CN108486605A - A kind of carbon coating selenizing nickel cobalt nano material and preparation method thereof with excellent electrolysis water performance - Google Patents
A kind of carbon coating selenizing nickel cobalt nano material and preparation method thereof with excellent electrolysis water performance Download PDFInfo
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- CN108486605A CN108486605A CN201810208694.6A CN201810208694A CN108486605A CN 108486605 A CN108486605 A CN 108486605A CN 201810208694 A CN201810208694 A CN 201810208694A CN 108486605 A CN108486605 A CN 108486605A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A kind of carbon-coated selenizing nickel cobalt with excellent electrolysis water performance（Ni0.67Co0.33Se2）Nano material and preparation method thereof.The method includes：First by Co (NO3)2·6H2O、Ni(NO3)2·6H2O, polyvinylpyrrolidone（PVP‑K30）It is dissolved in N with terephthalic acid (TPA), in N dimethylformamides (DMF) and the mixed solution of ethyl alcohol, it is then transferred into the autoclave of polytetrafluoroethyllining lining, drying and grinding is washed after pyroreaction synthesis Co Ni MOFs materials, it is put into tube furnace after being mixed with selenium powder, the high temperature anneal is carried out in a nitrogen atmosphere, obtains carbon-coated selenizing nickel cobalt（Ni0.67Co0.33Se2）Nano material.The carbon-coated Ni that the present invention obtains0.67Co0.33Se2Nano material, which has, prepares the excellent specific properties such as speed is fast, yield is high, stability is good, has important application value in terms of electrolysis water catalysis under alkaline condition.
Description
Technical field
The present invention relates to a kind of carbon coating selenizing nickel cobalts with excellent electrolysis water performance（Ni0.67Co0.33Se2）Nanometer
Material and preparation method thereof.
Background technology
With the aggravation of reduction and the environmental pollution of fossil fuel, the development of future society will have to dependent on sustainable
The renewable sources of energy.The method that electrolysis water prepares cleaning hydrogen fuel is generally considered a kind of promising sustainable development solution party
Case.However because water splitting processes are cells with non-spontaneous reactions, including oxygen evolution reaction（OER）It is needed with evolving hydrogen reaction (HER) very high
Overpotential, the practical application of electrolysis water has significant limitation.Currently, metal oxide containing precious metals, such as RuO2And IrO2, it is most to have
The OER elctro-catalysts of effect, but the shortcomings of it is expensive, and reserves are limited seriously limit its large-scale promotion application, equally
The electro catalytic activity of the noble metals such as Pt, Pd, Rh in Electrocatalytic Activity for Hydrogen Evolution Reaction reaction it is higher, but its is with high costs, and resource has
Limit, strongly limits its large-scale commercial application.Therefore, exploitation elctro-catalyst that is cheap, efficient, stablizing has become electric now
Chemical energy source stores and conversion devices develop the huge challenge faced.In this respect, transition metal selenides, sulfide,
Oxide and phosphide are most potential electrolysis water catalyst.In the electrolysis water catalysis material prepared based on base metal,
Transition metals cobalt and nickel are because its is of low cost, and rich reserves derive from a wealth of sources, good electric conductivity, and with as platinum class
The characteristics such as hydrogen adsorption free energy to prepare Cheap highly effective electrolysis water catalyst.
Metal-organic framework materials（MOFs）Be by organic ligand and metal ion or metal cluster self assembly and formed one
Class has the Porous coordination polymer of periodical reticular structure, therefore can pass through the choosing to metal center atom and machine ligand
Select, modify to design the MOFs materials of different structure, and organic ligand can be converted into high-temperature annealing process it is more
The nano particle of hole carbon, amorphous carbon, the carbon package of formation can effectively improve stability, along with its pore structure orderly may be used
Many excellent specific properties such as tune, large specific surface area, structure diversity, therefore the MOFs of complex functionality can be first designed as sacrificial mold
Plate is directly prepared by high-temperature annealing process with the porous nanocarbon/metal of good electrocatalysis characteristic without adding Additional carbon sources
Oxide material, this prepares carbon coating cobalt nickel selenides electrolysis water catalyst by presoma of MOFs materials for us and provides reason
By support.
Invention content
The technical problem to be solved in the present invention is the shortcoming overcome in the technology of preparing of existing transition metal selenides,
Develop a kind of carbon coating selenizing nickel cobalt with excellent electrolysis water performance（Ni0.67Co0.33Se2）Nano material and preparation method thereof.
Carbon coating selenizing nickel cobalt in the present invention（Ni0.67Co0.33Se2）The exemplary synthesis of nano material is by appropriate Co
(NO3)2·6H2O、Ni(NO3)2·6H2O, polyvinylpyrrolidone (PVP-K30) and terephthalic acid (TPA) are dissolved in N, N- dimethyl
It in formamide (DMF) and the mixed solution of ethyl alcohol, is then transferred into the autoclave of polytetrafluoroethyllining lining, pyroreaction synthesis
Dry and grind into powder is washed after Co-Ni-MOFs materials, is put into tube furnace after being mixed with selenium powder, high annealing, it is final to make
It is standby go out carbon-coated selenizing nickel cobalt（Ni0.67Co0.33Se2）Nano material.
A kind of heretofore described carbon coating selenizing nickel cobalt with excellent electrolysis water performance（Ni0.67Co0.33Se2）It receives
Rice material and preparation method thereof, including step in detail below：
（1）By 0.1746 gram of Co (NO3)2·6H2O and 0.3489 gram of Ni (NO3)2·6H2The 9.375 milliliters of N, N- bis- that O is added to
In the mixed solution of methylformamide (DMF) and 5.625 milliliters of ethyl alcohol, 0.36 gram of polyvinylpyrrolidone (PVP- is added
K30) this mixed solution is transferred in autoclave, 120 with 0.1995 gram of terephthalic acid (TPA), stirring and dissolving to homogeneous solution
24 hours are kept the temperature under degree Celsius to take out and cool down at room temperature after synthesis Co-Ni-MOFs materials.
（2）Step（1）Gained Co-Ni-MOFs materials are washed with deionized water and ethyl alcohol under twice, 80 degrees Celsius respectively
Vacuum drying 2 hours, grind into powder is spare after cooling.
（3）Weigh 0.1 gram of step（2）Gained powder and 0.5 gram of selenium powder, are put into tube furnace, and be passed through after mixing
Nitrogen is protected, and the high temperature anneal is then carried out, and wherein heating rate is 10 degrees celsius/minutes, and annealing temperature is taken the photograph for 450
Family name's degree.
Compared with prior art, a kind of carbon coating selenizing nickel cobalt with excellent electrolysis water performance provided by the present invention
（Ni0.67Co0.33Se2）The preparation method of nano material at least has the advantages that：
（1）The embodiment of the present invention provides a kind of carbon coating selenizing nickel cobalt with excellent electrolysis water performance（Ni0.67Co0.33Se2）
The preparation method great advantage of nano material is that cost of material is cheap, derives from a wealth of sources, preparation process is simple；
（2）The carbon coating selenizing nickel cobalt that the embodiment of the present invention is provided（Ni0.67Co0.33Se2）Nano material yield height, monodisperse
Property is good, can preserve for a long time at ambient temperature；
（3）The carbon coating selenizing nickel cobalt that the embodiment of the present invention is provided（Ni0.67Co0.33Se2）Nano material has specific surface area
Greatly, the advantages that active site is more, easy adsorption reaction object；
（4）The embodiment of the present invention provides a kind of carbon coating selenizing nickel cobalt with electrolysis water performance（Ni0.67Co0.33Se2）Nanometer
The preparation method of material only needs some conventional equipments such as reaction kettle, quartz boat, tube furnace, baking oven, and technical process is simple and is easy to
Operation；
（5）The carbon coating selenizing nickel cobalt that the embodiment of the present invention is provided（Ni0.67Co0.33Se2）Nano material is to electric in alkaline environment
Xie Shui has excellent catalytic activity, while with good stability.
Description of the drawings
Fig. 1 a are using 200 field emission scanning electron microscopes of Sirion to carbon coating selenizing nickel cobalt
（Ni0.67Co0.33Se2）The photo that nano material is shot, Fig. 1 b are its high resolution transmission electron microscopy（HRTEM）Photo,
Fig. 2 is Ni0.67Co0.33Se2Carbon（C）, nickel（Ni）, cobalt（Co）And selenium（Se）The mapping of element（EDX mapping）, thus
It is found that Ni0.67Co0.33Se2It is uniformly coated in carbon-coating.
Fig. 3 is Ni0.67Co0.33Se2The X-ray diffracting spectrum of nano material, as seen from the figure：Carbon prepared by the present invention
The Ni of cladding0.67Co0.33Se2Nano material, diffraction peak is in NiSe2And CoSe2Standard diffraction peak between, and do not have
The division at peak, this, which is further illustrated the present invention, prepares really actually carbon-coated Ni0.67Co0.33Se2Nano material.
Fig. 4-6 is in occasion China 760e electrochemical test systems, to being coated in nickel foam（NF）On it is carbon-coated
Ni0.67Co0.33Se2The electrochemistry collection of illustrative plates that nano material is tested, is named as Ni0.67Co0.33Se2/NF.Fig. 4 a are foams
Nickel（NF）And Ni0.67Co0.33Se2The polarization curve of/NF liberations of hydrogen, sweep speed are 5 mv s（mV/s）, Fig. 4 b are turned by Fig. 4 a
The Tafel curve changed；Fig. 5 a are nickel foams（NF）And Ni0.67Co0.33Se2/ NF analyses the polarization curve of oxygen, and sweep speed is
5 mv s（mV/s）, Fig. 5 b are the Tafel curves being transformed by Fig. 5 a；Fig. 6 a are Ni0.67Co0.33Se2/ NF complete solution water
Polarization curve, Fig. 6 b are stability test collection of illustrative plates, illustrate prepared Ni0.67Co0.33Se2Not only there is excellent catalytic activity
And still there is preferable stability after 1000 circle of cycle.Fig. 4 a, 5a, 6a and 6b abscissa be Potential/V
vs.RHE（That is electrode potential, unit V）, ordinate is (j/mA cm-2)（That is current density, unit are mA cm-2）；Fig. 4 b
Abscissa with 5b is Log values, that is, Log (j/mA cm of current density-2), ordinate is Overpotential (V)（That is electrode
Potential, unit V）.
Specific implementation mode
Prepare the Co (NO that the present invention uses first3)2·6H2O、Ni(NO3)2·6H2O, N,N-dimethylformamide
(DMF), ethyl alcohol, polyvinylpyrrolidone (PVP-K30) and terephthalic acid (TPA)；Then respectively by Co (NO3)2·6H2O、Ni
(NO3)2·6H2O, PVP-K30 and terephthalic acid (TPA) are dissolved into DMF and the mixed solution of ethyl alcohol；Solution shifts after stirring evenly
It reacts, after reaction the Co-Ni-MOFs materials of synthesis are washed dry and grinds to autoclave high temperature；Finally and selenium powder
Mixing obtains carbon coating selenizing nickel cobalt through high annealing（Ni0.67Co0.33Se2）Nano material.
Present disclosure is described in further detail with reference to specific implementation example, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained under the premise of not making the creative labor belongs to the protection model of the present invention
It encloses.
Embodiment 1
A kind of carbon coating selenizing nickel cobalt with excellent electrolysis water performance（Ni0.67Co0.33Se2）The preparation method packet of nano material
Containing following steps：
（1）By 0.1746 gram of Co (NO3)2·6H2O and 0.3489 gram of Ni (NO3)2·6H2The 9.375 milliliters of N, N- bis- that O is added to
In the mixed solution of methylformamide (DMF) and 5.625 milliliters of ethyl alcohol, 0.36 gram of polyvinylpyrrolidone (PVP- is added
K30) this mixed solution is transferred in water heating kettle, 120 with 0.1995 gram of terephthalic acid (TPA), stirring and dissolving to homogeneous solution
Synthesis Co-Ni-MOFs materials taking-up in 24 hours is kept the temperature under degree Celsius to cool down at room temperature.
（2）By step（1）Gained Co-Ni-MOFs materials are washed twice with deionized water and ethyl alcohol respectively, and 80 degrees Celsius true
Sky is 2 hours dry, and grind into powder is spare after cooling.
（3）Weigh 0.1 gram of step（2）Gained powder and 0.5 gram of selenium powder, are put into tube furnace, and be passed through after mixing
Nitrogen is protected, and the high temperature anneal is then carried out, and wherein heating rate is 10 degrees celsius/minutes, and annealing temperature is taken the photograph for 450
Family name's degree.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (3)
1. a kind of carbon-coated selenizing nickel cobalt with excellent electrocatalysis characteristic（Ni0.67Co0.33Se2）The preparation side of nano material
Method, it is characterised in that：
Preparation process can be divided into two steps, Co-Ni-MOFs materials first be synthesized, using high annealing selenidation process；
（1）Prepare carbon-coated selenizing nickel cobalt（Ni0.67Co0.33Se2）Nano material is spherical shape, about 1 microns of size；
（2）Prepare carbon-coated selenizing nickel cobalt（Ni0.67Co0.33Se2）Nano material, Ni elements and Co element ratios are 2:1,
Its ratio can be regulated and controled by rate of charge when synthesizing MOFs presomas；
（3）Carbon-coated selenizing nickel cobalt（Ni0.67Co0.33Se2）Nano material has good stability in room temperature environment；
（4）Carbon-coated selenizing nickel cobalt（Ni0.67Co0.33Se2）Nano material under alkaline condition there is excellent electrolysis water to be catalyzed
Activity, while there is very outstanding stability.
2. a kind of a kind of carbon-coated selenizing nickel cobalt with excellent electrocatalysis characteristic described in claim 1
（Ni0.67Co0.33Se2）Nano material and preparation method thereof, it is characterized in that including the following steps：
（1）By 0.1746 gram of Co (NO3)2·6H2O and 0.3489 gram of Ni (NO3)2·6H2The 9.375 milliliters of N, N- bis- that O is added to
In the mixed solution of methylformamide (DMF) and 5.625 milliliters of ethyl alcohol, 0.36 gram of polyvinylpyrrolidone (PVP- is added
K30) this mixed solution is transferred in water heating kettle, 120 with 0.1995 gram of terephthalic acid (TPA), stirring and dissolving to homogeneous solution
Kept the temperature under degree Celsius 24 hours synthesis Co-Ni-MOFs materials after take out after cool down at room temperature；
（2）By step（1）Gained mixed solution is washed twice with deionized water and ethyl alcohol respectively, and 80 DEG C are dried in vacuo 2 hours, cold
But grind into powder is spare after；
（3）Weigh 0.1 gram of step（2）Gained powder and 0.5 gram of selenium powder, are put into tube furnace, and be passed through nitrogen after mixing
It is protected, then carries out the high temperature anneal, wherein heating rate is 10 degrees celsius/minutes, and annealing temperature is 450 Celsius
Degree, Ni is named as according to annealing temperature by gained sample0.67Co0.33Se2 。
3. a kind of carbon-coated Ni with excellent electrolysis water Hydrogen Evolution Performance0.67Co0.33Se2Nano material, it is characterised in that：
Current density is 10 mA cm-2When, it is 114.8 mV dec that liberation of hydrogen overpotential, which only has 143 mV, Tafel slope,-1；Analyse oxygen mistake
It is 24.9 mV dec that potential, which only has 311 mV Tafel slopes,-1；Complete solution water overpotential only has 1.69 V, has excellent catalysis
Activity.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110085834A (en) * | 2019-04-29 | 2019-08-02 | 齐鲁工业大学 | A kind of preparation method of two nickelous selenide high-performance anode material of lithium-ion batteries of Fe2O3 doping |
| CN110614105A (en) * | 2019-09-25 | 2019-12-27 | 上海应用技术大学 | Mo for hydrogen evolution2C/NiCoSex heterojunction electrocatalytic material and preparation method thereof |
| CN110853937A (en) * | 2019-11-29 | 2020-02-28 | 江苏理工学院 | Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor |
| CN111243871A (en) * | 2020-01-17 | 2020-06-05 | 湖北大学 | Novel NiSe2Coated mesoporous hollow carbon sphere composite material, preparation method thereof and application thereof in super capacitor |
| CN111359637A (en) * | 2020-03-18 | 2020-07-03 | 龙岩学院 | Hydrogen production catalyst nickel diselenide nanoparticle @ carbon nanosheet composite material and preparation method and application thereof |
| CN111514910A (en) * | 2020-06-17 | 2020-08-11 | 台州学院 | Co containing cobalt vacancy18Ni2Se20Compound (I) |
| CN112108160A (en) * | 2020-09-03 | 2020-12-22 | 华中科技大学 | Preparation method of dodecahedron hollow cobalt nickel selenide/iron oxyhydroxide composite catalyst |
| CN113327774A (en) * | 2021-05-31 | 2021-08-31 | 青岛科技大学 | Preparation method of carbon-based metal selenide composite material |
| CN113422032A (en) * | 2021-07-02 | 2021-09-21 | 上海电力大学 | Negative electrode material NiSe of sodium ion battery2Preparation method and application of @ C microspheres |
| CN113604838A (en) * | 2021-08-17 | 2021-11-05 | 江苏大学 | Preparation method and application of nickel-cobalt bimetallic selenide heterostructure electrocatalyst |
| CN113666344A (en) * | 2021-08-19 | 2021-11-19 | 安徽工业大学 | Transition metal selenide-carbon composite material and preparation method and application thereof |
| CN113666343A (en) * | 2021-08-19 | 2021-11-19 | 安徽工业大学 | Organic metal frame structure nickel-cobalt selenide and preparation method and application thereof |
| CN113725433A (en) * | 2021-08-31 | 2021-11-30 | 广东省国研科技研究中心有限公司 | N-doped carbon Ni0.6Co0.4Se2Preparation method and application of @ rGO composite material |
| CN114214636A (en) * | 2021-11-22 | 2022-03-22 | 江西师范大学 | Method for preparing cobalt-based nanosheet self-supporting electrode by selenium-containing ligand and application of cobalt-based nanosheet self-supporting electrode |
| CN114525546A (en) * | 2022-03-30 | 2022-05-24 | 合肥工业大学 | Preparation method of binary nickel cobalt selenide nanosheet material |
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| CN114892210A (en) * | 2022-06-07 | 2022-08-12 | 济南大学 | Method for preparing Ni @ Ru nano electrocatalyst with sandwich-like structure by one-pot method |
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| CN110614105B (en) * | 2019-09-25 | 2022-05-31 | 上海应用技术大学 | Mo for hydrogen evolution2C/NiCoSex heterojunction electrocatalytic material and preparation method thereof |
| CN110614105A (en) * | 2019-09-25 | 2019-12-27 | 上海应用技术大学 | Mo for hydrogen evolution2C/NiCoSex heterojunction electrocatalytic material and preparation method thereof |
| CN110853937A (en) * | 2019-11-29 | 2020-02-28 | 江苏理工学院 | Preparation method of nickel-cobalt bimetallic selenide/carbon composite for supercapacitor |
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| CN114702014B (en) * | 2022-04-15 | 2023-09-01 | 西安建筑科技大学 | Nickel-cobalt-selenium nano material with network structure and preparation method and application thereof |
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