CN105261489A - Preparation method and application of PPy/MoS2/Ni3S2 composite material - Google Patents

Preparation method and application of PPy/MoS2/Ni3S2 composite material Download PDF

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CN105261489A
CN105261489A CN201510752176.7A CN201510752176A CN105261489A CN 105261489 A CN105261489 A CN 105261489A CN 201510752176 A CN201510752176 A CN 201510752176A CN 105261489 A CN105261489 A CN 105261489A
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composite material
ppy
preparation
mos
nickel foam
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CN105261489B (en
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王秀华
高杰
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Anhui Normal University
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Anhui Normal University
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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 preparation method and application of PPy/MoS2/Ni3S2 composite material. The preparation method of PPy/MoS2/Ni3S2 composite material comprises the steps: in the hydrochloric acid solution or sodium hyposulfite solution, pyrroles monomers are polymerized on the surface of nickel foam, and a layer of polypyrrole is formed on the cleaned surface of nickel foam; chemical liquid phase deposition reaction for the layer of polypyrrole, MoO3 and thiourea occurs in the aqueous solution; and then the linear PPy/MoS2/Ni3S2 composite material can be obtained. The preparation method of PPy/MoS2/Ni3S2 composite material has the advantages of being simple in preparation technology, being low in cost, having a super long one-dimensional morphology structure, being superior in performance, being high in specific capacitance, and being high in cycling stability, and can be used as the electrode material for a super capacitor.

Description

A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material and application
Technical field
Composite material technology of preparing of the present invention and electrochemistry crossing domain, be specifically related to a kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material and application.
Background technology
In the sulfide of transition metal, due to the character that it has unique physics and chemistry, thus have a wide range of applications in fields such as catalysis, electrochemistry and gas sensors, thus cause the high interest of people.Conducting polymer due to its high-energy-density, low cost, be easy to the feature such as synthesis, good thermal stability and environmental friendliness, be also the focus of research.But the composite material of transient metal sulfide and conducting polymer is but seldom in the news.
Summary of the invention
The invention provides a kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, the present invention utilizes liquid phase synthesizing method to prepare PPy/MoS 2/ Ni 3s 2composite material.Its preparation technology is simple, with low cost, and has the one dimension appearance structure of overlength, superior performance.
Present invention also offers PPy/MoS 2/ Ni 3s 2composite material is as the application of electrode material for super capacitor.
The technical scheme that the present invention takes is:
A kind of PPy/MoS 2/ Ni 3s 2composite material, described composite material is polymerized by the surface of pyrrole monomer in nickel foam in hydrochloric acid solution or hypo solution, forms one deck polypyrrole on nickel foam surface, then by itself and MoO 3, thiocarbamide composition the aqueous solution to carry out chemical liquid deposition reaction obtained.
The invention also discloses a kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, described preparation method comprises the following steps:
(a) cleaning nickel foam;
Nickel foam after (b) cleaning and pyrroles's stirring reaction in reactant liquor, cleaning, dry, obtain the nickel foam that surface recombination has polypyrrole;
C surface recombination is had nickel foam, the MoO of polypyrrole by () 3, thiocarbamide reacts in aqueous, cleaning, dry, can obtain PPy/MoS 2/ Ni 3s 2composite material.
Reaction time in described step (b) is 8 ~ 16 hours.
Reactant liquor in described step (b) be PH be less than 7 hydrochloric acid solution or concentration be the hypo solution of 1.6 ~ 1.7g/L.
In described step (b), the mass concentration of pyrroles is 10 ~ 20mg/ml, and the top surface area of nickel foam is 6cm with the ratio of the volume of reactant liquor 2: (25 ~ 90) ml.
Reaction temperature in described step (c) is 155-170 DEG C, and the time is 10-12h; Being preferably reaction temperature is 160 DEG C, time 11.5h.
In described step (c), MoO 3, thiocarbamide mass concentration be respectively 1.0 ~ 1.5mg/mL, 2.0 ~ 2.5mg/mL; The top surface area of nickel foam is 6cm with the ratio of the volume of the aqueous solution 2: (25 ~ 40) ml; Be preferably, MoO 3, thiocarbamide mass concentration be respectively 1.3 ~ 1.5mg/mL, 2.0 ~ 2.2mg/mL; The top surface area of nickel foam is 6cm with the ratio of the volume of the aqueous solution 2: 30ml.
Described PPy/MoS 2/ Ni 3s 2composite material is linear nano structure.
Present invention also offers the PPy/MoS prepared by described preparation method 2/ Ni 3s 2composite material is as the application of electrode material for super capacitor.PPy/MoS 2/ Ni 3s 2composite material possesses that ratio capacitance is large, the performance of good cycling stability, can be used as the electrode material of ultracapacitor.
The present invention is by hydrochloric acid solution or hypo solution, and pyrrole monomer is polymerized on the surface of nickel foam, forms one deck polypyrrole on the nickel foam surface cleaned up, then by itself and MoO 3, thiocarbamide carries out chemical liquid deposition reaction at the aqueous solution, thus obtains the PPy/MoS of wire 2/ Ni 3s 2composite material.
PPy/MoS disclosed by the invention 2/ Ni 3s 2the preparation method of composite material, be a kind of simple to operate, with low cost, mild condition, environmental protection chemical liquid deposition.Without the need to adding any stabilizer, template or surfactant in course of reaction, the convenient post-treatment of product, is easy to regulate and control the size of material and pattern, is applicable to large-scale production.
PPy/MoS disclosed by the invention 2/ Ni 3s 2the PPy/MoS that the preparation method of composite material obtains 2/ Ni 3s 2composite material is the electrode material of the ultracapacitor of excellent performance, under 1A/g current density, and PPy/MoS 2/ Ni 3s 2the ratio capacitance of composite material can reach 2213.2F/g; After 3000 cycle charge-discharges, PPy/MoS 2/ Ni 3s 2the electric capacity of composite material is still identical with initial capacitance, and PPy/MoS is described 2/ Ni 3s 2composite material has good stability.
Accompanying drawing explanation
Fig. 1 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2scanning electron microscopy (SEM) figure of composite material;
Fig. 2 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2transmission electron microscope (TEM) figure of composite material;
Fig. 3 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2x-ray energy spectrum (EDX) figure of composite material;
Fig. 4 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2x-ray photoelectron spectroscopy (XPS) figure of composite material;
Fig. 5 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2x-ray diffraction pattern (XRD) figure of composite material;
Fig. 6 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2the AC impedance curve of composite material before discharge and recharge and after 100 circle circulations;
Fig. 7 be enforcement 1 prepare PPy/MoS 2/ Ni 3s 2the cyclic voltammetry curve of composite material;
Fig. 8 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2the constant current charge-discharge curve of composite material under different current density;
Fig. 9 is PPy/MoS prepared by enforcement 1 2/ Ni 3s 2composite material is circulation-ratio capacitance curve when current density is 4A/g.
Embodiment
The present invention's nickel foam used, pyrroles, MoO 3, thiocarbamide all sale producer from the market directly can buy and obtains.
Embodiment 1
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 15min;
B nickel foam after cleaning is positioned in 250mL beaker by (), add the hydrochloric acid solution 90ml that PH is 3, stirs and adds 1mL pyrroles, Keep agitation 12h, react rear to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, Pt/Polypyrrole composite material one;
C () adds MoO in a kettle. successively 340mg, after thiocarbamide 60mg, 30mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 160 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 2
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam after cleaning is positioned in 100mL beaker by (), add the hydrochloric acid solution 65ml that PH is 4, stirs and adds 1mL pyrroles, Keep agitation 14h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 343mg, after thiocarbamide 65mg, 30mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 160 DEG C, reacts 11.5h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 3
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam after cleaning is positioned in 250mL beaker by (), add the hydrochloric acid solution 50ml that PH is 5, stirs and adds 1mL pyrroles, Keep agitation 13h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 338.5mg, after thiocarbamide 62mg, 30mL deionized water and stirring 20min, adds the obtained composite material of step (b), at 160 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 4
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam after cleaning is positioned in 100mL beaker by (), add the hydrochloric acid solution 30ml that PH is 1.5, stirs and adds 0.6mL pyrroles, Keep agitation 8h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 340mg, after thiocarbamide 66mg, 30mL deionized water and stirring 20min, adds the obtained composite material of step (b), at 160 DEG C, reacts 10h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 5
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 15min;
B nickel foam after cleaning is positioned in 200mL beaker by (), add the hydrochloric acid solution 85ml that PH is 6.5, stirs and adds 0.85mL pyrroles, Keep agitation 16h, take out nickel sheet to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 342mg, after thiocarbamide 61mg, 30mL deionized water and stirring 20min, adds the obtained composite material of step (b), at 160 DEG C, reacts 11h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 6
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 15min;
B nickel foam after cleaning is positioned in 100mL beaker by (), add the hydrochloric acid solution 40ml that PH is 2.5, stirs and adds 0.8mL pyrroles, Keep agitation 10h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 342mg, after thiocarbamide 61mg, 30mL deionized water and stirring 20min, adds the obtained composite material of step (b), at 160 DEG C, reacts 11h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 7
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 15min;
B nickel foam after cleaning is positioned in 100mL beaker by (), add the hydrochloric acid solution 20ml that PH is 0..5, stirs and adds 0.2mL pyrroles, Keep agitation 8h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 339mg, after thiocarbamide 62.5mg, 30mL deionized water and stirring 20min, adds the obtained composite material of step (b), at 160 DEG C, reacts 11h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 8
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 15min;
B nickel foam after cleaning is positioned in 250mL beaker by (), add the hydrochloric acid solution 90ml that PH is 3, stirs and adds 1mL pyrroles, Keep agitation 12h, react rear to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, Pt/Polypyrrole composite material one;
C () adds MoO in a kettle. successively 325mg, after thiocarbamide 50mg, 25mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 155 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 9
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam after cleaning is positioned in 100mL beaker by (), add the hydrochloric acid solution 65ml that PH is 4, stirs and adds 1mL pyrroles, Keep agitation 14h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 352.5mg, after thiocarbamide 80.5mg, 35mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 165 DEG C, reacts 11.5h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 10
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam after cleaning is positioned in 250mL beaker by (), add the hydrochloric acid solution 50ml that PH is 5, stirs and adds 1mL pyrroles, Keep agitation 13h, and take out nickel sheet and rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry, obtain composite material one.
C () adds MoO in a kettle. successively 352mg, after thiocarbamide 80mg, 40mL deionized water and stirring 20min, adds the obtained composite material of step (b), at 170 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 11
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam is put into 100ml beaker by (), add deionized water 30mL, sodium thiosulfate 0.05g, stirs and adds pyrroles 0.3mL, and nickel foam in step 1, Keep agitation 15h.Take out nickel sheet to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry.
C () adds MoO in a kettle. successively 345mg, after thiocarbamide 63.5mg, 30mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 160 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 12
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam is put into 100ml beaker by (), add deionized water 50mL, sodium thiosulfate 0.08g, stirs and adds pyrroles 0.5mL, and nickel foam in step 1, Keep agitation 10h.Take out nickel sheet to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry.
C () adds MoO in a kettle. successively 340mg, after thiocarbamide 60mg, 30mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 160 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 13
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam is put into 100ml beaker by (), add deionized water 80mL, sodium thiosulfate 0.13g, stirs and adds pyrroles 1mL, and nickel foam in step 1, Keep agitation 8h.Take out nickel sheet to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry.
C () adds MoO in a kettle. successively 345mg, after thiocarbamide 63.5mg, 30mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 160 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 14
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam is put into 100ml beaker by (), add deionized water 20mL, sodium thiosulfate 0.032g, stirs and adds pyrroles 0.4mL, and nickel foam in step 1, Keep agitation 15h.Take out nickel sheet to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry.
C () adds MoO in a kettle. successively 345mg, after thiocarbamide 80mg, 40mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 170 DEG C, reacts 12h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 15
A kind of PPy/MoS 2/ Ni 3s 2the preparation method of composite material, comprises the following steps:
A () is by nickel foam (2 × 3cm) priority absolute ethyl alcohol and deionized water ultrasonic cleaning 10min;
B nickel foam is put into 100ml beaker by (), add deionized water 90mL, sodium thiosulfate 0.15g, stirs and adds pyrroles 0.9mL, and nickel foam in step 1, Keep agitation 15h.Take out nickel sheet to rinse with deionized water and absolute ethyl alcohol respectively, 60 DEG C of oven dry.
C () adds MoO in a kettle. successively 337.5mg, after thiocarbamide 50mg, 25mL deionized water and stirring 15min, adds the obtained composite material of step (b), at 170 DEG C, reacts 10h.Cooling uses deionized water and absolute ethanol washing 3 times after taking out respectively, 60 DEG C of oven dry.
Embodiment 16
PPy/MoS 2/ Ni 3s 2the sign of composite material:
(1) carry out morphology analysis by scanning electron microscopy (SEM) to embodiment 1 products therefrom, result as shown in Figure 1, shows that prepared sample is the nanostructure of wire.
(2) analyze embodiment 1 products therefrom composition with X-ray energy spectrum (EDX), result as shown in Figure 2.Indicate MoS in this sample 2, Ni 3s 2, pyrroles can well be coupled.
(3) analyze product elemental chemical valence embodiment 1 gained by x-ray photoelectron power spectrum (XPS), result is as Fig. 3, and the chemical valence of molybdenum element is+4, and corresponding compound should be MoS 2; The chemical valence of nickel element is+2, and corresponding compound should be Ni 3s 2; The functional group of pyrroles also can well be detected.So can show that the compound of embodiment 1 gained is PPy/MoS 2/ Ni 3s 2composite material.
(4) detect enforcement 1 products therefrom with X-ray diffraction (XRD), result as shown in Figure 4, obtains collection of illustrative plates and the Ni corresponding to JCPDS standard card NO.44-1418 3s 2diffraction maximum and the MoS corresponding to JCPDS standard card NO.37-1492 2diffraction maximum fit like a glove.About 17 degree occur diffraction maximums be the diffraction maximum of PPy, this XRD figure can well prove that this material is PPy/MoS 2/ Ni 3s 2composite material.
Embodiment 17
A kind of PPy/MoS 2/ Ni 3s 2composite material is as the application of electrode material for super capacitor.
Below test instrument and be CHI660E electrochemical workstation, Shanghai Chen Hua Instrument Ltd. manufactures.
Below test and all adopt three-electrode system, wherein, by PPy/MoS prepared by embodiment 1 2/ Ni 3s 2composite material, is cut into 1cm × 1cm size, as work electrode; Using platinum electrode and saturated calomel electrode (SCE) as to electrode and reference electrode; Using 3MNaOH solution as electrolyte.
(1) electrochemical impedance spectroscopy test
PPy/MoS is drawn by electrochemical impedance spectroscopy 2/ Ni 3s 2the ac impedance spectroscopy of composite electrode after the circle discharge and recharge of the front and back 100 of discharge and recharge, as shown in Figure 6,0 represents PPy/MoS 2/ Ni 3s 2aC impedance curve before composite electrode discharge and recharge, 100 represent PPy/MoS 2/ Ni 3s 2aC impedance curve when nano line electrode 100 encloses charge and discharge cycles.
Ac impedance spectroscopy is divided into high frequency region part and low frequency range part, is made up of the arc of one section of semicircle of high frequency region and a skew lines of low frequency range.Be PPy/MoS at the intersection point of high frequency region impedance spectrum and real axis 2/ Ni 3s 2the internal resistance of composite electrode, comprises the contact resistance of the resistance of active material itself, the resistance of electrolyte and active material and electrolyte.PPy/MoS can be found in high frequency region 2/ Ni 3s 2curve approximation when composite electrode is before discharge and recharge and after 100 cycle charge-discharges, the electrode material of the curve of high frequency region more close excellent ultracapacitor before discharge and recharge and after cycle charge-discharge, indicates PPy/MoS thus 2/ Ni 3s 2nano line electrode can as the electrode material of ultracapacitor.
(2) cyclic voltammetry (CV) test
Respectively with 10mVs -1, 20mVs -1, 50mVs -1and 100mVs -1sweep speed scan, draw the PPy/MoS in embodiment 1 2/ Ni 3s 2as shown in Figure 7, the potential range of this curve is 0v ~ 0.5V to the cyclic voltammetry curve of composite material.
(3) chronoptentiometry (CP) test
Respectively at 1Ag -1, 2Ag -1, 3Ag -1and 4Ag -1under carry out constant current charge-discharge detection, draw the PPy/MoS in embodiment 1 2/ Ni 3s 2the constant current charge-discharge curve of composite material under different current density, as shown in Figure 8.Wherein, the ordinate of this curve and voltage range are 0 ~ 0.5V.The ratio capacitance discharge and recharge under different current density is gone out by following formulae discovery.Ratio capacitance is calculated, i.e. PPy/MoS by discharge and recharge figure 2/ Ni 3s 2nano wire at 1Ag -1under current density, ratio capacitance is 2213.2Fg -1, PPy/MoS is described 2/ Ni 3s 2nano wire has the performance of excellent storage electricity.Wherein, capacitance calculation formula is: C m=C/m=(It)/(△ Vm), I is size of current, and t is discharge time, and △ V is voltage difference, and m is the quality of sample on work electrode sheet.
(4) constant current charge-discharge detects
At 4Ag -1under current density, constant current charge-discharge 3000 times, obtains the PPy/MoS in embodiment 1 2/ Ni 3s 2composite material is circulation-ratio capacitance curve when current density is 4A/g, and termination capacity and initial capacity as shown in Figure 9, contrast known by result, identical with initial capacitance after 3000 cycle charge-discharges, and PPy/MoS is described 2/ Ni 3s 2nano wire has excellent stability.
Above-mentioned reference embodiment is to PPy/MoS 2/ Ni 3s 2the detailed description that the preparation method of composite material and application are carried out; illustrative instead of determinate; several embodiments can be listed according to institute's limited range, therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.

Claims (10)

1. a PPy/MoS 2/ Ni 3s 2the preparation method of composite material, is characterized in that, described preparation method comprises the following steps:
(a) cleaning nickel foam;
Nickel foam after (b) cleaning and pyrroles's stirring reaction in reactant liquor, cleaning, dry, obtain the nickel foam that surface recombination has polypyrrole;
C surface recombination is had nickel foam, the MoO of polypyrrole by () 3, thiocarbamide reacts in aqueous, cleaning, dry, can obtain PPy/MoS 2/ Ni 3s 2composite material.
2. preparation method according to claim 1, is characterized in that, the reaction time in described step (b) is 8 ~ 16 hours.
3. preparation method according to claim 1 and 2, is characterized in that: the reactant liquor in described step (b) be PH be less than 7 hydrochloric acid solution or concentration be the hypo solution of 1.6 ~ 1.7g/L.
4. preparation method according to claim 1 and 2, is characterized in that: in described step (b), and the mass concentration of pyrroles is 10 ~ 20mg/ml, and the top surface area of nickel foam is 6cm with the ratio of the volume of reactant liquor 2: (25 ~ 90) ml.
5. preparation method according to claim 1, is characterized in that, the reaction temperature in described step (c) is 155-170 DEG C, and the time is 10-12h.
6. preparation method according to claim 1 or 5, it is characterized in that, the reaction temperature in described step (c) is 160 DEG C, and the time is 11.5h.
7. the preparation method according to claim 1 or 6, is characterized in that, in described step (c), and MoO 3, thiocarbamide mass concentration be respectively 1.0 ~ 1.5mg/mL, 2.0 ~ 2.5mg/mL; The top surface area of nickel foam is 6cm with the ratio of the volume of the aqueous solution 2: (25 ~ 40) ml.
8. preparation method according to claim 7, is characterized in that: in described step (c), MoO 3, thiocarbamide mass concentration be respectively 1.3 ~ 1.5mg/mL, 2.0 ~ 2.2mg/mL; The top surface area of nickel foam is 6cm with the ratio of the volume of the aqueous solution 2: 30ml.
9. preparation method according to claim 1, is characterized in that, described PPy/MoS 2/ Ni 3s 2composite material is linear nano structure.
10. the PPy/MoS that the preparation method according to claim 1-9 any one prepares 2/ Ni 3s 2composite material is as the application of electrode material for super capacitor.
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CN111540609A (en) * 2020-05-07 2020-08-14 电子科技大学 Crystalline-amorphous MoO for super capacitor3@Ni3S2Method for producing a material
CN113058622A (en) * 2021-03-26 2021-07-02 安徽大学 Nickel sulfide/molybdenum disulfide composite nano array for photoelectrocatalysis killing of drug-resistant bacteria and preparation method thereof
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CN106057498A (en) * 2016-06-15 2016-10-26 齐鲁工业大学 Preparation method and application of molybdenum disulfide/polypyrrole supercapacitor electrode material
CN106501455A (en) * 2016-11-03 2017-03-15 山东师范大学 A kind of preparation method of the highly sensitive stretchable biosensor in situ detection
CN106501455B (en) * 2016-11-03 2019-05-28 山东师范大学 A kind of preparation method of the highly sensitive stretchable biosensor in situ detection
CN107086132A (en) * 2017-04-26 2017-08-22 安徽师范大学 Flower-shaped nickel nano film of vanadic anhydride/curing three and its preparation method and application
CN107086132B (en) * 2017-04-26 2019-07-19 安徽师范大学 Flower-shaped three nickel nano film of vanadic anhydride/curing and its preparation method and application
CN107968208B (en) * 2017-12-01 2020-09-25 吉林大学 Nano lamellar structure of trinickel disulfide/molybdenum disulfide composite material and preparation method thereof
CN107968208A (en) * 2017-12-01 2018-04-27 吉林大学 A kind of nano-lamellar structure of three nickel of curing/molybdenum disulfide composite material and preparation method thereof
CN108155028A (en) * 2017-12-29 2018-06-12 安徽大学 The preparation method of the flower-shaped molybdenum disulfide high-performance super capacitor electrode of one type
CN109455774A (en) * 2018-12-27 2019-03-12 西安交通大学 A kind of Ni-Fe-OH/MoS2/Ni3S2Composite nano plate/carbon cloth, preparation method and application
CN109455774B (en) * 2018-12-27 2020-03-13 西安交通大学 Ni-Fe-OH/MoS2/Ni3S2Composite nano sheet/carbon fiber cloth, preparation method and application
CN110075873A (en) * 2019-04-29 2019-08-02 苏州大学 It is layered the Fe-MoS of self assembly2/Ni3S2/ NF composite nano materials and the preparation method and application thereof
CN110075873B (en) * 2019-04-29 2021-11-23 苏州大学 Layered self-assembled Fe-MoS2/Ni3S2/NF composite nano material and preparation method and application thereof
CN111540609A (en) * 2020-05-07 2020-08-14 电子科技大学 Crystalline-amorphous MoO for super capacitor3@Ni3S2Method for producing a material
CN111540609B (en) * 2020-05-07 2021-04-30 电子科技大学 Crystalline-amorphous MoO for super capacitor3@Ni3S2Method for producing a material
CN113058622A (en) * 2021-03-26 2021-07-02 安徽大学 Nickel sulfide/molybdenum disulfide composite nano array for photoelectrocatalysis killing of drug-resistant bacteria and preparation method thereof
WO2024083850A1 (en) 2022-10-18 2024-04-25 ETH Zürich Electrocatalyst

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