CN114622217B - Iron-cobalt phosphide catalyst and preparation method and application thereof - Google Patents
Iron-cobalt phosphide catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an iron-cobalt phosphide catalyst, a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, mixing iron salt, cobalt salt and acetic acid solution containing chitosan, sequentially stirring, drying, and performing pyrolysis treatment at 300-700 ℃ for 1-4 h to obtain an iron-cobalt phosphide precursor; the ratio of the mass sum of the ferric salt and the cobalt salt to the mass of the chitosan is (1.2-1.8): 1; the molar ratio of Fe in the ferric salt to Co in the cobalt salt is (3-7): (3-7); s2, putting the iron-cobalt phosphide precursor in an inert atmosphere for phosphating to obtain an iron-cobalt phosphide catalyst; the temperature of the phosphating treatment is 250-450 ℃, and the time of the phosphating treatment is 1-4 h; the mass ratio of the iron-cobalt phosphide precursor to the phosphorus source for phosphating is 2: (40-100). The invention provides an iron-cobalt phosphide catalyst which is used in a full-hydrolysis reaction, has a lower overpotential under a high current density and can meet the requirement of industrial application of electrocatalytic full-hydrolysis.
Description
Technical Field
The invention relates to the technical field of catalysts, and particularly relates to an iron-cobalt phosphide catalyst and a preparation method and application thereof.
Background
At present, hydrogen is mainly prepared by cracking reaction of fossil energy, but excessive use of fossil energy can aggravate energy crisis and cause environmental pollution, so that a new hydrogen production method is urgently needed to deal with the increasingly severe energy crisis. Electrocatalytic full-hydrolysis is a green, environment-friendly and sustainable hydrogen production mode. Electrocatalytic total hydrolysis involves two half-reactions under alkaline conditions: hydrogen evolution reaction (HER, 2H) 2 O+2e - →H 2 +2OH - ) And oxygen evolution reaction (OER, 2 OH) - →1/2O 2 +H 2 O+2e - ). Therefore, it is of great importance to find a bifunctional electrocatalyst with both HER and OER activity. Platinum-based catalysts generally show significant HER activity but poor OER activity, while iridium-based catalysts show only good OER activity. Furthermore, their use on an industrial scale is impractical due to their high cost and scarcity. Therefore, there is a need to search for a new bifunctional electrocatalyst based on low cost and high abundance in the earth.
The Chinese invention patent CN109499596A discloses a method for preparing a bifunctional electrocatalyst by reacting modified chitosan with metal salt, the electrocatalyst prepared by the method can be used for catalyzing water electrolysis hydrogen production and Oxygen Reduction Reaction (ORR), and has oxygen reduction performance superior to that of a commercial Pt/C catalyst, but phosphorus and nitrogen doping in the catalyst mainly influences the electroneutrality of carbon, so that the adsorption of oxygen is facilitated, and the ORR performance is improved. The OER is an oxygen evolution reaction, the active center of the OER is mainly an oxide or oxyhydroxide converted from high-valence metal ions, and the OER requires the catalyst to have stronger desorption capacity to oxygen, which is opposite to the theory of the ORR, so that the catalyst is used for low or even no OER activity, and further cannot be used for electrocatalytic full-hydrolysis.
Disclosure of Invention
The invention aims to overcome the problem that the existing bifunctional electrocatalyst cannot be used for electrocatalytic full-hydrolysis, and provides a preparation method of an iron-cobalt phosphide catalyst, wherein the catalyst prepared by the method is used for electrocatalytic full-hydrolysis at the current density of 100 mA-cm -2 The overpotential is less than 1.9V.
It is another object of the present invention to provide an iron cobalt phosphide catalyst.
It is a further object of the present invention to provide the use of the above iron cobalt phosphide catalyst.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of an iron-cobalt phosphide catalyst comprises the following steps:
s1, mixing iron salt, cobalt salt and acetic acid solution containing chitosan, sequentially stirring, drying, and performing pyrolysis treatment at 300-700 ℃ for 1-4 h to obtain an iron-cobalt phosphide precursor;
the ratio of the mass sum of the ferric salt and the cobalt salt to the mass of the chitosan is (1.2-1.8): 1;
the molar ratio of Fe in the iron salt to Co in the cobalt salt is (3-7): (3-7);
s2, putting the iron-cobalt phosphide precursor in an inert atmosphere for phosphating to obtain an iron-cobalt phosphide catalyst; the temperature of the phosphating treatment is 250-450 ℃, and the time of the phosphating treatment is 1-4 h;
the mass ratio of the iron-cobalt phosphide precursor to the phosphorus source subjected to phosphating treatment is 2: (40-100).
The invention prepares an iron-cobalt precursor by controlling the proportion of iron and cobalt coordinated with chitosan, further introduces phosphorus to regulate the electronic structure of iron-cobalt alloy, and prepares an iron-cobalt phosphide catalyst which can be used for electrocatalytic full-water electrolysis, has great advantages in acid water electrolysis hydrogen production, alkaline water electrolysis hydrogen production and water electrolysis oxygen production, and has wide application prospect.
Preferably, the ratio of the mass sum of the iron salt and the cobalt salt to the mass of the chitosan is (1.3-1.5): 1. more preferably 1.4:1.
preferably, the molar ratio of Fe in the iron salt to Co in the cobalt salt is (3-5): (5-7). More preferably 3:7.
preferably, the pyrolysis treatment temperature is 400 to 600 ℃. More preferably 500 deg.c.
Iron and cobalt salts, which are conventional in the art, may be used in the present invention. Preferably, the iron salt is selected from iron nitrate and the cobalt salt is selected from cobalt nitrate.
Preferably, the phosphating temperature is 300-400 ℃. More preferably 300 deg.c.
In the invention, the phosphorization treatment is to place a phosphorus source in an upper tuyere and place an iron-cobalt phosphide precursor in a lower tuyere, and treat for 1-4 h at the temperature of 250-450 ℃ in an inert atmosphere.
Preferably, the mass ratio of the iron-cobalt phosphide precursor to the phosphorus source for phosphating is 2: (50-70).
Phosphorus sources conventional in the art may be used in the present invention. The phosphorus source is preferably sodium hypophosphite.
Acetic acid solutions of concentrations conventional in the art may be used in the present invention. Preferably, the concentration of the acetic acid solution is 1.25wt%.
An iron-cobalt phosphide catalyst is prepared by the method.
When the iron-cobalt phosphide catalyst is used for full-hydrolysis, the overpotential is lower under the high current density, and the iron-cobalt phosphide catalyst can be used for electrocatalytic full-hydrolysis. Therefore, the application of the iron-cobalt phosphide catalyst in electrocatalytic total-hydrolysis water also falls within the protection scope of the invention.
Compared with the prior art, the invention has the beneficial effects that:
the catalyst with nanoparticle stacking appearance and synergistic effect of FeCo, coP and FeCoP is prepared by a sol-gel method, pyrolysis treatment and phosphating treatment, can realize efficient hydrogen evolution and efficient oxygen evolution under acidic and alkaline conditions, and has full-hydrolytic performance of hydrogen evolution and oxygen evolution simultaneously under high current density in an alkaline solution. In addition, the catalyst provided by the invention has excellent stability, and can meet the requirements of industrial application of electrocatalytic full-hydrolytic water.
Drawings
FIG. 1 is an XRD pattern of an iron cobalt phosphide catalyst provided in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of an iron cobalt phosphide catalyst provided in example 1 of the present invention;
FIG. 3 shows the reaction of the iron-cobalt-phosphide catalyst provided in example 1 of the present invention in 1M HClO 4 An electrocatalytic hydrogen evolution polarization curve diagram in the solution;
FIG. 4 is a graph showing the polarization of electrocatalytic hydrogen evolution of an iron-cobalt phosphide catalyst in a 1M KOH solution according to example 1 of the present invention;
FIG. 5 is a graph showing the polarization of electrocatalytic oxygen evolution of an iron-cobalt-phosphide catalyst in a 1M KOH solution according to example 1 of the present invention;
FIG. 6 is a graph of the polarization of electrocatalytic full-hydrolysis of Fe-Co phosphide catalyst in 1M KOH solution provided in example 1 of the present invention;
FIG. 7 is a graph showing the stability of the FeCoP catalyst in a 1M KOH solution according to example 1 of the present invention.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.
Example 1
The preparation method of the iron-cobalt phosphide catalyst comprises the following steps:
s1, dissolving 2g of chitosan in 1.25wt% of acetic acid solution, stirring at constant temperature until the solution is transparent, and adding Fe: continuously stirring ferric nitrate nonahydrate and cobalt nitrate hexahydrate with the Co molar ratio of 3:7 at the constant temperature of 80 ℃ for 2 hours until the solution slowly flows, taking out the solution, drying the solution in an oven at the temperature of 50 ℃ for 12 hours, and then putting a sample in a tubular furnace for pyrolysis treatment, wherein the temperature of the pyrolysis treatment is 500 ℃ and the pyrolysis time is 2 hours to obtain an iron-cobalt phosphide precursor; the ratio of the mass sum of the ferric nitrate nonahydrate and the cobalt nitrate hexahydrate to the mass of the chitosan is 1.4:1;
s2, respectively loading sodium hypophosphite and an iron-cobalt phosphide precursor into a corundum crucible, respectively placing the corundum crucible and the iron-cobalt phosphide precursor into an upper air inlet and a lower air inlet in a tubular furnace, introducing 200ml/min of nitrogen, heating to 300 ℃ at a heating rate of 2 ℃/min, and keeping for 2 hours to complete phosphating treatment to obtain an iron-cobalt phosphide catalyst; the mass ratio of the iron-cobalt phosphide precursor to the sodium hypophosphite is 2:60.
example 2
Unlike example 1, the temperature of the phosphating treatment in step S2 of this example was 400 ℃.
Example 3
Unlike example 1, the temperature of the phosphating treatment in step S2 of this example was 250 ℃ and the time of the phosphating treatment was 4 hours.
Example 4
Unlike example 1, the temperature of the phosphating treatment in step S2 of this example was 450 ℃ and the time of the phosphating treatment was 1 hour.
Example 5
Unlike example 1, the pyrolysis treatment temperature in step S1 of this example was 300 ℃ and the pyrolysis treatment time was 4 hours.
Example 6
Unlike example 1, the pyrolysis treatment temperature in step S1 of this example was 700 ℃ and the pyrolysis treatment time was 1 hour.
Example 7
Unlike example 1, the temperature of the pyrolysis treatment in step S1 of this example was 400 ℃.
Example 8
Unlike example 1, the temperature of the pyrolysis treatment in step S1 of this example was 600 ℃.
Example 9
Unlike example 1, in step S1 of this example, fe: iron nitrate nonahydrate and cobalt nitrate hexahydrate with a Co molar ratio of 7:3.
Example 10
Unlike example 1, in step S1 of this example, fe: iron nitrate nonahydrate and cobalt nitrate hexahydrate with a Co molar ratio of 5:5.
Example 11
Unlike example 1, in step S1 of this example, the ratio of the sum of the masses of the iron nitrate nonahydrate and the cobalt nitrate hexahydrate to the mass of the chitosan was 1.2:1.
example 12
Unlike example 1, in step S1 of this example, the ratio of the sum of the masses of the iron nitrate nonahydrate and the cobalt nitrate hexahydrate to the mass of the chitosan was 1.3:1.
example 13
Unlike example 1, in step S1 of this example, the ratio of the sum of the masses of iron nitrate nonahydrate and cobalt nitrate hexahydrate to the mass of chitosan was 1.5:1.
example 14
Unlike example 1, in step S1 of this example, the ratio of the sum of the masses of the iron nitrate nonahydrate and the cobalt nitrate hexahydrate to the mass of the chitosan was 1.8:1.
example 15
Different from embodiment 1, in step S2 of this embodiment, the mass ratio of the iron-cobalt phosphide precursor to the sodium hypophosphite is 2:40.
example 16
Different from the embodiment 1, in the step S2 of the present embodiment, the mass ratio of the iron-cobalt phosphide precursor to the sodium hypophosphite is 2:50.
example 17
Different from the embodiment 1, in the step S2 of the present embodiment, the mass ratio of the iron-cobalt phosphide precursor to the sodium hypophosphite is 2:70.
example 18
Different from the embodiment 1, in the step S2 of the present embodiment, the mass ratio of the iron-cobalt phosphide precursor to the sodium hypophosphite is 2:100.
comparative example 1
The present comparative example provides an iron phosphide catalyst, the preparation method of which is as follows:
s1, dissolving 2g of chitosan in 1.25wt% of acetic acid solution, stirring at a constant temperature until the solution is transparent, adding 3.6g of ferric nitrate nonahydrate, continuously stirring at a constant temperature of 80 ℃ for 2h until the solution slowly flows, taking out, drying in an oven at 50 ℃ for 12h, and then placing a sample in a tubular furnace for pyrolysis treatment, wherein the temperature of the pyrolysis treatment is 500 ℃, and the pyrolysis time is 2h to obtain an iron phosphide precursor; the mass ratio of the ferric nitrate nonahydrate to the chitosan is 1.8:1;
s2, respectively loading sodium hypophosphite and an iron phosphide precursor into a corundum crucible, respectively placing the corundum crucible and the iron phosphide precursor into an upper air inlet and a lower air inlet in a tubular furnace, introducing 200ml/min of nitrogen, heating to 300 ℃ at a heating rate of 2 ℃/min, and keeping for 2h to complete phosphating treatment to obtain an iron phosphide catalyst; the mass ratio of the iron phosphide precursor to the sodium hypophosphite is 2:60.
comparative example 2
The comparative example provides a cobalt phosphide catalyst, and the preparation method comprises the following steps:
s1, dissolving 2g of chitosan in 1.25wt% of acetic acid solution, stirring at constant temperature until the solution is transparent, adding 2.48g of cobalt nitrate hexahydrate, continuously stirring at constant temperature of 80 ℃ for 2h until the solution flows slowly, taking out, drying in an oven at 50 ℃ for 12h, and then putting a sample in a tubular furnace for pyrolysis treatment, wherein the pyrolysis treatment temperature is 500 ℃, and the pyrolysis time is 2h, so as to obtain a cobalt phosphide precursor; the mass ratio of the cobalt nitrate hexahydrate to the chitosan is 1.24:1;
s2, respectively loading sodium hypophosphite and a cobalt phosphide precursor into a corundum crucible, respectively placing the corundum crucible and the cobalt phosphide precursor into an upper air inlet and a lower air inlet of a tubular furnace, introducing 200ml/min nitrogen, heating to 300 ℃ at a heating rate of 2 ℃/min, and keeping for 2 hours to complete phosphating treatment to obtain a cobalt phosphide catalyst; the mass ratio of the cobalt phosphide precursor to the sodium hypophosphite is 2:60.
comparative example 3
The present comparative example provides a copper phosphide catalyst, the preparation method of which is as follows:
s1, dissolving 2g of chitosan in 1.25wt% of acetic acid solution, stirring at a constant temperature until the solution is transparent, adding 1.48g of copper nitrate, continuously stirring at a constant temperature of 80 ℃ for 2h until the solution slowly flows, taking out, drying in an oven at 50 ℃ for 12h, and putting a sample in a tubular furnace for pyrolysis treatment at 500 ℃ for 2h to obtain a copper phosphide precursor; the mass ratio of the copper nitrate to the chitosan is 0.74:1;
s2, respectively loading sodium hypophosphite and a copper phosphide precursor into a corundum crucible, respectively placing the corundum crucible and the copper phosphide precursor into an upper air inlet and a lower air inlet in a tubular furnace, introducing 200ml/min of nitrogen, heating to 300 ℃ at a heating rate of 2 ℃/min, and keeping for 2h to complete phosphating treatment to obtain a copper phosphide catalyst; the mass ratio of the copper phosphide precursor to the sodium hypophosphite is 2:60.
comparative example 4
The present comparative example provides a nickel cobalt phosphide catalyst, the preparation method of which is as follows:
s1, dissolving 2g of chitosan in 1.25wt% of acetic acid solution, stirring at constant temperature until the solution is transparent, and adding Ni: continuously stirring nickel nitrate hexahydrate and cobalt nitrate hexahydrate with the Co molar ratio of 7:3 at the constant temperature of 80 ℃ for 2 hours until the solution slowly flows, taking out the solution, drying the solution in an oven at the temperature of 50 ℃ for 12 hours, and then putting a sample in a tubular furnace for pyrolysis treatment, wherein the temperature of the pyrolysis treatment is 500 ℃ and the pyrolysis time is 2 hours to obtain a nickel cobalt phosphide precursor; the mass ratio of the sum of the nickel nitrate hexahydrate and the cobalt nitrate hexahydrate to the chitosan is 1.25:1;
s2, respectively loading sodium hypophosphite and a nickel cobalt phosphide precursor into a corundum crucible, respectively placing the corundum crucible and the nickel cobalt phosphide precursor into an upper air inlet and a lower air inlet of a tubular furnace, introducing 200ml/min nitrogen, heating to 300 ℃ at a heating rate of 2 ℃/min, and keeping for 2 hours to complete phosphating treatment to obtain a nickel cobalt phosphide catalyst; the mass ratio of the nickel cobalt phosphide precursor to the sodium hypophosphite is 2:60.
characterization of the test
XRD (X-ray diffraction) and scanning electron microscope analysis are carried out on the iron-cobalt phosphide catalysts of the examples 1-18, and the XRD pattern and the SEM pattern of the iron-cobalt phosphide catalyst of the example 1 are respectively shown in figure 1 and figure 2, and as can be seen from figure 1, the iron-cobalt phosphide catalyst is successfully prepared in the example 1; as can be seen from fig. 2, the morphology of the iron-cobalt phosphide catalyst prepared in example 1 is stacked in the form of particles. The XRD patterns and SEM patterns of the iron-cobalt-phosphide catalysts described in examples 2 to 18 are similar to those of fig. 1 and 2, respectively.
The iron-cobalt phosphide catalysts described in examples 1 to 18 were subjected to polarization curve testing under room temperature using a three-electrode system (in which a graphite electrode was used as a counter electrode, a mercury oxide electrode was used as a reference electrode, and a platinum sheet electrode holder was used as a working electrode), carbon paper was used as a carrier for the catalyst, and 1M HClO was used 4 Or 1M KOH as electrolyte, and the line is processed under the condition that the scanning speed is 2mV/sAnd (4) performing sexual sweep voltammetry testing.
FIG. 3 is a graph of the iron-cobalt-phosphide catalyst of example 1 in 1M HClO 4 Polarization curve diagram of electrocatalytic hydrogen evolution in solution. As can be seen from FIG. 3, when the current density was 10mA cm -2 At 1M HClO 4 The overpotential for hydrogen evolution in the solution is 78mV. Examples 2-18 iron cobalt phosphide catalysts in 1M HClO 4 The polarization curve of electrocatalytic hydrogen evolution in solution is similar to that of example 1 when the current density is 10mA cm -2 When in 1M HClO 4 The hydrogen evolution overpotential of the solution is lower than 95mV.
FIG. 4 is a graph showing the polarization of electrocatalytic hydrogen evolution of the iron-cobalt-phosphide catalyst described in example 1 in a 1M KOH solution. As can be seen from FIG. 4, when the current density was 10mA cm -2 The overpotential for hydrogen evolution in 1M KOH solution was 194mV. The Fe-Co-phosphide catalysts described in examples 2 to 18 exhibited a current density of 10mA cm -2 The overpotential for hydrogen evolution in 1M KOH solution is shown in Table 1.
TABLE 1
| overpotential/mV | |
| Example 1 | 194 |
| Example 2 | 203 |
| Example 3 | 201 |
| Example 4 | 206 |
| Example 5 | 210 |
| Example 6 | 215 |
| Example 7 | 213 |
| Example 8 | 215 |
| Example 9 | 220 |
| Example 10 | 215 |
| Example 11 | 217 |
| Example 12 | 210 |
| Example 13 | 207 |
| Example 14 | 205 |
| Example 15 | 210 |
| Example 16 | 208 |
| Example 17 | 211 |
| Example 18 | 207 |
FIG. 5 is a graph of the electrocatalytic oxygen evolution polarization of the iron cobalt phosphide catalyst described in example 1 in 1M KOH solution. As can be seen from FIG. 5, when the current density was 1A cm -2 The overpotential for oxygen evolution in a 1M KOH solution was 360mV. The electrocatalytic oxygen evolution polarization curves of the iron-cobalt-phosphide catalysts described in examples 2-18 in a 1M KOH solution are similar to those of example 1, when the current density is 1A cm -2 The oxygen evolution overpotential of the catalyst in a 1M KOH solution is lower than 400mV.
FIG. 6 is a graph of the electrocatalytic full-hydrolysis polarization of the iron-cobalt-phosphide catalyst described in example 1 in a 1M KOH solution. As can be seen from FIG. 6, when the current density was 100mA cm -2 The overpotential for the total hydrolysis in 1M KOH solution was 1.75V. The Fe-Co-phosphide catalysts described in examples 2 to 18 and the catalysts described in comparative examples 1 to 4 were used when the current density was 100mA cm -2 The overpotential for total hydrolysis in 1M KOH solution is shown in Table 2.
TABLE 2
FIG. 7 is a graph showing the stability of the iron-cobalt-phosphide catalyst of example 1, and it can be seen from FIG. 7 that the catalyst can be used at a current density of 40mA cm -2 The test piece is smoothly operated for 48 hours, and the test piece has excellent stability. The stability test patterns of the iron-cobalt phosphide catalysts described in examples 2 to 18 all showed excellent stability similarly to example 1.
From the above test results, embodiment 1 to E of the present invention18 can be used for electrocatalytic full-hydrolysis at a current density of 100 mA-cm -2 When the catalyst is used, the overpotential is not higher than 1.9V, and from the above results, it is understood that the catalyst can be used also in hydrogen production by acidic electrolysis of water, hydrogen production by alkaline electrolysis of water, and oxygen production by electrolysis of water, and that the catalyst has excellent stability and has a current density of 40mA cm -2 And the operation can be carried out for 48h. In contrast, in comparative examples 1 to 3, the catalyst prepared by using the monometal to coordinate with chitosan and phosphating had significantly poorer full-hydrolytic performance. Comparative example 4 the catalyst obtained was also inferior in full water splitting performance by complexing and phosphating the chitosan with nickel cobalt bimetallic.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The preparation method of the iron-cobalt phosphide catalyst is characterized by comprising the following steps of:
s1, mixing iron salt, cobalt salt and acetic acid solution containing chitosan, sequentially stirring, drying, and performing pyrolysis treatment for 1-4 hours at 300-700 ℃ to obtain an iron-cobalt phosphide precursor;
the ratio of the mass sum of the ferric salt and the cobalt salt to the mass of the chitosan is (1.2-1.8): 1;
the molar ratio of Fe in the ferric salt to Co in the cobalt salt is (3-7): (3-7);
s2, putting the iron-cobalt phosphide precursor in an inert atmosphere for phosphating to obtain an iron-cobalt phosphide catalyst; the phosphating temperature is 250-450 ℃, and the phosphating time is 1-4 h;
the mass ratio of the iron-cobalt phosphide precursor to the phosphorus source for phosphating is 2: (40-100).
2. The method for preparing the iron-cobalt phosphide catalyst according to claim 1, wherein the ratio of the mass sum of the iron salt and the cobalt salt to the mass of the chitosan is (1.3-1.5): 1.
3. the method of claim 1, wherein the molar ratio of Fe in the iron salt to Co in the cobalt salt is (3-5): (5-7).
4. The method of claim 1, wherein the pyrolysis treatment temperature is from 400 to 600 ℃.
5. The method of claim 1, wherein the iron salt is selected from the group consisting of ferric nitrate and the cobalt salt is selected from the group consisting of cobalt nitrate.
6. The method of claim 1, wherein the phosphating temperature is from 300 to 400 ℃.
7. The method for preparing the Fe-Co-phosphide catalyst as claimed in claim 1, wherein the phosphating treatment comprises the steps of placing a phosphorus source in an upper tuyere, placing an Fe-Co phosphide precursor in a lower tuyere and treating for 1-4 h at the temperature of 250-450 ℃ in an inert atmosphere.
8. The method for preparing the iron-cobalt phosphide catalyst according to claim 1, wherein the mass ratio of the iron-cobalt phosphide precursor to the phosphorus source for phosphating is 2: (50-70).
9. An iron-cobalt phosphide catalyst, characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. Use of the iron-cobalt phosphide catalyst of claim 9 in electrocatalytic total hydrolysis of water.
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