CN113186564B - Preparation method and application of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material - Google Patents
Preparation method and application of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material Download PDFInfo
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- CN113186564B CN113186564B CN202110479510.1A CN202110479510A CN113186564B CN 113186564 B CN113186564 B CN 113186564B CN 202110479510 A CN202110479510 A CN 202110479510A CN 113186564 B CN113186564 B CN 113186564B
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method and application of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material, which comprises the following steps: 1) preparing nickel foam self-supporting nickel ruthenium layered double metal hydroxide; 2) preparing a nickel phosphide-ruthenium phosphide/foamed nickel three-dimensional self-supporting electrode material; the application of the nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material in the electrolytic water. The preparation process is convenient and simple, the cost of the electrocatalyst can be greatly reduced, the electrocatalyst has excellent performance in the aspect of alkaline electrocatalytic hydrogen evolution, excellent catalytic performance is also shown in the aspects of alkaline electrocatalytic oxygen evolution and total hydrolysis, the three-dimensional porous foam nickel carrier has excellent conductivity, the loading capacity of active sites can be improved, and the transfer speed of electrons and protons is accelerated; the in-situ growth method can effectively promote the interaction between the nickel phosphide-ruthenium phosphide and the carrier foam nickel, thereby enhancing the electrocatalytic stability of the catalyst.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method and application of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material.
Background
The electrocatalytic water decomposition technology efficiently stores a large amount of electric energy in chemical bonds by electrolyzing water to produce hydrogen and oxygen, thereby solving the problem that the electric energy is difficult to store and simultaneously obtaining hydrogen energy with zero pollution, high heat value and recycling use. Now thatOne of the major challenges facing effective large-scale water electrolysis today is the use of highly efficient electrocatalysts (e.g., Pt/C, RuO) in conventional water electrolysis hydrogen production technologies2、IrO2Etc.) are expensive rare metal catalysts, greatly improving the hydrogen production cost and greatly limiting the large-scale application of the water electrolysis hydrogen production technology. In recent years, scientists at home and abroad are dedicated to design and develop an electrocatalyst which is abundant, cheap, efficient and stable on the earth, improve the efficiency of water electrolysis and reduce the cost of the catalyst.
Disclosure of Invention
The invention aims to provide a preparation method and application of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material.
The invention relates to a preparation method of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material, which comprises the following steps:
1) preparation of foamed nickel self-supporting nickel ruthenium layered double metal hydroxide (NiRu LDH): dissolving nickel nitrate hexahydrate (2-3 mmol), ruthenium trichloride (0.5-0.75 mmol), sodium dodecyl sulfate (0.5-0.75 mmol) and urea (16-25 mmol) in 40-60 mL of water/ethylene glycol mixed solution (volume ratio is 1:3), stirring to obtain solution A, transferring the solution A into a reaction kettle of 50-100 mL, immersing foamed nickel (with the length of 2-5 cm and the thickness of 100-200 nm) into the solution A, keeping the temperature at 100-150 ℃ for 12h, washing the foamed nickel for 5 times by using methanol and ultrapure water respectively, and performing vacuum drying at 50-80 ℃ to obtain a sample I, namely the nickel ruthenium layered double metal hydroxide (NiRu) self-supported by the foamed nickel;
2) preparation of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material (Ni)2P-Ru2P/NF): and respectively placing the sodium hypophosphite and the sample I in the upper source and the middle of the tubular furnace, raising the temperature to 280-400 ℃ at the speed of 2-10 ℃/min under the atmosphere of protective gas, preserving the temperature for 2-5 hours, and cooling to obtain a sample II, namely the nickel phosphide-ruthenium phosphide/foamed nickel.
The protective gas in the step 2) is one of high-purity argon, nitrogen and helium.
And in the step 2), the distance between the sodium hypophosphite and the sample I is 4-10 cm.
The nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material disclosed by the invention is applied to electrolytic water.
Compared with the prior art, the invention has the following beneficial effects.
The preparation process is convenient and simple, the cost of the electrocatalyst can be greatly reduced, and the nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material provided by the invention has excellent performance in alkaline electrocatalytic hydrogen evolution and also has excellent catalytic performance in alkaline electrocatalytic oxygen evolution and total hydrolysis. The reason for this is summarized as follows: the three-dimensional porous foam nickel carrier has excellent conductivity, can improve the loading capacity of active sites, and accelerates the transfer speed of electrons and protons. The in-situ growth method can avoid the use of an adhesive, effectively promote the interaction between the nickel phosphide-ruthenium phosphide and the carrier foam nickel, prevent the separation of active species and further enhance the electrocatalytic stability of the catalyst. In addition, the nickel phosphide-ruthenium phosphide heterojunction can regulate and control the electronic structure of the nano particles and promote the performance of water electrolysis.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
FIG. 2 is an X-ray powder diffraction pattern of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention.
FIGS. 3(a) to (c) are Scanning Electron Microscope (SEM) photographs of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention
FIGS. 4(a) to (c) are Transmission Electron Microscope (TEM) and high-resolution transmission electron microscope (HRTEM) photographs of the nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention.
FIG. 5 is a graph showing the oxygen evolution performance of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention under alkaline conditions.
FIG. 6 is a graph showing the hydrogen evolution performance of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention under alkaline conditions.
FIG. 7 is a graph showing the full water splitting performance of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention under alkaline conditions.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The invention relates to a preparation method of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material, which comprises the following steps:
1) preparation of foamed nickel self-supporting nickel ruthenium layered double metal hydroxide (NiRu LDH): dissolving 2mmol of nickel nitrate hexahydrate, 0.5mmol of ruthenium trichloride, 0.5mmol of sodium dodecyl sulfate and 16.7mmol of urea in 40mL of water/ethylene glycol mixed solution (volume ratio is 1:3), stirring to obtain a solution A, and transferring the solution A to a 50mL reaction kettle; immersing foamed nickel (2 cm in length and 150nm in thickness); keeping the temperature at 100 ℃ for 12h, respectively washing the foamed nickel with methanol and ultrapure water for 5 times, and performing vacuum drying at 50 ℃ to obtain a sample I, namely the nickel ruthenium layered double metal hydroxide (NiRu LDH) self-supported by the foamed nickel;
2) preparation of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material (Ni)2P-Ru2P/NF): and respectively placing the sodium hypophosphite and the sample I in the upper source and the middle of the tubular furnace, introducing argon, heating to 280 ℃ at the speed of 2 ℃/min, preserving the heat for 2 hours, and cooling to obtain a sample II, namely the nickel phosphide-ruthenium phosphide/foamed nickel.
FIG. 2 is an X-ray powder diffraction pattern of the resulting sample. From this figure it can be seen that the resulting material comprises nickel phosphide and ruthenium phosphide.
FIG. 3(a) - (c) shows Scanning Electron Microscope (SEM) photographs of the nickel phosphide-ruthenium phosphide/nickel foam obtained in FIGS. As can be seen from the figure, the nanoparticles are deposited on the nickel foam.
FIGS. 4(a) to (c) are Transmission Electron Microscope (TEM) and high-resolution transmission electron microscope (HRTEM) photographs of the obtained nickel phosphide-ruthenium phosphide/nickel foam. From this figure, it can be seen that there are significant interfaces and corresponding lattice striations between the nickel and ruthenium phosphide nanoparticles.
Example 2
The invention relates to a preparation method of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material, which comprises the following steps:
1) preparation of foamed nickel self-supporting nickel ruthenium layered double metal hydroxide (NiRu LDH): dissolving 3mmol of nickel nitrate hexahydrate, 0.75mmol of ruthenium trichloride, 0.75mmol of sodium dodecyl sulfate and 25mmol of urea in 60mL of water/ethylene glycol mixed solution (volume ratio is 1:3), stirring to obtain a solution A, and transferring the solution A to a 100mL reaction kettle; immersing foamed nickel (5 cm in length and 150nm in thickness); keeping the temperature at 150 ℃ for 12h, respectively washing the foamed nickel with methanol and ultrapure water for 5 times, and performing vacuum drying at 80 ℃ to obtain a sample I, namely the nickel ruthenium layered double metal hydroxide (NiRu LDH) self-supported by the foamed nickel;
2) preparation of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material (Ni)2P-Ru2P/NF): and respectively placing the sodium hypophosphite and the sample I in the upper source and the middle of the tubular furnace, introducing nitrogen, heating to 400 ℃ at the speed of 10 ℃/min, preserving the heat for 5 hours, and cooling to obtain a sample II, namely the nickel phosphide-ruthenium phosphide/foamed nickel.
Example 3
The invention relates to a preparation method of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material, which comprises the following steps:
1) preparation of foamed nickel self-supporting nickel ruthenium layered double metal hydroxide (NiRu LDH): dissolving 2.5mmol of nickel nitrate hexahydrate, 0.6mmol of ruthenium trichloride, 0.6mmol of sodium dodecyl sulfate and 20mmol of urea in 50mL of water/ethylene glycol mixed solution (volume ratio is 1:3), stirring to obtain a solution A, and transferring the solution A to a 100mL reaction kettle; immersing foamed nickel (3 cm in length and 150nm in thickness); keeping the temperature at 120 ℃ for 12h, respectively washing the foamed nickel with methanol and ultrapure water for 5 times, and performing vacuum drying at 65 ℃ to obtain a sample I, namely the nickel-ruthenium layered double metal hydroxide (NiRu LDH) self-supported by the foamed nickel;
2) preparation of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material (Ni)2P-Ru2P/NF): respectively placing sodium hypophosphite and the sample I in the upper source and the middle of a tubular furnace, introducing helium gas, heating to 320 ℃ at the speed of 6 ℃/min, preserving heat for 3 hours, and cooling to obtain a sample II, namely the nickel phosphide-ruthenium phosphide/foamed nickel.
Example 4
The invention relates to an application of nickel phosphide-ruthenium phosphide/nickel foam in the oxygen production by electrolyzing water, which comprises the following steps:
using the nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1, a three-electrode system was usedThe working electrode is the obtained sample, the counter electrode is a graphite rod electrode, the reference electrode is a mercury/mercury oxide electrode, the electrolyte is 1.0M KOH solution, and the sweep rate of the polarization curve is 1mV s-1。
FIG. 5 is a graph of the oxygen evolution performance of the resulting nickel phosphide-ruthenium phosphide/nickel foam under alkaline conditions. As can be seen from the figure, the obtained electrode material only needs 160mV overpotential to enable the current density to reach 10mA cm-2And is superior to commercial ruthenium dioxide catalyst (320 mV).
Example 5
The invention discloses an application of nickel phosphide-ruthenium phosphide/nickel foam in hydrogen production by electrolyzing water, which comprises the following steps:
using the nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1, a three-electrode system was employed, the working electrode was the sample obtained, the counter electrode was a graphite rod electrode, the reference electrode was a mercury/mercury oxide electrode, the electrolyte was a 1.0M KOH solution, and the sweep rate of the polarization curve was 1mV s-1。
FIG. 6 is a graph showing the hydrogen evolution performance of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention under alkaline conditions. As can be seen from the figure, the obtained electrode material needs 99.8mV of overpotential to enable the current density to reach 10mA cm-2Slightly above commercial platinum carbon catalyst (39.8 mV).
Example 6
The application of the nickel phosphide-ruthenium phosphide/nickel foam in the full-hydrolysis water comprises the following steps:
using the nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1, a two-electrode system was employed, in which all the working electrodes were the samples obtained, the electrolyte was 1.0M KOH solution, and the sweep rate of the polarization curve was 1mV s-1。
FIG. 7 is a graph showing the full water splitting performance of nickel phosphide-ruthenium phosphide/nickel foam obtained in example 1 of the present invention under alkaline conditions. As can be seen from the figure, the obtained electrode material needs 1.45V of potential to ensure that the current density reaches 10mA cm-2。
Claims (2)
1. A preparation method of a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material is characterized by comprising the following steps:
1) preparation of foamed nickel self-supporting nickel ruthenium layered double metal hydroxide nirudhl: dissolving 2-3 mmol of nickel nitrate hexahydrate, 0.5-0.75 mmol of ruthenium trichloride, 0.5-0.75 mmol of sodium dodecyl sulfate and 16-25 mmol of urea in 40-60 mL of mixed solution with the volume ratio of water to ethylene glycol being 1:3, stirring to obtain solution A, transferring the solution A to a reaction kettle with 50-100 mL, soaking foamed nickel with the length of 2-5 cm and the thickness of 100-200 nm into the solution A, keeping the temperature at 100-150 ℃ for 12 hours, respectively washing the foamed nickel for 5 times by using methanol and ultrapure water, and drying at 50-80 ℃ in vacuum to obtain a sample I, namely the nickel ruthenium layered double metal hydroxide NiRuLDH self-supported by foamed nickel;
2) preparing a nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material Ni2P-Ru 2P/NF: respectively placing sodium hypophosphite and a sample I in the upper source and the middle of a tubular furnace, heating to 280-400 ℃ at the speed of 2-10 ℃/min under the atmosphere of protective gas, preserving heat for 2-5 hours, and cooling to obtain a sample II, namely nickel phosphide-ruthenium phosphide/foamed nickel;
in the step 2), the protective gas is one of high-purity argon, nitrogen and helium, and the distance between the sodium hypophosphite and the sample I is 4-10 cm.
2. Use of the nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material as defined in claim 1 in electrolytic water.
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| CN202110479510.1A CN113186564B (en) | 2021-04-30 | 2021-04-30 | Preparation method and application of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material |
| PCT/CN2021/135742 WO2022227576A1 (en) | 2021-04-30 | 2021-12-06 | Preparation method and application of nickel phosphide-ruthenium phosphide/foamed nickel three-dimensional self-supporting electrode material |
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| CN202110479510.1A CN113186564B (en) | 2021-04-30 | 2021-04-30 | Preparation method and application of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material |
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| CN113186564B (en) * | 2021-04-30 | 2022-05-03 | 济宁学院 | Preparation method and application of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material |
| WO2022250120A1 (en) * | 2021-05-26 | 2022-12-01 | 国立大学法人東京工業大学 | Catalyst, and method for producing catalyst |
| CN114941157B (en) * | 2022-05-30 | 2023-11-28 | 安徽工业大学 | Electrocatalyst material and preparation method thereof |
| CN117604569A (en) * | 2024-01-17 | 2024-02-27 | 海南深远海新能源科技有限公司 | Preparation method and application of heterostructure catalyst for hydrogen production by water electrolysis |
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| US20160289849A1 (en) * | 2015-03-31 | 2016-10-06 | Yujie Sun | Bifunctional water splitting catalysts and associated methods |
| CN110257859B (en) * | 2019-06-28 | 2021-02-02 | 青岛科技大学 | Co2P/Ni2P/Al2O3/NF multi-stage structure composite electrode and preparation method thereof |
| CN110512228B (en) * | 2019-09-16 | 2021-06-22 | 燕山大学 | Preparation method of nickel phosphide/nickel foam electrochemical functional hydrogen evolution material |
| CN113201764A (en) * | 2021-04-30 | 2021-08-03 | 济宁学院 | Preparation method and application of nickel phosphide-iron phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material |
| CN113186564B (en) * | 2021-04-30 | 2022-05-03 | 济宁学院 | Preparation method and application of nickel phosphide-ruthenium phosphide/nickel foam three-dimensional self-supporting electrode material |
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| CN107088432A (en) * | 2017-04-12 | 2017-08-25 | 南京师范大学 | A kind of two-dimentional Ru doping Ni2P plate-like nano flakes and its preparation method and application |
| CN109364963A (en) * | 2018-11-22 | 2019-02-22 | 重庆工商大学 | A kind of ruthenium-phosphorus is modified nickel composite catalyst and preparation method thereof altogether |
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