CN111054378B - High-entropy oxide type electrocatalytic anode oxygen evolution catalyst material and preparation method thereof - Google Patents
High-entropy oxide type electrocatalytic anode oxygen evolution catalyst material and preparation method thereof Download PDFInfo
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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- C25B11/077—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide
- C25B11/0771—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound the compound being a non-noble metal oxide of the spinel type
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material and a preparation method thereof, belonging to the field of functional materials. The high-entropy spinel oxide catalyst which can be used for catalyzing the electrocatalytic anodic oxygen evolution reaction is prepared by an alloying ball milling method, has a single spinel structure, is uniform in grain distribution, and has no second phase. The specific method comprises the following steps: the required raw materials are MnO, CoO, NiO and Fe3O4Powder, weighing four kinds of oxide powder according to the set mole ratio of each element, pouring the weighed powder into a ball milling tank, setting the parameters of a ball mill, and carrying out alloying ball milling to obtain the powder containing CoFe2O4Novel high entropy spinel oxides of spinel structure. The high-entropy oxide material prepared by the invention has high-stability electrocatalytic anode oxygen evolution performance, only needs one-step synthesis, and has simple, efficient and safe preparation process.
Description
Technical Field
The invention discloses a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material and a preparation method thereof, belonging to the field of functional materials.
Background
Energy and environment are two major challenges facing human beings. Nowadays, fossil fuel is still the main energy used by human, but with the rapid increase of the usage amount of fossil fuel, the pollution to the global environment is more serious, and the non-renewable resources are increasingly exhausted, which urgently requires people to develop a new clean, pollution-free and renewable energy. H2 is a renewable energy source, not only can deal with resource shortage, but also generates water after hydrogen is combusted, and is the cleanest energy source in the world. The hydrogen evolution of the electrolyzed water is an important means for industrially preparing hydrogen at present, but the main problem of the electrolyzed water is that the anodic oxygen evolution reaction needs higher activation potential. At present, the electrocatalytic anode oxygen evolution catalyst materials widely used commercially are still noble metal oxides such as RuO2 and IrO2, however, the price of the catalyst is very high, the preparation cost is very high, and the requirement of large-scale use cannot be met. Therefore, the development of the electrocatalytic anode oxygen evolution catalytic material which is rich in resources, low in price and high in efficiency is a problem which needs to be solved urgently in the current society.
High Entropy Oxides (HEOs) are novel High Entropy materials formed by adding non-metallic elements on the basis of High Entropy alloys in recent years. The existing methods for preparing high-entropy oxide ceramics mainly comprise solid-phase sintering, mechanical alloying, solution combustion synthesis and the like. The spinel type high-entropy oxide is mixed with spinel (CoFe)2O4) The compounds with the same structure have higher entropy and lower Gibbs free energy, show excellent performance in the aspects of electricity, optics, magnetism and the like, have extremely wide application prospect, and are one of the important discoveries in the field of high-entropy materials in recent years.
In the invention, a plurality of common oxide powders are used, a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material is prepared by mechanical alloying, and the material is found to have excellent performance in the aspect of electrocatalytic anode oxygen evolution catalysis. At present, no report related to the preparation of the high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material by a mechanical alloying method is found.
Disclosure of Invention
The technical problem is as follows: the invention provides a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material and a preparation method thereof, which expand the functional application of the high-entropy oxide material, and have the advantages of simple, safe and efficient preparation method, and excellent and stable catalytic performance of the material.
The invention discloses a high-entropy oxide electrocatalytic anode oxygen evolution catalyst material and a preparation method thereofThe distribution is uniform and no second phase exists. The specific method comprises the following steps: the required raw materials are MnO, CoO, NiO and Fe3O4Powder, weighing four kinds of oxide powder according to the set mole ratio of each element, pouring the weighed powder into a ball milling tank, setting the parameters of a ball mill, and carrying out alloying ball milling to obtain the powder containing CoFe2O4Novel high entropy spinel oxides of spinel structure. The high-entropy oxide material prepared by the invention has high-stability electrocatalytic anode oxygen evolution performance, only needs one-step synthesis, and has simple, efficient and safe preparation process.
The technical scheme is as follows: in the first aspect of the invention, the high-entropy oxide type electrocatalytic anode oxygen evolution catalyst is prepared by adopting the following high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material. At present, no report related to the high-entropy oxide type electrocatalytic anode oxygen evolution catalyst is found.
In a second aspect of the invention, a high entropy oxide electrocatalytic anode oxygen evolution catalyst material is protected, having CoFe2O4The spinel crystal structure, wherein the lattice positions occupied by Co element are occupied by the mixture of Co, Mn, Ni and Fe element, the molar ratio of Co element is 10% -30%, the molar ratio of Mn element is 10% -30%, the molar ratio of Ni element is 10% -30%, the balance is Fe element, and the total molar ratio of elements is ensured to be 100%.
Simultaneously discloses a preparation method of the high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material, which comprises the following steps:
step 1: with CoO, MnO, NiO, Fe3O4The powder is taken as a raw material and is weighed according to the set mole ratio of each element;
step 2, putting the weighed four oxide powders into the same ball milling tank, covering a sealing cover, and then installing the ball milling tank on a ball mill for mechanical ball milling, wherein the ball milling tank is a hard alloy tank; the grinding ball is a hard alloy ball, and the ball material ratio is about 10: 1;
step 3, the ball milling process is as follows: firstly, performing ball milling for 1h at the rotation speed of 500 plus 600rpm, then pausing for 15min, and performing ball milling for 1h after 15min, wherein the rotation speed of 500 plus 600rpm is taken as a ball milling period, and the total ball milling time is 60-65 h;
step 4, taking out oxide mixture powder obtained after alloying and ball milling, putting the oxide mixture powder into a drying box for drying, and sieving the dried oxide mixture powder;
and 5: weighing 80-100mg of sieved powder, putting into a test tube, dripping 2mL of absolute ethyl alcohol, performing ultrasonic oscillation for 20-30min, adding 5-10 mu L of Nafion solution with the mass fraction of 5 wt%, and performing ultrasonic oscillation for 20-30 min;
step 6: sucking a little of the solution prepared in the step 6 by using a dropper, uniformly dripping the solution on the surface of hydrophilic carbon paper with the area of 1cm2, and taking the hydrophilic carbon paper as a working electrode after the alcohol is completely volatilized;
and 7: performing electrochemical activity CV activation on a working electrode, wherein a reference electrode is an Ag/AgCl electrode; the counter electrode is a Pt electrode; the electrolyte is 1M KOH solution; the activation interval is-0.6V to-0.3V; the number of activation cycles is 800-1000.
The invention also discloses application of the material, namely application of the high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material in an electrocatalytic anode material.
Has the advantages that: (1) the invention discloses a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material and a preparation method thereof, wherein the high-entropy oxide does not have a second phase and is mixed with typical spinel (CoFe)2O4) The structure of the compound is the same. The system is very stable due to the large mixing entropy and the low Gibbs free energy. Compared with the common spinel oxide, the spinel oxide has more potential new properties and larger application space.
(2) The invention is to CoO, NiO, MnO and Fe3O4Before the powder is alloyed and ball-milled, the ball-milling tank does not need to be vacuumized and protective gas is introduced into the vacuum glove box, the alloying ball-milling process is simple and feasible, and the time is saved. The synthesis method is an alloying ball milling method, only one-step synthesis operation is needed, no complex post-treatment is needed, and the preparation process is simple, efficient and safe.
Drawings
FIG. 1 is an XRD pattern of a high entropy oxide electrocatalytic anode oxygen evolution catalyst;
FIG. 2 is an SEM picture of a high entropy oxide type electrocatalytic anode oxygen evolution catalyst;
FIG. 3 is an EDS picture of a high entropy oxide type electrocatalytic anode oxygen evolution catalyst;
FIG. 4 is a polarization curve of a high entropy oxide type electrocatalytic anodic oxygen evolution catalyst material of example compositions in a 1mol/L KOH solution.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments:
example 1
As shown in fig. 1 to 4, a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material has a chemical formula: (Co)0.25Ni0.25Mn0.25Fe0.25)Fe2O4The preparation method comprises the following steps:
step 1: with CoO, MnO, NiO, Fe3O4The powder is taken as a raw material, and four kinds of oxide powder are weighed according to the molar ratio of Co element of 25%, Mn element of 25%, Ni element of 25% and Fe element of 25%.
Step 2, putting the weighed four oxide powders into the same ball milling tank, covering a sealing cover, and then installing the ball milling tank on a ball mill for mechanical ball milling, wherein the ball milling tank is a hard alloy tank; the grinding ball is a hard alloy ball, and the ball material ratio is about 10: 1;
step 3, the ball milling process is as follows: firstly, carrying out ball milling for 1h at the rotation speed of 500rpm, then pausing for 15min, and carrying out ball milling for 1h after 15min, wherein the rotation speed is 500rpm and is taken as a ball milling period, and the total ball milling time is 60 h;
step 4, taking out oxide mixture powder obtained after alloying and ball milling, putting the oxide mixture powder into a drying box for drying, and sieving the dried oxide mixture powder;
and 5: weighing 80mg of sieved powder, putting the powder into a test tube, dripping 2mL of absolute ethyl alcohol, performing ultrasonic oscillation for 20min, adding 5 mu L of Nafion solution with the mass fraction of 5 wt%, and performing ultrasonic oscillation for 20 min;
step 6: sucking a little of the solution prepared in step 6 by a dropper, and uniformly dropping the solution in an area of 1cm2After the alcohol is completely volatilized, the surface of the hydrophilic carbon paper can be used as a working electrode;
and 7: performing CV activation on the working electrode, wherein the reference electrode is an Ag/AgCl electrode; the counter electrode is a Pt electrode; the electrolyte is 1M KOH solution; the activation interval is-0.6V to-0.3V; the number of CV activation cycles was 800-1000.
Example two: the difference between the embodiment and the embodiment one is that the molar ratio of Co element in the step 1 is 10%; the molar ratio of Mn element is 10%; the molar ratio of the Ni element is 10 percent; the four oxide powders were weighed so that the molar ratio of Fe element was 70%, and the rotation speed in step 3 was 600 rpm. The rest is the same as the first embodiment.
Example three: the difference between the embodiment and the embodiment one is that the molar ratio of Co element in the step 1 is 30%; the molar ratio of Mn element is 30%; the molar ratio of the Ni element is 30 percent; the four kinds of oxide powder are weighed with the molar ratio of Fe element of 10%, and the ball milling time in the step 3 is 65 h. The rest is the same as the first embodiment.
Example four: the difference between the embodiment and the embodiment one is that the molar ratio of Co element in the step 1 is 30%; the molar ratio of Mn element is 20%; the molar ratio of the Ni element is 30 percent; the four oxide powders were weighed so that the molar ratio of Fe was 20%, and the weighed amount of the powder in step 5 was 90 mg. The rest is the same as the first embodiment.
Example five: the difference between the embodiment and the embodiment one is that the molar ratio of Co element in the step 1 is 10%; the molar ratio of Mn element is 40%; the molar ratio of the Ni element is 40 percent; the four oxide powders were weighed so that the molar ratio of Fe was 10%, and the weighed amount of the powder in step 5 was 100 mg. The rest is the same as the first embodiment.
Example six: the difference between this embodiment and the first embodiment is that the rotation speed in step 3 is 550rpm, and the ultrasonic oscillation time in step 5 is 25 min. The rest is the same as the first embodiment.
Example seven: the difference between this embodiment and the first embodiment is that the rotation speed in step 3 is 550rpm, and the ultrasonic oscillation time in step 5 is 30 min. The rest is the same as the first embodiment.
Example eight: this example differs from the first example in that the rotation speed in step 3 is 600rpm and the amount of Nafion solution added in step 5 is 8. mu.L. The rest is the same as the first embodiment.
Example nine: the difference between this example and the first example is that the rotation speed in step 3 is 600rpm, and the amount of Nafion solution added in step 5 is 10. mu.L. The rest is the same as the first embodiment.
Example ten: this example differs from the first example in that the amount of Nafion solution added in step 5 was 8 μ L and the number of cycles of electrochemically active CV in step 7 was 900. The rest is the same as the first embodiment.
Example eleven: this example differs from the first example in that the amount of Nafion solution added in step 5 was 10 μ L and the number of cycles of electrochemically active CV in step 7 was 1000. The rest is the same as the first embodiment.
The invention successfully synthesizes a high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material by adopting an alloying ball milling method, wherein the high-entropy oxide does not have impurity phase and is mixed with typical spinel (CoFe)2O4) Class of same structureA compound is provided. The system is very stable due to the large mixing entropy and the low Gibbs free energy. Compared with the common spinel oxide, the spinel oxide has more potential new properties and larger application space.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by one of ordinary skill in the art and related arts based on the embodiments of the present invention without any creative effort, shall fall within the protection scope of the present invention.
Claims (1)
1. A high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material is characterized in that: having CoFe2O4The spinel crystal structure is characterized in that lattice positions occupied by Co are occupied by Co, Mn, Ni and Fe in a mixed mode, the molar ratio of Co is 10% -30%, the molar ratio of Mn is 10% -30%, the molar ratio of Ni is 10% -30%, the balance is Fe, and the total molar ratio of the elements is 100%;
the preparation method of the high-entropy oxide type electrocatalytic anode oxygen evolution catalyst material comprises the following steps:
step 1: with CoO, MnO, NiO, Fe3O4The powder is taken as a raw material and is weighed according to the set mole ratio of each element;
step 2, putting the weighed four oxide powders into the same ball milling tank, covering a sealing cover, and then installing the ball milling tank on a ball mill for mechanical ball milling, wherein the ball milling tank is a hard alloy tank; the grinding ball is a hard alloy ball, and the ball material ratio is 10: 1;
step 3, the ball milling process is as follows: firstly, performing ball milling for 1h at the rotation speed of 500 plus 600rpm, then pausing for 15min, and performing ball milling for 1h after 15min, wherein the rotation speed of 500 plus 600rpm is taken as a ball milling period, and the total ball milling time is 60-65 h;
step 4, taking out oxide mixture powder obtained after alloying and ball milling, putting the oxide mixture powder into a drying box for drying, and sieving the dried oxide mixture powder;
and 5: weighing 80-100mg of sieved powder, putting into a test tube, dripping 2mL of absolute ethyl alcohol, performing ultrasonic oscillation for 20-30min, adding 5-10 mu L of Nafion solution with the mass fraction of 5 wt%, and performing ultrasonic oscillation for 20-30 min;
step 6: sucking a little of the solution prepared in the step 5 by using a dropper, uniformly dripping the solution on the surface of the hydrophilic carbon paper, and taking the hydrophilic carbon paper as a working electrode after the alcohol is completely volatilized;
and 7: performing electrochemical activity CV activation on a working electrode, wherein a reference electrode is an Ag/AgCl electrode; the counter electrode is a Pt electrode; the electrolyte is 1M KOH solution; the activation interval is-0.6V to-0.3V; the number of activation cycles is 800-1000.
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