sheet layer material.Therefore, in reality
Border is used during 2D sheet layer materials, it is necessary to solve the problems, such as to reunite.
PPy as conducting polymer important component, with electrical conductivity higher, preferable chemical stability and height
Specific capacitance and paid close attention to by domestic and foreign scholars.Yet with conductive polymer electrodes material mechanical property it is not good,
Cyclical stability is poor, so as to limit the extensive use of material.While the material of one-dimensional nano structure, due to the one of its uniqueness
Dimension structure, and has specific surface area and excellent electrical conductivity higher, much with special construction (core shell structure, shuttle-type and fixed
To arrangement) electrode material be reported out, and with excellent performance of the supercapacitor.Therefore, by one-dimensional material
(PPy fibers) and inorganic material (MoS2) be combined, it is the extremely feasible direction of the electrode material that excellent performance is obtained.
The content of the invention
The purpose of the present invention is exactly to provide a kind of sulphur of three-dimensional tubulose two for the defect for overcoming above-mentioned prior art to exist
Change molybdenum/polypyrrole composite electrode material for super capacitor and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor, including as inorganic skeleton
3D MoS2, and with the 3D MoS2It is crosslinked and constitutes the PPy nanofibers of network structure.
As the preferred of above-mentioned technical proposal, described 3D MoS2A diameter of 400-500nm；
3D MoS2It is 1 with the mass ratio of PPy:10-2:1.
A kind of preparation method of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor, including it is following
Step：
(1) 3D MoS are taken2Add into the mixed solution of oxalic acid and absolute ethyl alcohol, and carry out ultrasonic disperse；
(2) again toward the MoS of step (1)2CTAB (cetyl trimethylammonium bromide) is added in solution, stirring forms uniform
The 3D MoS of stabilization2Dispersion liquid；
(3) again by 3D MoS obtained in step (2)2Dispersion liquid is placed in low temperature environment, adds pyrrole monomer, and stirring makes pyrrole
Monomer absorption is coughed up in 3D MoS2Surface；
(4) continue to instill ammonium persulfate solution toward the solution of step (3), react, separate, wash, dry, that is, obtain mesh
Product 3D MoS2/ PPy ultracapacitor composites.
As the preferred of above-mentioned technical proposal, the 3D MoS described in step (1)2It is made by the following method：
Take S powder and ammonium molybdate is added into the mixed solvent of n-octyl amine and absolute ethyl alcohol, stir, be transferred to reactor
Interior, heating response, cooling is separated, and washing is dried, that is, obtain 3D MoS2。
As the further preferred of above-mentioned technical proposal, the ratio between the addition of S powder, ammonium molybdate, n-octyl amine and absolute ethyl alcohol
It is 1g：(2-3)g：(0.15-0.2)L：(0.15-0.2)L；
The process conditions of heating response are：18-36h is reacted at 180-220 DEG C.
As the preferred of above-mentioned technical proposal, step (1) 3D MoS2Concentration be 0.05-0.3g/60mL；
Described solvent is sour and absolute ethyl alcohol mixed solvent, wherein, both volume ratios are 1:1, acid is oxalic acid or salt
Acid.It is furthermore preferred that the concentration of oxalic acid is 0.35M, the concentration of hydrochloric acid is 1M.It is furthermore preferred that acid is oxalic acid.Oxalic acid is compared to salt
Acid, can improve the energy storage property of PPy, improve the ability that electrolyte ion enters material.
Used as the preferred of above-mentioned technical proposal, the concentration of CTAB is 0.06-0.15M in step (2).It is too low to form particle
The PPy of shape；When too high, the PPy of sheet can be formed.
Used as the preferred of above-mentioned technical proposal, the temperature of the low temperature environment described in step (3) is 0-5 DEG C.Temperature is too low
When, it is unfavorable for the generation of reaction, reduce efficiency；When temperature is too high, reaction can be made acutely to occur, pattern homogeneous cannot be controlled.
As the preferred of above-mentioned technical proposal, 3D MoS in step (3)2It is 1 with the mass ratio of pyrrole monomer:10-2:1.
If not in this range, too low or too high, the chemical property of electrode material can be all reduced.
Used as the preferred of above-mentioned technical proposal, the ammonium persulfate instilled in step (4) is 1 with the mol ratio of pyrrole monomer:
1, the reaction time is 18-36h.The too short reaction time can be such that the reaction cannot carries out completely；The long reaction time will reduce anti-
The efficiency answered.
Used as the preferred of such scheme, the time of ultrasonic disperse is 30-60min in step (1)；Stirring in step (2)
Time is 6h；The time of stirring is 5-6h in step (3)；The specific method of washing is in step (4)：Absolute ethyl alcohol and deionization
Water alternating centrifugal is washed to neutrality, and centrifugal rotational speed is 4000r/min, and centrifugation time is 5min；Drying condition is vacuum at 60 DEG C
Dry.
Described electrode material is 3D MoS at low ambient temperatures2As inorganic skeleton, using cetyl trimethyl bromine
Change ammonium (CTAB) as surfactant, ammonium persulfate is oxidant, by situ chemical oxidative polymerization method, will conductance higher
The PPy of rate is first with 3D MoS2It is hard template, is coated on 3D MoS2Surface, then forms nanofiber by soft template of CTAB,
So as to form the network structure being cross-linked with each other, there is provided good conductive network passage.Obtained composite of the invention has
Larger specific surface area, electrical conductivity higher and excellent chemical property, are that a kind of ultracapacitor of excellent performance is born
Pole material.When current density is 1A/g, specific capacity reaches 462F/g, and after discharge and recharge 2000 times, capacity can still retain original
The 82% of beginning capacity.Preparation method of the present invention is simple, the advantages of repeatable high.
The present invention is using 3D MoS2As composite inorganic skeleton, by the method for in situ chemical oxidative polymerization, will lead
Electric PPy fibers are successfully combined with it, form good conductive network passage, have been obtained with Fabrication of High Specific Capacitance and stable circulation
The electrode material for super capacitor of excellent performance.3D MoS2With larger specific surface area, specific capacity high and excellent circulation
Stability, and PPy nanofibers have electrical conductivity higher, while fake capacitance can be produced and there is specific capacity higher.
By PPy and 3D MoS2It is compound, it is possible to use the cooperative effect of the two, improve the overall chemical property of electrode material.
Compared with prior art, the present invention has advantages below：
(1) 3D MoS prepared by the present invention2/ PPy combination electrode materials, can be used as a kind of level capacitor of super excellent performance
Negative material.
(2) it is of the invention with pyrroles as monomer, in 3D MoS2Surface in situ oxidation polymerization, preparation method is simple, and yield is high.
(3) present invention is with 3D MoS2It is inorganic skeleton, it is to avoid sheet MoS2The problem easily reunited, meanwhile, also improve
The overall reactivity site of composite, while for electrolyte ion provides quick passage, improve composite
Ion transport capacity and storage capacity.
(4) 3D MoS of the present invention2/ PPy composite electrode material for super capacitor combines 3D MoS2With PPy fibers
Respective advantage, using the cooperative effect of the two, improves the overall specific capacitance and its electrochemical cycle stability of composite
Performance.
Brief description of the drawings
Fig. 1 is 3D MoS prepared by the present invention2Transmission electron microscope (TEM) shape appearance figure；
Fig. 2 is the 3D MoS of embodiment 12Flied emission Scanning Electron microscope (FESEM) of/PPy composite powder materials；
Fig. 3 is the different 3D MoS that the present invention is prepared2The performance of the supercapacitor of/PPy composite powder materials；
Fig. 4 is the 3D MoS in embodiment 12The stable circulation performance of/PPy composite powder materials.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of 3D MoS2/ PPy composite electrode material for super capacitor, the composite is to use 3D MoS2As composite wood
Material inorganic skeleton, by in-situ polymerization, by conducting polymer PPy fibers and 3D MoS2It is combined, has been obtained with height
Specific volume and the excellent composite electrode material for super capacitor of stable circulation performance.3D MoS in composite2With pyrrole monomer
Mass ratio is 1:5.
The above-mentioned electrode material preparation method with excellent performance of the supercapacitor is as follows：
(1)3D MoS2Preparation：The ammonium molybdate of the S powder of 77.0mg and 185.4mg is added to 14mL n-octyl amines and 13mL
In the mixed solvent of both absolute ethyl alcohols, after stirring 20min, it is transferred in the ptfe autoclave of 80mL.It is anti-at 200 DEG C
Answer 24h.Reaction terminate after, after being cooled to room temperature, be centrifuged and with deionized water, absolute ethyl alcohol cyclic washing after, 60 DEG C very
Dried to constant weight in empty baking oven.Can obtain 3D MoS2。
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.1g2Add to 30mL 1M HCl and 30mL without
In water-ethanol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to adding CTAB 1.82g, magnetic in solution
Power stirs 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control after 2 DEG C or so, add 0.5g
Pyrrole monomer, magnetic agitation 5h makes pyrrole monomer uniform adsorption in 3D MoS2Surface.1.6580g persulfuric acid will then be dissolved
The 10mL aqueous solution of ammonium is added dropwise in above-mentioned mixed dispersion liquid, and 24h is reacted at 2 DEG C.After question response terminates, it is centrifuged and spends
After ionized water and absolute ethyl alcohol cyclic washing, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D MoS2/ PPy is combined
Dusty material, is designated as 5PW1Mo.
Pure PPy is prepared using identical step, is designated as W-PPy.
(3) Fig. 1 is pure 3D MoS2Transmission electron micrograph, as shown in Figure 1, pure 3D MoS2In a tubular form, and diameter
Size is 400-500nm.Fig. 2 is the three-dimensional tubulose 3D MoS for obtaining2The scanning electron microscope diagram piece of/PPy composites, it is multiple
After conjunction, PPy is first with tubulose 3D MoS2It is hard template, is coated on 3D MoS2Surface, then with CTAB as soft template, forms PPy
Nanofibrous structures, so as to form the network structure being cross-linked with each other, there is provided good conductive network passage.
(4) electrochemical property test is pressed active material, acetylene black and binding agent using three electrode test systems of standard
After ratio is well mixed, it is coated in nickel foam as working electrode, 1x1cm2Platinized platinum make to electrode, saturated calomel electrode conduct
Reference electrode, electrolyte solution is 0.5M Na2SO4.Carry out cyclic voltammetry and different electric currents under different scanning rates
Constant current charge-discharge under density, and potential range is-0.2-- 0.8V.Fig. 3 is the cyclic voltammetric in the case where sweep speed is 5mV/s
Curve (a) and current density be 1A/g under, it is constant current charge-discharge curve (b) to measure.From calculating, obtained combination electrode
When current density is 1A/g, specific capacity is 462F/g to material.Fig. 4 is the electrochemical cycle stability performance of combination electrode material,
Under the current density of 3A/g, after discharge and recharge 2000 times, specific capacity still maintains the 82% of initial capacity, is being filled far above pure PPy
After electric discharge 2000 times, the 55% of initial capacity is maintained
Embodiment 2
A kind of 3D MoS2/ PPy composite electrode material for super capacitor, the composite is to use 3D MoS2As composite wood
Material inorganic skeleton, by in-situ polymerization, by conducting polymer PPy fibers and 3D MoS2It is combined, has been obtained with height
Specific volume and the excellent composite electrode material for super capacitor of stable circulation performance.3D MoS in composite2With pyrrole monomer
Mass ratio is 1:1.
The above-mentioned electrode material preparation method with excellent performance of the supercapacitor is as follows：
(1)3D MoS2Preparation according to embodiment 1.
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.1g2Add to 30mL 0.35M oxalic acid and 30mL
In absolute ethyl alcohol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to adding CTAB 1.82g in solution,
Magnetic agitation 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control after 2 DEG C or so, add
The pyrrole monomer of 0.1g, magnetic agitation 5h makes pyrrole monomer uniform adsorption in 3D MoS2Surface.0.3280g mistakes will then be dissolved
The 10mL aqueous solution of ammonium sulfate is added dropwise in above-mentioned mixed dispersion liquid, and 24h is reacted at 2 DEG C.After question response terminates, centrifugation is simultaneously
After with deionized water and absolute ethyl alcohol cyclic washing, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D MoS2/PPy
Composite powder material, is designated as 1PW1Mo.
Under conditions of current density is 1A/g, specific capacity is 248F/g to obtained combination electrode material.
Embodiment 3
A kind of 3D MoS2/ PPy composite electrode material for super capacitor, the composite is to use 3D MoS2As composite wood
Material inorganic skeleton, by in-situ polymerization, by conducting polymer PPy fibers and 3D MoS2It is combined, has been obtained with height
Specific volume and the excellent composite electrode material for super capacitor of stable circulation performance.3D MoS in composite2With pyrrole monomer
Mass ratio is 2:1.
The above-mentioned electrode material preparation method with excellent performance of the supercapacitor is as follows：
(1)3D MoS2Preparation according to embodiment 1.
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.2g2Add to 30mL 0.35M oxalic acid and 30mL
In absolute ethyl alcohol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to adding CTAB 1.82g in solution,
Magnetic agitation 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control after 2 DEG C or so, add
The pyrrole monomer of 0.1g, magnetic agitation 5h makes pyrrole monomer uniform adsorption in 3D MoS2Surface.0.3280g mistakes will then be dissolved
The 10mL aqueous solution of ammonium sulfate is added dropwise in above-mentioned mixed dispersion liquid, and 24h is reacted at 2 DEG C.After question response terminates, centrifugation is simultaneously
After with deionized water and absolute ethyl alcohol cyclic washing, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D MoS2/PPy
Composite powder material, is designated as 1PW2Mo.
Under conditions of current density is 1A/g, specific capacity is 211F/g to obtained combination electrode material
Embodiment 4
A kind of 3D MoS2/ PPy composite electrode material for super capacitor, the composite is to use 3D MoS2As composite wood
Material inorganic skeleton, by in-situ polymerization, by conducting polymer PPy and MoS2Be combined, be obtained with Fabrication of High Specific Capacitance and
The excellent composite electrode material for super capacitor of stable circulation performance.3D MoS in composite2With the mass ratio of pyrrole monomer
It is 1:2, it is designated as 2PW1Mo.
The above-mentioned electrode material preparation method with excellent performance of the supercapacitor is as follows：
(1)3D MoS2Preparation according to embodiment 1.
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.1g2Add to 30mL 0.35M oxalic acid and 30mL
In absolute ethyl alcohol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to being added to CTAB in solution
1.82g, magnetic agitation 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control after 2 DEG C or so,
Adding the pyrrole monomer of 0.2g, magnetic agitation 5h makes pyrrole monomer uniform adsorption in 3D MoS2Surface.Then will dissolving
The 10mL aqueous solution of 0.6540g ammonium persulfates is added dropwise in above-mentioned mixed dispersion liquid, and 24h is reacted at 2 DEG C.Question response terminates
Afterwards, be centrifuged and with deionized water and absolute ethyl alcohol cyclic washing after, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D
MoS2/ PPy composite powder materials, are designated as 2PW1Mo.
Under conditions of current density is 1A/g, specific capacity is 257F/g to obtained combination electrode material；
Embodiment 5
A kind of 3D MoS2/ PPy composite electrode material for super capacitor, the composite is to use 3D MoS2As composite wood
Material inorganic skeleton, by in-situ polymerization, by conducting polymer PPy fibers and MoS2It is combined, has been obtained and has compared with high
Hold and the excellent composite electrode material for super capacitor of stable circulation performance.3DMoS in composite2With the quality of pyrrole monomer
Than being 1:10.
The above-mentioned electrode material preparation method with excellent performance of the supercapacitor is as follows：
(1)3D MoS2Preparation according to embodiment 1.
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.1g2Add to 30mL 1M HCl and 30mL without
In water-ethanol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to adding CTAB 1.82g, magnetic in solution
Power stirs 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control after 2 DEG C or so, add 1.0g
Pyrrole monomer, magnetic agitation 5h makes pyrrole monomer uniform adsorption in 3D MoS2Surface.3.3160g persulfuric acid will then be dissolved
The 10mL aqueous solution of ammonium is added dropwise in above-mentioned mixed dispersion liquid, and 24h is reacted at 2 DEG C.After question response terminates, it is centrifuged and spends
After ionized water and absolute ethyl alcohol cyclic washing, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D MoS2/ PPy is combined
Dusty material, is designated as 10PW1Mo.
Under conditions of current density is 1A/g, specific capacity is 183F/g to obtained combination electrode material.
Embodiment 6
The 3D MoS of the present embodiment2/ PPy composites compared with Example 1, except 3D MoS2Preparation technology it is different
Outward, remaining is all.
Specially：
3D MoS2Preparation：By the ammonium molybdate of the S powder of 70.0mg and 140.0mg add to 14mL n-octyl amines and 14mL without
In the mixed solvent of both water-ethanols, after stirring 20min, it is transferred in the ptfe autoclave of 80mL.Reacted at 220 DEG C
18h.Reaction terminate after, after being cooled to room temperature, be centrifuged and with deionized water, absolute ethyl alcohol cyclic washing after, in 60 DEG C of vacuum
Dried to constant weight in baking oven.Can obtain 3D MoS2。
Embodiment 7
The 3D MoS of the present embodiment2/ PPy composites compared with Example 1, except 3D MoS2Preparation technology it is different
Outward, remaining is all.
Specially：
3D MoS2Preparation：The ammonium molybdate of the S powder of 60.0mg and 180.0mg is added anhydrous with 9mL to 9mL n-octyl amines
In the mixed solvent of both ethanol, after stirring 20min, it is transferred in the ptfe autoclave of 80mL.Reacted at 180 DEG C
36h.Reaction terminate after, after being cooled to room temperature, be centrifuged and with deionized water, absolute ethyl alcohol cyclic washing after, in 60 DEG C of vacuum
Dried to constant weight in baking oven.Can obtain 3D MoS2。
Embodiment 8
A kind of electrode material with excellent performance of the supercapacitor, its preparation method is as follows：
(1)3D MoS2Preparation according to embodiment 1.
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.1g2Add to 30mL 1M HCl and 30mL without
In water-ethanol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to CTAB is added in solution, make its concentration
About 0.06M, magnetic agitation 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control at 0 DEG C or so
Afterwards, adding the pyrrole monomer of 0.5g, magnetic agitation 5.5h makes pyrrole monomer uniform adsorption in 3D MoS2Surface.Then will dissolving
The 10mL aqueous solution of 1.6580g ammonium persulfates is added dropwise in above-mentioned mixed dispersion liquid, and 36h is reacted at 0 DEG C.Question response terminates
Afterwards, be centrifuged and with deionized water and absolute ethyl alcohol cyclic washing after, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D
MoS2/ PPy composite powder materials.
Embodiment 9
A kind of electrode material with excellent performance of the supercapacitor, its preparation method is as follows：
(1)3D MoS2Preparation according to embodiment 1.
(2)3D MoS2The preparation of/PPy composites：By the 3D MoS of 0.1g2Add to 30mL 0.35M oxalic acid and 30mL
In absolute ethyl alcohol mixed solution, ultrasonic 30min makes 3D MoS2It is dispersed；Then to CTAB is added in solution, make its dense
Degree is about 0.06M, magnetic agitation 6h；After uniform dispersion liquid to be formed, using circulating condensing machine and make solution temperature control on 1 DEG C of left side
Behind the right side, the pyrrole monomer of 1.0g, magnetic agitation 6h is added to make pyrrole monomer uniform adsorption in 3D MoS2Surface.Then will dissolving
The 10mL aqueous solution of 3.3160g ammonium persulfates is added dropwise in above-mentioned mixed dispersion liquid, and 18h is reacted at 1 DEG C.Question response terminates
Afterwards, be centrifuged and with deionized water and absolute ethyl alcohol cyclic washing after, dried to constant weight in 60 DEG C of vacuum drying ovens.Can obtain 3D
MoS2/ PPy composite powder materials.
The above-mentioned description to embodiment is to be understood that and use invention for ease of those skilled in the art.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel announcement of the invention, does not depart from improvement that scope made and modification all should be of the invention
Within protection domain.
Claims (10)
1. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor, it is characterised in that including as nothing
The 3D MoS of machine skeleton2, and with the 3D MoS2It is crosslinked and constitutes the PPy nanofibers of network structure.
2. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 1, its
It is characterised by, described 3D MoS2A diameter of 400-500nm.
3. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 1, its
It is characterised by, 3D MoS2It is 1 with the mass ratio of PPy:10-2:1.
4. three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor as described in claim 1-3 is any
Preparation method, it is characterised in that comprise the following steps：
(1) 3D MoS are taken2Add into solvent, and carry out ultrasonic disperse；
(2) again toward the MoS of step (1)2CTAB is added in solution, stirring forms uniform and stable 3D MoS2Dispersion liquid；
(3) again by 3D MoS obtained in step (2)2Dispersion liquid is placed in low temperature environment, adds pyrrole monomer, stirring；
(4) continue to instill ammonium persulfate solution toward the solution of step (3), react, separate, wash, dry, that is, obtain purpose product
Thing 3D MoS2/ PPy ultracapacitor composites.
5. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 4
Preparation method, it is characterised in that the 3D MoS described in step (1)2It is made by the following method：
Take S powder and ammonium molybdate added into the mixed solvent of n-octyl amine and absolute ethyl alcohol, stir, be transferred in reactor,
Heating response, cooling is separated, and washing is dried, that is, obtain 3D MoS2。
6. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 5
Preparation method, it is characterised in that the ratio between addition of S powder, ammonium molybdate, n-octyl amine and absolute ethyl alcohol is 1g：(2-3)g：(0.15-
0.2)L：(0.15-0.2)L；
The process conditions of heating response are：18-36h is reacted at 180-220 DEG C.
7. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 4
Preparation method, it is characterised in that step (1) 3D MoS2Concentration be 0.05-0.3g/60mL；
Described solvent is sour and absolute ethyl alcohol mixed solvent, wherein, both volume ratios are 1:1, acid is oxalic acid or hydrochloric acid.
8. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 4
Preparation method, it is characterised in that the concentration of CTAB is 0.06-0.15M in step (2).
9. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 4
Preparation method, it is characterised in that the temperature of the low temperature environment described in step (3) is 0-5 DEG C；
3D MoS in step (3)2It is 1 with the mass ratio of pyrrole monomer:10-2:1.
10. a kind of three-dimensional tubulose molybdenum bisuphide/polypyrrole composite electrode material for super capacitor according to claim 4
Preparation method, it is characterised in that the ammonium persulfate instilled in step (4) is 1 with the mol ratio of pyrrole monomer:1, the reaction time is
18-36h。
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| CN110331124A (en) * | 2019-06-14 | 2019-10-15 | 浙江大学 | A kind of electric polypyrrole/extracellular matrix laminated film and preparation method thereof |
| CN110885555A (en) * | 2019-09-07 | 2020-03-17 | 宁波大学 | Metal sulfide/conductive polymer composite material and preparation method thereof |
| CN112490449A (en) * | 2020-11-30 | 2021-03-12 | 胡冲丽 | Three-dimensional tubular molybdenum disulfide composite bacterial cellulose membrane electrode material and preparation method thereof |
| CN112713011A (en) * | 2020-12-23 | 2021-04-27 | 杭州电子科技大学 | Method for preparing super capacitor with double-conducting network |
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| CN110885555B (en) * | 2019-09-07 | 2022-02-01 | 宁波大学 | Metal sulfide/conductive polymer composite material and preparation method thereof |
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