CN107587161A - A kind of preparation method of bar-shaped NiFeSe/C electrolysis waters catalyst - Google Patents
A kind of preparation method of bar-shaped NiFeSe/C electrolysis waters catalyst Download PDFInfo
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- CN107587161A CN107587161A CN201710684000.1A CN201710684000A CN107587161A CN 107587161 A CN107587161 A CN 107587161A CN 201710684000 A CN201710684000 A CN 201710684000A CN 107587161 A CN107587161 A CN 107587161A
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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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention relates to a kind of new NiFeSe/C composite nanorods and preparation method thereof, belong to technical field of inorganic nano-material preparation.The present invention prepares NiFeSe/C composite nanorods using Ni/Fe bimetallics metal organic frame as presoma by selenizing.Comprise the following steps that：It is that Ni/Fe bimetallics metal organic frame is made as presoma by hydro-thermal method in reactant first using nickel nitrate, iron chloride, terephthalic acid (TPA) and sodium hydroxide；Further selenizing being carried out under nitrogen protection to presoma using selenium powder, NiFeSe/C composite nanorods are made.Products obtained therefrom has excellent electrolysis water catalytic performance.
Description
Technical field
The present invention relates to a kind of bar-shaped NiFeSe/C combined electrolysis water catalyst and preparation method thereof, belong to inorganic nano material
Expect preparation field.
Background technology
Because having the characteristics of cleaning, be efficient, facilitating, preparing hydrogen and oxygen using electrochemical method splitting water is considered as
It is to solve one of important means of global problem such as energy crisis and the environmental pollution of current serious.By using suitably urging
The overpotential that agent reduces electrolysis water process is to reduce electric energy consumption, improves the important means of electrolysis water conversion efficiency.Platinum family
Metal has an excellent electrolysis water catalytic performance, but its reserves are low, expensive on earth, be unfavorable for electrolysis water technology
Extensive use.Therefore, designing and preparing has important practical significance based on non-noble metal Novel electrolytic water catalyst.
In recent years, metal organic frame is widely used in due to the Modulatory character with appearance structure and chemical constituent
Prepare various new function materials.Because metal organic frame has the high design feature of porosity so that be used as forerunner using it
Material prepared by body is also tended to porous.The carbon enriched in metal organic frame can be easily incorporated into it and be spread out
In green material, have the function that to improve material property.Simultaneously as metal organic frame has confinement effect, can effectively hinder
Only in chemical reaction process metal nanoparticle isoreactivity component reunion, improve the stability of catalyst.
The sulfide of the transition metal such as iron, cobalt, nickel, phosphide, selenides etc. often have excellent electrolysis water catalytic
Energy.Meanwhile such material storage is abundant, cheap, is advantageous to the extensive use of electrolysis water technology.Recently, researcher has found
The methods of passing through doping, multi-component nano material is prepared based on transition metal such as iron, cobalt, nickel, shown in terms of electrolysis water
More excellent catalytic performance.For example, the NiCoP nano wires of the components of R. Zhang et al. three, under the conditions of different acid-base values
All show excellent electrolysis water catalytic performance（Adv. Mater. 2017, 1605502）.As it was previously stated, metal organic frame
Component Modulatory character with height, can easily be made with the metal organic frame containing two kinds of metallic elements as presoma
Standby multi-component electrolysis water catalyst.
The content of the invention
It is an object of the invention to provide a kind of preparation method of novel clubbed NiFeSe/C composite nano materials.The present invention
This preparation method process provided is simple, it is not necessary to which special instrument and equipment, cost is cheap, gained NiFeSe/C nanometer rods tool
There is excellent electrolysis aquatic products hydrogen catalysis performance, be a kind of excellent elctro-catalyst.
The purpose of the present invention is achieved through the following technical solutions, a kind of preparation of new NiFeSe/C composite nanorods
Method, comprise the following steps：
1）Nickel nitrate, iron chloride, terephthalic acid (TPA) and sodium hydroxide are weighed respectively according to certain mol proportion and are dissolved in N, N '-two
In NMF；
2）Step 1 gained mixed solution is transferred in ptfe autoclave, 100 oCIt is lower to react 12 hours and drop naturally
Ni/Fe bimetallic metal organic frames are can obtain after to room temperature；
3）Step 2 gained Ni/Fe bimetallic metal organic frames are put into quartz boat one end, and certain mass is added in the other end
Selenium powder；
4）Quartz boat is put into the high temperature process furnances of nitrogen protection, pays attention to the one end for holding selenium powder being placed in overdraught side
Position, NiFeSe/C composite nanorods are obtained after heating.
Beneficial effects of the present invention：
（1）The invention provides a kind of preparation method of new NiFeSe/C composite nanorods, i.e., prepares Ni/ first with hydro-thermal method
Fe bimetallic metal organic frames, then selenylation reaction is carried out to it product is made.Preparation method is simple, it is not necessary to which specific apparatus is set
Standby, cost is relatively low, has potential large-scale application value；
（2）Product prepared by the present invention is NiFeSe/C composite nanorods, product morphology size uniform；
（3）NiFeSe/C composite nanorods prepared by the present invention have excellent catalytic performance for electrocatalytic decomposition water.
Brief description of the drawings
Fig. 1 is that the NiFeSe/C composite nanorods prepared by the inventive method project electricity with the EX of JEOL JEM 2010
The projection Electronic Speculum shot after the micro- sem observation of son（TEM）Photo；
Fig. 2 is the NiFeSe/C composite nanorods U.S. FEI QUANTA FEG250 scanning electrons prepared by the inventive method
The ESEM shot after micro- sem observation（SEM）Photo；
Fig. 3 is the X-ray diffraction of the NiFeSe/C composite nanorods prepared by the inventive method（XRD）Figure；
Fig. 4 is the x-ray photoelectron energy spectrum diagram of the NiFeSe/C composite nanorods prepared by the inventive method；
Fig. 5 is the NiFeSe/C composite nanorod occasion China 660D electrochemical workstations test gained prepared by the inventive method
Electrolytic water electric current density-potential energy diagram.
Embodiment
Present disclosure is described in further detail below by specific implementation example with reference, but these embodiments
It is not intended to limit protection scope of the present invention.
Embodiment 1
Compound concentration first is 0.033 mole every liter of nickel nitrate, 0.067 mole every liter of iron chloride, 0.1 mole every liter of pair
Phthalic acid and 0.08 mole every liter of sodium hydroxide mixed solution（Solvent is N, N '-dimethyl formamide）, it is then transferred to
In ptfe autoclave.Above-mentioned reactant is reacted 12 hours in 100 degrees Celsius of baking ovens, produced after being down to room temperature naturally
To Ni/Fe bimetallic metal organic frames.Above-mentioned 30 milligrams above-mentioned Ni/Fe bimetallics metal organic frames are placed on quartz boat
One end, and put 90 milligrams of selenium powder in the other end.Quartz boat is put into the high temperature process furnances of nitrogen protection, paid attention to
The one end for holding selenium powder is placed in overdraught orientation, tubular type furnace temperature is risen into 450 with the heating rate of 3 centigrade per minutes takes the photograph
Simultaneously insulation reaction is naturally cooling to obtain NiFeSe/C composite nanorods after room temperature family name's degree after 1 hour.
Embodiment 2
Compound concentration first is 0.03 mole every liter of nickel nitrate, 0.06 mole every liter of iron chloride, 0.1 mole every liter to benzene
Dioctyl phthalate and 0.08 mole every liter of sodium hydroxide mixed solution（Solvent is N, N '-dimethyl formamide）, it is then transferred to poly-
In tetrafluoroethene reactor.Above-mentioned reactant is reacted 12 hours in 110 degrees Celsius of baking ovens, obtained after being down to room temperature naturally
Ni/Fe bimetallic metal organic frames.Above-mentioned 40 milligrams above-mentioned Ni/Fe bimetallics metal organic frames are placed on quartz boat
One end, and put 120 milligrams of selenium powder in the other end.Quartz boat is put into the high temperature process furnances of nitrogen protection, paid attention to
The one end for holding selenium powder is placed in overdraught orientation, tubular type furnace temperature is risen into 450 with the heating rate of 3 centigrade per minutes takes the photograph
Simultaneously insulation reaction is naturally cooling to obtain NiFeSe/C composite nanorods after room temperature family name's degree after 1 hour.
Embodiment 3
The electrolysis water catalytic activity of NiFeSe/C composite nanorods is tested using occasion China 660D electrochemical workstations.With platinum
Silk is that silver/silver chlorate is reference electrode to electrode, to be loaded with the foam nickel sheet of NiFeSe/C composite nanorods as work electricity
Pole, 1.0 moles of every liter of KOH aqueous solution are electrolyte solution.In 1.0 to 1.9 V voltage ranges, per second speed is swept with 5 milliamperes
Carry out linear voltammetric scan, you can obtain the polarization curve of NiFeSe/C composite nanorod catalytic electrolysis aquatic products hydrogen.
Claims (4)
1. a kind of NiFeSe/C composite nanorods, the nanometer rods are using Ni/Fe bimetallics metal organic frame as forerunner's system
Standby, length is about 150 nanometers, and width is about 40 nanometers.
2. a kind of preparation method of NiFeSe/C composite nanorods, it is characterised in that as follows the step of preparation method：
1) hydro-thermal method is used, Ni/Fe bimetallics are made by reactant of nickel nitrate, iron chloride, terephthalic acid (TPA) and sodium hydroxide
Metal organic frame is presoma；
2) one end being transferred to step 1 gained Ni/Fe bimetallic metal organic frames in quartz boat, and put in the other end
The selenium powder of certain mass quality；Quartz boat is put into the high temperature process furnances of nitrogen protection, the one end for holding selenium powder is put
In overdraught orientation, tubular type furnace temperature is risen to after 450 degrees Celsius and insulation reaction certainly with the heating rate of 3 centigrade per minutes
So being cooled to room temperature obtains NiFeSe/C composite nanorods.
3. the preparation method of NiFeSe/C composite nanorods according to claim 2, it is characterised in that the NiFeSe/C
The preparation of composite nanorod is using Ni/Fe bimetallics metal organic frame as presoma.
4. the preparation method of NiFeSe/C composite nanorods according to claim 2, it is characterised in that the Ni/Fe is double
The mass ratio of metallized metal organic frame and selenium powder is 1:3.
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Cited By (15)
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| CN108439549A (en) * | 2018-04-03 | 2018-08-24 | 北京工业大学 | A kind of preparation of array structure transition metal selenides electrode and its application in electrolysis water |
| CN108486605A (en) * | 2018-03-14 | 2018-09-04 | 济南大学 | A kind of carbon coating selenizing nickel cobalt nano material and preparation method thereof with excellent electrolysis water performance |
| CN108842167A (en) * | 2018-06-20 | 2018-11-20 | 中国石油大学(华东) | A kind of preparation method and its usage similar to coralliform NiSe@NC |
| CN109811365A (en) * | 2019-01-25 | 2019-05-28 | 同济大学 | A kind of ferronickel base nano-chip arrays and its preparation and application based on carbon cloth growth |
| CN109830692A (en) * | 2018-12-28 | 2019-05-31 | 中国矿业大学 | Novel lithium-air battery three-dimensional self-supporting positive electrode and its preparation method and application |
| CN110079823A (en) * | 2019-05-15 | 2019-08-02 | 中山大学 | Electrode material, using and preparation method thereof |
| CN110354872A (en) * | 2018-03-26 | 2019-10-22 | 济南大学 | A kind of carbon coating Fe doping NiSe nano material and preparation method thereof with excellent electrolysis elutriation oxygen performance |
| CN110681402A (en) * | 2019-09-10 | 2020-01-14 | 广东工业大学 | Carbon paper-loaded Fe-NiCoP heterostructure and preparation method and application thereof |
| CN111193011A (en) * | 2020-01-08 | 2020-05-22 | 青岛科技大学 | FeS2/FeNiS2Preparation and application of nanoparticles |
| CN112138701A (en) * | 2020-10-20 | 2020-12-29 | 中国石油大学(华东) | Ni0.85Preparation method of Se @ NC electro-catalytic material |
| CN112678784A (en) * | 2020-12-28 | 2021-04-20 | 天目湖先进储能技术研究院有限公司 | Preparation method and application of composite cathode material of sodium-ion battery |
| CN113373476A (en) * | 2021-06-07 | 2021-09-10 | 山东大学深圳研究院 | Phosphorus-doped bimetallic selenide electrocatalyst material with adjustable single metal element electronic structure and preparation method and application thereof |
| CN114621457A (en) * | 2022-04-21 | 2022-06-14 | 安徽大学 | Modified iron-based metal organic framework material and preparation method and application thereof |
| CN115627497A (en) * | 2022-12-21 | 2023-01-20 | 广东工业大学 | Preparation method and application of NiFeSe/NF catalyst |
| CN117463342A (en) * | 2023-12-27 | 2024-01-30 | 山东海化集团有限公司 | Preparation method of porous hollow tubular heterojunction catalyst for electrolyzing seawater and oxygen evolution application of porous hollow tubular heterojunction catalyst |
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| CN108486605A (en) * | 2018-03-14 | 2018-09-04 | 济南大学 | A kind of carbon coating selenizing nickel cobalt nano material and preparation method thereof with excellent electrolysis water performance |
| CN110354872A (en) * | 2018-03-26 | 2019-10-22 | 济南大学 | A kind of carbon coating Fe doping NiSe nano material and preparation method thereof with excellent electrolysis elutriation oxygen performance |
| CN110354872B (en) * | 2018-03-26 | 2022-04-19 | 济南大学 | Carbon-coated Fe-doped NiSe nano material with excellent electrolytic water oxygen evolution performance and preparation method thereof |
| CN108439549B (en) * | 2018-04-03 | 2021-07-09 | 北京工业大学 | Preparation of array structure transition metal selenide electrode and application thereof in electrolytic water |
| CN108439549A (en) * | 2018-04-03 | 2018-08-24 | 北京工业大学 | A kind of preparation of array structure transition metal selenides electrode and its application in electrolysis water |
| CN108842167A (en) * | 2018-06-20 | 2018-11-20 | 中国石油大学(华东) | A kind of preparation method and its usage similar to coralliform NiSe@NC |
| CN109830692A (en) * | 2018-12-28 | 2019-05-31 | 中国矿业大学 | Novel lithium-air battery three-dimensional self-supporting positive electrode and its preparation method and application |
| CN109830692B (en) * | 2018-12-28 | 2021-08-03 | 中国矿业大学 | Preparation method and application of three-dimensional self-supporting positive electrode material of lithium-air battery |
| CN109811365A (en) * | 2019-01-25 | 2019-05-28 | 同济大学 | A kind of ferronickel base nano-chip arrays and its preparation and application based on carbon cloth growth |
| CN110079823A (en) * | 2019-05-15 | 2019-08-02 | 中山大学 | Electrode material, using and preparation method thereof |
| CN110681402B (en) * | 2019-09-10 | 2022-03-25 | 广东工业大学 | Carbon paper-loaded Fe-NiCoP heterostructure and preparation method and application thereof |
| CN110681402A (en) * | 2019-09-10 | 2020-01-14 | 广东工业大学 | Carbon paper-loaded Fe-NiCoP heterostructure and preparation method and application thereof |
| CN111193011A (en) * | 2020-01-08 | 2020-05-22 | 青岛科技大学 | FeS2/FeNiS2Preparation and application of nanoparticles |
| CN112138701A (en) * | 2020-10-20 | 2020-12-29 | 中国石油大学(华东) | Ni0.85Preparation method of Se @ NC electro-catalytic material |
| CN112678784A (en) * | 2020-12-28 | 2021-04-20 | 天目湖先进储能技术研究院有限公司 | Preparation method and application of composite cathode material of sodium-ion battery |
| CN112678784B (en) * | 2020-12-28 | 2023-11-21 | 天目湖先进储能技术研究院有限公司 | Preparation method and application of sodium ion battery composite anode material |
| CN113373476A (en) * | 2021-06-07 | 2021-09-10 | 山东大学深圳研究院 | Phosphorus-doped bimetallic selenide electrocatalyst material with adjustable single metal element electronic structure and preparation method and application thereof |
| CN114621457A (en) * | 2022-04-21 | 2022-06-14 | 安徽大学 | Modified iron-based metal organic framework material and preparation method and application thereof |
| CN115627497A (en) * | 2022-12-21 | 2023-01-20 | 广东工业大学 | Preparation method and application of NiFeSe/NF catalyst |
| CN117463342A (en) * | 2023-12-27 | 2024-01-30 | 山东海化集团有限公司 | Preparation method of porous hollow tubular heterojunction catalyst for electrolyzing seawater and oxygen evolution application of porous hollow tubular heterojunction catalyst |
| CN117463342B (en) * | 2023-12-27 | 2024-04-05 | 山东海化集团有限公司 | Preparation method of porous hollow tubular heterojunction catalyst for electrolyzing seawater and oxygen evolution application of porous hollow tubular heterojunction catalyst |
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