CN114735667B - High-entropy metal phosphide FeCoNiCrMnP x Is prepared by the preparation method of (2) - Google Patents
High-entropy metal phosphide FeCoNiCrMnP x Is prepared by the preparation method of (2) Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 31
- 239000002184 metal Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 230000005496 eutectics Effects 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims abstract description 6
- 235000019983 sodium metaphosphate Nutrition 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 4
- 238000013478 data encryption standard Methods 0.000 claims abstract 5
- 150000003839 salts Chemical class 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims description 4
- 229910001510 metal chloride Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229940068886 polyethylene glycol 300 Drugs 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 238000005303 weighing Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000010411 electrocatalyst Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 150000002843 nonmetals Chemical class 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
- C01B25/088—Other phosphides containing plural metal
-
- 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
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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
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Engineering & Computer Science (AREA)
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Abstract
The application discloses a high-entropy metal phosphide FeCoNiCrMnP x Is prepared by the preparation method of (1). Comprising the following steps: weighing polyethylene glycol 200 and urea in a molar ratio of 2:1, and forming a eutectic solvent in an oil bath at 60 ℃; weighing FeCl with the same molar mass 3 ·6H 2 O、CoCl 2 ·6H 2 O、NiCl 2 ·6H 2 O、CrCl 3 ·6H 2 O、MnCl 2 ·4H 2 O, adding DESs to form a eutectic solvent system; transferring the formed DESs system into a reaction kettle, placing the reaction kettle into an oven for reaction, naturally cooling to room temperature after the reaction is finished, filtering, collecting solids, and drying; and (3) placing the dried product in a tubular furnace, heating an upstream region, placing sodium metaphosphate, roasting in an inert gas atmosphere, and cooling along with the furnace. The application has simple preparation operation and low preparation cost, and can be produced in large scale, and the FeCoNiCrMnP is obtained x The size of the nano particles of the material is controllable, and the material has a better crystal form.
Description
Technical Field
The application belongs to the technical field of electrocatalytic materials and preparation thereof, and in particular relates to a high-entropy metal phosphide FeCoNiCrMnP x Is prepared by the preparation method of (1).
Background
Developing clean and sustainable energy resources is an effective strategy to address energy crisis and environmental pollution. The rational utilization of rich water resources has received great attention and has become an effective strategy to solve this problem. Electrocatalytic water decomposition has proven to be a highly efficient and cost-effective energy conversion technology over the past decades, with promise of significant roles in reducing environmental pollution. To effectively achieve electrochemical water decomposition including Hydrogen Evolution Reaction (HER) and Oxygen Evolution Reaction (OER) in order to accommodate the need for rapid development, it is essential to explore advanced electrocatalysts with excellent activity and stability in catalytic reactions.
High entropy materials have been of great interest over the past few years due to their superior physicochemical properties. In particular, high entropy materials are considered to be potentially high performance advanced electrocatalysts due to the particular crystal structure and diversity of multi-elements. Generally, high entropy materials can be classified into high entropy alloys and high entropy compounds; the former contains five or more metallic elements, and the latter combines metallic and nonmetallic elements. In the field of catalysis, high entropy alloys used as electrocatalysts exhibit excellent catalytic activity with very high selectivity and stability. The formation of single high entropy compounds is more difficult than the synthesis of high entropy alloys due to the incompatibility between the different metals and non-metals, and thus few reports of synthesizing high entropy compounds are available. The current synthesis strategy of the high-entropy compound is complex and complicated in steps and high in cost. High entropy compounds such as high entropy oxides and high entropy sulfides have been reported; however, they are almost not single phase but complex phase. This is mainly because the formation of compounds depends on the binding forces and coordination numbers between metals and non-metals. The differences in these aspects between metals make it difficult to control the multielement to form a single phase. Thus, developing new strategies for synthesizing high entropy compounds remains a significant challenge.
Transition metal phosphides with unique electrochemical properties are considered to be very promising electrocatalysts in water splitting and are of particular interest due to their high catalytic activity due to hydrogenase-like catalytic mechanisms. The phosphorus element has metallic property and phosphorus in phosphide can adjust electronic structure, thereby improving catalytic activity. Due to the synergistic effect, multimetal phosphides, such as bimetallic or trimetallic phosphides, generally exhibit better catalytic activity than monometal phosphides. In contrast, high Entropy Metal Phosphides (HEMPs) with more metal elements can further increase OER and HER activity by adjusting the composition to achieve optimal adsorption of the reaction intermediates. However, for the above reasons, it is extremely difficult to achieve single-phase combination of the multi-metal element with phosphorus, and thus synthesis of tetra-metal phosphide, even high-entropy metal phosphide (HEMPs) with more improved performance, has been rarely studied and found.
Disclosure of Invention
Based on the defects of the prior art, the application aims to provide a high-entropy metal phosphide FeCoNiCrMnP x The preparation method has the advantages of simple preparation process, mild condition, low preparation cost, industrial production and no environmental pollution. The FeCoNiCrMnP is obtained x Has excellent electrocatalytic hydrogen evolution performance.
In order to achieve the aim, the application provides a high-entropy metal phosphide FeCoNiCrMnP x The preparation method of (2) comprises the following steps:
1) Mixing polyethylene glycol with urea, and heating to form a eutectic solvent (DESs);
2) Mixing Fe salt, co salt, ni salt, cr salt and Mn salt, adding the eutectic solvent (DESs) prepared in the step 1), and heating to form a eutectic solvent system;
3) Transferring the formed eutectic solvent system into a reaction kettle, reacting, cooling to room temperature after the reaction is finished, filtering, collecting solids, and drying;
4) And (3) placing the dried product in a tubular furnace, placing sodium metaphosphate in a heating upstream area, roasting in an inert gas atmosphere, and cooling along with the furnace to obtain the product.
In the step 1) of the method, the molar ratio of the polyethylene glycol to the urea is 10:1-1:1, and can be specifically 2:1;
the polyethylene glycol can be polyethylene glycol 200, polyethylene glycol 300,
the heating can be performed in an oil bath at 40-120 ℃ (specifically 60 ℃);
in step 2), the Fe salt, co salt, ni salt, cr salt and Mn salt are mixed in equimolar amounts (in terms of the number of moles of each metal contained) of 0.001 to 0.003mol, specifically 0.002mol, 0.001mol or 0.003mol;
the Fe salt can be FeCl 3 ·6H 2 O；
The Co salt may be CoCl 2 ·6H 2 O；
The Ni salt can be NiCl 2 ·6H 2 O；
The Cr salt can be CrCl 3 ·6H 2 O；
The Mn salt can be MnCl 2 ·4H 2 O；
The Fe salt, co salt, ni salt, cr salt and Mn salt are mixed with respective metal chloride hydrate, and the ratio of the metal chloride hydrate to the eutectic solvent (DESs) can be specifically 0.001-0.005mol:15mL; specifically, it may be 0.002mol:15mL, 0.001mol:15mL or 0.003mol:15mL,
The heating can be performed in an oil bath at 40-120 ℃ (specifically 60 ℃);
in step 3), the reaction is performed in an oven, and the temperature of the reaction may be 150 to 300 ℃, specifically 200 to 250 ℃, the time may be 2 to 48 hours, specifically 10 to 16 hours, more specifically 210 ℃ for 12 hours, 200 ℃ for 14 hours or 250 ℃ for 10 hours.
The volume of the eutectic solvent system transferred to the reaction kettle can be 5-100 mL, and can be 15mL in particular;
in the step 4), the roasting conditions are as follows: heating to 200-400 ℃ at a heating rate of 1-10 ℃/min, and preserving heat for 0.5-6 h, wherein the heating rate can be specifically 2 ℃/min to 200 ℃, and preserving heat for 2h;
the inert atmosphere can be N 2 Or an Ar atmosphere.
The obtained high-entropy metal phosphide FeCoNiCrMnP x Consists of nano particles.
The high-entropy metal phosphide FeCoNiCrMnP prepared by the method x And also falls within the scope of the present application.
The high-entropy metal phosphide FeCoNiCrMnP x The application of the catalyst as an electrocatalytic hydrogen evolution catalyst in hydrogen production by water decomposition also belongs to the protection scope of the application.
The preparation method of the application has simple operation, low preparation cost and easy operationIndustrialized production, and the obtained high-entropy metal phosphide FeCoNiCrMnP x The appearance is regular, and the crystal form is good.
Drawings
FIG. 1 is a high entropy metal phosphide FeCoNiCrMnP prepared in example 1 of the present application x SEM photographs of (2).
FIG. 2 is a high entropy metal phosphide FeCoNiCrMnP prepared in example 1 of the present application x Is a XRD pattern of (C).
FIG. 3 shows the high entropy metal phosphide FeCoNiCrMnP prepared in examples 1-3 of the present application x HER curve of (c).
Detailed Description
The following detailed description of the application is provided in connection with the accompanying drawings that are presented to illustrate the application and not to limit the scope thereof. The examples provided below are intended as guidelines for further modifications by one of ordinary skill in the art and are not to be construed as limiting the application in any way.
The experimental methods in the following examples, unless otherwise specified, are conventional methods, and are carried out according to techniques or conditions described in the literature in the field or according to the product specifications. Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
Accurately weighing polyethylene glycol 200 and urea in a molar ratio of 2:1, and forming a eutectic solvent (DESs) in an oil bath at 60 ℃; 0.002mol FeCl is respectively and accurately weighed 3 ·6H 2 O、C℃l 2 ·6H 2 O、NiCl 2 ·6H 2 O、CrCl 3 ·6H 2 O、MnCl 2 ·4H 2 O, adding 15mL of synthesized DESs, and forming a eutectic solvent (DESs) system in an oil bath at 60 ℃; the DESs formed were transferred to a reaction vessel and placed in an oven for reaction (210 ℃ C. For 12 h). And after the reaction is finished, naturally cooling to room temperature, filtering, collecting solids, washing with ethanol and deionized water for three times respectively, and drying. Placing the dried product in a tube furnace, heating the upstream region, placing sodium metaphosphate in N 2 Baking under atmosphereFiring and roasting conditions: heating to 200 ℃ at 2 ℃/min, preserving heat for 2 hours, and cooling along with the furnace.
Example 2
Accurately weighing polyethylene glycol 200 and urea in a molar ratio of 2:1, and forming a eutectic solvent (DESs) in an oil bath at 60 ℃; accurately weigh 0.001mol FeCl 3 ·6H 2 O、C℃l 2 ·6H 2 O、NiCl 2 ·6H 2 O、CrCl 3 ·6H 2 O、MnCl 2 ·4H 2 O, adding 15mL of synthesized DESs, and forming a eutectic solvent (DESs) system in an oil bath at 60 ℃; the DESs formed were transferred to a reaction vessel and placed in an oven for reaction (reaction at 200 ℃ C. For 14 h). And after the reaction is finished, naturally cooling to room temperature, filtering, collecting solids, washing with ethanol and deionized water for three times respectively, and drying. Placing the dried product in a tube furnace, heating the upstream region, placing sodium metaphosphate in N 2 Roasting under atmosphere, wherein the roasting conditions are as follows: heating to 200 ℃ at 2 ℃/min, preserving heat for 2 hours, and cooling along with the furnace.
Example 3
Accurately weighing polyethylene glycol 200 and urea in a molar ratio of 2:1, and forming a eutectic solvent (DESs) in an oil bath at 60 ℃; accurately weigh 0.003mol FeCl 3 ·6H 2 O、C℃l 2 ·6H 2 O、NiCl 2 ·6H 2 O、CrCl 3 ·6H 2 O、MnCl 2 ·4H 2 O, adding 15mL of synthesized DESs, and forming a eutectic solvent (DESs) system in an oil bath at 60 ℃; the DESs formed were transferred to a reaction vessel and placed in an oven for reaction (reaction at 250 ℃ C. For 10 h). And after the reaction is finished, naturally cooling to room temperature, filtering, collecting solids, washing with ethanol and deionized water for three times respectively, and drying. Placing the dried product in a tube furnace, heating the upstream region, placing sodium metaphosphate in N 2 Roasting under atmosphere, wherein the roasting conditions are as follows: heating to 200 ℃ at 2 ℃/min, preserving heat for 2 hours, and cooling along with the furnace.
The product obtained in example 1 was characterized in terms of morphology. Wherein the morphology of the product is observed by SEM, and the composition and crystal form of the product are identified by XRD.
FIG. 1 shows the high entropy gold prepared in example 1 of the present applicationBelonging to phosphide FeCoNiCrMnP x As can be seen from the SEM pictures of (c), the material prepared consisted of nanoparticles;
FIG. 2 is a high entropy metal phosphide FeCoNiCrMnP prepared in example 1 of the present application x From the figure it can be seen that the XRD diffraction peaks of all samples can be attributed to CrP of No. PDF#29-0456;
table 1 shows the high entropy metal phosphide FeCoNiCrMnP prepared in example 1 of the present application x From the table, it can be seen that the synthesized high entropy metal phosphide FeCoNiCrMnP x The mole fractions of the elements Fe, co, ni, cr and M are respectively 22%,19%,21%,17% and 21%.
TABLE 1
FIG. 3 shows the high entropy metal phosphide FeCoNiCrMnP prepared in examples 1-3 of the present application x From the HER performance graph, it can be seen that the synthesized high-entropy metal phosphide FeCoNiCrMnP x Has excellent hydrogen evolution performance.
The present application is described in detail above. It will be apparent to those skilled in the art that the present application can be practiced in a wide range of equivalent parameters, concentrations, and conditions without departing from the spirit and scope of the application and without undue experimentation. While the application has been described with respect to specific embodiments, it will be appreciated that the application may be further modified. In general, this application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains.
Claims (7)
1. High-entropy metal phosphide FeCoNiCrMnP x The preparation method of (2) comprises the following steps:
1) Mixing polyethylene glycol with urea, and heating to form a eutectic solvent DESs;
2) Mixing Fe salt, co salt, ni salt, cr salt and Mn salt, adding the eutectic solvent (DESs) prepared in the step 1), and heating to form a eutectic solvent system;
3) Transferring the formed eutectic solvent system into a reaction kettle, reacting, cooling to room temperature after the reaction is finished, filtering, collecting solids, and drying;
4) Placing the dried product in a tube furnace, placing sodium metaphosphate in a heating upstream area, roasting in an inert atmosphere, and cooling along with the furnace to obtain the product;
in the step 1), the molar ratio of the polyethylene glycol to the urea is 10:1-1:1;
the polyethylene glycol is polyethylene glycol 200 and polyethylene glycol 300;
the Fe salt is FeCl 3 ·6H 2 O；
The Co salt is CoCl 2 ·6H 2 O；
The Ni salt is NiCl 2 ·6H 2 O；
The Cr salt is CrCl 3 ·6H 2 O；
The Mn salt is MnCl 2 ·4H 2 O。
2. The method according to claim 1, characterized in that: the heating is 40-120 o And C, carrying out in an oil bath pot.
3. The method according to claim 1 or 2, characterized in that: in step 2), the Fe salt, co salt, ni salt, cr salt and Mn salt are mixed in equimolar amounts of 0.001 to 0.003mol in terms of the number of moles of each metal contained.
4. A method according to claim 3, characterized in that: the Fe salt, the Co salt, the Ni salt, the Cr salt and the Mn salt are mixed by respective metal chloride hydrate, and the ratio of the metal chloride hydrate to the eutectic solvent DESs is 0.001-0.005mol:15 And (3) mL.
5. The method according to claim 1, characterized in that: in step 3), the reactionThe reaction is carried out in an oven, and the temperature of the reaction is 150-300 DEG C o And C, the time is 2-48 h.
6. The method according to any one of claims 1-5, wherein: in the step 4), the roasting conditions are as follows: 1 to 10 o C/min heating rate is increased to 200-400 o C, preserving heat for 0.5-6 hours;
the inert atmosphere is N 2 Or an Ar atmosphere.
7. The method according to any one of claims 1-6, wherein: the obtained high-entropy metal phosphide FeCoNiCrMnP x Consists of nano particles.
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| US11359266B2 (en) * | 2018-11-20 | 2022-06-14 | City University Of Hong Kong | High entropy alloy structure and a method of preparing the same |
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