CN114481209A - Preparation method of Ru-modified iron-based self-supporting hydrogen evolution electrode - Google Patents
Preparation method of Ru-modified iron-based self-supporting hydrogen evolution electrode Download PDFInfo
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- CN114481209A CN114481209A CN202210132058.6A CN202210132058A CN114481209A CN 114481209 A CN114481209 A CN 114481209A CN 202210132058 A CN202210132058 A CN 202210132058A CN 114481209 A CN114481209 A CN 114481209A
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Abstract
The invention discloses a preparation method of a Ru-modified iron-based self-supporting hydrogen evolution electrode, which comprises the following specific processes: cutting the foam iron, ultrasonically cleaning the foam iron in absolute ethyl alcohol, and ultrasonically cleaning the foam iron by using dilute hydrochloric acid to obtain a material A; mixing the ruthenium trichloride solution with pure water and absolute ethyl alcohol, and fully stirring to obtain a material B; adding the material A into the material B, stirring at normal temperature, and introducingObtaining a material C through a spontaneous metal corrosion process; and (3) cleaning the material C by using pure water and absolute ethyl alcohol, and then drying the material C in a forced air drying oven at 80 ℃ to obtain the target product Ru-modified iron-based self-supporting hydrogen evolution electrode. The invention adopts a metal corrosion strategy to regulate and control the corrosion process, and the preparation process is green, clean, simple and efficient, and RuO2The synergistic effect of the two phases of FeOOH ensures that the self-supporting electrode has excellent hydrogen evolution reaction activity, and further has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation of self-supporting hydrogen evolution electrodes, and particularly relates to a preparation method of a Ru modified iron-based self-supporting hydrogen evolution electrode.
Background
Natural resources composed of carbon elements such as petroleum and coal are excessively exploited and used, which causes serious energy crisis and environmental deterioration, and therefore, development and application of green clean energy are important for energy transformation and carbon emission reduction. Hydrogen energy is considered as one of the most important energy sources in the 21 st century because of its outstanding advantages of abundant resources, high energy density, zero pollution and the like. Among several industrial hydrogen production methods such as hydrogen production by fossil fuel, hydrogen production by industrial by-products, hydrogen production by water electrolysis and the like, hydrogen production by water electrolysis is an important means for realizing cheap hydrogen production and green hydrogen production. The electric energy generated by clean solar energy and wind energy is utilized to drive the water electrolysis device, so that the electrocatalytic hydrogen evolution reaction can be carried out, and the wide application prospect of sustainable development is shown. However, the hydrogen evolution reaction, which is one of the basic half reactions for water electrolysis, has a high activation energy barrier and requires a large overpotential, resulting in excessive power consumption and a reduction in the conversion efficiency of the electrolyzer. The commercial Pt/C catalyst used at present has the problem of high cost, which limits the large-scale application of the catalyst. Therefore, the design of an electrocatalytic hydrogen evolution electrode which is low in synthesis cost, clean and efficient in synthesis process and simple in process is urgently needed.
In recent years, transition metal hydroxides have attracted interest from many scholars due to advantages such as abundant resources and unique electronic structures, but their catalytic activity is still to be further improved. The noble metal-based catalyst has excellent catalytic activity, the activity and stability of the catalyst can be obviously improved by compounding the transition metal and the noble metal, and the consumption of the noble metal is greatly reduced, so that the production cost of the catalyst is reduced. The conventional powder catalyst needs to use a binder to prepare a hydrogen evolution electrode, resulting in problems of reduced electrode conductivity, difficult exposure of active sites, limited catalyst loading capacity, and the like. The self-supporting electrode avoids the steps of adding an adhesive and coating the catalyst by growing the electrocatalyst in situ on the metal substrate with good conductivity, and can anchor the catalyst and accelerate charge transfer. However, the synthesis process of the self-supporting hydrogen evolution electrocatalyst is complicated, and the energy consumption, the waste and the waste liquid yield in the preparation process are high, so that the large-scale application of the self-supporting hydrogen evolution electrocatalyst is greatly limited. The metal corrosion strategy has the outstanding advantages of simple preparation process, low energy consumption, low waste liquid yield and the like, and is expected to realize industrial production. According to the invention, the foam iron is used as a substrate, and the iron corrosion process which is spontaneously carried out at normal temperature is regulated and controlled by changing the composition of the solution, so that the Ru modified iron-based self-supporting hydrogen evolution electrode with good electrocatalytic activity is prepared, however, no relevant literature report on the content of the aspect exists at present.
Disclosure of Invention
The invention solves the technical problem of providing a clean and efficient preparation method of a Ru-modified iron-based self-supporting hydrogen evolution electrode with a simple process, which takes foam iron as a substrate and grows RuO with a nano-sheet structure in situ through a metal corrosion process of the foam iron in a mixed solution of ruthenium trichloride, pure water and ethanol at normal temperature2The prepared self-supporting hydrogen evolution catalyst can provide rich active sites for hydrogen evolution reaction, and effectively reduces overpotential of the hydrogen evolution reaction; in addition, the spontaneous corrosion process of the foam iron can be effectively regulated and controlled by adding the non-conductive solvent ethanol, the uniform synthesis of an active corrosion layer and the controllable construction of the shape of the nanosheet are facilitated, and the Ru-modified iron-based self-supporting hydrogen evolution electrode with rich active sites is finally prepared.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the Ru modified iron-based self-supporting hydrogen evolution electrode is characterized by comprising the following specific processes:
step S1: cutting the foamed iron, ultrasonically cleaning the foamed iron in absolute ethyl alcohol for 3-5 min, and ultrasonically cleaning the foamed iron for 15-20 min by using dilute hydrochloric acid to obtain a material A;
step S2: mixing the ruthenium trichloride solution with pure water and absolute ethyl alcohol, and fully stirring to obtain a material B;
step S3: putting the material A into the material B, stirring for 120-180 min at normal temperature, and obtaining a material C through a spontaneous metal corrosion process, wherein the material A is a self-supporting substrate, and the addition of a non-conductive solvent ethanol in the material B is used for regulating and controlling the metal corrosion process and promoting the uniform synthesis of an active corrosion layer;
step S4: and (3) cleaning the material C by using pure water and absolute ethyl alcohol, and then drying the material C in a forced air drying oven at 80 ℃ to obtain the target product Ru-modified iron-based self-supporting hydrogen evolution electrode.
Further preferably, in the step S2, the molar concentration of ruthenium trichloride in the material B is 1-5 mM, and the volume ratio of pure water to absolute ethyl alcohol in the material B is 1: 0-5.
Further preferably, the volume ratio of the pure water to the absolute ethyl alcohol in the material B in the step S2 is 1: 0.1-2.
Further preferably, the volume ratio of the pure water to the absolute ethyl alcohol in the material B in the step S2 is 2: 1.
The preparation method of the Ru modified iron-based self-supporting hydrogen evolution electrode is characterized by comprising the following steps of:
step S1: cutting foam iron, ultrasonically cleaning in absolute ethyl alcohol for 3min, and ultrasonically cleaning with dilute hydrochloric acid for 18min to obtain a material A;
step S2: mixing ruthenium trichloride with pure water and absolute ethyl alcohol, wherein the volume ratio of the pure water to the absolute ethyl alcohol is 2:1, the molar concentration of the ruthenium trichloride is 2mM, and fully stirring to obtain a material B;
step S3: putting the material A into the material B, stirring for 160min at normal temperature, and obtaining a material C through a spontaneous metal corrosion process, wherein the material A is a self-supporting substrate, and the addition of a non-conductive solvent ethanol in the material B is used for regulating and controlling the metal corrosion process and promoting the uniform synthesis of an active corrosion layer;
step S4: washing the material C with pure water and absolute ethanol, and blowing at 80 deg.CDrying in a drying oven for 3h to obtain a target product Ru-modified iron-based self-supporting hydrogen evolution electrode with a nanosheet structure, wherein the Ru-modified iron-based self-supporting hydrogen evolution electrode is 1mol L-1Performing electrochemical test in KOH electrolyte, and preparing the Ru modified iron-based self-supporting hydrogen evolution electrode at 100mA cm-2The overpotential for the hydrogen evolution reaction under the current density of (2) is 110-130 mV.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention adopts foamed iron as a substrate, and RuO with a nanosheet structure grows in situ through a metal corrosion process which is spontaneously carried out under normal-temperature stirring2the/FeOOH composite hydrogen evolution electrocatalyst provides more active sites for the electrocatalytic reaction process;
2. according to the invention, the absolute ethyl alcohol is added into the mixed solution, and the non-conductivity of the absolute ethyl alcohol is utilized, so that the reaction speed of the foamed iron in the mixed solution of ruthenium trichloride and pure water can be obviously reduced, and the uniform synthesis of an active corrosion layer and the growth of the nano-sheet morphology are facilitated;
3. the Ru modified iron-based self-supporting hydrogen evolution electrode prepared by the method is 1mol L-1Electrochemical testing was performed in KOH electrolyte at 100mA cm-2Under the current density, the overpotential of the hydrogen evolution reaction of the Ru modified iron-based self-supporting hydrogen evolution electrode is 110-130 mV.
Drawings
FIG. 1 is a scanning electron micrograph of product D1 prepared according to example 1;
FIG. 2 is an X-ray diffraction pattern of products D1-D3 prepared in examples 1-3;
FIG. 3 is a corrosion polarization curve for products D1-D3 prepared in examples 1-3;
FIG. 4 is an electrochemical impedance plot of products D1-D3 prepared in examples 1-3;
FIG. 5 is a linear sweep voltammogram of the products D1-D3 prepared in examples 1-3.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
Step S1: cutting foam iron, ultrasonically cleaning the foam iron in absolute ethyl alcohol for 3min, and ultrasonically cleaning the foam iron for 18min by using dilute hydrochloric acid to obtain a material A1;
step S2: mixing a ruthenium trichloride solution with pure water and absolute ethyl alcohol, wherein the molar concentration of ruthenium trichloride is 2mM, and the volume ratio of pure water to absolute ethyl alcohol is 2:1, and fully stirring to obtain a material B1;
step S3: putting the material A1 into the material B1, stirring for 160min at normal temperature, and obtaining a material C1 through a spontaneous metal corrosion process, wherein the material A1 is a self-supporting substrate, and the addition of a non-conductive solvent ethanol in the material B1 is used for regulating and controlling the metal corrosion process and promoting the uniform synthesis of an active corrosion layer;
step S4: the material C1 was washed with pure water and absolute ethanol, and the material C1 was dried in a forced air drying oven at 80 ℃ for 3 hours to give the product D1.
Example 2
Step S1: cutting foam iron, ultrasonically cleaning in absolute ethyl alcohol for 3min, and ultrasonically cleaning with dilute hydrochloric acid for 18min to obtain a material A2;
step S2: mixing a ruthenium trichloride solution with pure water, wherein the molar concentration of ruthenium trichloride is 2mM, and fully stirring to obtain a material B2;
step S3: putting the material A2 into the material B2, stirring for 160min at normal temperature, and obtaining a material C2 through a spontaneous metal corrosion process, wherein the material A2 is a self-supporting substrate;
step S4: the material C2 was washed with pure water and absolute ethanol, and the material C2 was dried in a forced air drying oven at 80 ℃ for 3 hours to give the product D2.
Example 3
Step S1: cutting foam iron, ultrasonically cleaning in absolute ethyl alcohol for 3min, and ultrasonically cleaning with dilute hydrochloric acid for 18min to obtain a material A3;
step S2: mixing a ruthenium trichloride solution with absolute ethyl alcohol, wherein the molar concentration of ruthenium trichloride is 2mM, and fully stirring to obtain a material B;
step S3: putting the material A3 into the material B3, stirring for 160min at normal temperature, and obtaining a material C3 through a spontaneous metal corrosion process, wherein the material A3 is a self-supporting substrate;
step S4: the material C3 was washed with pure water and absolute ethanol, and the material C3 was dried in a forced air drying oven at 80 ℃ for 3 hours to give the product D3.
Example 4
Cutting to 1 × 0.5cm2The Ru-modified iron-based self-supporting hydrogen evolution electrode D1 product was fixed with a platinum sheet electrode clamp as a working electrode. Working electrodes for products D2, D3 and Iron Foam (IF) were prepared in the same manner and were used in comparison with the product D1. All electrochemical tests adopt a three-electrode system, an Hg/HgO electrode and a carbon rod are respectively used as a reference electrode and a counter electrode, and the electrolyte is 1mol L-1Aqueous KOH solution. The scanning speed of the Linear Sweep Voltammetry (LSV) test is 5mV s-1The scanning range is 0 to-0.4V (vs. RHE).
The properties of the samples in all examples are characterized as follows: as shown in fig. 1, which is a scanning electron micrograph of the product D1 obtained in example 1, the nanosheet structure is evident. As shown in FIG. 3, for the corrosion polarization curves of products D1-D3 prepared in examples 1-3, product D1 corroded to an extent intermediate between that of product D2 and product D3. As shown in FIG. 5, for the linear sweep voltammograms of products D1-D3 prepared in examples 1-3, product D1 was at 100mA cm-2The overpotential of the hydrogen evolution reaction at the current density is 114 mV. The results show that the product D1 has good electrocatalytic hydrogen evolution performance, and the preparation process has the obvious advantages of cleanness, high efficiency, greenness and simplicity, and has wide prospects in practical application.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (5)
1. A preparation method of a Ru-modified iron-based self-supporting hydrogen evolution electrode is characterized by comprising the following specific processes:
step S1: cutting the foamed iron, ultrasonically cleaning the foamed iron in absolute ethyl alcohol for 3-5 min, and ultrasonically cleaning the foamed iron for 15-20 min by using dilute hydrochloric acid to obtain a material A;
step S2: mixing the ruthenium trichloride solution with pure water and absolute ethyl alcohol, and fully stirring to obtain a material B;
step S3: putting the material A into the material B, stirring for 120-180 min at normal temperature, and obtaining a material C through a spontaneous metal corrosion process, wherein the material A is a self-supporting substrate, and the addition of a non-conductive solvent ethanol in the material B is used for regulating and controlling the metal corrosion process and promoting the uniform synthesis of an active corrosion layer;
step S4: and (3) cleaning the material C by using pure water and absolute ethyl alcohol, and then drying the material C in a forced air drying oven at 80 ℃ to obtain the target product Ru-modified iron-based self-supporting hydrogen evolution electrode.
2. The method for preparing the Ru-modified iron-based self-supporting hydrogen evolution electrode according to claim 1, wherein the method comprises the following steps: in the step S2, the molar concentration of ruthenium trichloride in the material B is 1-5 mM, and the volume ratio of pure water to absolute ethyl alcohol in the material B is 1: 0-5.
3. The method for preparing the Ru-modified iron-based self-supporting hydrogen evolution electrode according to claim 1, wherein the method comprises the following steps: and S2, the volume ratio of the pure water to the absolute ethyl alcohol in the material B is 1: 0.1-2.
4. The method for preparing the Ru-modified iron-based self-supporting hydrogen evolution electrode according to claim 1, wherein the method comprises the following steps: and in the step S2, the volume ratio of the pure water to the absolute ethyl alcohol in the material B is 2: 1.
5. The preparation method of the Ru-modified iron-based self-supporting hydrogen evolution electrode according to claim 1, which comprises the following steps:
step S1: cutting foam iron, ultrasonically cleaning in absolute ethyl alcohol for 3min, and ultrasonically cleaning with dilute hydrochloric acid for 18min to obtain a material A;
step S2: mixing ruthenium trichloride with pure water and absolute ethyl alcohol, wherein the volume ratio of the pure water to the absolute ethyl alcohol is 2:1, the molar concentration of the ruthenium trichloride is 2mM, and fully stirring to obtain a material B;
step S3: putting the material A into the material B, stirring for 160min at normal temperature, and obtaining a material C through a spontaneous metal corrosion process, wherein the material A is a self-supporting substrate, and the addition of a non-conductive solvent ethanol in the material B is used for regulating and controlling the metal corrosion process and promoting the uniform synthesis of an active corrosion layer;
step S4: washing the material C with pure water and absolute ethyl alcohol, and then placing the material C in a forced air drying oven at 80 ℃ for drying for 3h to obtain a target product Ru-modified iron-based self-supporting hydrogen evolution electrode with a nanosheet structure, wherein the Ru-modified iron-based self-supporting hydrogen evolution electrode is 1mol L-1Performing electrochemical test in KOH electrolyte, and preparing the Ru modified iron-based self-supporting hydrogen evolution electrode at 100mA cm-2The overpotential for the hydrogen evolution reaction under the current density of (2) is 110-130 mV.
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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 |
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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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