CN112808284A - Ni2Novel preparation method of P/Ni composite electrode material and application of P/Ni composite electrode material in aspect of hydrogen production catalysis by electrolyzing water - Google Patents
Ni2Novel preparation method of P/Ni composite electrode material and application of P/Ni composite electrode material in aspect of hydrogen production catalysis by electrolyzing water Download PDFInfo
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- CN112808284A CN112808284A CN201911124308.6A CN201911124308A CN112808284A CN 112808284 A CN112808284 A CN 112808284A CN 201911124308 A CN201911124308 A CN 201911124308A CN 112808284 A CN112808284 A CN 112808284A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000001257 hydrogen Substances 0.000 title claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000007772 electrode material Substances 0.000 title claims abstract description 9
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 153
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 47
- 238000000576 coating method Methods 0.000 claims abstract description 18
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 14
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 14
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- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
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- 229910052723 transition metal Inorganic materials 0.000 abstract description 17
- 150000003624 transition metals Chemical class 0.000 abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 6
- 239000011574 phosphorus Substances 0.000 abstract description 6
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
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- 239000011261 inert gas Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000011160 research Methods 0.000 description 7
- 238000002791 soaking Methods 0.000 description 6
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 5
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- 238000004502 linear sweep voltammetry Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
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- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
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- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- VAKIVKMUBMZANL-UHFFFAOYSA-N iron phosphide Chemical compound P.[Fe].[Fe].[Fe] VAKIVKMUBMZANL-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- -1 metal oxides iridium dioxide Chemical class 0.000 description 1
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- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
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Images
Classifications
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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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- B01J35/33—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/28—Phosphorising
-
- 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
-
- 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
Ni2The invention relates to the field of electrochemical catalysis, in particular to a novel preparation method of a P/Ni composite electrode material and an application technology thereof in hydrogen catalysis of electrolytic water, and creatively adopts a coating and annealing mode to synthesize self-supporting Ni on foamed nickel2The P electrode is also applied to the catalysis field of hydrogen production by electrolyzing water. The technical problem solved is to explore transition metal phosphide (Ni)2P) is environment-friendly, and the environment is protected,non-toxic, simple and efficient preparation method and process. The key point of the technical scheme for solving the problem is 1, uniformly coating an organic polymer phosphorus source, namely phytic acid 2 on the foamed nickel, annealing the precursor (800 ℃) in a tube furnace at a certain heating rate under the atmosphere of inert gas and preserving heat for 2 hours. The invention is mainly applied to the electrolytic water Hydrogen Evolution Reaction (HER) nano catalytic material to reduce the overpotential of the hydrogen evolution reaction.
Description
Technical Field
The invention relates to the field of electrochemical catalysis, and creatively synthesizes self-supporting Ni on foamed nickel by adopting a coating and high-temperature reaction mode2The P electrode is also applied to the catalysis field of hydrogen production by electrolyzing water.
Background
The energy crisis and the environmental problem are two major problems of human sustainable development, and the two problems are closely related, so that the search for green energy which has no pollution to the environment and can be continuously regenerated is a goal of modern scientists in all the time. With the development of industrial society and economy, the consumption of fossil fuels such as petroleum and coal by human beings is increasing, and the problem of global environmental pollution is becoming more severe. But the reserves of these fossil energy sources are limited and these resources will eventually be exhausted. Therefore, the search for a clean and sustainable alternative energy source is a key problem to be solved by the human social letter. Because wind energy, solar energy and other energy sources are difficult to store and transport, development, storage and transportation of convenient and efficient energy sources become the key point of common research of scientists in various countries. Because hydrogen has the characteristics of light weight, large combustion heat value, cleanness, no pollution and the like, and is an environment-friendly low-carbon energy source, the development of hydrogen energy becomes one of the hot spots of research in the field of new energy. The products of hydrogen combustion do not produce CO in addition to water, as compared to other fossil fuels2Carbon-containing compounds such as CO and other pollutants harmful to the environment such as particles and dust, and therefore hydrogen energy is considered to be the cleanest energy source in the 21 st century. At present, hydrogen energy is mainly obtained from traditional fossil fuel, so how to continuously and efficiently prepare hydrogen gas becomes a key target of research of scientists in various countries, and the method also has important significance for reducing the use of the fossil fuel.
Electrochemistry plays an important role in industrial production, such as chemical biological reaction, environmental protection, production and production of clean energy, particularly water energy and solar energy, while Hydrogen Evolution Reaction (HER) by photo/chemical hydrolysis is an important means for producing hydrogen energy, and Oxygen Evolution Reaction (OER), Oxygen Reduction Reaction (ORR) used in fuel cells, etc. can be used for producing clean hydrogen energy. However, these reactions require catalysts to accelerate the reaction process, and current studies show that noble metal platinum (Pt) and noble metal oxides iridium dioxide, ruthenium dioxide (IrO)2，RuO2) Etc. have been proven to possess good catalytic properties and have been put to industrial use. However, it is possible to use a single-layer,the above-mentioned catalysts have limitations in their use, such as low selectivity, poor current durability, and susceptibility to adverse environmental effects, and more importantly, their high cost has limited their wide-scale commercial use, and therefore, it is certainly important to develop a non-noble metal nano-electrocatalyst.
Non-noble metal phosphides are of great interest because of their excellent electrocatalytic properties and versatility. Since the discovery of transition metal phosphides in the 19 th century, transition metal phosphides have been increasingly used in the field of electrocatalysis, and in the early days, most of them were produced by phosphating a phosphorus source precursor at high temperature or by grinding metal, for example, in the synthesis of iron phosphide, mainly by phosphating metallic iron at 900 ℃ with red phosphorus as a phosphorus source. The reaction not only easily produces high-activity and spontaneous combustion byproducts, but also easily causes danger and is difficult to separate products. Nevertheless, these synthetic methods are still widely used to prepare TMPs. Reducing the temperature is an effective method. For example, using a phosphorus source (e.g., NaH) having a lower decomposition or evaporation temperature2PO2), but the reaction releases exhaust gas PH which is a strong pollutant to the environment and human body3And liquid phase reactions to produce Transition Metal Phosphides (TMPs), and these processes generally involve the use of organic phosphorus, such as Triphenylphosphine (TOP). Since triphenylphosphine (as is the case with other commonly used organophosphorous sources) is insoluble in water, its decomposition temperature is high, making the chemical reaction highly flammable. And the extremely corrosive nature of the reactants means that they can only be carried out in a strictly oxygen-free environment, and it is very much urgent to develop a novel method for preparing transition metal phosphides because the development and application of TMP are hindered by the disadvantages of solid state reaction or solution phase reaction.
Disclosure of Invention
The invention adopts a novel method to prepare the transition metal phosphide loaded on the nickel foam to research the electrocatalytic hydrogen evolution performance of the nickel foam. In the research, phytic acid is uniformly coated on the surface of the foamed nickel by a coating method, and then the transition metal phosphide is prepared by one-step high-temperature treatment. And then, the morphology and microstructure of the prepared transition metal phosphide are further represented, the electrocatalytic performance of the transition metal phosphide is tested, and a new thought and a new method are provided for preparing novel transition metal phosphide materials.
In order to achieve the purpose of the invention, the following technical scheme is provided:
in-situ phosphorization synthesis of Ni from foamed nickel by two-step method2The preparation method of P/Ni is as follows:
(1) foam nickel (Ni) pretreatment
The pure nickel net is cleaned before use, and the method comprises the following steps: the mixture is soaked in acetone for 30 minutes and is subjected to ultrasonic treatment for 5 minutes, then is washed clean by deionized water, and is soaked in 2M/L hydrochloric acid for 30 minutes and then is repeatedly washed by deionized water. Finally, washing for many times by adopting absolute ethyl alcohol and storing for later use.
(2) Synthesis of precursor (coating method)
Selecting a piece of clean foam nickel, measuring 250uL phytic acid (analytically pure) by using a titration gun, uniformly coating the surface of the foam nickel in a manual coating mode, and drying the foam nickel in an oven at 60 ℃ for 12 hours. And the dried sample is the PA/Ni precursor loaded with the phytic acid.
(3) One-step annealing phosphating process
Taking out the dried foam nickel loaded with the PA/Ni precursor, placing the foam nickel in a quartz boat, placing the quartz boat in a central temperature area of a vacuum tube furnace, respectively heating to 700 ℃, 800 ℃ and 900 ℃ according to a set program with the heating rate of 5 ℃/min, and preserving heat for 2h to finish the whole phosphating process.
Self-supporting Ni in comparison to other hydrogen evolution catalysts2The synthesis method of the P/Ni electrode has the following advantages:
1. the method develops a new way for a classical method for preparing the transition metal phosphide nano material without using sodium hypophosphite to carry out phosphorization, and organic polymers are used as phosphorus sources to carry out one-step phosphorization, so that toxic gases such as phosphine and the like which are harmful to the environment are not generated in the experimental process, and the method is non-toxic and pollution-free.
2. The whole experiment process is carried out by adopting a coating and annealing method, the prepared transition metal phosphide material has better HER electrocatalytic activity, and the operation method is simple and easy to implement.
The invention adopts a novel method to prepare transition metal phosphide loaded on foamed nickel to research the electro-catalytic hydrogen evolution performance of the nickel. In the research, phytic acid is uniformly coated on the surface of the foamed nickel by a coating method, and then the transition metal phosphide is prepared by one-step high-temperature treatment. And then, the morphology and microstructure of the prepared transition metal phosphide are further represented, the electrocatalytic performance of the transition metal phosphide is tested, and a new thought and a new method are provided for preparing novel transition metal phosphide materials.
Drawings
FIG. 1 shows the phosphorized Ni of example 2 of the present invention2Scanning electron microscope photo of P/Ni catalyst material;
FIG. 2 shows the phosphorous synthesized Ni in example 2 of the present invention2Elemental analysis photographs of the P/Ni catalyst material;
FIG. 3 shows the phosphorous synthesized Ni in example 2 of the present invention2An X-ray diffraction pattern of the P/Ni catalyst material;
FIG. 4 shows the phosphorized Ni of example 2 of the present invention2A polarization curve comparison graph of the P/Ni catalyst material and pure foam nickel;
Detailed Description
The following provides a detailed description of specific embodiments of the present invention.
Example 1
Cutting a pure nickel net purchased in the market into a plurality of strips with the size of 1cm multiplied by 2cm, soaking the strips in acetone for 30 minutes and carrying out ultrasonic treatment for 5 minutes, then washing the strips clean by deionized water, then soaking the strips in 2M/L hydrochloric acid for 30 minutes, respectively washing the strips for 3 times by using the deionized water and ethanol, and then naturally airing the strips for later use. Selecting a piece of clean foam nickel, measuring 250uL phytic acid (analytically pure) by using a titration gun, uniformly coating the surface of the foam nickel in a manual coating mode, and drying the foam nickel in an oven at 60 ℃ for 12 hours. And the dried sample is the PA/Ni precursor loaded with the phytic acid. Taking out the dried foam nickel loaded with the PA/Ni precursor, placing the foam nickel in a quartz boat, placing the quartz boat in a central temperature area of a vacuum tube furnace, and continuously introducing argon at a proper flow rateRespectively heating to 700 ℃ according to a set program with the heating rate of 5 ℃/min, preserving heat for two hours, taking out a sample after the temperature of the tube furnace is reduced, and obtaining 700-Ni2P/Ni electrode material.
Example 2
Cutting a pure nickel net purchased in the market into a plurality of strips with the size of 1cm multiplied by 2cm, soaking the strips in acetone for 30 minutes and carrying out ultrasonic treatment for 5 minutes, then washing the strips clean by deionized water, then soaking the strips in 2M/L hydrochloric acid for 30 minutes, respectively washing the strips for 3 times by using the deionized water and ethanol, and then naturally airing the strips for later use. Selecting a piece of clean foam nickel, measuring 250uL phytic acid (analytically pure) by using a titration gun, uniformly coating the surface of the foam nickel in a manual coating mode, and drying the foam nickel in an oven at 60 ℃ for 12 hours. And the dried sample is the PA/Ni precursor loaded with the phytic acid. Taking out a piece of dried foamed nickel loaded with PA/Ni precursor, placing the foamed nickel in a quartz boat, placing the quartz boat in a central temperature area of a vacuum tube furnace, continuously introducing argon at a proper flow rate, respectively heating to 700 ℃ according to a set program with the heating rate of 5 ℃/min, preserving heat for two hours, taking out a sample after the temperature of the tube furnace is reduced, and obtaining 800-Ni2P/Ni electrode material.
Example 3
Cutting a pure nickel net purchased in the market into a plurality of strips with the size of 1cm multiplied by 2cm, soaking the strips in acetone for 30 minutes and carrying out ultrasonic treatment for 5 minutes, then washing the strips clean by deionized water, then soaking the strips in 2M/L hydrochloric acid for 30 minutes, respectively washing the strips for 3 times by using the deionized water and ethanol, and then naturally airing the strips for later use. Selecting a piece of clean foam nickel, measuring 250uL phytic acid (analytically pure) by using a titration gun, uniformly coating the surface of the foam nickel in a manual coating mode, and drying the foam nickel in an oven at 60 ℃ for 12 hours. And the dried sample is the PA/Ni precursor loaded with the phytic acid. Taking out a piece of dried foamed nickel loaded with PA/Ni precursor, placing the foamed nickel in a quartz boat, placing the quartz boat in a central temperature area of a vacuum tube furnace, continuously introducing argon at a proper flow rate, respectively heating to 700 ℃ according to a set program with the heating rate of 5 ℃/min, preserving heat for two hours, taking out a sample after the temperature of the tube furnace is reduced,thus obtaining 900-Ni2P/Ni electrode material.
Respectively synthesizing 700-Ni2P/Ni，800-Ni2P/Ni，900-Ni2The performance test process of the P/Ni nano-structured catalyst for the Hydrogen Evolution Reaction (HER) by electrolysis water is as follows:
and (3) respectively washing the samples with deionized water and ethanol for three times, and after the natural drying is finished, testing the catalytic performance of hydrogen evolution by electrolyzing water by using an electrochemical workstation.
Linear Sweep Voltammetry (LSV) is a method of recording the electrolytic current on the working electrode by applying a linearly varying voltage on the working electrode, i.e. the electrode potential is linearly varied with the applied voltage, and the LSV of this experiment was mainly measured at CHI760E (shanghai chenhua production) electrochemical workstation, where the sweeping speed of the LSV was 5mv/s and the influence of solution resistance etc. on the test was eliminated by IR compensation. This was tested in a classical three-electrode system with carbon rods as counter electrode and Hg/HgO as reference electrode, using the catalyst materials synthesized in examples 1, 2 and 3 as working electrodes, respectively, and using a 1M KOH solution as electrolyte. During testing, argon is continuously introduced into the electrolytic cell to remove impurity gases in the electrolyte. The results of the hydrogen evolution performance test are shown in table 1 below. As can be seen from the table, the hydrogen evolution catalytic activity of the annealing phosphating treatment at 800 ℃ is the best, and is 10mA/cm2Only 137mV of overpotential is shown at the same current density, which is 99mV lower than the overpotential (238mV) measured by pure nickel foam.
TABLE 1 electrochemical hydrogen evolution Performance
FIG. 4 shows 800-Ni synthesized in example 2 of the present invention2Comparison of polarization curves for electrochemical hydrogen evolution Performance of P/Ni composite nanostructured catalysts with pure Nickel foam (Nickel foam), where the composite catalyst was at 10mA/cm2Only exhibits an overpotential of 137mV at the current density of (a). And can be seen from the above tableThe overpotential (238mV) measured at the same current density was reduced by 99mV compared to that measured for pure nickel foam. Thus 800-Ni synthesized by the present invention2The P/Ni has excellent application potential in the field of hydrogen evolution reaction catalysts.
The above description is only an example of the present invention, and is not limited thereto. Any simple changes, equivalent substitutions or modifications made based on the present invention to solve substantially the same technical problems or achieve substantially the same technical effects are within the scope of the present invention.
Claims (4)
1. Ni2The novel preparation method of the P/Ni composite electrode material and the application thereof in the aspect of hydrogen production catalysis by electrolyzing water are characterized by comprising the following steps:
(1) foam nickel (Ni) pretreatment
The pure nickel net is cleaned before use, and the method comprises the following steps: the mixture is soaked in acetone for 30 minutes and is subjected to ultrasonic treatment for 5 minutes, then is washed clean by deionized water, and is soaked in 2M/L hydrochloric acid for 30 minutes and then is repeatedly washed by deionized water. Finally, washing for many times by adopting absolute ethyl alcohol and storing for later use.
(2) Synthesis of precursor (coating method)
Selecting a piece of clean foam nickel, measuring 250uL phytic acid (analytically pure) by using a titration gun, uniformly coating the surface of the foam nickel in a manual coating mode, and drying the foam nickel in an oven at 60 ℃ for 12 hours. And the dried sample is the PA/Ni precursor loaded with the phytic acid.
(3) One-step annealing phosphating process
Taking out the dried foam nickel loaded with the PA/Ni precursor, placing the foam nickel in a quartz boat, placing the quartz boat in a central temperature area of a vacuum tube furnace, respectively heating to 700 ℃, 800 ℃ and 900 ℃ according to a set program with the heating rate of 5 ℃/min, and preserving heat for 2h to finish the whole phosphating process.
2. Ni according to claim 12The preparation method of the P/Ni composite nano-structure catalyst for hydrogen production by water electrolysis is characterized by comprising the following steps: the substrate of the material in the step (1) is foamed nickel.
3. Ni according to claim 12The preparation method of the P/Ni composite nano-structure catalyst for hydrogen production by water electrolysis is characterized by comprising the following steps: the dosage of the phytic acid in the step (2) is 250 ul.
4. Ni according to claim 12The preparation method of the P/Ni composite nano-structure catalyst for hydrogen production by water electrolysis is characterized by comprising the following steps: the temperature of the phosphorization annealing in the step (3) is 700 ℃, 800 ℃, 900 ℃ and the duration time is 2h respectively. The sample with the best catalytic performance on hydrogen evolution reaction is a phosphatized sample at 800 ℃, namely 800-Ni2P/Ni。
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