CN116970974A - Preparation method of Ru/F-FeCoOOH heterojunction electrocatalyst based on hydrogen overflow strategy - Google Patents
Preparation method of Ru/F-FeCoOOH heterojunction electrocatalyst based on hydrogen overflow strategy Download PDFInfo
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 19
- 239000001257 hydrogen Substances 0.000 title claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000013535 sea water Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 44
- 239000006260 foam Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910052742 iron Inorganic materials 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910017855 NH 4 F Inorganic materials 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 238000005868 electrolysis reaction Methods 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000011521 glass Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000001308 synthesis method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229910002588 FeOOH Inorganic materials 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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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
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
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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
-
- 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
- C25B11/061—Metal or alloy
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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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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to the field of interface engineering materials, and particularly relates to a preparation method of an F-doped Ru/FeCoOOH heterojunction HER electrocatalyst catalyst and application of the catalyst in high-current electrolysis of seawater. Ru/F-FeCoOOH grows on the self-supporting material through molten salt, and the final F-doped Ru/FeCoOOH electrocatalyst (Ru/F-FeCoOOH) is obtained through a ruthenium trichloride soaking method. Under the condition of industrial seawater electrolysis (electrolyte: 6M KOH seawater, temperature: 60 ℃) only 1.73V of working voltage is needed to reach 2A/cm 2 And is capable of stable circulation for 100h under industrial seawater conditions. Compared with the traditional method for preparing the dual-function electrocatalyst, the invention solves the problem of electrolysis by utilizing a hydrogen overflow strategyThe problems of slow dynamics and the like in the alkaline seawater process are solved, high-efficiency catalysis is ensured, meanwhile, the catalysis stability can be maintained under the condition of high current density, and the method has important value in the future practical application.
Description
Technical Field
The invention belongs to the field of interface engineering materials, and particularly relates to a preparation method of an F-doped Ru/FeCoOOH heterojunction HER electrocatalyst catalyst and application of the catalyst in high-current electrolysis of seawater.
Background
Hydrogen has higher volatility and energy density, and is an ideal green energy source for replacing fossil fuel. The hydrogen evolution reaction is a cathode reaction in the water electrolysis process and has an important influence on the hydrogen production rate in the water electrolysis process. For alkaline water electrolysis, the dissociation of water in alkaline medium is slow, resulting in an insufficient proton supply, which is detrimental to HER kinetics and thus challenging. Under alkaline conditions, electrolysis of seawater at high current densities typically produces hydroxide deposition at the cathode, resulting in slower reaction kinetics than pure water electrolysis. Therefore, there is an urgent need to design a highly efficient catalyst (ΔG) that can accelerate the rate of hydrolysis and optimize the free energy of hydrogen adsorption H )。
Ruthenium (Ru) and its compounds have attracted attention for basic HER because of their water binding capacity similar to Pt, and more importantly their excellent activity. However, poor desorption of the intermediate product and insufficient proton supply in the alkaline solution slows down HER kinetics of the ruthenium-based material. To solve this problem, design E with metals and carriers f The matched carrier can induce the overflow of hydrogen, thereby accelerating the desorption process of hydrogen and improving the activity of HER. Due to E f The quantitative relation exists between the material work function (phi), and the reduction of the phi heterostructure gap can reduce the accumulation of interface charges, so that the H trapping of the interface is weakened, and the interface hydrogen overflow is facilitated.
Disclosure of Invention
1. The invention aims to provide a synthesis method of an F-doped Ru/FeCoOOH heterojunction material. Ru/F-FeCoOOH grows on the self-supporting material through molten salt, and the final F-doped Ru/FeCoOOH electrocatalyst (Ru/F-FeCoOOH) is obtained through a ruthenium trichloride soaking method. Compared with the traditional method for preparing the bifunctional electrocatalyst, the method solves the problems of slow dynamics and the like in the process of electrolyzing alkaline seawater by utilizing a hydrogen overflow strategy, ensures high-efficiency catalysis, can maintain the catalysis stability under the condition of high current density, and has important value in the future practical application.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an F-doped Ru/FeCoOOH heterojunction electrocatalyst, which can be realized by the following technical route:
(1) Pretreatment of self-supporting materials: cutting the self-supporting material (foam iron) into proper size, respectively immersing in hydrochloric acid, acetone and deionized water for ultrasonic treatment, and drying in a vacuum oven.
(2) Preparing an F-FeCoOOH precursor: NH is added to 4 F and Co (NO) 3 ) 2 ·6H 2 Heating O to 125-250 deg.C in a baking oven, putting into foam iron for reaction for 1-60 min, and naturally cooling. And repeatedly washing the reacted foam iron with deionized water and ethanol, and drying in a vacuum oven.
(3) Ru/F-FeCoOOH preparation: immersing the reacted foam iron into ruthenium trichloride solution, and reacting at the temperature of 0-120 ℃; taking out the prepared sample and cleaning the sample by deionized water to obtain Ru/F-FeCoOOH.
The preparation method according to the technical route is characterized in that: in the step (1), the foam iron is cut into the size of 1cm or 2cm, and is immersed into hydrochloric acid, acetone and deionized water respectively for ultrasonic treatment for 10-40 min and then dried, so that organic matters and oxides on the surface of the foam nickel are removed.
The preparation method according to the technical route is characterized in that: and (3) placing molten salt into the step (2) for reaction for 5min to synthesize a flaky F-FeCoOOH precursor with uniform morphology and size.
The preparation method according to the technical route is characterized in that: the temperature in the step (3) is 0.5-2.0 g.
The preparation method according to the technical route is characterized in that: and (3) in the step (4), the reaction time in the oven is 0-10 h.
The invention also provides application of the F-doped Ru/FeCoOOH heterojunction material in industrial seawater electrolysis hydrogen production.
As a further feature of the present invention: the F-doped Ru/FeCoOOH heterojunction material prepared by the preparation method is used as an HER electrocatalyst for industrial electrolysis of seawater, and has excellent electrochemical performance. Under the condition of industrial seawater electrolysis (electrolyte: 6MKOH seawater, temperature: 60 ℃) the working voltage of only 1.73V can reach 2A/cm 2 And is capable of stable circulation for 100h under industrial seawater conditions.
The invention provides a preparation method of an F-doped Ru/FeCoOOH heterojunction HER electrolytic seawater electrocatalyst. F-FeCoOOH grows on the self-supporting material through a molten salt method, and a hydrogen overflow strategy of the metal-carrier is constructed by further utilizing a ruthenium trichloride soaking method, so that the F-doped Ru/FeCoOOH heterojunction material is finally prepared. Compared with the traditional method for preparing the bifunctional electrocatalyst, the method provided by the invention can maintain the catalytic stability under the condition of high current density while ensuring high-efficiency catalysis, and has important value in future practical application.
Detailed Description
The technical features of the present invention will be described with reference to the following specific experimental schemes and drawings, but the present invention is not limited thereto. The test methods described in the examples below, unless otherwise specified, are all conventional; the apparatus and materials are commercially available unless otherwise specified.
Example 1
A synthesis method of F-doped Ru/FeCoOOH heterojunction for preparing hydrogen by electrolyzing seawater comprises the following steps:
(1) In the embodiment, 1cm x 2cm of foam iron is cut, the foam iron is placed in hydrochloric acid, acetone and deionized water for respectively carrying out ultrasonic treatment for 30min, and vacuum drying is carried out for later use.
(2) Weigh 7gNi (NO) 3 ) 2 ·6H 2 O and 0.55. 0.55gNH 4 F was placed in a 25mL glass bottle. The glass vials were then placed in an oven at 150 ℃ for 60 minutes until the salt melted. Immersing the pretreated foam nickel in the molten salt for reaction for 5min, naturally cooling, washing with deionized water and ethanol for multiple times, and drying to obtain F-FeCoOOH product, which is X-rayThe diffraction (XRD) results are shown in the figure (fig. 1), demonstrating the presence of FeOOH phases, F in doped form, in the material.
(3) Immersing the reacted foam iron into 0.05g ruthenium trichloride solution, and reacting at the temperature of 60 ℃; taking out the prepared sample and cleaning with deionized water, and proving that FeOOH and Ru phases exist in the material and heterojunction exists. For the synthesized material, the scanning electron microscope is shown (fig. 2), and the material continues to maintain the sheet morphology of the precursor. The X-ray diffraction (XRD) results for the Ru/F-FeCoOOH material are shown (FIG. 3), which continues to maintain the phase of the Ru/F-FeCoOOH product. In the process of testing the dual-function electrocatalyst, the conditions of industrial electrolysis of seawater (electrolyte: 6MKOH seawater, temperature: 60 ℃) were adopted in this example, and the prepared materials were simultaneously used as the cathode and anode of the two-electrode system electrolytic cell. The prepared difunctional electrocatalyst can reach 2A/cm with the working voltage of only 1.73V 2 And is capable of stabilizing the cycle for 100h (fig. 5) under industrial seawater conditions (fig. 4).
Example 2
A synthesis method of F-doped Ru/FeCoOOH heterojunction for preparing hydrogen by electrolyzing seawater comprises the following steps:
(1) In the embodiment, 1cm x 2cm of foam iron is cut, the foam iron is placed in hydrochloric acid, acetone and deionized water for respectively carrying out ultrasonic treatment for 30min, and vacuum drying is carried out for later use.
(2) The pretreated foam iron was treated with 7gNi (NO 3 ) 2 ·6H 2 O，0.55gNH 4 F was placed in a 25mL glass bottle. The glass vials were then placed in an oven at 150 ℃ for 60 minutes until the salt melted. Immersing the pretreated foam iron into the molten salt for reaction for 10min, naturally cooling, washing with deionized water and ethanol for multiple times, and drying to obtain the F-FeCoOOH product.
(3) Immersing the reacted foam iron into 0.05g ruthenium trichloride solution, and reacting at the temperature of 60 ℃; and taking out the prepared sample, and cleaning the sample by deionized water to obtain the Ru/F-FeCoOOH product. During the dual-function electrocatalyst test, the material prepared in this example served as both a cathode and anode dual-function cell (fig. 6) and was able to be cycled stably for 100h under industrial seawater conditions.
Example 3
A synthesis method of F-doped Ru/FeCoOOH heterojunction for preparing hydrogen by electrolyzing seawater comprises the following steps:
(1) In the embodiment, 1cm x 2cm of foam iron is cut, the foam iron is placed in hydrochloric acid, acetone and deionized water for respectively carrying out ultrasonic treatment for 30min, and vacuum drying is carried out for later use.
(2) The pretreated foam iron was treated with 7gNi (NO 3 ) 2 ·6H 2 O，0.55gNH 4 F was placed in a 25mL glass bottle. The glass vials were then placed in an oven at 150 ℃ for 60 minutes until the salt melted. Immersing the pretreated foam iron into the molten salt for reaction for 15min, naturally cooling, washing with deionized water and ethanol for multiple times, and drying to obtain the F-FeCoOOH product.
(3) Immersing the reacted foam iron into 0.05g ruthenium trichloride solution, and reacting at the temperature of 60 ℃; and taking out the prepared sample, and cleaning the sample by deionized water to obtain the Ru/F-FeCoOOH product. In the course of the dual-function electrocatalyst test, the material prepared in this example served as both a cathode and anode dual-function cell and was able to be cycled stably for 100h under industrial seawater conditions.
Description of the drawings:
fig. 1: x-ray diffraction pattern of F-FeCoOOH obtained in example 1;
fig. 2: a scanning electron microscope image of F-FeCoOOH obtained in example 1;
fig. 3: x-ray diffraction pattern of Ru/F-FeCoOOH obtained in example 1;
fig. 4: the two-electrode linear sweep voltammogram of the dual-function alkaline marine water electrolyzer assembled in example 1 of the present invention. Wherein the X-axis is the working potential (V) and the Y-axis is the current density (A/cm) 2 )。
Fig. 5: the two-electrode timing current curve of the assembled dual-function alkaline seawater electrolytic cell of the embodiment 1 of the invention. Wherein the X-axis is time (h) and the Y-axis is current density (V).
Fig. 6: example 2 of the invention assembled two-way alkaline seawater electrolyzerThe electrode scans the voltammogram linearly. Wherein the X-axis is the working potential (V) and the Y-axis is the current density (A/cm) 2 )。
Claims (6)
1. A preparation method of a Ru/F-FeCoOOH heterojunction electrocatalyst based on a hydrogen overflow strategy is characterized by comprising the following steps of: the self-supporting material is subjected to simple cleaning treatment, F-FeCoOOH grows on the self-supporting material by a molten salt method, and finally the self-supporting material is subjected to further modification treatment by a ruthenium trichloride soaking method. The obtained modified F-FeCoOOH electrocatalyst can realize high-efficiency preparation of hydrogen under the condition of industrial seawater, and can maintain long-time stability.
2. The method for cleaning and treating self-supporting material according to claim 1, wherein the self-supporting material (foam iron) is cut into a proper size, and the foam iron is immersed in hydrochloric acid, acetone and deionized water, respectively, and subjected to ultrasonic treatment.
3. The molten salt process according to claim 1, wherein NH 4 F and Ni (NO) 3 ) 2 ·6H 2 Heating O to 125-250 deg.C in an oven, placing into foam nickel for reaction for 1-60 min, and naturally cooling. And repeatedly washing the reacted foam iron with deionized water and ethanol, and drying in a vacuum oven to obtain F-FeCoOOH.
4. The soaking method according to claim 1, wherein the reacted foam iron is immersed in ruthenium trichloride solution and reacted at a temperature of 0 to 120 ℃; taking out the prepared sample and cleaning the sample by deionized water to obtain Ru/F-FeCoOOH.
5. The Ru/F-FeCoOOH heterojunction electrocatalyst based on a hydrogen flooding strategy as claimed in claim 1, wherein: the electrocatalyst may be used as a cathode in an alkaline industrial marine water electrolyzer.
6. The process according to claim 1, wherein the electrolyte is prepared from natural seawater and the temperature of the electrolyte is maintained at 60 ℃ when the seawater is electrolyzed.
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| CN117443410A (en) * | 2023-12-22 | 2024-01-26 | 四川大学 | ROS scavenging biocatalysis material and preparation and application thereof |
| CN117443410B (en) * | 2023-12-22 | 2024-03-12 | 四川大学 | ROS scavenging biocatalysis material and preparation and application thereof |
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