CN115044933B - Ni (nickel) 12 P 5 Or Ni 2 Preparation method and application of P nano array - Google Patents

Ni (nickel) 12 P 5 Or Ni 2 Preparation method and application of P nano array Download PDF

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CN115044933B
CN115044933B CN202210498874.9A CN202210498874A CN115044933B CN 115044933 B CN115044933 B CN 115044933B CN 202210498874 A CN202210498874 A CN 202210498874A CN 115044933 B CN115044933 B CN 115044933B
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carrier
preparation
nickel
washing
drying
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CN115044933A (en
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田新龙
封苏阳
李静
邓培林
罗俊明
沈义俊
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Hainan Deep Sea New Energy Technology Co ltd
Hainan University
Sanya Research Institute of Hainan University
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Hainan Deep Sea New Energy Technology Co ltd
Hainan University
Sanya Research Institute of Hainan University
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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
    • 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
    • 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
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/061—Metal or alloy
    • 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
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • 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

Abstract

The application discloses Ni 12 P 5 Or Ni 2 A preparation method of a P nano array relates to the technical field of catalyst preparation, and comprises the following steps: pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array; preparation of Ni 12 P 5 Or Ni 2 P: coating phosphate on pretreated carrier, heating to 250-350deg.C under inert atmosphere, maintaining for 0.5-4 hr, washing the obtained product, and drying to obtain Ni 12 P 5 Support or Ni 2 P/vector. Preparation of Ni by the method of the present application 12 P 5 Support or Ni 2 The P/carrier can obtain single phosphide, the preparation method is simple and easy to control, and the P/carrier has excellent catalytic performance and stability when applied to long-term electrolysis in electrolytic seawater.

Description

Ni (nickel) 12 P 5 Or Ni 2 Preparation method and application of P nano array
Technical Field
The application relates to the technical field of catalyst preparation, in particular to Ni 12 P 5 Or Ni 2 A preparation method and application of a P nano array.
Background
Along with the development of society, people are increasingly dependent on fossil energy, and meanwhile, the environmental problem is particularly serious, and currently, a new energy source with high energy density and no pollution to the environment is sought. The research of hydrogen energy sources shows that hydrogen has the characteristics of high energy density, no pollution to environment caused by water generated by combustion, and the like. The electrolytic seawater hydrogen production has great development potential, but still has a plurality of problems, is mainly limited by the price, low yield and other disadvantages of the noble metal catalyst, and is also limited by the complicated environment of the seawater mainly comprising the selective reaction of the anode and the corrosion problem of Cl-on the surface of the electrode. Based on the above problems, transition metal catalysts have been explored for the electrolysis of seawater to produce hydrogen.
Transition metal phosphides have excellent electrochemical properties and are widely focused by researchers, and researches show that the phosphides are easy to prepare stable nano-and micro-structures, and the nano-and micro-structures have remarkably strong stability and increased catalytic activity in electrolyzed water and are excellent electrode materials. Recent studies have shown that nickel phosphide possesses a variety of compounds such as: ni (Ni) 3 P、Ni 2 P、NiP 2 、NiP、Ni 5 P 4 、Ni 7 P 3 、Ni 12 P 5 Etc. the bonding mode of nickel and phosphorus is more special, and the phosphide NiP with different proportions is obtained by a general synthesis method X Obtaining a single phosphide often requires a relatively complex synthesis formulation and scheme, which is not beneficial to the application of nickel phosphide in the electrode material direction.
Disclosure of Invention
The application provides Ni 12 P 5 Or Ni 2 The preparation method and application of the P nano array at least solve the technical problems in the prior art.
The first aspect of the application provides a Ni 12 P 5 Or Ni 2 A method of preparing a P-nanoarray, the method comprising:
pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array;
preparation of Ni 12 P 5 Or Ni 2 P: coating phosphate on pretreated carrier, heating to 250-350deg.C under inert atmosphere, maintaining for 0.5-4 hr, washing the obtained product, and drying to obtain Ni 12 P 5 Support or Ni 2 P/vector.
In one embodiment, the carrier is nickel foam, nickel-copper foam or nickel-iron foam.
In one embodiment, the carrier pretreatment comprises:
ultrasonic washing the carrier with acid solution for 10-30min;
ultrasonic washing the carrier with organic solvent for 5-20min;
and drying the washed carrier to obtain the pretreated carrier.
In one embodiment, the phosphate comprises one of orthophosphate, hypophosphite, or phosphite.
In one embodiment, the mass ratio of phosphate to carrier is 3-6:1.
In a second aspect, the application provides a NiSe 2 /TiN@Ni 12 P 5 Preparation method of a Supported catalyst, ni 12 P 5 The carrier is Ni according to the above 12 P 5 Or Ni 2 The preparation method of the P nano array comprises the following steps:
NiCl is added 2 -6H 2 O、SeO 2 And TiN are uniformly dissolved in the deionized water to obtain a mixed solution;
at the place of will beAdding the mixed solution into polytetrafluoroethylene lining, heating to 130-160deg.C at 1-10deg.C/min, maintaining for 5 hr, filtering, washing, and drying to obtain NiSe 2 /TiN@Ni 12 P 5 A supported catalyst.
In a third aspect the application provides a NiSe 2 /TiN@Ni 2 Preparation method of P/carrier catalyst, ni 2 The P/carrier is Ni according to the above 12 P 5 Or Ni 2 The preparation method of the P nano array comprises the following steps:
NiCl is added 2 -6H 2 O、SeO 2 And TiN are uniformly dissolved in the deionized water to obtain a mixed solution;
adding the mixed solution into a polytetrafluoroethylene lining, heating to 130-160 ℃ at 1-10 ℃/min, preserving heat for 5h, filtering, washing and drying the obtained product to obtain NiSe 2 /TiN@Ni 2 P/supported catalyst.
In a fourth aspect of the application, there is provided Ni 3 Se 2 /MoO 2 @Ni 12 P 5 Preparation method of a Supported catalyst, ni 12 P 5 The carrier is Ni according to the above 12 P 5 Or Ni 2 The preparation method of the P nano array comprises the following steps:
mixing ethylene glycol with choline chloride, and stirring at 50-100deg.C to obtain eutectic solvent;
then NiCl is added into the eutectic solvent 2 -6H 2 O、(NH 4 ) 2 MoO 4 、C 6 H 8 O 7 And SeO 2 Stirring again to obtain a deposition solution;
the oxidation-reduction reaction is carried out on the surface of the working electrode under the three-electrode system by an electrodeposition method to obtain Ni 3 Se 2 /MoO 2 @Ni 12 P 5 A supported catalyst.
In one embodiment, the electrodeposition method includes: with Ni 12 P 5 The carrier is a working electrode, the platinum column is a counter electrode, the silver wire is a reference electrode,deposition potential: 0.85V, deposition of 10C cm -2. The catalyst electrode surface was then rinsed with deionized water and finally dried.
A fifth aspect of the present application provides a Ni 12 P 5 Support or Ni 2 Application of P/carrier in electrolysis of seawater to prepare Ni 12 P 5 Support or Ni 2 The P/carrier is used as an anode catalyst for oxygen evolution reaction of the electrolyzed seawater.
In the above-described aspect of the present application, ni is produced by the method of the present application 12 P 5 Support or Ni 2 The P/carrier can obtain single phosphide, the preparation method is simple and easy to control, and the P/carrier has excellent catalytic performance and stability when applied to long-term electrolysis in electrolytic seawater.
Drawings
FIG. 1 is Ni obtained in example 1 12 P 5 XRD pattern of/NF;
FIG. 2 is Ni obtained in example 1 12 P 5 SEM and TEM images of/NF;
FIG. 3 is Ni obtained in example 1 12 P 5 Performing LSV test on NF under different systems;
FIG. 4 is Ni obtained in example 1 12 P 5 200h long term stability profile of/NF;
FIG. 5 is Ni obtained in example 1 12 P 5 LSV performance comparison graphs of materials before and after 200 hours of NF electrolysis;
FIG. 6 is an XRD pattern for example 1 after 200 hours of electrolysis;
FIG. 7 is a LSV test performed on different materials prepared in example 4;
FIG. 8 shows LSV testing performed on different materials prepared in example 5.
Detailed Description
In order to make the objects, features and advantages of the present application more comprehensible, the technical solutions according to the embodiments of the present application will be clearly described in the following with reference to the accompanying drawings, and it is obvious that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The application provides Ni 12 P 5 Or Ni 2 A method of preparing a P-nanoarray, the method comprising:
step S1, pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array;
step S2, preparing Ni 12 P 5 Or Ni 2 P: coating phosphate on pretreated carrier, heating to 250-350deg.C under inert atmosphere, maintaining for 0.5-4 hr, washing the obtained product, and drying to obtain Ni 12 P 5 Support or Ni 2 P/vector.
In one embodiment, wherein the carrier is Nickel Foam (NF), nickel-copper foam (NCF), or nickel-iron foam (NIF).
In one embodiment, the carrier pretreatment comprises:
ultrasonic washing the carrier with acid solution for 10-30min;
ultrasonic washing the carrier with organic solvent for 5-20min;
and drying the washed carrier to obtain the pretreated carrier.
In one embodiment, the phosphate comprises one of orthophosphate, hypophosphite, or phosphite.
In one embodiment, the mass ratio of phosphate to carrier is 3-6:1.
The present application will be described in detail with reference to specific examples.
Example 1
Ni (nickel) 12 P 5 A method of preparing a nanoarray, the method comprising:
step S11, pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array;
wherein the carrier is foam Nickel (NF), cutting the foam nickel into 1cm multiplied by 2cm, respectively ultrasonic washing with 1.0mol/L hydrochloric acid solution and absolute ethyl alcohol for 20min and 10min, removing oxide and organic impurities on the surface of the foam nickel, placing the washed foam nickel in a vacuum drying oven at 40 ℃, and drying for 2h.
Step S12, ni is prepared 12 P 5 Nano array: putting 4 pieces of pretreated foam nickel into a porcelain boat, weighing 1g of anhydrous sodium hypophosphite to cover the foam nickel, putting the porcelain boat into a tube furnace, heating to 300 ℃ under the protection of nitrogen, and preserving heat for 2 hours; wherein the temperature rising interval is 20-300 ℃, the temperature rising rate is 5 ℃/min, and the flow rate of the introduced nitrogen is as follows: 2L/min; repeatedly washing the obtained product with deionized water, placing in a vacuum drying oven at 40deg.C, and drying for 12 hr to obtain Ni 12 P 5 The nano array is marked as Ni 12 P 5 /NF。Ni 12 P 5 NF characterization and performance test:
(1) XRD characterization: as shown in FIG. 1, the diffraction pattern obtained by XRD analysis is shown for Ni 12 P 5 The presence of NF and Ni on the diffraction pattern of/NF 12 P 5 Is a characteristic peak of (2);
(2) Electron microscope image: ni was measured using a Scanning Electron Microscope (SEM) and a Transmission Electron Microscope (TEM) 12 P 5 Characterization of the micro-morphology of/NF, as shown in FIG. 2, FIG. 2 (a) is Ni 12 P 5 SEM image of/NF, having a nanoarray structure; FIG. 2 (b) is Ni 12 P 5 TEM image of/NF.
(3)Ni 12 P 5 Catalytic performance testing of/NF with different electrolyte systems: ni (Ni) 12 P 5 The NF catalyst was tested in a three electrode system and simultaneously in an alkaline solution with 1.0M KOH and 1.0M KOH plus 0.5M NaCl as electrolyte, as shown in FIG. 3, the performance of the test system tested in 1.0M KOH plus 0.5M NaCl electrolyte was better than that of the test system tested in 1.0M KOH at 100mA cm -2 Only 233mV overpotential is needed, which is comparable to noble metals.
(4)Ni 12 P 5 Stability test of NF: as shown in FIGS. 4 and 5, when the current density reaches 100mA cm -2 Time-resolved seawaterThe potential of the electrolytic fresh water is 91mV lower than that of the electrolytic fresh water, and when the current density reaches 100mA cm in the electrolytic seawater -2 Only 233mV overpotential was required, and the material had excellent stability, and the final product Ni was tested in a 1.0M KOH plus 0.5M NaCl system 12 P 5 Stability of/NF, it can be seen that at 100mA cm -2 After 200 hours of continuous electrolysis, the potential is not increased but reduced by 22.9mV. Analysis showed that the XRD pattern of the catalyst after 200 hours of electrolysis, as shown in FIG. 6, resulted in surface reconstruction of the catalyst surface to Ni (OH) after electrolysis 2 。
Example 2
Ni (nickel) 2 A method of preparing a P-nanoarray, the method comprising:
step S21, pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array;
wherein the carrier is foam Nickel (NF), cutting the foam nickel into 1cm multiplied by 2cm, respectively ultrasonically washing for 10min and 5min by using 1.0mol/L hydrochloric acid solution and propanol, removing oxide and organic impurities on the surface of the foam nickel, and placing the washed foam nickel in a vacuum drying oven at 40 ℃ for drying for 2h.
Step S22, ni is prepared 2 P nanoarray: putting 5 pieces of pretreated foam nickel into a porcelain boat, weighing 1g of anhydrous sodium hypophosphite to cover the foam nickel, putting the porcelain boat into a tube furnace, heating to 250 ℃ under the protection of nitrogen, and preserving heat for 2 hours; wherein the temperature rising interval is 20-250 ℃, the temperature rising rate is 2.5 ℃/min, and the flow rate of the introduced nitrogen is as follows: 2L/min; repeatedly washing the obtained product with deionized water, placing in a vacuum drying oven at 40deg.C, and drying for 12 hr to obtain Ni 2 The P nano array is marked as Ni 2 P/NF。
Example 3
Ni (nickel) 12 P 5 A method of preparing a nanoarray, the method comprising:
step S31, pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array;
wherein the carrier is foam Nickel Copper (NCF), cutting the foam nickel copper into 1cm multiplied by 2cm, respectively ultrasonically washing for 30min and 20min by using 1.0mol/L hydrochloric acid solution and absolute ethyl alcohol to remove oxide and organic impurities on the surface of the foam nickel copper, and placing the washed foam nickel copper in a vacuum drying oven at 40 ℃ for drying for 2h.
Step S32, ni preparation 12 P 5 Nano array: putting 4 pieces of pretreated foam nickel-copper into a porcelain boat, weighing 1g of sodium orthophosphate to cover the foam nickel-copper, putting the porcelain boat into a tube furnace, heating to 350 ℃ under the protection of nitrogen, and preserving the temperature for 0.5h; wherein the temperature rising interval is 20-350 ℃, the temperature rising rate is 5 ℃/min, and the flow rate of the introduced nitrogen is as follows: 2L/min; repeatedly washing the obtained product with deionized water, placing in a vacuum drying oven at 40deg.C, and drying for 12 hr to obtain Ni 12 P 5 The nano array is marked as Ni 12 P 5 /NCF。
Example 4
NiSe 2 /TiN@Ni 12 P 5 Process for preparing a/NF catalyst wherein Ni 12 P 5 The preparation method of/NF was the same as in example 1, and the method included:
step S41, 2.3mmol L -1 NiCl 2 -6H 2 O、10mmol L -1 SeO 2 And 0.16mmol L -1 Uniformly dissolving TiN in 100mL of deionized water to obtain a mixed solution;
step S42, adding the mixed solution obtained in the step S41 into a polytetrafluoroethylene lining, heating to 140 ℃ at a heating rate of 5 ℃/min, and preserving heat for 5 hours to obtain NiSe 2 /TiN@Ni 12 P 5 a/NF catalyst.
Performance test: niSe 2 /TiN@Ni 12 P 5 NF catalyst, ni 12 P 5 UOR system with/NF catalyst and NF application to urea-assisted oxidation, LSV curve is shown in FIG. 7, where Ni 12 P 5 catalyst/NF at 100mA cm -2 Is only 1.447V; niSe 2 /TiN@Ni 12 P 5 catalyst/NF at 500mA cm -2 Is 1.962V.
Example 5
Ni (nickel) 3 Se 2 /MoO 2 @Ni 12 P 5 Process for preparing a/NF catalyst wherein Ni 12 P 5 The preparation method of the/NF is the same as in example 1, and comprises the following steps:
step S51, mixing ethylene glycol and choline chloride according to a mass ratio of 2:1, and stirring at 75 ℃ to obtain a eutectic solvent;
step S52, adding 0.25mol/L NiCl into the eutectic solvent 2 -6H 2 O、0.05mol/L(NH 4 ) 2 MoO 4 、0.2mol/L C 6 H 8 O 7 And 20mmol/L SeO 2 Stirring again to obtain a deposition solution;
step S53, carrying out oxidation-reduction reaction on the surface of the working electrode under a three-electrode system by an electrodeposition method to obtain Ni 3 Se 2 /MoO 2 @Ni 12 P 5 a/NF catalyst. The method comprises the following steps: with Ni 12 P 5 NF is the working electrode, platinum column is the counter electrode and silver wire is the reference electrode, deposition potential: 0.85V, deposition of 10C cm -2. Then washing the surface of the catalyst electrode with deionized water at 55 ℃, and finally vacuum drying to obtain Ni 3 Se 2 /MoO 2 @Ni 12 P 5 a/NF catalyst.
Performance test: ni (Ni) 3 Se 2 /MoO 2 @Ni 12 P 5 NF catalyst, ni 12 P 5 Application of NF catalyst and NF to UOR System for Urea-assisted Oxidation, LSV Curve is shown in FIG. 8, when industry Standard current Density of 500mA cm is reached at Urea oxidation -2 Time Ni 3 Se 2 /MoO 2 @Ni 12 P 5 the/NF catalyst only requires 1.797V.
The basic principles of the present application have been described above in connection with specific embodiments, however, it should be noted that the advantages, benefits, effects, etc. mentioned in the present application are merely examples and not intended to be limiting, and these advantages, benefits, effects, etc. are not to be considered as essential to the various embodiments of the present application. Furthermore, the specific details disclosed herein are for purposes of illustration and understanding only, and are not intended to be limiting, as the application is not necessarily limited to practice with the above described specific details.
Terms such as "comprising," "including," "having," and the like, as used herein, are open-ended terms that include, but are not limited to, and are used interchangeably therewith. The terms "or" and "as used herein refer to and are used interchangeably with the term" and/or "unless the context clearly indicates otherwise. The term "such as" as used herein refers to, and is used interchangeably with, the phrase "such as, but not limited to.
It is also pointed out that in the method according to the application, the steps can be decomposed and/or recombined, which are to be regarded as equivalents of the application.
The previous description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other aspects without departing from the scope of the application. Thus, the present application is not intended to be limited to the aspects shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The foregoing description has been presented for purposes of illustration and description. Furthermore, this description is not intended to limit embodiments of the application to the form disclosed herein. Although a number of example aspects and embodiments have been discussed above, a person of ordinary skill in the art will recognize certain variations, modifications, alterations, additions, and subcombinations thereof.

Claims (2)

1. NiSe 2 /TiN@Ni 12 P 5 Process for the preparation of a supported catalyst, characterized in that
In that Ni is used as 12 P 5 The preparation method comprises the following steps of:
NiCl is added 2 -6H 2 O、SeO 2 And TiN are uniformly dissolved in the deionized waterObtaining a mixed solution in the child water;
adding the mixed solution and the matrix into a polytetrafluoroethylene lining, heating to 130-160 ℃ at 1-10 ℃/min, preserving heat for 5-h, filtering, washing and drying the obtained product to obtain NiSe 2 /TiN@Ni 12 P 5 A supported catalyst;
wherein the Ni 12 P 5 The preparation method of the carrier comprises the following steps:
pretreatment of a carrier: removing oxide and organic impurities on the surface of a carrier, wherein the carrier is used for providing a nickel source and also used for providing a space for in-situ growth of the nano array; the carrier is foam nickel, foam nickel-copper alloy or foam nickel-iron alloy;
preparation of Ni 12 P 5 : coating phosphate on the pretreated carrier, and then coating the carrier on an idler
Heating to 300-350deg.C under an air atmosphere, maintaining the temperature for 0.5-4 hr, washing the obtained product, and drying to obtain Ni 12 P 5 A carrier;
the phosphate comprises one of orthophosphate, hypophosphite or phosphite;
the mass ratio of the phosphate to the carrier is 3-6:1.
2. The method of claim 1, wherein the carrier pretreatment comprises:
ultrasonic washing the carrier with acid solution for 10-30min;
ultrasonic washing the carrier with organic solvent for 5-20min;
and drying the washed carrier to obtain the pretreated carrier.
CN202210498874.9A 2022-05-09 2022-05-09 Ni (nickel) 12 P 5 Or Ni 2 Preparation method and application of P nano array Active CN115044933B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103263939A (en) * 2013-06-08 2013-08-28 安徽工业大学 Method for preparing Ni2P catalyst
CN111701607A (en) * 2020-06-15 2020-09-25 西北大学 MnCo2O4@Ni2P/NF difunctional full-hydrolysis catalyst and preparation method and application thereof
CN113684501A (en) * 2021-07-19 2021-11-23 中国海洋大学 Nickel-iron-based phosphide electrocatalytic material and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103263939A (en) * 2013-06-08 2013-08-28 安徽工业大学 Method for preparing Ni2P catalyst
CN111701607A (en) * 2020-06-15 2020-09-25 西北大学 MnCo2O4@Ni2P/NF difunctional full-hydrolysis catalyst and preparation method and application thereof
CN113684501A (en) * 2021-07-19 2021-11-23 中国海洋大学 Nickel-iron-based phosphide electrocatalytic material and preparation method and application thereof

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"Heterogeneous structured Ni3Se2/MoO2@Ni12P5 catalyst for durable urea oxidation reaction";S. Feng等;《MATERIALS TODAY PHYSICS》;第23卷;第1-7页 *
"Hierarchical self-supported NiSe2/TiN@Ni12P5 on nickel foam for the urea oxidation reaction";Suyang Feng等;《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》;第47卷(第87期);第36814-36822页 *
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