CN113751037B - Metal carbide Fe combined with organic metal framework 3 C/Mo 2 Preparation and use of C - Google Patents

Metal carbide Fe combined with organic metal framework 3 C/Mo 2 Preparation and use of C Download PDF

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CN113751037B
CN113751037B CN202010492146.8A CN202010492146A CN113751037B CN 113751037 B CN113751037 B CN 113751037B CN 202010492146 A CN202010492146 A CN 202010492146A CN 113751037 B CN113751037 B CN 113751037B
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CN113751037A (en
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李林林
于涵芝
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Nanjing University of Aeronautics and Astronautics
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/22—Carbides
    • B01J35/33—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/086—Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
    • 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
    • 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 invention discloses a preparation method and application of metal carbide combined with a metal organic framework, which has a unique nano cube and nano sheet composite structure. The preparation method of the material comprises the following steps: 1) Firstly, compounding an iron salt inorganic compound and an organic high molecular material to obtain Fe-MOFs of an iron-based metal organic framework; 2) Mixing Fe-MOFs and a molybdate according to a certain mass ratio, uniformly stirring, and naturally evaporating and drying water at 60 ℃; 3) Then uniformly dispersing the sample prepared in the step 3) and dopamine in an alkaline solution according to a certain mass ratio, stirring, collecting the precipitate, and centrifugally drying; 4) Finally, annealing the dried sample prepared in the step 3) in a nitrogen atmosphere to obtain a final product Fe 3 C/Mo 2 C. The electrocatalyst prepared by the invention is applied to Oxygen Evolution Reaction (OER) in electrolyzed water, compared with commercialized RuO 2 、IrO 2 And most other electrocatalysts, the material prepared by the invention has higher reaction activity, catalytic performance and cycling stability.

Description

Metal carbide Fe combined with organic metal framework 3 C/Mo 2 Preparation and use of C
Technical Field
The invention relates to the field of organic metal frameworks and electrocatalysis, in particular to preparation of organic metal frameworks, preparation of an electrode material for electrocatalysis oxygen evolution and performance exploration of the electrode material.
Background
Future economic and strategic developments in human society leave sustainable energy systems. As a renewable alternative energy source to fossil fuels, hydrogen energy has clean, efficient, and friendly characteristics, and can play an important role in green energy and chemical conversion. Recently, more and more hydrogen evolution reaction catalysts have been reported, and in addition, they have conducted extensive studies on electrochemical water decomposition. Electrochemical water splitting is divided into two half-reactions: hydrogen Evolution Reaction (HER), oxygen Evolution Reaction (OER), wherein the development of electrochemical water splitting is severely limited due to higher overpotential and poorer cycle performance in the electrochemical reaction of OER.
The effective oxygen evolution catalysts found so far are: (1) Noble metal oxides, e.g. IrO 2 And RuO 2 Etc.; (2) Perovskite materials having catalytic activity, e.g. LaCoO 4 And PrCoO 4 Etc.; (3) Metal oxides, e.g. Co 3 O 4 And NiO 2 And so on. These materials are materials with excellent performance in the electrolytic water oxygen evolution reaction, but still have some problems which cannot be solved in a short time, such as expensive precious metals, low reserves, low conductivity of perovskite materials and the like. It has been shown that the activity and cycling stability of electrocatalysts in hydrolysis reactions are related to their microscopic crystal size structure. In recent years, research reports about Metal Organic Framework (MOF) materials have been widely applied to electrochemical hydrolysis reactions. The materials have a hollow structure, high material compatibility and extremely high size controllability, so that the materials can achieve high activity, good conductivity and stable cycle performance in a catalytic reaction. However, the metal organic framework has low catalytic performance and needs to be further compounded with other materials.
Therefore, it is of great significance to research and develop an OER electrode catalyst with higher activity, conductivity and low price and abundant reserves.
Disclosure of Invention
The invention provides an oxygen evolution reaction electrocatalyst combined with a metal organic framework, which aims to solve the problem that a common catalyst in the prior art is low in catalytic performance in the OER reaction process.
The invention also provides an oxygen evolution reaction electrocatalyst combined with the organic metal framework, which is prepared by the method and has a unique nano cube and nano sheet composite structure and OER activity.
The invention also provides the oxygen evolution reaction electrocatalyst combined with the organic metal framework, which is prepared by the method and has good conductivity and cycling stability.
The experimental scheme adopted by the invention for solving the technical problems is as follows:
an electrocatalyst for oxygen evolution reactions, characterized in that said catalyst is a composite material consisting of a metal organic framework and a metal carbide; the metal carbide of the material is interacted on the surface of the composite metal organic framework through molecules to form a lamellar structure and be compounded with a cubic structure with a certain shape.
In the technical scheme, the metal carbide is prepared by coating and calcining metal salt carbon.
The oxygen evolution reaction electrocatalyst is prepared by firstly preparing a required metal organic framework, preparing a precursor from the metal organic framework and metal salt with different mass ratios, and then carrying out heat treatment on the precursor to obtain a product of the lamellar structure and a cubic structure with a certain shape.
In the above technical scheme, the ratio of the metal organic framework to the metal salt is 2: 1, 1: 2, 1: 4.
A preparation method of an oxygen evolution reaction electrocatalyst combined with a metal organic framework comprises the following steps:
(1) Compounding an iron salt inorganic compound and an organic polymer material, uniformly stirring, heating at constant temperature, centrifuging, collecting precipitate, cleaning and drying to obtain the Fe-MOFs of the iron-based metal organic framework.
(2) Mixing the iron-based metal organic frame prepared in the step (1) with molybdate according to a certain mass ratio, then carrying out ultrasonic dispersion, and then stirring at a certain temperature until water is evaporated, so that the molybdate is coated on the surface of Fe-MOFs to form Fe-MOFs/molybdate.
(3) And (3) uniformly dispersing the dried sample obtained in the step (2) and dopamine in an alkaline solution according to a certain mass ratio, stirring for a certain time, finally collecting and cleaning the precipitate, and drying in vacuum.
(4) And (4) annealing the product obtained in the step (3) at a high temperature for a certain time under the protection of a nitrogen atmosphere to obtain a final product.
In the above technical scheme, the iron salt selected in step (1) includes ferric nitrate nonahydrate, ferric chloride hexahydrate, potassium ferricyanide, and the like, and the organic polymer material includes polyvinylpyrrolidone, terephthalic acid, trimesic acid, and the like. Preferably, potassium ferricyanide and polyvinylpyrrolidone are used in the present invention.
In the step (1), the constant temperature heating is carried out in water bath for 30-50 hours at 60-80 ℃. The centrifugal speed is 8000-10000 r/l, and the time is 8-10 min. Preferably, the method adopts a thermostatic water bath with the temperature of 80 ℃ for 48 hours, and centrifuges the mixture for 8 minutes at 10000 revolutions.
In the technical scheme, the proportion of Fe-MOFs to molybdate in the step (2) is 2: 1, 1: 2 and 1: 4. Preferably, the molybdate adopted by the invention is ammonium molybdate, and the ratio is 1: 2.
In the step (2), the ultrasonic dispersion time is 30-60 minutes, and the stirring temperature is 60-80 ℃. Preferably, the invention adopts ultrasonic dispersion for 30 minutes, and stirring evaporation is carried out at 60 ℃.
In the technical scheme, the mass ratio of the sample to the dopamine in the step (3) is 90-105: 45-60, and the mass ratio of the sample to the alkaline solution is 90-105: 120-140. The alkaline solution is generally Tris buffer solution, the pH value of the solution is 7.0-9.0, and the stirring time is 20-30 hours. Preferably, the mass ratio of the sample to the dopamine is 90: 45, the mass ratio of the sample to the alkaline solution is 90: 120, the pH value of the solution is 8.8, and the stirring time is 24 hours.
And (4) centrifugally collecting and cleaning precipitates in the step (3), wherein the centrifugal rotating speed is 8000-10000 r, the centrifugal time is 8-15 minutes, and the vacuum drying temperature is 60 ℃ for 10-12 hours. Preferably, the invention adopts the centrifugal rotating speed of 8000 min and vacuum drying at 60 ℃ for 12 h.
In the technical scheme, the annealing temperature of the sample in the step (4) is 700-900 ℃, and the time is 1-3 hours. Preferably, the annealing temperature adopted by the invention is 800 ℃ and the time is 2 hours.
The beneficial effects of the invention are:
the invention provides a simple and convenient method for synthesizing the material with the unique nano cubic block and nano lamellar composite structure, the cubic blocks have the same size, uniform distribution and uniform lamellar thickness, and the structural characteristics of the metal organic framework are fully utilized. Compared with the traditional electrocatalyst and the commercialized RuO 2 、IrO 2 The invention prepares Fe 3 C/Mo 2 C has higher catalytic activity, good stability and structural novelty. And the raw material reserves are abundant, the cost is lower, and the problems of high cost, scarce resources and the like of the noble metal catalyst are solved to a certain extent.
Drawings
FIG. 1 shows Fe obtained in example 1 of the present invention 3 C/Mo 2 X-ray diffraction pattern (XRD) of C.
FIG. 2 shows Fe obtained in example 1 of the present invention 3 C/Mo 2 Electron Micrograph (SEM) of C.
FIG. 3 shows Fe obtained in example 1 of the present invention 3 C/Mo 2 High resolution transmission electron microscopy (HR-TEM) image of C.
FIG. 4 shows Fe prepared by the present invention 3 C/Mo 2 C、Fe 3 C、Mo 2 C with commercial RuO 2 OER polarization profile of the catalyst.
FIG. 5 shows Fe prepared by the present invention 3 C/Mo 2 C、Fe 3 C、Mo 2 C with commercial RuO 2 The Tafel profile of the catalyst in the OER reaction corresponds.
Detailed Description
Example 1
131.7mg of K 3 [Fe(CN) 6 ]And 3.0g PVP (K30) was dissolved in 40ml 0.01M HCl solution and stirred for 30 minutes to disperse it homogeneously. Then putting into a hot water bath, and heating at the constant temperature of 80 ℃ for 48h. And after the constant temperature is finished, centrifuging to collect precipitates, wherein the centrifugal speed is 10000 r, and the centrifugal time is 8 minutes. The sample was washed three times with deionized water and two times with ethanol. And drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain the Fe-MOFs.
100mg of pre-prepared Fe-MOFs was mixed with 200mg (NH) 4 ) 6 Mo 7 O 2 ·4H 2 O is dispersed in 15ml of water and dispersed by ultrasonic. And then stirring the solution at 60 ℃, and coating a layer of molybdate on the surface of the Fe-MOFs after water is evaporated. The dried solid powder and dopamine were uniformly dispersed in Tris base buffer at pH 8.8 and stirred for 24 hours. Finally collecting and cleaning the precipitate, drying the precipitate, and calcining the dried precipitate for 2 hours at 800 ℃ in a nitrogen atmosphere to obtain black powder Fe 3 C/Mo 2 And C, a composite material.
Example 2
The procedure is as in example 1, except that Fe-MOFs and (NH) 4 ) 6 Mo 7 O 2 ·4H 2 The amount of O is changed to 100 mg: 100mg, and the O is dispersed in 10ml of water.
Example 3
The procedure is as in example 1, except that Fe-MOFs and (NH) 4 ) 6 Mo 7 O 2 ·4H 2 The amount of O was changed to 100 mg: 400mg, and dispersed in 30ml of water.
Example 4
The procedure is as in example 1, except that Fe-MOFs and (NH) 4 ) 6 Mo 7 O 2 ·4H 2 The amount of O was changed to 200mg to 100mg, dispersed in 15ml of water.
Example 5
The procedure of example 1 was followed except that the temperature of the final nitrogen heat treatment was changed to 700 ℃.
Example 6
The procedure was followed as in example 1, except that the temperature of the final nitrogen heat treatment was changed to 900 ℃.
Example 7
The procedure is as in example 1, except that the pH of the Tris base buffer is changed to 7.4.
Example 8
The procedure is as in example 1, except that the pH of the Tris base buffer is changed to 8.0.
Comparative example 1
131.7mg of K 3 [Fe(CN) 6 ]And 3.0g PVP (K30)) Dissolved in 40ml of 0.01M HCl solution and stirred for 30 minutes to disperse it homogeneously. Then placing into a hot water bath, and heating at 80 ℃ for 48h. And after the constant temperature is finished, centrifuging and collecting the precipitate, wherein the centrifugal speed is 10000 revolutions, and the centrifugal time is 8 minutes. The sample was washed three times with deionized water and two times with ethanol. And drying in a vacuum drying oven at 60 ℃ for 12 hours to obtain Fe-MOFs.
The prepared 0.4g Fe-MOFs and 0.2g dopamine were uniformly dispersed in Tris base buffer solution of pH 8.8, stirred for 24 hours, then the washed precipitate was collected and dried in a vacuum oven at 60 ℃ for 10 hours. Finally, the product is heated and treated for 2 hours in nitrogen at 800 ℃ to obtain a solid sample Fe 3 C。
Comparative example 2
0.8g of (NH) 4 ) 6 Mo 7 O 2 ·4H 2 O and 0.2g of dopamine are uniformly dispersed in Tris alkali buffer solution with the pH value of 8.8, and the sample is uniformly dispersed by ultrasonic treatment for 60 minutes. Then stirring and reacting for 6 hours, centrifugally separating for 10min at the rotating speed of 10000 r/min, washing the solid by water, and drying for 12 hours in a vacuum drying oven at 60 ℃. Finally, the product is heated and treated for 2 hours in nitrogen at 800 ℃ to obtain a solid sample Mo 2 C。
Test example 1
Fe obtained in Experimental example 1 3 C/Mo 2 C and Fe obtained in comparative examples 1 and 2 3 C、Mo 2 C, carrying out an X-ray diffraction (XRD) test, wherein the test result is shown in figure 1, and the obtained samples are target products by comparing the XRD pattern of the sample with a standard JCPDF card.
Detection example 2
Fe obtained in example 1 3 C/Mo 2 And C, respectively carrying out Scanning Electron Microscope (SEM) and high-resolution transmission electron microscope (HR-TEM) tests, wherein the test results are respectively shown in the figure 2 and the figure 3. As can be seen from FIG. 2, the catalyst prepared by the invention is a composite structure of nano-cubic blocks and nano-lamellar, the cubic blocks are regular in shape and uniform in size, the size is about 200nm, and the lamellar structure is uniform in thickness and distribution. From fig. 3, it can be seen that in the high-resolution transmission electron microscope (HR-TEM) image, the existence of crystal images of the two substances is clearly shown.
Detection example 3
Fe obtained in example 1 3 C/Mo 2 C. Fe obtained in comparative examples 1 and 2 3 C、Mo 2 C and commercial RuO 2 The catalyst powder was used as a test sample, and an electrode was prepared as follows:
mixing 950 μ L of anhydrous ethanol and 50 μ L of 5% Nafion solution, adding 5mg of sample, performing ultrasonic dispersion for 30min to obtain liquid sample, dropping 10 μ L of sample on disc electrode (ring disc electrode), and air drying to obtain electrode with catalyst loading of 40mg cm -2 。
And carrying out OER electrochemical performance test on the prepared electrode in a 1.0M KOH solution by adopting a three-electrode system. Measured Fe 3 C/Mo 2 C. Fe3C, mo2C and commercial RuO 2 The OER polarization curve of the catalyst is shown in FIG. 4. As can be seen from FIG. 4, when 10mA cm is reached -2 Current density of (1), fe 3 C/Mo 2 The overpotential required for C is 275mV, lower than that of Fe 3 C、Mo 2 C and commercial RuO 2 This indicates that it has superior activity in catalyzing OER in alkaline media.
As can be seen from FIG. 5, fe 3 C/Mo 2 Tafel slope fit to C was 36.18mV dec -1 Is significantly less than Fe 3 C(66.23mV dec -1 )、 Mo 2 C(102.51mV dec -1 ) And RuO 2 (50.82mV dec -1 ) And shows better OER dynamic performance.
The above LSVs and Tafel results collectively demonstrate that this metal organic framework-bound oxygen evolution reaction electrocatalyst, fe 3 C/Mo 2 The high activity of C in catalyzing oxygen evolution indicates that C can be used as an excellent electrode material for electrochemical oxygen evolution reaction.

Claims (2)

1. Metallic carbide Fe 3 C/Mo 2 The preparation method of the material C comprises the following steps:
1) 131.7mg of K 3 [Fe(CN) 6 ]And 3.0g PVP in 40ml 0.01M HCl solution, stirring 3Uniformly dispersing the mixture in hot water bath for 0 minute, heating the mixture at the constant temperature of 80 ℃ for 48 hours, centrifuging the mixture after the constant temperature is finished, collecting precipitates, centrifuging the precipitates at the rotation speed of 10000 r/min for 8 minutes, washing the precipitates with three times of deionized water and two times of ethanol, and drying the precipitates in a vacuum drying oven at the temperature of 60 ℃ for 12 hours to obtain an intermediate;
2) 100mg of the intermediate prepared in step 1) are admixed with 200mg of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 Dispersing O in 15ml of water, performing ultrasonic dispersion, stirring the solution at 60 ℃, wrapping a layer of molybdate on the surface of an intermediate after water is evaporated, uniformly dispersing dried solid powder and dopamine in Tris buffer solution with the pH of 8.8, stirring for 24 hours, collecting and cleaning precipitates, drying, and calcining at 800 ℃ in nitrogen atmosphere for 2 hours to obtain black powder Fe 3 C/Mo 2 C, a composite material;
preparation of the resulting Fe 3 C/Mo 2 The C composite material is a structure compounded by nano cubic blocks and nano lamellar, the cubic blocks are regular in shape and uniform in size, the size is about 200nm, and the lamellar structure is uniform in thickness and distribution.
2. A metal carbide Fe prepared by the method of claim 1 3 C/Mo 2 The application of the material C in electrocatalytic oxygen evolution reaction.
CN202010492146.8A 2020-06-01 2020-06-01 Metal carbide Fe combined with organic metal framework 3 C/Mo 2 Preparation and use of C Active CN113751037B (en)

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