CN107475743A - Foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method - Google Patents
Foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method Download PDFInfo
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- CN107475743A CN107475743A CN201610403915.6A CN201610403915A CN107475743A CN 107475743 A CN107475743 A CN 107475743A CN 201610403915 A CN201610403915 A CN 201610403915A CN 107475743 A CN107475743 A CN 107475743A
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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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
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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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- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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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 present invention relates to a kind of foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method thereof, belong to materials science field and electro-catalysis hydrogen preparation field.For the electrode using three-dimensional foam nickel as carrier, nickel sulphur coating is surface-active layer, and by composite electroplating by CeO2In the composite mixed sulphur coating to nickel, the Ni-based NiS/CeO of foam is formed2Combination electrode.Using composite electroplating, nickel sulphur coating deposition is carried out in three-dimensional foam nickel surface.Meanwhile in electrodeposition process, using magnetic agitation by the nanoscale CeO in composite plating bath2It is doped in nickel sulphur coating.Hydrogen-precipitating electrode prepared by the present invention has the characteristics that overpotential is low, electrode stability is strong, and preparation technology is simple, suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method thereof, belong to material
Expect science and technology field and electro-catalysis hydrogen preparation field.
Background technology
Hydrogen energy source causes countries in the world to be paid close attention to remarkable advantages such as high, the renewable, cleanliness without any pollution of its fuel value.Although
Fossil fuel hydrogen manufacturing using methane steam reforming as representative is most economical hydrogen production process at present, but it is in process of production not only
A large amount of fossil fuels are consumed, and produce great amount of carbon dioxide, it is impossible to fundamentally solve energy crisis and environmental problem.Alkalescence
Electrolysis water conduct is most ancient, the most ripe electrolysis water mode of technology, is following most potential low cost, high efficiency, greenization
Extensive hydrogen producing technology.At present, reduce energy consumption and improve the primary solution that production stability is water electrolysis hydrogen production large-scale application
Certainly problem.
In electrolytic hydrogen production, the selection of hydrogen-precipitating electrode, the design of structure and the optimization of preparation technology are always electrolysis water system
The key of hydrogen, its energy consumption and stability to electrolysis has vital effect, while influences the extensive of electrolytic hydrogen production again
Industrialized production.The noble metals such as platinum palladium have excellent electrocatalytic hydrogen evolution activity, but are limited to the price of costliness, it is difficult in industry
Widely applied in production.Therefore, the new evolving hydrogen electrode tool cheap, overpotential of hydrogen evolution is low and stability is high is researched and developed
There is very important meaning.
The content of the invention
It is an object of the invention to provide the foamed nickel supported doping of a kind of low cost, high catalytic activity and high stability analysis
CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method thereof, it is higher to solve existing hydrogen-precipitating electrode cost, catalytic activity it is not high and
The shortcomings of less stable.
The technical scheme is that：
A kind of foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur, the electrode is using three-dimensional foam nickel as carrier, nickel
Sulphur coating is surface-active layer, and by composite electroplating by CeO2In the composite mixed sulphur coating to nickel, it is Ni-based to form foam
NiS/CeO2Combination electrode.
Described foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur, carrier be purity 99.9wt% three-dimensional it is more
Hole nickel foam, surface density are 400~550g/m2。
Described foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur, adulterate CeO2Nickel sulphur thickness of coating for 2~
4 μm, CeO in nickel sulphur coating2Doping be 12~20wt.%.
Described foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur preparation method, comprise the following steps：
(1) at room temperature, by nickel foam 5~15min of degreasing degreasing in acetone, cleaned with ultra-pure water；Then, it is put into
3~10min of activation process is acidified in 1~3M HCl；Finally, it is put into ultra-pure water and is cleaned by ultrasonic 1~5min and dries stand-by；
(2) pretreated nickel foam in step (1) is put into composite plating bath, anode is made with nickel plate, nickel foam is made cloudy
Pole, 20~50mm distances are kept between two electrodes；Under the magnetic agitation effect that stir speed (S.S.) is 150~300r/min, control
Current density is 5~20mA/cm2, 30~50min of composite electrodeposition；
The composite plating bath composition includes：250~300g/L of nickel sulfate, 40~50g/L of nickel chloride, 35~50g/L of boric acid,
0.05~0.1g/L of lauryl sodium sulfate, 80~120g/L of sodium thiosulfate, nanoscale 5~15g/L of ceria, remaining is
Water；
(3) by step (2) prepared by NiS/CeO2Combination electrode is put into 0.5~1.5M NaOH, in 5~15mA/cm2
Under current density, catholyte activates 10~30min；Then, 3~10min is cleaned with ultra-pure water, it is standby after drying.
Described foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur preparation method, in step (2), prison in time
Bath pH value is controlled, with volume ratio 3:1 hydrochloric acid and the mixed liquor of sulfuric acid, make plating solution pH be maintained between 3.5~4.0.
The present invention is after adopting the above technical scheme, main have the advantage that and beneficial effect：
(1) catalytic activity of hydrogen evolution is good.NiS alloys provide electro-chemical activity site, promote hydrone O-H keys to be broken rapidly.
It is composite mixed enter coating CeO2Nano-particle provides reasonable adsorption potential for H atom, discharges NiS avtive spots, avoid due to
Excessive hydrogen covering on electrode surface and caused by electrode inactivate, while accelerate H desorption processes.
(2) stability is good.CeO of the present invention2Compound particle produces steric effect, solid S effects, slows down S active dissolution.Together
When, composite nanoparticle also acts the effect of dispersion-strengtherning, strengthens electrode mechanical strength, it is strong to improve the resistance to bubble impact of electrode
Degree.
(3) preparation technology is simple, cost is low.Under same aperture, nickel foam has bigger specific surface area compared to nickel wire net
And price advantage.Moreover, electroplating technology technical maturity, process transplanting convenient to carry out.Electroplating device less investment, processing and safeguard into
This is low.
Brief description of the drawings
Fig. 1 is the microcosmic electron microscope of electrode prepared by the present invention.
Fig. 2 is the energy spectrum diagram of electrode prepared by the present invention.
Fig. 3 is electrode and the Hydrogen Evolution Performance correlation curve of contrast experiment prepared by the present invention.
Embodiment
The present invention is discussed in detail for specific embodiment below, there is provided embodiment is for the ease of understanding the present invention, is definitely not
The limitation present invention.
Embodiment 1
In the present embodiment, the Ni-based NiS/CeO of foam2The preparation method of combination electrode, using composite electroplating, in three-dimensional
Foam nickel surface carries out nickel sulphur coating deposition.Meanwhile in electrodeposition process, using magnetic agitation by the nanometer in composite plating bath
Level CeO2It is doped in nickel sulphur coating, comprises the following steps that：
(1) nickel foam selection and pretreatment
The purity of the three-dimensional porous foams nickel is 99.9%, surface density 480g/m2.At room temperature, by nickel foam third
Degreasing degreasing 10min in ketone, is cleaned with ultra-pure water；Then, it is put into 2M (molar concentration) HCl and is acidified activation process
5min；Finally, it is put into ultra-pure water and is cleaned by ultrasonic 2min and dries stand-by.
(2) the Ni-based NiS/CeO of foam is prepared2Combination electrode
Pretreated nickel foam in step (1) is put into composite plating bath, anode is made with nickel plate, nickel foam makees negative electrode,
30mm distances are kept between two electrodes.Under the magnetic agitation effect that stir speed (S.S.) is 180r/min, control electric current density is
10mA/cm2, composite electrodeposition 30min.The composite plating bath composition includes：Nickel sulfate 300g/L, nickel chloride 45g/L, boric acid
38g/L, lauryl sodium sulfate 0.1g/L, sodium thiosulfate 100g/L, nanoscale ceria 10g/L, remaining is water.Together
When, it is necessary to bath pH value be monitored in time, with the mixed liquor of hydrochloric acid and sulfuric acid (volume ratio 3:1) plating solution pH is maintained at 3.5~4.0
Between.
(3) activation process of combination electrode
By the Ni-based NiS/CeO of foam prepared by step (2)2Combination electrode is put into 1MNaOH, in 10mA/cm2Electric current is close
Under degree, catholyte activation 10min；Then, 5min is cleaned with ultra-pure water, it is standby after drying.In the present embodiment, CeO is adulterated2's
Nickel sulphur thickness of coating is 2~3 μm, CeO in nickel sulphur coating2Doping be 12~16wt.%.
As shown in figure 1, find out from the microcosmic electron microscope of prepared electrode, electrode surface without obvious crackle, and surface have it is bright
Aobvious particulate inclusion.
As shown in Fig. 2 the energy spectrum diagram from prepared electrode is found out, source/drain removes Ni-S coating and CeO2The outer nothing of particle
Other impurities, and amount containing S is higher.
As shown in figure 3, the Hydrogen Evolution Performance correlation curve from prepared electrode and contrast experiment finds out that prepared electrode has
Higher hydrogen evolution activity.
Embodiment 2
In the present embodiment, the Ni-based NiS/CeO of foam2The preparation method of combination electrode, using composite electroplating, in three-dimensional
Foam nickel surface carries out nickel sulphur coating deposition.Meanwhile in electrodeposition process, using magnetic agitation by the nanometer in composite plating bath
Level CeO2It is doped in nickel sulphur coating, comprises the following steps that：
(1) nickel foam selection and pretreatment
The purity of the three-dimensional porous foams nickel is 99.9%, surface density 550g/m2.At room temperature, by nickel foam third
Degreasing degreasing 10min in ketone, is cleaned with ultra-pure water；Then, it is put into 2M HCl and is acidified activation process 5min；Finally, put
Enter to be cleaned by ultrasonic in ultra-pure water 2min and dry stand-by.
(2) the Ni-based NiS/CeO of foam is prepared2Combination electrode
Pretreated nickel foam in step (1) is put into composite plating bath, anode is made with nickel plate, nickel foam makees negative electrode,
30mm distances are kept between two electrodes.Under the magnetic agitation effect that stir speed (S.S.) is 300r/min, control electric current density is
10mA/cm2, composite electrodeposition 30min.The composite plating bath composition includes：Nickel sulfate 300g/L, nickel chloride 45g/L, boric acid
38g/L, lauryl sodium sulfate 0.1g/L, sodium thiosulfate 120g/L, nanoscale ceria 10g/L, remaining is water.Together
When, it is necessary to bath pH value be monitored in time, with the mixed liquor of hydrochloric acid and sulfuric acid (volume ratio 3:1) plating solution pH is maintained at 3.5~4.0
Between.
(3) activation process of combination electrode
By the Ni-based NiS/CeO of foam prepared by step (2)2Combination electrode is put into 1M NaOH, in 10mA/cm2Electric current
Under density, catholyte activation 20min；Then, 5min is cleaned with ultra-pure water, it is standby after drying.In the present embodiment, CeO is adulterated2
Nickel sulphur thickness of coating be 2~3 μm, CeO in nickel sulphur coating2Doping be 14~18wt.%.
Embodiment 3
In the present embodiment, the Ni-based NiS/CeO of foam2The preparation method of combination electrode, using composite electroplating, in three-dimensional
Foam nickel surface carries out nickel sulphur coating deposition.Meanwhile in electrodeposition process, using magnetic agitation by the nanometer in composite plating bath
Level CeO2It is doped in nickel sulphur coating, comprises the following steps that：
(1) nickel foam selection and pretreatment
The purity of the three-dimensional porous foams nickel is 99.9%, surface density 500g/m2.At room temperature, by nickel foam third
Degreasing degreasing 10min in ketone, is cleaned with ultra-pure water；Then, it is put into 2M HCl and is acidified activation process 5min；Finally, put
Enter to be cleaned by ultrasonic in ultra-pure water 2min and dry stand-by.
(2) the Ni-based NiS/CeO of foam is prepared2Combination electrode
Pretreated nickel foam in step (1) is put into composite plating bath, anode is made with nickel plate, nickel foam makees negative electrode,
30mm distances are kept between two electrodes.Under the magnetic agitation effect that stir speed (S.S.) is 250r/min, control electric current density is
10mA/cm2, composite electrodeposition 40min.The composite plating bath composition includes：Nickel sulfate 300g/L, nickel chloride 45g/L, boric acid
38g/L, lauryl sodium sulfate 0.1g/L, sodium thiosulfate 80g/L, nanoscale ceria 10g/L, remaining is water.Meanwhile
Need to monitor bath pH value in time, with the mixed liquor of hydrochloric acid and sulfuric acid (volume ratio 3:1) by plating solution pH be maintained at 3.5~4.0 it
Between.
(3) activation process of combination electrode
By the Ni-based NiS/CeO of foam prepared by step (2)2Combination electrode is put into 1M NaOH, in 10mA/cm2Electric current
Under density, catholyte activation 15min；Then, 5min is cleaned with ultra-pure water, it is standby after drying.In the present embodiment, CeO is adulterated2
Nickel sulphur thickness of coating be 3~4 μm, CeO in nickel sulphur coating2Doping be 16~20wt.%.
Embodiment result shows that the hydrogen-precipitating electrode prepared by the present invention has the characteristics that overpotential is low, electrode stability is strong,
And preparation technology is simple, suitable for large-scale production.Above-mentioned embodiment is in order to illustrate the features of the present invention, still
The present invention is not limited to above-described embodiment, in those of ordinary skill in the art's possessed knowledge, can also not take off
Various change is made obtaining on the premise of from present inventive concept, also should be regarded as protection scope of the present invention.
Claims (5)
- A kind of 1. foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur, it is characterised in that the electrode using three-dimensional foam nickel as Carrier, nickel sulphur coating are surface-active layer, and by composite electroplating by CeO2In the composite mixed sulphur coating to nickel, bubble is formed The Ni-based NiS/CeO of foam2Combination electrode.
- 2. according to the foamed nickel supported doping CeO described in claim 12The compound hydrogen-precipitating electrode of nickel sulphur, it is characterised in that carrier For purity 99.9wt% three-dimensional porous foams nickel, surface density is 400~550g/m2。
- 3. according to the foamed nickel supported doping CeO described in claim 12The compound hydrogen-precipitating electrode of nickel sulphur, it is characterised in that doping CeO2Nickel sulphur thickness of coating be 2~4 μm, CeO in nickel sulphur coating2Doping be 12~20wt.%.
- A kind of 4. foamed nickel supported doping CeO described in claim 12The compound hydrogen-precipitating electrode of nickel sulphur preparation method, its feature It is, comprises the following steps：(1) at room temperature, by nickel foam 5~15min of degreasing degreasing in acetone, cleaned with ultra-pure water；Then, it is put into 1~ 3~10min of activation process is acidified in 3M HCl；Finally, it is put into ultra-pure water and is cleaned by ultrasonic 1~5min and dries stand-by；(2) pretreated nickel foam in step (1) being put into composite plating bath, anode is made with nickel plate, nickel foam makees negative electrode, and two 20~50mm distances are kept between electrode；Under the magnetic agitation effect that stir speed (S.S.) is 150~300r/min, control electric current is close Spend for 5~20mA/cm2, 30~50min of composite electrodeposition；The composite plating bath composition includes：250~300g/L of nickel sulfate, 40~50g/L of nickel chloride, boric acid 35~50g/L, 12 0.05~0.1g/L of sodium alkyl sulfate, 80~120g/L of sodium thiosulfate, nanoscale 5~15g/L of ceria, remaining is water；(3) by step (2) prepared by NiS/CeO2Combination electrode is put into 0.5~1.5M NaOH, in 5~15mA/cm2Electric current Under density, catholyte activates 10~30min；Then, 3~10min is cleaned with ultra-pure water, it is standby after drying.
- 5. according to the foamed nickel supported doping CeO described in claim 42The compound hydrogen-precipitating electrode of nickel sulphur preparation method, its feature It is, in step (2), monitors bath pH value in time, with volume ratio 3:1 hydrochloric acid and the mixed liquor of sulfuric acid, keep plating solution pH Between 3.5~4.0.
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| CN201610403915.6A CN107475743A (en) | 2016-06-07 | 2016-06-07 | Foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method |
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| CN201610403915.6A CN107475743A (en) | 2016-06-07 | 2016-06-07 | Foamed nickel supported doping CeO2The compound hydrogen-precipitating electrode of nickel sulphur and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108097269A (en) * | 2017-12-19 | 2018-06-01 | 南京晓庄学院 | A kind of ultra-thin porous Ce-Ni-O-S nanometer sheets and its preparation method and application |
| CN111686743A (en) * | 2020-05-20 | 2020-09-22 | 上海应用技术大学 | La/NF hydrogen evolution material and preparation method and application thereof |
| CN111841553A (en) * | 2020-08-17 | 2020-10-30 | 吉林大学 | Foam nickel-based Nano-K2Fe4O7Catalyst, preparation method and application of catalyst in high-efficiency electrocatalytic hydrolysis |
-
2016
- 2016-06-07 CN CN201610403915.6A patent/CN107475743A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| ZHEN ZHENG等: "Electrochemical synthesis of NieS/CeO2 composite electrodes for hydrogen evolution reaction", 《JOURNAL OF POWER SOURCES》 * |
| 袁铁锤: "电沉积Ni-S合金析氢阴极材料及析氢机理的研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108097269A (en) * | 2017-12-19 | 2018-06-01 | 南京晓庄学院 | A kind of ultra-thin porous Ce-Ni-O-S nanometer sheets and its preparation method and application |
| CN108097269B (en) * | 2017-12-19 | 2018-10-30 | 南京晓庄学院 | A kind of ultra-thin porous Ce-Ni-O-S nanometer sheets and its preparation method and application |
| CN111686743A (en) * | 2020-05-20 | 2020-09-22 | 上海应用技术大学 | La/NF hydrogen evolution material and preparation method and application thereof |
| CN111841553A (en) * | 2020-08-17 | 2020-10-30 | 吉林大学 | Foam nickel-based Nano-K2Fe4O7Catalyst, preparation method and application of catalyst in high-efficiency electrocatalytic hydrolysis |
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Application publication date: 20171215 |