CN107761128A - A kind of FeNiNC electrode materials, preparation method and applications - Google Patents
A kind of FeNiNC electrode materials, preparation method and applications Download PDFInfo
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- CN107761128A CN107761128A CN201711101347.5A CN201711101347A CN107761128A CN 107761128 A CN107761128 A CN 107761128A CN 201711101347 A CN201711101347 A CN 201711101347A CN 107761128 A CN107761128 A CN 107761128A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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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- 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
The invention discloses a kind of FeNiNC electrode materials, preparation method and applications.The present invention first mixes Fe(NO3)39H2O, urea, trisodium citrate and water, and solution hydro-thermal reaction generates colloid after mixing；Then nickel foam is immersed in colloid and soaked, after immersion terminates, nickel foam taken out and is put into vacuum drying chamber drying；Finally calcining obtains FeNiNC electrode materials.FeNiNC materials prepared by the present invention have the bulk multi-hole structure similar to nickel foam, and cost of material is low, and liberation of hydrogen works well, and is expected to towards industrialization development.
Description
Technical field
The present invention relates to hydrogen energy source technical field, specifically, be related to a kind of FeNiNC electrode materials, preparation method and its
Using.
Background technology
The energy and environment are the main problems that human social is related to.The energy requirement in the whole world 80% at present
From fossil fuel, this will finally cause the exhaustion of fossil fuel, and it uses and also leads to serious environmental pollution.From
Fossil fuel progressively turn to using the free of contamination non-fossil energy of sustainable development be development inexorable trend.Hydrogen is preferably clear
One of clean energy is also the industrial chemicals of weight, is widely paid attention to by countries in the world.Water electrolysis hydrogen production is to realize industrialize, be cheap
Prepare the important means of hydrogen.Water electrolysis hydrogen production has the advantages that easy, pollution is small, product purity is high, but its liberation of hydrogen is anti-
Answer (2H++2e→H2Or 2H2O+2e→H2+2OH-) more serious cathodic polarization be present, cause higher hydrogen manufacturing cost, be not suitable for
Large-scale application.Electrocatalytic hydrogen evolution (the ElectrocatalyticHydrogen Evolution that developed recently gets up
Reaction, HER) be considered as great application prospect green hydrogen producing technology.This hydrogen producing technology in the presence of catalyst,
Overpotential of hydrogen evolution can be greatly lowered, there is low energy consumption, efficiency high, advantages of environment protection.Based on noble metals such as Pt, Pd
It is low that catalyst not only originates overpotential, and activity and stability are all fine, are the best catalyst of current Hydrogen Evolution Performance.But
These noble metals are expensive, are unfavorable for practical application.
Base metal liberation of hydrogen catalyst mainly have the phosphide based on transition metal such as Mo, W, Fe, Co, Ni, sulfide with
And their alloy etc..Because the content (about 0.00011%) of Mo and W in the earth's crust is far below Fe (6.8%), Co
(0.003%), Ni (0.0089%) content, therefore, develop the electrocatalytic hydrogen evolution catalyst based on Fe, Co, Ni and be more beneficial for
The extensive industrialization of electrocatalytic hydrogen evolution technology.In recent years the electrocatalytic hydrogen evolution catalyst based on Fe, Co, Ni has obtained sending out energetically
Exhibition, is prepared for the catalyst of many excellent performances, good impetus is served to electrocatalytic hydrogen evolution technological industrialization.This
A little catalyst mainly include Fe, Co, Ni alloy, phosphide, sulfide etc.,
R.B.Levy has been found that carbide possesses similar Pt catalytic property with M.Boudart, and this is primarily due to it
There are similar Pt d having electronic states, based on this discovery, also (alcohol decomposes and activation from heterogeneous catalysis for the application of tungsten carbide
Oxygen) expand to fuel cell electrolysis, electrolyzer etc..The special construction of carbide, determine that it possesses good property on HER
Can, therefore, the catalyst using carbide as matrix is also just gradually applied to these new fields.
The content of the invention
For technical problem existing for prior art, the present invention proposes a kind of low nitrogen co-doped FeNiNC electrodes of carbon of cost
Material, preparation method, and have studied its application in terms of electrocatalytic hydrogen evolution.Described hybrid catalyst is urged than existing electricity
Agent cost is low, and the overpotential when introducing of nonmetalloid reduces electrocatalytic hydrogen evolution, improves electrocatalytic hydrogen evolution
Effect, the catalyst stability is good, and preparation method is simple, enhances the performance of electrocatalytic hydrogen evolution.
The present invention provides a kind of preparation method of FeNiNC electrode materials, first by Fe(NO3)39H2O, urea, citric acid
Trisodium and water mixing, solution carries out hydro-thermal reaction after mixing, and reaction removes the unnecessary moisture of supernatant, generates colloid after terminating；So
Nickel foam is immersed in colloid afterwards and soaked, after immersion terminates, nickel foam is taken out and is put into vacuum drying chamber drying；Finally calcine
Obtain FeNiNC electrode materials.
In the present invention, nickel foam each soaks 10~20min of ultrasound before using in water, acetone, ethanol.
In the present invention, the mass ratio of Fe(NO3)39H2O, urea and trisodium citrate is (0.5~1)：(0.5~5)：
(0.0008~0.0016).Trisodium citrate is added to control colloidal particle size, allows colloidal solid to disperse more uniform.
In the present invention, the mass ratio of Fe(NO3)39H2O and water is 1:50~1:100.
In the present invention, the temperature of hydro-thermal reaction is 140~160 DEG C；Reaction time is 22~26h.
In the present invention, soak time is 10~15h；Drying temperature is 50~65 DEG C.
In the present invention, calcining heat is 750~850 DEG C, and calcination time is 1~3h.
The present invention also provides the FeNiNC electrode materials that a kind of above-mentioned preparation method obtains.
The present invention further provides a kind of application of above-mentioned FeNiNC electrode materials in electrocatalytic hydrogen evolution reaction.Using
Method comprises the following steps：
(1) Nation solution 0.2-0.5wt% is matched somebody with somebody.Weigh the above-mentioned hybrid catalysts of 1mg and be dissolved in what 100 μ L were prepared
In Nation solution, the dispersed half an hour under ultrasound.Then the solution is drawn into 6-24 μ L on glass-carbon electrode again, from
So dry.
(2) electrolyte of the 0.5M aqueous sulfuric acid as electro-catalysis is prepared, nitrogen is passed through and throws out air, with 0.5M sulphur
Acid solution cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemical operation
Stand, measure the performance of the hybrid catalyst electrocatalytic hydrogen evolution in an acidic solution.
Compared to the prior art, the beneficial effects of the present invention are：
The Tafel slopes and overpotential of the electrode material are low, therefore liberation of hydrogen works well, and the introducing of nonmetalloid is led
Cause having good stability for catalyst.
Using the present invention electrocatalytic hydrogen evolution electrode material in acid medium electrolysis water, find liberation of hydrogen of the present invention by contrast
Effect, overpotential is low, and cost is relatively low.Wherein, electrocatalysis characteristic test is carried out in 0.5M sulfuric acid solution.
In the present invention, as transition metal, its own can be by adjusting electronic structure for ferro element and nickel element
To improve electro-chemical activity, cause the material bulk multi-hole after carbonization using the skeleton of nickel foam, enhance catalyst in acidity
Proton adsorption ability in solution, so as to enhance the ability of electrocatalytic hydrogen evolution.Nonmetallic introducing not only passes through electric charge transfer
And/or it is adjoint it is structurally-modified adjust the electronic structure of metal host significantly, so as to urging for significant raising base metal center
Change efficiency, and the stability of electrode material can be improved.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.
Various raw materials used, are commercially available unless otherwise specified in various embodiments of the present invention.
Embodiment 1
Fe(NO3)39H2O 0.7g
Urea 0.9g
Trisodium citrate 1.3mg
Nickel foam is a piece of (1cm*4cm)
Surplus is distilled water
It is prepared by the preparation method of above-mentioned composite as follows：
Fe(NO3)39H2O is made into 1M solution, urea is made into 0.5M solution, and trisodium citrate is made into the molten of 0.01M
Liquid, 1.5mL iron nitrate solutions are then measured, 6mL urea liquids and 2mL citric acid three sodium solutions add in 100mL beakers
70mL distilled water dilutings, solution is put into high temperature water heating kettle into hydro-thermal 20h in 150 DEG C, will be upper after cooling into ferric hydroxide colloid
Clear unnecessary moisture is gone.It is some to get out 1cm*4cm nickel foam, each immersion is ultrasonic in water, acetone, ethanol by it
15min, it is put into baking oven and dries.Then the nickel foam Jing Guo pre-treatment is immersed in ferric hydroxide colloid and soaks a night, so
Nickel foam is taken out afterwards and is put into vacuum drying chamber drying, is finally passed through nitrogen, 2h is calcined at 800 DEG C and obtains FeNiNC electrode materials
Material.
Application Example 1
The product of embodiment 1 is ground, glassy carbon electrode surface is clean using 0.05 μm of alumina lap, remove
Residual sample, rinsed well, dried using second alcohol and water.
(1) Nation solution 0.5wt% is matched somebody with somebody with absolute methanol.Weigh the above-mentioned hybrid catalysts of 1mg and be dissolved in 100 μ L preparations
In good Nation solution, dispersed two hours under ultrasound.Then the solution is drawn into 18 μ L on glass-carbon electrode again,
Naturally dry.
(2) electrolyte of the 0.5M aqueous sulfuric acid as electro-catalysis is prepared, nitrogen is passed through and throws out air, with 0.5M sulphur
Aqueous acid cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemistry work
Stand, measure the performance of the electrode material electrocatalytic hydrogen evolution in an acidic solution, material Tafel slopes are 96mV dec-1,
Current density is 10mA cm-2Overpotential be 213mV.
Embodiment 2
Fe(NO3)39H2O 1.1g
Urea 0.9g
Trisodium citrate 1.3mg
Nickel foam is a piece of
Surplus is distilled water
The preparation method of above-mentioned composite as follows：
Fe(NO3)39H2O is made into 1M solution, urea is made into 0.5M solution, and trisodium citrate is made into the molten of 0.01M
Liquid, 2.5mL iron nitrate solutions are then measured, 6mL urea liquids and 2mL citric acid three sodium solutions add in 100mL beakers
70mL distilled water dilutings, solution is put into high temperature water heating kettle into hydro-thermal 24h in 150 DEG C, will be upper after cooling into ferric hydroxide colloid
Clear unnecessary moisture is gone.It is some to get out 1cm*4cm nickel foam, each immersion is ultrasonic in water, acetone, ethanol by it
15min, it is put into baking oven and dries.Then the nickel foam Jing Guo pre-treatment is immersed in ferric hydroxide colloid and soaks a night, so
Nickel foam is taken out afterwards and is put into vacuum drying chamber drying, is finally passed through nitrogen, 2h is calcined at 800 DEG C and obtains FeNiNC electrode materials
Material.
Application Example 2
The product of embodiment 2 is ground, glassy carbon electrode surface is clean using 0.05 μm of alumina lap, remove
Residual sample, rinsed well, dried using second alcohol and water.
(1) Nation solution 0.6wt% is matched somebody with somebody with absolute methanol.Weigh the above-mentioned hybrid catalysts of 1mg and be dissolved in 100 μ L preparations
In good Nation solution, dispersed two hours under ultrasound.Then the solution is drawn into 18 μ L on glass-carbon electrode again,
Naturally dry.
(2) electrolyte of the 0.5M aqueous sulfuric acid as electro-catalysis is prepared, nitrogen is passed through and throws out air, with 0.5M sulphur
Aqueous acid cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemistry work
Stand, measure the performance of the electrode material electrocatalytic hydrogen evolution in an acidic solution, material Tafel slopes are 128mV dec-1,
It is 10mA cm in current density-2Overpotential be 250mV.
Embodiment 3
Fe(NO3)39H2O 0.7g
Urea 0.9g
Trisodium citrate 2.5mg
Nickel foam is a piece of
Surplus is distilled water
The preparation method of above-mentioned composite as follows：
Fe(NO3)39H2O is made into 1M solution, urea is made into 0.5M solution, and trisodium citrate is made into the molten of 0.01M
Liquid, 1.5mL iron nitrate solutions are then measured, 6mL urea liquids and 4mL citric acid three sodium solutions add in 100mL beakers
70mL distilled water dilutings, solution is put into high temperature water heating kettle into hydro-thermal 24h in 150 DEG C, will be upper after cooling into ferric hydroxide colloid
Clear unnecessary moisture is gone.It is some to get out 1cm*4cm nickel foam, each immersion is ultrasonic in water, acetone, ethanol by it
15min, it is put into baking oven and dries.Then the nickel foam Jing Guo pre-treatment is immersed in ferric hydroxide colloid and soaks a night, so
Nickel foam is taken out afterwards and is put into vacuum drying chamber drying, is finally passed through nitrogen, 2h is calcined at 800 DEG C and obtains FeNiNC electrode materials
Material.
Application Example 3
The product of embodiment 3 is ground, glassy carbon electrode surface is clean using 0.05 μm of alumina lap, remove
Residual sample, rinsed well, dried using second alcohol and water.
(1) Nation solution 0.5wt% is matched somebody with somebody with absolute methanol.Weigh the above-mentioned hybrid catalysts of 1mg and be dissolved in 100 μ L preparations
In good Nation solution, dispersed two hours under ultrasound.Then the solution is drawn into 24 μ L on glass-carbon electrode again,
Naturally dry.
(2) electrolyte of the 0.5M aqueous sulfuric acid as electro-catalysis is prepared, nitrogen is passed through and throws out air, with 0.5M sulphur
Aqueous acid cleans the electrode surface of glass-carbon electrode, and glass-carbon electrode, Ag/AgCl electrodes, platinum electrode then are connected into electrochemistry work
Stand, measure the performance of the electrode material electrocatalytic hydrogen evolution in an acidic solution, material Tafel slopes are 113mV dec-1,
It is 10mA cm in current density-2Overpotential be 236mV.
Claims (9)
1. a kind of preparation method of FeNiNC electrode materials, it is characterised in that first by Fe(NO3)39H2O, urea, citric acid
Trisodium and water mixing, solution carries out hydro-thermal reaction after mixing, and reaction removes the unnecessary moisture of supernatant, generates colloid after terminating；So
The good nickel foam of pre-treatment is immersed in colloid afterwards and soaked, after immersion terminates, nickel foam is taken out and is put into vacuum drying chamber drying；
Finally calcining obtains FeNiNC electrode materials.
2. preparation method according to claim 1, it is characterised in that nickel foam is respective in water, acetone, ethanol before using
Soak 10~20min of ultrasound.
3. preparation method according to claim 1, it is characterised in that Fe(NO3)39H2O, urea and trisodium citrate
Mass ratio is (0.5~1)：(0.5~5)：(0.0008~0.0016).
4. preparation method according to claim 1, it is characterised in that the mass ratio of Fe(NO3)39H2O and water is 1:50~
1:100。
5. preparation method according to claim 1, it is characterised in that the temperature of hydro-thermal reaction is 140~160 DEG C；Reaction
Time is 22~26h.
6. preparation method according to claim 1, it is characterised in that soak time is 10~15h；Drying temperature be 50~
65℃。
7. preparation method according to claim 1, it is characterised in that calcining heat is 750~850 DEG C, calcination time 1
~3h.
A kind of 8. FeNiNC electrode materials that preparation method according to one of claim 1~7 obtains.
A kind of 9. application of FeNiNC electrode materials according to claim 8 in electrocatalytic hydrogen evolution reaction.
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| CN109967080A (en) * | 2019-03-28 | 2019-07-05 | 浙江大学 | A kind of preparation method and application for amorphous (Ni, Fe) the OOH film elctro-catalyst being supported on foam nickel surface |
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| CN116078398A (en) * | 2023-02-13 | 2023-05-09 | 中国石油大学(华东) | Porous MnFe catalyst and preparation method and application thereof |
| CN116078398B (en) * | 2023-02-13 | 2024-04-19 | 中国石油大学(华东) | Porous MnFe catalyst and preparation method and application thereof |
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