CN114250487B - Carbon paper-supported ruthenium manganide catalyst and preparation method and application thereof - Google Patents
Carbon paper-supported ruthenium manganide catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a carbon paper-loaded ruthenium manganite catalyst and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing a precursor manganese salt, polyvinylpyrrolidone and a ruthenium trichloride solution to obtain a precursor mixed solution; dipping the cleaned carbon paper in the precursor mixed solution, taking out and drying; ventilating the dried carbon paper under hydrogen at normal temperature, heating, sintering and cooling; the ion concentration ratio of ruthenium element in ruthenium trichloride to manganese element in manganese salt is 1:1, and the manganese salt is selected from manganese trichloride and Mn (NO) 3 ) 3 Or Mn 2 (SO 4 ) 3 (ii) a The carbon paper-supported ruthenium manganite catalyst is applied to the acidic electrolytic water oxygen precipitation reaction as an electrode; according to the invention, the ruthenium manganese alloy catalyst grows in situ on the carbon paper, so that the bonding bond strength of ruthenium is greatly enhanced, the stability is obviously enhanced, the dissolution speed is reduced, a ruthenium oxide with stronger bond is formed on the surface through oxidation, and the stability of the ruthenium-based catalyst in acidic electrolyzed water is further greatly improved.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to a carbon paper-supported ruthenium manganite catalyst, and a preparation method and application thereof.
Background
Acidic electrolysis water oxygen evolution mainly depends on noble metal ruthenium (Ru) and iridium (Ir) based catalyst, wherein Ir noble metal reserves are extremely low, and in contrast, ru has higher catalytic performance and lower price, but Ru based catalyst has relatively poor stability. At present, ru is doped with synthetic alloy or oxide, so that the performance and stability of the Ru are improved.
The proton exchange membrane electrolyzed water has the characteristics of compact structure, low impedance, high current density and the like, and the strong acid environment of the proton exchange membrane and the high voltage of the electrolyzed water have strong corrosion effect on the catalyst, so that most base metals can be dissolved out. At present, most of catalysts which can be used in acidity are noble metal Ru and Ir-based catalysts, and the extreme rarity of Ir limits the wide application of Ir. Ru and electrochemical Oxygen Evolution (OER) catalysts have excellent catalytic performance but weaker stability, and the constant voltage test (10 mA/cm) of acidic environment electrolyzed water catalysts in the literature 2 Corresponding voltage value) or constant current stability (10 mA/cm) 2 ) The test duration mostly does not exceed 50h. The low stability of Ru-based catalysts limits their further widespread use in acidic oxygen evolution reactions.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a carbon paper-supported ruthenium manganite catalyst as well as a preparation method and application thereof. The catalyst grows in situ by a dip-coating method, namely, a carbon paper (CFP) surface is dipped with precursor mixed liquid, and then reduction sintering is carried out in a hydrogen atmosphere to obtain the in-situ grown carbon paper ruthenium manganese (RuMn) alloy catalyst.
In order to achieve the purpose, the solution of the invention is as follows:
in a first aspect, the invention provides a preparation method of a carbon paper-supported RuMn catalyst, which comprises the following steps:
(1) And subjecting the precursor manganese saltPolyvinylpyrrolidone (PVP) and ruthenium trichloride (RuCl) 3 ) Mixing the solutions to obtain a precursor mixed solution;
(2) Dipping the cleaned carbon paper in the precursor mixed solution, taking out and drying;
(3) Ventilating the dried carbon paper in the step (2) in a hydrogen atmosphere at normal temperature, heating, sintering and cooling to obtain the carbon paper-loaded RuMn catalyst;
in step (1), ruCl 3 The ion concentration ratio of the medium Ru element to the Mn element in the manganese salt is 1:1.
As a preferred embodiment of the present invention, in the step (1), the manganese salt is selected from MnCl 3 、Mn(NO 3 ) 3 And Mn 2 (SO 4 ) 3 More than one of them.
As a preferred embodiment of the present invention, in the step (2), the time for the immersion is 10 to 20 seconds.
As a preferred embodiment of the invention, in the step (2), the drying temperature is 40-70 ℃, and the drying time is 10-20min.
As a preferred embodiment of the invention, in the step (3), the aeration time at normal temperature is 1-2h.
As a preferred embodiment of the present invention, in the step (3), the rate of temperature rise during heating is 4 to 6 ℃/min, and the heating temperature is 800 to 1000 ℃.
As a preferred embodiment of the present invention, in the step (3), the sintering time is 7-8h.
In a second aspect, the present invention provides a carbon paper supported RuMn catalyst, which is obtained by the above preparation method.
In a third aspect, the invention provides an application of the carbon paper-supported RuMn catalyst as an electrode in an acidic electrolyzed water oxygen evolution reaction. The invention adopts an in-situ growth mode to directly prepare the electrode for the oxygen precipitation reaction of the acidic electrolyzed water.
Due to the adoption of the scheme, the invention has the beneficial effects that:
the invention greatly enhances the bonding strength of Ru by growing the RuMn alloy catalyst in situ on the carbon paper, therebyThe stability of the catalyst is obviously enhanced, the dissolution rate is reduced, and Ru oxide with stronger bond is formed on the surface by oxidation, so that the stability of the Ru-based catalyst in acid electrolyzed water is further greatly improved, and the catalyst can be used at constant current (10 mA/cm) 2 ) The product is stable for 720h in the environment and has super-durability.
In addition, the in-situ growth catalyst stabilizes a Ru-based catalyst under the doping action of Mn, and synthesizes RuZn, ruCo, ruCr and an undoped Ru alloy catalyst by using the same method for comparison, and electrochemical tests show that the carbon paper-loaded RuMn catalyst shows excellent stability in the process of testing the catalytic performance of the catalyst by CV circulation.
Drawings
FIG. 1 is a schematic view of CV cycle scans of (a) Ru, (b) RuCo, (c) RuCr, (d) RuZn and (e) RuMn according to the present invention.
FIG. 2 shows the constant current test (10 mA/cm) of the RuMn catalyst on carbon paper of the present invention 2 ) Schematic representation.
FIG. 3 is SEM images of the growth of (a) Ru, (b) RuCo, (c) RuCr, (d) RuZn and (e) RuMn particles of the present invention on a CFP.
FIG. 4 is TEM images of particles and chemical element distribution of RuMn catalyst on carbon paper before (a), (b) and after (c), (d) electrochemical test.
Detailed Description
The invention provides a carbon paper-loaded RuMn catalyst and a preparation method and application thereof.
< preparation method of RuMn catalyst carried on carbon paper >
The preparation method of the carbon paper-supported RuMn catalyst comprises the following steps:
(1) Preparing RuCl 3 A solution;
(2) The precursor manganese salt, PVP and RuCl 3 Mixing the solution with ultrapure water, and stirring overnight to obtain a precursor mixed solution;
(3) Cleaning the carbon paper, cutting the carbon paper into a size of 1cm multiplied by 2cm, dipping the carbon paper in the precursor mixed solution, and drying the carbon paper dipped with the solution in a drying oven in vacuum;
(4) And putting the dried carbon paper into a tubular furnace, introducing a hydrogen-argon mixer with the hydrogen content of 5%, heating after introducing the hydrogen, sintering, and naturally cooling to obtain the carbon paper-loaded RuMn catalyst.
Wherein, in the step (1), ruCl is added 3 The solution with fixed concentration is prepared and then mixed with other solutions.
In the step (2), the manganese salt is selected from MnCl 3 、Mn(NO 3 ) 3 And Mn 2 (SO 4 ) 3 More than one of (1), mnCl 3 、Mn(NO 3 ) 3 And Mn 2 (SO 4 ) 3 Purchased from aladine corporation.
In step (2), ruCl 3 The ion concentration ratio of the medium Ru element to the Mn element in the manganese salt is 1:1, the ratio can achieve the stable effect, and the catalyst synthesized in other ratios has relatively weak bond energy in the characterization process and poor electrochemical stability.
In the step (2), PVP is added into the precursor solution to adjust the viscosity of the solution, and meanwhile, the dispersion uniformity of the catalyst is improved.
In step (3), the time for immersion may be 10 to 20s, preferably 10s.
In the step (3), the drying temperature can be 40-70 ℃, preferably 50 ℃; the drying time can be 10-20min, preferably 20min.
In the step (4), the normal temperature aeration time may be 1h to 2h, preferably 2h.
In the step (4), the heating rate during heating can be 4-6 ℃/min, preferably 5 ℃/min; the temperature of the heating may be 800-1000 deg.C (which is advantageous for forming an alloy), preferably 800 deg.C.
In step (4), the sintering time may be 7-8h (this time is suitable for forming an alloy), preferably 7h.
< RuMn catalyst on carbon paper >
The carbon paper supported RuMn catalyst of the invention is obtained by the preparation method.
In the electrochemical test, the surface reconstruction is accelerated by scanning electrochemical Cyclic Voltammetry (CV), the scanning range is 1.25-1.75V (vs. rhe), and after scanning, a stable RuOx amorphous layer is formed on the surface of the carbon paper-supported RuMn catalyst, so that the stability is achieved. Specifically, the surface reconstruction of the carbon paper-supported RuMn catalyst occurs in a high-voltage environment (CV and constant current are both environments), so that a RuOx amorphous layer is formed and is stabilized. From electrochemical test results, when the catalyst is stabilized, an amorphous layer is formed on the surface, and the stability of the catalyst is improved by the amorphous layer on the surface in literature (lateral demonstration); on the other hand, the XPS result shows that the Ru bond energy of the carbon paper supported RuMn catalyst is the strongest, so that the stability of the catalyst is greatly enhanced, the dissolution rate is reduced, and finally an oxide is formed in an oxidizing environment (main reason).
In addition, ruMn alloy is grown in situ on the surface of the Ti felt (Ti mesh), and the electrode can also become a self-assembly stable electrode; the same loading effect can be achieved by dripping the precursor mixture on the surface of a substrate (carbon paper, etc.) and then sintering.
As shown in FIG. 1, ru, ruZn, ruCo and RuCr all undergo significant attenuation in the initial 10-turn test, the strong attenuation of the catalyst performance makes it useless as an effective catalyst, while the carbon paper-supported RuMn catalyst shows excellent stability performance in the 20,000-turn test and can be used at a constant current (10 mA/cm) 2 ) The stability test in the environment is 720h, and since the four catalysts of Ru, ruZn, ruCo and RuCr can be seen to be rapidly attenuated in the CV test, the stability is extremely poor so as not to be used as an effective OER catalyst, so that the constant current test is not carried out on the catalysts.
As shown in fig. 4, the carbon paper supported RuMn catalyst before the test has distribution in the surface, and the particles after the reaction, surface area has no Mn element, it can be proved that the Mn element on the surface is leached out during the test, and finally, only Ru is left on the surface.
Application of RuMn catalyst carried on carbon paper
The carbon paper-supported RuMn catalyst can be applied to the acidic electrolyzed water oxygen precipitation reaction as an electrode, namely the super-durable RuMn electrode suitable for the acidic electrolyzed water oxygen precipitation reaction.
The technical content of the present invention will be further described with reference to examples. The following examples are illustrative and not intended to be limiting, and are not intended to limit the scope of the invention. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The present invention will be further described with reference to the following examples.
Example (b):
the preparation method of the in-situ growth carbon paper supported RuMn catalyst comprises the following steps:
(1) Preparing RuCl 3 The concentration of the solution was 0.345mmol/mL.
(2) 0.1385g of MnCl 3 Precursor with 0.16g PVP and 2mL RuCl 3 Mixing the solution with 1mL of ultrapure water, and stirring overnight to form 3mL of precursor mixed solution; wherein the ion concentration ratio of Ru to Mn is 1:1, and the content is 0.7mmol.
(3) Cleaning the carbon paper, cutting the carbon paper into a size of 1cm multiplied by 2cm, dipping the carbon paper in the precursor mixed solution for 10s, and drying the carbon paper dipped with the solution in an oven at 50 ℃ in vacuum for 20min.
(4) And putting the dried carbon paper into a tubular furnace, introducing a hydrogen-argon mixer with the hydrogen content of 5%, heating after introducing the hydrogen for 2h at the heating rate of 5 ℃/min to 800 ℃, sintering for 7h, and naturally cooling to obtain the carbon paper-loaded RuMn catalyst.
The embodiments described above are presented to facilitate one of ordinary skill in the art to make and use the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (6)
1. A preparation method of a carbon paper-supported ruthenium manganite catalyst is characterized by comprising the following steps: which comprises the following steps:
(1) Mixing a precursor manganese salt, 0.16g of polyvinylpyrrolidone and 2mL of ruthenium trichloride solution with ultrapure water to obtain 3mL of precursor mixed solution;
(2) Dipping the cleaned carbon paper in the precursor mixed solution, and drying after taking out;
(3) At normal temperature, ventilating the dried carbon paper in the step (2) in a hydrogen atmosphere, heating, sintering and cooling to obtain the carbon paper-loaded ruthenium manganese catalyst;
in the step (1), the ion concentration ratio of the ruthenium element in the precursor mixed solution to the manganese element in the manganese salt is 1:1, and the contents of the ruthenium element and the manganese element are both 0.7mmol;
in the step (2), the dipping time is 10-20s;
in the step (3), the heating rate is 4-6 ℃/min during heating, and the heating temperature is 800-1000 ℃;
in the step (3), the sintering time is 7-8h.
2. The method for preparing the carbon paper-supported ruthenium manganite catalyst according to claim 1, which is characterized in that: in the step (1), the manganese salt is selected from manganese trichloride and Mn (NO) 3 ） 3 And Mn 2 （SO 4 ） 3 More than one of them.
3. The method for preparing the carbon paper-supported ruthenium manganite catalyst according to claim 1, wherein the method comprises the following steps: in the step (2), the drying temperature is 40-70 ℃, and the drying time is 10-20min.
4. The method for preparing the carbon paper-supported ruthenium manganite catalyst according to claim 1, wherein the method comprises the following steps: in the step (3), the normal-temperature ventilation time is 1-2h.
5. A carbon paper-supported ruthenium manganite catalyst is characterized in that: which is obtained by the production method according to any one of claims 1 to 4.
6. Use of the carbon paper-supported ruthenium manganite catalyst as claimed in claim 5 as an electrode in an acidic electrolysis water oxygen evolution reaction.
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Citations (5)
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| DE3167797D1 (en) * | 1980-05-02 | 1985-01-31 | Gen Electric | Anode catalyst and generation of oxygen |
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| CN113026051A (en) * | 2021-03-12 | 2021-06-25 | 中国科学技术大学 | Ruthenium-manganese oxide solid solution, preparation method thereof and application of ruthenium-manganese oxide solid solution as acidic oxygen precipitation reaction electrocatalyst |
| CN113026032A (en) * | 2021-03-10 | 2021-06-25 | 东华大学 | Ruthenium atom-level loaded manganese oxide catalyst and preparation method and application thereof |
| CN113611884A (en) * | 2021-08-03 | 2021-11-05 | 中国科学技术大学 | Ruthenium-doped alpha-manganese dioxide composite material, preparation method and application thereof |
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2021
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| DE3167797D1 (en) * | 1980-05-02 | 1985-01-31 | Gen Electric | Anode catalyst and generation of oxygen |
| CN112458495A (en) * | 2020-11-27 | 2021-03-09 | 浙江大学衢州研究院 | Electrocatalyst of ruthenium-based transition metal oxide solid solution and preparation method and application thereof |
| CN113026032A (en) * | 2021-03-10 | 2021-06-25 | 东华大学 | Ruthenium atom-level loaded manganese oxide catalyst and preparation method and application thereof |
| CN113026051A (en) * | 2021-03-12 | 2021-06-25 | 中国科学技术大学 | Ruthenium-manganese oxide solid solution, preparation method thereof and application of ruthenium-manganese oxide solid solution as acidic oxygen precipitation reaction electrocatalyst |
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| Compensating Electronic Effect Enables Fast Site-to-Site Electron Transfer over Ultrathin RuMn Nanosheet Branches toward Highly Electroactive and Stable Water Splitting;Leigang Li et al.;《Adv. Mater.》;20211015;第1-11页 * |
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| Ru-Mn氧化物涂层钛阴极的制备及其析氢性能;王欣等;《金属热处理》;20091125(第11期);第34-37页 * |
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