CN105576216A - Preparation method and application of alpha-nickel sulfide/graphene composite material - Google Patents
Preparation method and application of alpha-nickel sulfide/graphene composite material Download PDFInfo
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- CN105576216A CN105576216A CN201610128883.3A CN201610128883A CN105576216A CN 105576216 A CN105576216 A CN 105576216A CN 201610128883 A CN201610128883 A CN 201610128883A CN 105576216 A CN105576216 A CN 105576216A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of an alpha-nickel sulfide/graphene composite material and application thereof as an electrochemical hydrogen evolution catalyst. The alpha-nickel sulfide/graphene composite material is mainly synthesized by virtue of a one-step hydrothermal method, ultrasonically dispersed and then modified onto a glassy carbon electrode to obtain an alpha-nickel sulfide/graphene composite material modified electrode. The alpha-nickel sulfide/graphene composite material modified electrode is mainly applied to electrochemical hydrogen evolution. The catalytic activity of the synthesized alpha-nickel sulfide/graphene composite material is detected by adopting a linear scanning curve (polarized curve), and a cycling voltage-current curve is used for testing the stability of the alpha-nickel sulfide/graphene composite material. By adequately utilizing the synergism of the alpha-nickel sulfide nano particles and graphene in the alpha-nickel sulfide/graphene composite material, the catalytic efficiency of the electrochemical hydrogen evolution is increased, the stability of the catalyst is effectively improved, and long-time application in an alkaline environment is facilitated.
Description
Technical field
The invention belongs to clean sustainable novel energy Application and preparation field, particularly a kind of preparation method of α-nickel sulfide/graphene composite material and application thereof.
Background technology
The energy is the important support of modern economy, is the important foundation of human society survival and development, plays indispensable important impetus to economy, social development.Along with the fast development of China's economic and increasing rapidly of population, the deterioration of the ecological environment problem caused by the while that increasing to the demand of the energy, energy resource consumption significantly increasing, traditional energy resource reduces day by day highlights day by day.Hydrogen has that aboundresources, calorific value are high, combustion process and product pollution-free and easily store and the feature such as transport, be considered to the new forms of energy carrier of most possible substitute fossil fuels.Electrocatalytic hydrogen evolution is one of method of producing hydrogen, traditional electrochemistry liberation of hydrogen catalyst is mostly the noble metal of platinum and so on, although show comparatively superior electrochemical catalysis hydrogen evolution activity, but noble metal catalyst preparation cost is high, earth storage capacity is few, limits it and further develop and practical application.
A kind of metal sulfide of nickel sulfide, the overpotential of hydrogen evolution lower because of it and become the study hotspot of hydrogen manufacturing, α-nickel sulfide is compared β-nickel sulfide and is had good conductivity and other excellent physical characteristics, it is made to have higher catalytic hydrogen evolution performance in the basic conditions, but in long electrochemical applications process, material morphology and structure can be destroyed, and reduce the stability of its catalysis, are unfavorable for long application.
Graphene is typical two-dimensional material, has the excellent properties such as very high specific area, superpower mechanical property, high conduction and heat conduction due to Graphene, can as the carrier of many nano materials.Therefore, the present invention uses the composite nanostructure material of Graphene and nickel sulfide as electrode, the conductivity that Graphene is excellent and stability, not only be conducive to accelerating the electron transmission in composite electrode course of reaction, reduce interface charge transfer resistance, and the effective morphology stability of reinforcing material in cyclic process, thus greatly promote its chemical property.
In prepared by NiS and composite material thereof, people carry out different probing into work.The people such as Yung-EunSung are with nickel acetylacetonate, and lauryl mercaptan, oleamide is raw material, and under logical protective gas, pyroreaction obtains NiS nano particle (Nanoscale, 2015,7,5157 – 5163).The method uses a large amount of organic reagents, should not remove and easily affect the performance of material itself in expensive external last handling process itself.The people such as NguyenVanHieu pass through two-step method, with the Ni first prepared (OH)
2for raw material is at H
2obtain α-nanometer nickel sulfide sheet (MaterialsLetters161 (2015) 282 – 285) under S atmosphere, not only preparation method is complicated and use more dangerous gas as presoma, inapplicable fairly large preparations and applicatio.
The object of the invention is for the deficiencies in the prior art, a kind of nickel sulfide and graphene composite material of α phase of morphology controllable are provided, its first time is applied to electrochemical catalysis liberation of hydrogen domain variability and shows good catalytic hydrogen evolution performance.This α-nickel sulfide/graphene composite material has the features such as preparation method is simple, workable, catalytic activity is high, good stability
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method and application thereof of α-nickel sulfide/graphene composite material are provided.
The object of the invention is to be achieved through the following technical solutions: a kind of preparation method of α-nickel sulfide/graphene composite material, step is as follows:
(1) be scattered in by graphene oxide in the mixed solution of ethylene glycol and water, ultrasonic acquisition concentration is the graphene oxide solution of 6 ~ 10mg/mL, then in graphene oxide solution, adds nickel chloride, thiocarbamide, and ultrasonic disperse is even, obtains mixed solution.
(2) mixed solution in step (1) is transferred in reactor, at 180 DEG C-220 DEG C, carry out hydro-thermal reaction obtain product, after product is centrifugal, repeatedly wash with deionized water, dry, obtain α-nickel sulfide/graphene composite material.
Further, in step (1), the volume ratio of ethylene glycol and water is 2:0.75 ~ 1.5.
Further, the graphene oxide in step (1) and the mass ratio of nickel chloride are 0.8 ~ 7:50, and the mass ratio of nickel chloride and thiocarbamide is 1:1 ~ 5.
Further, the mass ratio of described graphene oxide and nickel chloride is 4.5:50, and the mass ratio of nickel chloride and thiocarbamide is 1:5.
Further, in step (2), the reaction time of reactor is 16 ~ 20h.
An application for α-nickel sulfide/graphene composite material, described in be applied as: α-nickel sulfide/graphene composite material is applied to electrocatalytic hydrogen evolution.
The present invention take Graphene as substrate, and obtain α-nickel sulfide/graphene composite material, wherein α-nickel sulfide nano particle is evenly distributed on graphenic surface.The present invention adopts one-step method to prepare, make the graphene oxide that is not reduced by a large amount of negative electrical charge on its surface and functional group, the nickel ion that strong adsorption is positively charged, nickel chloride is made to have good dispersiveness, meanwhile, nickel chloride and surface of graphene oxide is made to have stronger valence bond active force and electrostatic force; Thiocarbamide is adopted to reduce to graphene oxide while absorption, and S source is provided, nickel chloride is replaced as the nickel sulfide with catalytic property, and the combination do not destroyed between nickel ion and Graphene, ensure the electric action between nickel sulfide and Graphene, form the α-nickel sulfide/graphene composite material of even structure.This material is by introducing Graphene, improve the electron transfer capacity of nickel sulfide, there is good conductivity and stability, effectively reduce it as the transfer resistance of interface charge during catalyst and the change of pattern and structure in long-time use procedure, make the nickel sulfide material catalyzes performance enhancement that α-nickel sulfide/graphene composite material is more independent, for the development of new catalytic hydrogen evolution electrode material provides Research foundation.
α-nickel sulfide of the present invention/graphene composite material electrode first time is applied in electrochemical catalysis liberation of hydrogen, has high catalytic hydrogen evolution performance and excellent cyclical stability.
Accompanying drawing explanation
Fig. 1 is α-nickel sulfide/graphene composite material scanning electron microscope diagram (SEM) prepared by the present invention.
Fig. 2 is that the present invention prepares α-nickel sulfide/graphene composite material transmission electron microscope figure (TEM).
Fig. 3 is that the present invention prepares α-nickel sulfide/graphene composite material high resolution transmission electron microscopy figure (HRTEM).
Fig. 4 is α-nickel sulfide/graphene composite material Raman spectrogram (Raman) prepared by the present invention.
Fig. 5 is the polarization curve (Polarizationcurves) that the present invention prepares α-nickel sulfide/graphene composite material electrochemistry liberation of hydrogen in 0.5MKOH.
Fig. 6 is that the present invention prepares the stability test curve (Durabilitytest) of α-nickel sulfide/graphene composite material in 0.5MKOH.
Embodiment
Below in conjunction with embodiment the invention will be further described technical solution of the present invention, these embodiments can not be interpreted as it is restriction to technical solution.
Embodiment 1: the present embodiment prepares α-nickel sulfide/graphene composite material, specifically comprises the following steps:
(1) graphene oxide solution (GO) being 9mg/mL by different volumes (0.1,0.5,0.75mL) concentration joins containing in the reagent bottle in 15mL ethylene glycol (EG) and water mixed solution (volume ratio of ethylene glycol and water is 2:1), ultrasonic half an hour, make graphene uniform be dispersed in mixed solution, obtain graphene oxide suspension.
(2) take 50mg nickel chloride respectively with electronic balance, 250mg thiocarbamide, join in the graphene oxide suspension in step (1) in the lump, within ultrasonic 20 minutes, obtain uniform mixed solution.
(3) mixed solution in step (2) is joined in the reactor of 25mL polytetrafluoroethylene, and react 18h at 200 DEG C.
(4) adding ethanol by the black product be obtained by reacting in step (3), is 8000rpm/min at rotating speed, each 10min, repeats 5 lower centrifuge washings, and at 60 DEG C vacuumize 24h, obtain α-nickel sulfide/Graphene composite wood.
Fig. 1,2 is respectively scanning electron microscope diagram (SEM) and the transmission electron microscope figure (HRTEM) of α-nickel sulfide/graphene complex prepared by the present invention (product that the graphene oxide of 0.5mL obtains), as can be seen from the figure α-nickel sulfide nano particle is evenly distributed on graphene film, and the lateral dimension size of particle is about 80nm.
Fig. 3 is α-nickel sulfide/graphene complex (product that the graphene oxide of 0.5mL obtains) high resolution transmission electron microscopy figure prepared by the present invention, lattice fringe spacing in figure is 0.296nm, corresponding to (100) face of nickel sulfide, corresponding with the α-nickel sulfide of previous report, illustrate and successfully synthesize α-nickel sulfide nano particle.
Fig. 4 is α-nickel sulfide/graphene complex (product that the graphene oxide of 0.5mL obtains) Raman spectrogram (Raman) prepared by the present invention.As can be seen from Figure at 1335cm
-1and 1585cm
-1two diffraction maximums at place are respectively feature D peak and the G peak of graphene oxide.The I of α-nickel sulfide/graphene complex
d/ I
gbe 1.23, compare graphene oxide 0.98 increases greatly, illustrates successfully to be reduced to Graphene by hydro-thermal reaction graphene oxide.
The nickel ion Electrostatic Absorption of electronegative Graphene and positively charged, take graphene platelet as substrate, nickel sulfide nano particle is uniformly distributed its surface, effectively prevent the cluster of nano particle and increases the contact with electrolyte, the conductivity that Graphene is good simultaneously, accelerates the transfer of electronics.In α-nickel sulfide/graphene composite material, the synergy of α-nickel sulfide nano particle and Graphene, improves the catalytic efficiency of electrochemistry liberation of hydrogen, and effectively raises the stability of catalyst, is convenient to the use of its long period under alkaline environment.
Embodiment 2,3 α-nickel sulfide/graphene composite materials that the present embodiment adopts the graphene oxide of embodiment 1 different volumes to prepare prepare glass-carbon electrode, be specially: it is in the deionized water-alcohol mixeding liquid of (3:1) that dried for 5mg α-nickel sulfide/graphene composite material is joined 1mL volume ratio, and to add 80uL mass fraction be in 5wt%Nafion solution, after ultrasonic half an hour, obtain suspension.Then be coated on glass-carbon electrode with the hanging drop that liquid-transfering gun measures 5uL, after natural drying, obtain the glass-carbon electrode of α-nickel sulfide/Graphene.
Embodiment 3: application of electrode embodiment 2 prepared, in electrochemistry liberation of hydrogen, is specially:
The glass-carbon electrode (GCE) modified α-nickel sulfide/graphene complex is work electrode (WE), saturated calomel electrode be reference electrode (RE), platinum filament for form three-electrode system to electrode (CE), take 1MKOH as electrolyte.Before carrying out electro-chemical test, pass into saturated nitrogen, the oxygen in removing solution.And positive SCE=RHE+1.08V is calibrated to electrode.The polarization curve (Polarizationcurves) of α-nickel sulfide/graphene complex that Fig. 5 is prepared for the present invention, as can be seen from the figure when overpotential is 192mV, current density reaches 10mA/cm
2.And when the mass ratio of graphene oxide and nickel chloride is 4.5:50, the composite material prepared has better catalytic hydrogen evolution characteristic compared to other two materials.The product obtained by the graphene oxide adding 0.5mL carries out stability test, and as shown in Figure 6, as can be seen from the figure circulate after 1000 times, the catalytic activity of α-nickel sulfide/graphene complex only has a small amount of reduction, shows higher stability.
α-nickel sulfide/graphene composite material the preparation method of morphology controllable prepared by the inventive method is simple, and repeatability is high, workable.As a kind of novel electrochemistry liberation of hydrogen catalyst, show excellent catalytic activity, relative to traditional nickel sulfide/graphene complex, its bias potential is only 91mV, and exchange current density is up to 0.126mA/cm
2, for the development of new catalytic hydrogen evolution electrode material provides Research foundation.
Claims (6)
1. a preparation method for α-nickel sulfide/graphene composite material, it is characterized in that, concrete steps are as follows:
(1) be scattered in by graphene oxide in the mixed solution of ethylene glycol and water, ultrasonic acquisition concentration is the graphene oxide solution of 6 ~ 10mg/mL, then in graphene oxide solution, adds nickel chloride, thiocarbamide, and ultrasonic disperse is even, obtains mixed solution.
(2) mixed solution in step (1) is transferred in reactor, at 180 DEG C-220 DEG C, carry out hydro-thermal reaction obtain product, after product is centrifugal, repeatedly wash with deionized water, dry, obtain α-nickel sulfide/graphene composite material.
2. preparation method as claimed in claim 1, is characterized in that, in step (1), the volume ratio of ethylene glycol and water is 2:0.75 ~ 1.5.
3. preparation method as claimed in claim 1, it is characterized in that, the graphene oxide in step (1) and the mass ratio of nickel chloride are 0.8 ~ 7:50, and the mass ratio of nickel chloride and thiocarbamide is 1:1 ~ 5.
4. method according to claim 3, is characterized in that, the mass ratio of described graphene oxide and nickel chloride is 4.5:50, and the mass ratio of nickel chloride and thiocarbamide is 1:5.
5. preparation method as claimed in claim 1, is characterized in that, in step (2), the reaction time of reactor is 16 ~ 20h.
6. the application of α-nickel sulfide/graphene composite material prepared of method described in claim 1, is characterized in that, described in be applied as: α-nickel sulfide/graphene composite material is applied to electrocatalytic hydrogen evolution.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105895882A (en) * | 2016-06-02 | 2016-08-24 | 广西大学 | Preparation method for nitrogen-doped graphene-coated nickel sulfide composite electrode material |
| CN106025227A (en) * | 2016-07-14 | 2016-10-12 | 上海应用技术学院 | Preparation method of nickel sulfide/graphene/polyaniline composite electrode material |
| CN106207111A (en) * | 2016-07-14 | 2016-12-07 | 上海应用技术学院 | A kind of lithium ion battery negative GO PANI Ni3s2the preparation method of composite |
| CN106876731A (en) * | 2017-01-23 | 2017-06-20 | 吉林大学 | A kind of molybdenum disulfide nano superstructure material and its application |
| CN107959029A (en) * | 2017-10-09 | 2018-04-24 | 中国科学院深圳先进技术研究院 | A kind of catalyst material, preparation method and application |
| CN108574106A (en) * | 2017-03-08 | 2018-09-25 | 中国科学技术大学 | Self-supporting N doping metallic catalyst and preparation method thereof |
| CN110070996A (en) * | 2019-05-28 | 2019-07-30 | 中山大学 | Nickel sulfide/graphene composite material preparation method and application |
| CN110697803A (en) * | 2019-09-05 | 2020-01-17 | 东南大学 | Preparation method of high-performance nickel sulfide-graphene composite electrode material |
| CN110773198A (en) * | 2019-11-19 | 2020-02-11 | 肇庆市华师大光电产业研究院 | Carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN112981448A (en) * | 2021-03-03 | 2021-06-18 | 西南大学 | Preparation and application of carbon sphere @ nickel sulfide compound hydrogen evolution catalyst |
| CN113718281A (en) * | 2021-09-26 | 2021-11-30 | 河海大学 | Graphene quantum dot/MXene nanosheet two-dimensional composite material and preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105895882A (en) * | 2016-06-02 | 2016-08-24 | 广西大学 | Preparation method for nitrogen-doped graphene-coated nickel sulfide composite electrode material |
| CN105895882B (en) * | 2016-06-02 | 2018-04-13 | 广西大学 | A kind of preparation method of nitrogen-doped graphene cladding nickel sulfide combination electrode material |
| CN106207111B (en) * | 2016-07-14 | 2018-07-13 | 上海应用技术学院 | A kind of negative electrode of lithium ion battery GO-PANI-Ni3S2The preparation method of composite material |
| CN106025227A (en) * | 2016-07-14 | 2016-10-12 | 上海应用技术学院 | Preparation method of nickel sulfide/graphene/polyaniline composite electrode material |
| CN106207111A (en) * | 2016-07-14 | 2016-12-07 | 上海应用技术学院 | A kind of lithium ion battery negative GO PANI Ni3s2the preparation method of composite |
| CN106876731A (en) * | 2017-01-23 | 2017-06-20 | 吉林大学 | A kind of molybdenum disulfide nano superstructure material and its application |
| CN108574106A (en) * | 2017-03-08 | 2018-09-25 | 中国科学技术大学 | Self-supporting N doping metallic catalyst and preparation method thereof |
| CN108574106B (en) * | 2017-03-08 | 2021-12-10 | 中国科学技术大学 | Self-supporting nitrogen-doped metal catalyst and preparation method thereof |
| CN107959029A (en) * | 2017-10-09 | 2018-04-24 | 中国科学院深圳先进技术研究院 | A kind of catalyst material, preparation method and application |
| CN110070996A (en) * | 2019-05-28 | 2019-07-30 | 中山大学 | Nickel sulfide/graphene composite material preparation method and application |
| CN110697803A (en) * | 2019-09-05 | 2020-01-17 | 东南大学 | Preparation method of high-performance nickel sulfide-graphene composite electrode material |
| CN110773198A (en) * | 2019-11-19 | 2020-02-11 | 肇庆市华师大光电产业研究院 | Carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN110773198B (en) * | 2019-11-19 | 2022-10-04 | 肇庆市华师大光电产业研究院 | Carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN112981448A (en) * | 2021-03-03 | 2021-06-18 | 西南大学 | Preparation and application of carbon sphere @ nickel sulfide compound hydrogen evolution catalyst |
| CN113718281A (en) * | 2021-09-26 | 2021-11-30 | 河海大学 | Graphene quantum dot/MXene nanosheet two-dimensional composite material and preparation method and application thereof |
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Application publication date: 20160511 |