CN110773212A - Iron carbide-porous carbon composite material and preparation method and application thereof - Google Patents
Iron carbide-porous carbon composite material and preparation method and application thereof Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 119
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 81
- 239000002131 composite material Substances 0.000 title claims abstract description 73
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 229910001567 cementite Inorganic materials 0.000 claims abstract description 23
- 239000011148 porous material Substances 0.000 claims abstract description 9
- 239000011258 core-shell material Substances 0.000 claims abstract description 8
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 6
- 238000004146 energy storage Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- YFOOEYJGMMJJLS-UHFFFAOYSA-N 1,8-diaminonaphthalene Chemical compound C1=CC(N)=C2C(N)=CC=CC2=C1 YFOOEYJGMMJJLS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000002105 nanoparticle Substances 0.000 claims description 12
- -1 1, 8-diaminonaphthalene ethanol Chemical compound 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 3
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 3
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 10
- 238000003763 carbonization Methods 0.000 abstract description 8
- 229920000642 polymer Polymers 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 230000009467 reduction Effects 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 7
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- 238000012360 testing method Methods 0.000 description 6
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- 229910052757 nitrogen Inorganic materials 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GNTONLAAGMSLOW-UHFFFAOYSA-N C(C)O.[Fe].C(C)(=O)CC(C)=O Chemical compound C(C)O.[Fe].C(C)(=O)CC(C)=O GNTONLAAGMSLOW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
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- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
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- 150000003624 transition metals Chemical class 0.000 description 1
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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—
-
- B01J35/398—
-
- B01J35/40—
-
- B01J35/615—
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- B01J35/643—
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
-
- 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
- Y02E60/50—Fuel cells
Abstract
The invention relates to an iron carbide-porous carbon composite material and a preparation method and application thereof, belonging to the technical field of nano materials. When the composite material is prepared, the metal-doped high polymer is taken as a template and is obtained through one-step carbonization. In the material, the iron carbide with the core-shell structure is coated in the porous carbon, so that the corrosion resistance of the material is further improved, and in addition, the porous carbon positioned on the outer layer has the characteristics of high specific surface area, unique pore channel structure and the like, so that the finally prepared composite material integrates the advantages of special electrical property of the iron carbide, good heat transfer performance of the porous carbon and the like, and has wide application prospect in the fields of catalysis, energy storage and the like. The preparation method of the composite material is simple and easy to operate, has low cost and is suitable for expanded production.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to an iron carbide-porous carbon composite material and a preparation method and application thereof.
Background
The porous carbon material has the characteristics of high specific area, low cost, easy preparation, unique pore channel structure, excellent chemical stability and the like, and is widely used as a lithium battery electrode material, a super capacitor electrode material, a catalyst carrier and the like. At present, there are several methods for synthesizing porous carbon materials: high polymer carbonization, biomass material carbonization, physical and chemical activation, chemical vapor deposition, and the like.
Among these methods, the high polymer carbonization method and the biomass carbonization method are the most widely used methods for preparing porous carbon because of their low cost, easy preparation, and large specific surface area of the produced carbon material. The biomass material carbonization method uses biomass materials as raw materials, but the biomass materials are influenced by different regions and different seasons, so that uncertainty exists, and the prepared materials can be different. The high polymer carbonization method has high repeatability because the high polymer is a specific species during carbonization, simultaneously has a plurality of usable substrates, and can prepare various porous carbons with different specific surface areas, unique pore channel structures and excellent electrochemical performance by a simple method at low cost.
The nano iron carbide is an excellent electro-catalyst and is widely applied to reactions such as electro-catalytic oxygen reduction, hydrogen evolution, oxygen evolution and the like. Because the conductivity of the iron carbide is low, and the porous carbon has excellent conductivity, the catalytic performance of the iron carbide can be further improved after the iron carbide and the porous carbon form a composite material. Moreover, the catalytic performance of the catalyst is greatly improved by doping other transition metals. Therefore, the research and development of the iron carbide-porous carbon composite material can expand the application range of the iron carbide, and simultaneously can ensure that the composite material has wide application prospects in the fields of catalysis, energy storage and the like.
Disclosure of Invention
In view of the above, an object of the present invention is to provide an iron carbide-porous carbon composite material; the second purpose is to provide a preparation method of the iron carbide-porous carbon composite material; the third purpose is to provide the application of the iron carbide-porous carbon composite material in catalysis and/or energy storage.
In order to achieve the purpose, the invention provides the following technical scheme:
1. the composite material consists of porous carbon and iron carbide nanoparticles coated in the porous carbon, wherein the iron carbide nanoparticles have a core-shell structure.
Preferably, the particle size of the iron carbide nanoparticles is 20-30 nm.
Preferably, the BET specific surface area of the porous carbon is 250-350m
2The pore size is less than or equal to 2 nm.
2. The preparation method of the iron carbide-porous carbon composite material comprises the following steps:
dropwise adding the ferric salt ethanol solution into the 1, 8-diaminonaphthalene ethanol solution under stirring to obtain a reaction solution, continuously stirring the reaction solution for 16-24h, centrifuging to obtain the iron-doped poly-1, 8-diaminonaphthalene, washing and drying the iron-doped poly-1, 8-diaminonaphthalene, heating to 350-plus-fluid temperature of 450 ℃ at the speed of 3-6 ℃/min under a protective atmosphere, then preserving heat for 1-2h, heating to 700-plus-fluid temperature of 1000 ℃ at the speed of 0.5-1.5 ℃/min, then preserving heat for 2-4h, and cooling to obtain the iron carbide-porous carbon composite material.
Preferably, the molar ratio of the 1, 8-diaminonaphthalene to the iron ions in the reaction solution is 7-12: 1.
Preferably, the ferric salt in the ferric salt ethanol solution is one of ferric trichloride hexahydrate, ferric acetylacetonate or ferric nitrate nonahydrate.
Preferably, the stirring speed during stirring and the stirring continuing is both 600-800 r/min.
Preferably, the washing solution used in the washing is ethanol; the drying is vacuum drying at 20-30 deg.C for 12-16 h.
Preferably, the protective atmosphere is hydrogen.
3. The iron carbide-porous carbon composite material is applied to catalysis and/or energy storage.
The invention has the beneficial effects that: the invention provides an iron carbide-porous carbon composite material and a preparation method and application thereof, wherein the iron carbide-porous carbon composite material is a hierarchical composite material formed by porous carbon-coated iron carbide with a core-shell structure, the iron carbide with the core-shell structure is coated in the porous carbon in the material, so that the corrosion resistance of the material is further improved, in addition, the porous carbon positioned at the outer layer has the characteristics of high specific surface area, unique pore channel structure and the like, so that the finally prepared composite material integrates the advantages of special electrical properties of the iron carbide, good heat transfer performance of the porous carbon and the like, and has wide application prospects in the fields of catalysis, energy storage and the like. The preparation method of the composite material is simple and easy to operate, has low cost and is suitable for expanded production.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a scanning electron micrograph of iron-doped poly-1, 8-diaminonaphthalene prepared in example 1;
FIG. 2 is a scanning electron micrograph of an iron carbide-porous carbon composite prepared in example 1;
FIG. 3 is a transmission electron micrograph of an iron carbide-porous carbon composite prepared in example 1;
FIG. 4 is an XRD pattern of the iron carbide-porous carbon composite prepared in example 1;
FIG. 5 is a graph of the desorption of nitrogen for the iron carbide-porous carbon composite prepared in example 1;
FIG. 6 is a nitrogen pore size distribution plot for the iron carbide-porous carbon composite prepared in example 1;
FIG. 7 is a scanning electron micrograph of an iron carbide-porous carbon composite prepared in example 2;
FIG. 8 is a transmission electron micrograph of an iron carbide-porous carbon composite prepared in example 2;
FIG. 9 is a scanning electron micrograph of an iron carbide-porous carbon composite prepared in example 3;
FIG. 10 is a transmission electron micrograph of an iron carbide-porous carbon composite prepared in example 3;
FIG. 11 is a graph showing the results of an electrocatalytic oxygen reduction performance test of the iron carbide-porous carbon composite prepared in example 1;
FIG. 12 is a graph showing the results of an electrocatalytic oxygen reduction performance test of the iron carbide-porous carbon composite prepared in example 2;
fig. 13 is a graph showing the results of the electrocatalytic oxygen reduction performance test of the iron carbide-porous carbon composite prepared in example 3.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Preparation of iron carbide-porous carbon composite material
Dropwise adding ferric trichloride hexahydrate ethanol solution into 1, 8-diaminonaphthalene ethanol solution under stirring at the speed of 700r/min to obtain reaction liquid, wherein the molar ratio of 1, 8-diaminonaphthalene to iron ions in the reaction liquid is 10:1, continuously stirring the reaction liquid at the speed of 700r/min for 24 hours, centrifuging to obtain iron-doped poly-1, 8-diaminonaphthalene, washing the iron-doped poly-1, 8-diaminonaphthalene with ethanol, carrying out vacuum drying at the temperature of 30 ℃ for 12 hours, heating to 400 ℃ at the speed of 5 ℃/min under hydrogen, then carrying out heat preservation for 1 hour, heating to 900 ℃ at the speed of 1 ℃/min, carrying out heat preservation for 2 hours, and naturally cooling to room temperature to obtain the iron carbide-porous carbon composite material.
FIG. 1 is a scanning electron micrograph of the iron-doped poly-1, 8-diaminonaphthalene prepared in example 1, from which it can be seen that the iron-doped poly-1, 8-diaminonaphthalene is in the form of a regular sphere with a particle size of 100-150 nm.
FIG. 2 is a scanning electron micrograph of the iron carbide-porous carbon composite prepared in example 1, from which it can be seen that the iron carbide-porous carbon composite has a regular spherical shape with a particle size of 100-150nm, indicating that the structure does not collapse during the calcination process.
Fig. 3 is a transmission electron microscope image of the iron carbide-porous carbon composite material prepared in example 1, from which it can be seen that the composite material is composed of porous carbon and iron carbide nanoparticles coated in the porous carbon, wherein the iron carbide nanoparticles have a core-shell structure and a particle size of 20-30 nm.
Fig. 4 is an XRD pattern of the iron carbide-porous carbon composite material prepared in example 1, from which it can be seen that the composite material is composed of iron carbide and carbon, in which the 26 ° peak is a peak of graphitized carbon, indicating that the material contains a large amount of carbon.
FIG. 5 is a graph showing the desorption of nitrogen gas from the iron carbide-porous carbon composite prepared in example 1, and FIG. 6 is a graph showing the pore size distribution of nitrogen gas from the iron carbide-porous carbon composite prepared in example 1, and it can be seen from FIGS. 5 and 6 that the BET specific surface area of the composite is 250-
2Per g, at 0<P/P
0<When the pressure is 0.1, the adsorption capacity of nitrogen is rapidly increased along with the increase of the relative pressure, which indicates that the composite material contains micropores, the pore size of the micropores is less than or equal to 2nm, and meanwhile, no hysteresis loop appears in desorption branches, which indicates that the composite material is a typical microporous material.
Example 2
Preparation of iron carbide-porous carbon composite material
Dropwise adding ferric nitrate nonahydrate ethanol solution into 1, 8-diaminonaphthalene ethanol solution under stirring at a speed of 600r/min to obtain reaction solution, wherein the molar ratio of 1, 8-diaminonaphthalene to iron ions in the reaction solution is 7:1, continuously stirring the reaction solution at a speed of 600r/min for 20h, centrifuging to obtain iron-doped poly-1, 8-diaminonaphthalene, washing the iron-doped poly-1, 8-diaminonaphthalene with ethanol, then carrying out vacuum drying at 20 ℃ for 16h, then heating to 450 ℃ at a speed of 6 ℃/min under hydrogen, then carrying out heat preservation for 1.5h, heating to 1000 ℃ at a speed of 1.5 ℃/min, carrying out heat preservation for 3h, and naturally cooling to room temperature to obtain the iron carbide-porous carbon composite material.
Fig. 7 is a scanning electron microscope image of the iron carbide-porous carbon composite material prepared in example 2, which shows that the iron carbide-porous carbon composite material is in a regular spherical shape and has a particle size of 100-150 nm.
Fig. 8 is a transmission electron microscope image of the iron carbide-porous carbon composite material prepared in example 2, from which it can be seen that the composite material is composed of porous carbon and iron carbide nanoparticles coated in the porous carbon, wherein the iron carbide nanoparticles have a core-shell structure and a particle size of 20-30 nm.
Example 3
Preparation of iron carbide-porous carbon composite material
Dropwise adding an acetylacetone iron ethanol solution into a 1, 8-diaminonaphthalene ethanol solution under stirring at a speed of 800r/min to obtain a reaction solution, wherein the molar ratio of 1, 8-diaminonaphthalene to iron ions in the reaction solution is 12:1, continuously stirring the reaction solution at a speed of 800r/min for 16h, centrifuging to obtain iron-doped poly-1, 8-diaminonaphthalene, washing the iron-doped poly-1, 8-diaminonaphthalene with ethanol, performing vacuum drying at 25 ℃ for 14h, heating to 350 ℃ at a speed of 3 ℃/min under hydrogen, then performing heat preservation for 2h, heating to 700 ℃ at a speed of 0.5 ℃/min, performing heat preservation for 4h, and naturally cooling to room temperature to obtain the iron carbide-porous carbon composite material.
FIG. 9 is a scanning electron micrograph of the iron carbide-porous carbon composite prepared in example 3, which shows that the iron carbide-porous carbon composite is in a regular spherical shape and has a particle size of 100-150 nm.
Fig. 10 is a transmission electron microscope image of the iron carbide-porous carbon composite material prepared in example 3, from which it can be seen that the composite material is composed of porous carbon and iron carbide nanoparticles coated in the porous carbon, wherein the iron carbide nanoparticles have a core-shell structure and a particle size of 20-30 nm.
Example 4
Application of iron carbide-porous carbon composite material in electrocatalytic oxygen reduction
1) Taking 2mg of each of the iron carbide-porous carbon composite materials prepared in the examples 1 to 3, respectively dispersing the iron carbide-porous carbon composite materials into 1mL of mixed solution formed by mixing water and ethanol according to the volume ratio of 1:1, respectively adding 20 mu L of 5% Nafion solution, and then carrying out continuous ultrasonic treatment for 10 minutes to obtain three kinds of dispersion liquid;
2) polishing the rotary disk electrode by using aluminum powder with the particle size of 0.3 mu m and 0.05 mu m respectively until the rotary disk electrode is flat and smooth, washing the rotary disk electrode by using deionized water, and airing for later use;
3) taking 5 mu L of each dispersion liquid obtained in the step (1), respectively dripping the dispersion liquid into the center of a rotating disk electrode, naturally drying to prepare three oxygen reduction test electrodes, and testing the oxygen reduction performance of the three oxygen reduction test electrodes, wherein the results are shown in fig. 11, fig. 12 and fig. 13, wherein fig. 11 is a graph of the test result of the electrocatalytic oxygen reduction performance of the iron carbide-porous carbon composite material prepared in the example 1, fig. 12 is a graph of the test result of the electrocatalytic oxygen reduction performance of the iron carbide-porous carbon composite material prepared in the example 2, fig. 13 is a graph of the test result of the electrocatalytic oxygen reduction performance of the iron carbide-porous carbon composite material prepared in the example 3, and as can be seen from fig. 11 to fig. 13, the half slope potentials of the iron carbide-porous carbon composite materials prepared in the examples 1, 2 and 3 are all around 0.8V vsRHE, showing good oxygen reduction performance, the iron carbide-porous carbon composite material has great potential in electrocatalysis.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. The iron carbide-porous carbon composite material is characterized by consisting of porous carbon and iron carbide nanoparticles coated in the porous carbon, wherein the iron carbide nanoparticles have a core-shell structure.
2. The iron carbide-porous carbon composite material according to claim 1, wherein the iron carbide nanoparticles have a particle size of 20 to 30 nm.
3. The iron carbide-porous carbon composite material according to claim 1, wherein the BET specific surface area of the porous carbon is 250-350m
2The pore size is less than or equal to 2 nm.
4. A method of preparing an iron carbide-porous carbon composite according to any one of claims 1 to 3, characterized in that it comprises:
dropwise adding the ferric salt ethanol solution into the 1, 8-diaminonaphthalene ethanol solution under stirring to obtain a reaction solution, continuously stirring the reaction solution for 16-24h, centrifuging to obtain the iron-doped poly-1, 8-diaminonaphthalene, washing and drying the iron-doped poly-1, 8-diaminonaphthalene, heating to 350-plus-fluid temperature of 450 ℃ at the speed of 3-6 ℃/min under a protective atmosphere, then preserving heat for 1-2h, heating to 700-plus-fluid temperature of 1000 ℃ at the speed of 0.5-1.5 ℃/min, then preserving heat for 2-4h, and cooling to obtain the iron carbide-porous carbon composite material.
5. The method according to claim 4, wherein the molar ratio of 1, 8-diaminonaphthalene to iron ions in the reaction solution is 7-12: 1.
6. The method of claim 4, wherein the iron salt in the ethanolic iron salt solution is one of ferric chloride hexahydrate, ferric acetylacetonate, or ferric nitrate nonahydrate.
7. The method as claimed in claim 4, wherein the stirring speed and the stirring continuation speed are both 600-800 r/min.
8. The method according to claim 4, wherein the washing solution used in the washing is ethanol; the drying is vacuum drying at 20-30 deg.C for 12-16 h.
9. The method of claim 4, wherein the protective atmosphere is hydrogen.
10. Use of an iron carbide-porous carbon composite according to any one of claims 1 to 3 in catalysis and/or energy storage.
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