CN116239150A - Preparation method of pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles - Google Patents
Preparation method of pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles Download PDFInfo
- Publication number
- CN116239150A CN116239150A CN202211530503.0A CN202211530503A CN116239150A CN 116239150 A CN116239150 A CN 116239150A CN 202211530503 A CN202211530503 A CN 202211530503A CN 116239150 A CN116239150 A CN 116239150A
- Authority
- CN
- China
- Prior art keywords
- moc
- carbon
- nano
- product
- molybdenum carbide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910039444 MoC Inorganic materials 0.000 title claims abstract description 56
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 11
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002114 nanocomposite Substances 0.000 claims abstract description 8
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910003481 amorphous carbon Inorganic materials 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000006227 byproduct Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 241001083505 Punica Species 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002223 garnet Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 239000011777 magnesium Substances 0.000 abstract description 3
- 239000006096 absorbing agent Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000002159 nanocrystal Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 description 12
- 239000007787 solid Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 150000002751 molybdenum Chemical class 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000219991 Lythraceae Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- -1 Transition metal carbides Chemical class 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- UPKIHOQVIBBESY-UHFFFAOYSA-N magnesium;carbanide Chemical compound [CH3-].[CH3-].[Mg+2] UPKIHOQVIBBESY-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- CNEOGBIICRAWOH-UHFFFAOYSA-N methane;molybdenum Chemical compound C.[Mo] CNEOGBIICRAWOH-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The preparation method of the pomegranate-shaped molybdenum carbide/carbon (MoC/C) nano composite particles takes pyrrole and phosphomolybdic acid as raw materials, and the pomegranate-shaped MoC/C nano composite material with the average particle size of about 70 nanometers is prepared through in-situ polymerization and subsequent magnesium thermal reaction, wherein 3-5 nm MoC nanocrystals are embedded in an amorphous carbon matrix. The preparation method is simple to operate, the reaction temperature can be obviously reduced by adjusting the solution proportion and the thermal reaction strategy, and the preparation process is simple, easy to control and good in repeatability, and can realize large-scale production. The MoC/C nano particles prepared by the method have uniform size and high phase purity, and can be used as a catalyst and a wave absorber material for potential hydrogen evolution reaction.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a preparation method of a garnet-like molybdenum carbide/carbon MoC/C nanocomposite.
Background
Transition metal carbides are one of the very promising types of materials for new functional areas, such as: the electro-catalyst used for the electrolytic water hydrogen evolution reaction has the advantages of high catalytic activity, high stability, flexible and various preparation methods and the like; the material used as the wave absorber has strong microwave loss capability. Molybdenum carbide has received attention because of its Pt-like electronic structure, chemical stability, low cost, and good electrical conductivity. The composition, the crystal phase and the structure of the prepared molybdenum carbide nano material have decisive influence on the performance of the molybdenum carbide nano material by adjusting the reaction conditions and the precursors in the synthesis process.
In general, carbide synthesis is achieved by carbonization reactions at high temperatures. For example, molybdenum carbide is generally obtained by performing a carbon reduction reaction at a high temperature with the aid of hydrogen gas, using a molybdenum salt as a precursor and using gaseous carbon (hydrocarbon gas) or solid carbon (biochar or the like) as a carbon source. The gas carbon source has very high requirements on experimental conditions and preparation processes, and certain potential safety hazards exist in operation. The solid carbon source has the interface reaction between solid and solid, the uniformity of the reaction product is poor, the specific surface area is low, and the performance of the molybdenum carbide is affected to a certain extent.
Furthermore, magnesia reduction has been shown to synthesize carbides at temperatures <700 ℃. Magnesium metal may react with carbon to form magnesium carbide, which undergoes solid state metathesis with metal oxides to form metal carbides. Therefore, the synthesis of the molybdenum carbide nano material with high specific surface area and uniform composition at a lower temperature can be realized through magnesian reduction.
Disclosure of Invention
The invention aims to provide a preparation method of a garnet-like molybdenum carbide/carbon MoC/C nanocomposite, wherein the garnet-like MoC/C nanocomposite is prepared at a low temperature, the particle size of the composite is 40-70 nanometers, and 3-5 nanometers of MoC particles are uniformly dispersed in an amorphous carbon matrix to form a garnet-like microstructure. The composite material prepared by the method has a wide application prospect and an advantage in the aspects of electrocatalysis and microwave absorption.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles is characterized by comprising the following steps of:
1) Mu.l of pyrrole solution is added into 20ml of absolute ethanol and stirred fully;
2) 1.2mmol of phosphomolybdic acid was added to 100ml of distilled water and stirred well to form a yellow solution;
3) Adding the solution obtained in the step 1 into the solution obtained in the step 2 to gradually form black mixed dispersion liquid, and stirring for 12 hours at room temperature;
4) Centrifugally washing the mixed dispersion liquid obtained in the step 3 with deionized water and ethanol solution for a plurality of times until supernatant is clear, and then drying in a vacuum drying oven at 60 ℃ to obtain a black product A;
5) Mixing the product A obtained in the step 4 with magnesium powder and sodium chloride according to the mass ratio of 1:1:5, heating and preserving heat to obtain a product B;
6) And (3) treating the product B obtained in the step (5) with a hydrochloric acid aqueous solution to remove magnesium oxide and other soluble byproducts, collecting insoluble products through centrifugation, and drying to obtain the black powder which is the punica granatum-shaped MoC/C nanocomposite.
The average particle size of the MoC/C nano particles is 70 nanometers, and the microstructure of the MoC/C nano particles is in a pomegranate shape, namely, the MoC particles with the particle size of 3-5 nanometers are uniformly dispersed in an amorphous carbon matrix.
And in the step 5, the temperature is raised to 550-700 ℃, the temperature raising rate is 5-10 ℃/min, and the heat preservation time is 4-8 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses pyrrole solution and phosphomolybdic acid as precursors, forms a nano spherical structure through in-situ polymerization, and combines the subsequent magnesium thermal reaction to prepare the pomegranate-shaped MoC/C nano particles with uniform size. The average grain diameter of the prepared nano composite particles is 70 nanometers, the size is uniform, no impurity phase exists, the whole preparation process is simple in steps, the operation is simple and convenient, and the repeatability is good.
The dosage of the molybdenum salt has an important regulation effect on the composition of the product, and a solid carbon source is adopted in the carbonization process, so that carbon deposition generated in the carbonization process can be reduced, and the regulation of the active surface area of MoC is facilitated.
Compared with the prior art, the invention has relatively low reaction temperature and greatly reduces the energy consumption.
In conclusion, the molybdenum source and the carbon source adopted by the invention are common reagents, and the preparation process is simple, easy to control and good in repeatability, and can realize large-scale production. Meanwhile, the product has high purity and uniform and controllable size, and the active substance MoC nano particles are uniformly dispersed in the amorphous carbon matrix, so that the active surface area is improved.
Drawings
FIG. 1 is a graph of MoC/C nanoparticle scanning electron microscopy and low power transmission electron microscopy;
FIG. 2 is a high power transmission electron microscope image of MoC/C nanoparticles;
FIG. 3 is a graph of the MoC/C nanoparticle X-ray diffraction pattern.
Detailed Description
The invention is further described below with reference to the drawings and examples.
According to the molybdenum carbide (MoC) nanoparticle, pyrrole and phosphomolybdic acid are used as raw materials, and the pomegranate-shaped MoC/C nanoparticle is prepared through magnesium thermal reaction.
Example 1
Adding 400 mu l of pyrrole solution into 20ml of absolute ethyl alcohol, and fully stirring to form a mixed solution A; 1.2mmol of phosphomolybdic acid was added to 100ml of distilled water and stirred well to form yellow solution B; dropwise adding the mixed solution A into the mixed solution B to form black mixed dispersion liquid, and stirring at room temperature for 12h; centrifugally washing the obtained product with a mixed solution of deionized water and ethanol for several times until supernatant is clear, and then drying the supernatant in a vacuum drying oven at 60 ℃ overnight to obtain a black product A; mixing the obtained product A with magnesium powder and sodium chloride according to the mass ratio of 1:1:5, heating to 650 ℃ at the heating rate of 5 ℃/min, preserving heat for 6 hours, naturally cooling to room temperature, and then treating the product with hydrochloric acid aqueous solution to remove magnesium oxide and other soluble byproducts. Insoluble product was collected by centrifugation and dried to give black powder as MoC/C nanoparticles. The MoC/C nano particles are shown in the figures 1 and 2; the d-value and relative intensity of the diffraction peak were consistent with those listed for the MoC PDF standard card (89-2868), as shown in fig. 3.
Example 2
Adding 350 μl of pyrrole solution into 20ml of absolute ethanol, and stirring thoroughly to form a mixed solution A; 1.2mmol of phosphomolybdic acid was added to 100ml of distilled water and stirred well to form yellow solution B; dropwise adding the mixed solution A into the mixed solution B to form black mixed dispersion liquid, and stirring at room temperature for 12h; centrifugally washing the obtained product with a mixed solution of deionized water and ethanol for several times until supernatant is clear, and then drying the supernatant in a vacuum drying oven at 60 ℃ overnight to obtain a black product A; mixing the obtained product A with magnesium powder and sodium chloride according to the mass ratio of 1:1:5, heating to 650 ℃ at the heating rate of 5 ℃/min, preserving heat for 6 hours, naturally cooling to room temperature, and then treating the product with hydrochloric acid aqueous solution to remove magnesium oxide and other soluble byproducts. Insoluble product was collected by centrifugation and dried to give black powder as MoC/C nanoparticles. The d value and the relative intensity of the diffraction peak are consistent with those of PDF standard card (89-2868) of MoC, and the diffraction peak is MoC/C nano-particle.
Example 3
Adding 450 mu l of pyrrole solution into 20ml of absolute ethyl alcohol, and fully stirring to form a mixed solution A; 1.2mmol of phosphomolybdic acid was added to 100ml of distilled water and stirred well to form yellow solution B; dropwise adding the mixed solution A into the mixed solution B to form black mixed dispersion liquid, and stirring at room temperature for 12h; centrifugally washing the obtained product with a mixed solution of deionized water and ethanol for several times until supernatant is clear, and then drying the supernatant in a vacuum drying oven at 60 ℃ overnight to obtain a black product A; mixing the obtained product A with magnesium powder and sodium chloride according to the mass ratio of 1:1:5, heating to 650 ℃ at the heating rate of 5 ℃/min, preserving heat for 6 hours, naturally cooling to room temperature, and then treating the product with hydrochloric acid aqueous solution to remove magnesium oxide and other soluble byproducts. Insoluble product was collected by centrifugation and dried to give black powder as MoC/C nanoparticles. The d value and the relative intensity of the diffraction peak are consistent with those of PDF standard card (89-2868) of MoC, and the diffraction peak is MoC/C nano-particle.
FIG. 1 is a scanning and low-magnification transmission electron micrograph of MoC/C nanoparticles prepared according to the present invention, showing that the average particle diameter is 70 nm.
FIG. 2 is a high-magnification transmission electron micrograph of carbonized MoC/C nanoparticles, illustrating MoC grain sizes of 3-5 nanometers.
FIG. 3 is an X-ray diffraction pattern of MoC/C nanoparticles, demonstrating their relatively high phase purity.
Claims (3)
1. The preparation method of the pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles is characterized by comprising the following steps of:
1) Adding 350-450 mu l of pyrrole solution into 20ml of absolute ethyl alcohol, and fully stirring;
2) 1.2mmol of phosphomolybdic acid was added to 100ml of distilled water and stirred well to form a yellow solution;
3) Adding the solution obtained in the step 1 into the solution obtained in the step 2 to gradually form black mixed dispersion liquid, and stirring for 12 hours at room temperature;
4) Centrifugally washing the mixed dispersion liquid obtained in the step 3 with deionized water and ethanol solution for a plurality of times until supernatant is clear, and then drying in a vacuum drying oven at 60 ℃ to obtain a black product A;
5) Mixing the product A obtained in the step 4 with magnesium powder and sodium chloride according to the mass ratio of 1:1:5, heating and preserving heat to obtain a product B;
6) And (3) treating the product B obtained in the step (5) with a hydrochloric acid aqueous solution to remove magnesium oxide and other soluble byproducts, collecting insoluble products through centrifugation, and drying to obtain the black powder which is the punica granatum-shaped MoC/C nanocomposite.
2. The method for preparing the garnet-like molybdenum carbide/carbon MoC/C nanoparticles according to claim 1, wherein the average particle size of the MoC/C nanoparticles is 70 nanometers, and the microstructure is in the shape of a garnet, namely, the MoC particles of 3-5 nanometers are uniformly dispersed in an amorphous carbon matrix.
3. The method for preparing the garnet-like molybdenum carbide/carbon MoC/C nano-particles according to claim 1, wherein the temperature is raised to 550-700 ℃ in the step 5, the temperature raising rate is 5-10 ℃/min, and the heat preservation time is 4-8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211530503.0A CN116239150A (en) | 2022-12-01 | 2022-12-01 | Preparation method of pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211530503.0A CN116239150A (en) | 2022-12-01 | 2022-12-01 | Preparation method of pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116239150A true CN116239150A (en) | 2023-06-09 |
Family
ID=86633794
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211530503.0A Pending CN116239150A (en) | 2022-12-01 | 2022-12-01 | Preparation method of pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116239150A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU1777311C (en) * | 1988-07-12 | 1994-10-15 | Институт структурной макрокинетики РАН | Process for preparing molybdenum carbide |
| CN107311176A (en) * | 2017-08-07 | 2017-11-03 | 太原理工大学 | A kind of preparation method of order mesoporous carbonization molybdenum |
| CA3030838A1 (en) * | 2016-07-15 | 2018-01-18 | Marc POROSOFF | Alkali metal doped molybdenum carbide supported on gamma-alumina for selective co2 hydrogenation into co |
| CN110479335A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of molybdenum carbide carbon composite and preparation method thereof that copper adulterates in situ |
| CN112864366A (en) * | 2021-03-05 | 2021-05-28 | 武汉科技大学 | alpha-MoC1-x/Si @ C microsphere, preparation method and application |
| CN113293400A (en) * | 2021-06-09 | 2021-08-24 | 济南大学 | Electro-catalytic nitrogen reduction catalyst MoS2-Mo2Preparation method of C |
| CN114804111A (en) * | 2022-04-08 | 2022-07-29 | 济南大学 | Porous molybdenum carbide and preparation method and application thereof |
| CN115092962A (en) * | 2022-05-20 | 2022-09-23 | 江苏师范大学 | Molybdenum dioxide/carbon composite electrode material and preparation method and application thereof |
| CN115341235A (en) * | 2022-08-29 | 2022-11-15 | 天津大学 | Defective carbon material prepared by molybdenum carbide and preparation method and application thereof |
-
2022
- 2022-12-01 CN CN202211530503.0A patent/CN116239150A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU1777311C (en) * | 1988-07-12 | 1994-10-15 | Институт структурной макрокинетики РАН | Process for preparing molybdenum carbide |
| CA3030838A1 (en) * | 2016-07-15 | 2018-01-18 | Marc POROSOFF | Alkali metal doped molybdenum carbide supported on gamma-alumina for selective co2 hydrogenation into co |
| CN107311176A (en) * | 2017-08-07 | 2017-11-03 | 太原理工大学 | A kind of preparation method of order mesoporous carbonization molybdenum |
| CN110479335A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of molybdenum carbide carbon composite and preparation method thereof that copper adulterates in situ |
| CN112864366A (en) * | 2021-03-05 | 2021-05-28 | 武汉科技大学 | alpha-MoC1-x/Si @ C microsphere, preparation method and application |
| CN113293400A (en) * | 2021-06-09 | 2021-08-24 | 济南大学 | Electro-catalytic nitrogen reduction catalyst MoS2-Mo2Preparation method of C |
| CN114804111A (en) * | 2022-04-08 | 2022-07-29 | 济南大学 | Porous molybdenum carbide and preparation method and application thereof |
| CN115092962A (en) * | 2022-05-20 | 2022-09-23 | 江苏师范大学 | Molybdenum dioxide/carbon composite electrode material and preparation method and application thereof |
| CN115341235A (en) * | 2022-08-29 | 2022-11-15 | 天津大学 | Defective carbon material prepared by molybdenum carbide and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| SANJAY UPADHYAY ET AL.: "Synthesis of Mo2C/MoC/C nanocomposite for hydrogen evolution reaction", 《JOURNAL OF SOLID STATE ELECTROCHEMISTRY》, vol. 26, 10 January 2022 (2022-01-10), pages 560 * |
| 陈裕雲: "钼基电极材料的可控制备及其电化学性能研究", 《中国博士学位论文全文数据库 工程科技I辑》, no. 1, 15 January 2021 (2021-01-15), pages 33 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109534307B (en) | g-C3N4 crystalline phase/amorphous homogeneous junction and preparation method and application thereof | |
| CN110548528B (en) | SiO with core-shell structure2SiC material and preparation method and application thereof | |
| Chen et al. | 2D ultrathin CoP modified Mn x Cd 1− x S with controllable band structure and robust photocatalytic performance for hydrogen generation | |
| CN105582909A (en) | Preparation method and application of bismuth tungstate/expanded graphite sheet nanocomposite | |
| CN101786598A (en) | Method for preparing nanometer zero-valent iron/ordered meshporous silicon oxide composite material | |
| CN104752074B (en) | A kind of preparation method of molybdenum oxide/carbon bead composite | |
| CN112609197B (en) | Preparation method of two-dimensional lamellar carbon-based molybdenum carbide composite material | |
| CN108273488B (en) | Preparation method of nano-sheet cerium dioxide/porous carbon composite material | |
| CN113600223B (en) | Fe (Fe) 2 P/nitrogen vacancy g-C 3 N 4 Preparation method and application of nanosheet photocatalyst | |
| CN113000061A (en) | Preparation method of strip-shaped graphite carbon nitride nanosheet | |
| CN109174143B (en) | Perovskite-based composite nano photocatalytic material and preparation method and application thereof | |
| CN115196605A (en) | Preparation method and application of graphite phase carbon nitride nanosheet | |
| CN108658059B (en) | Preparation method of tungsten trioxide/nitrogen-doped graphene compound | |
| CN108620110B (en) | Vanadium carbide/graphene nanosheet composite material, preparation method and application thereof in hydrogen production through water cracking | |
| CN116239150A (en) | Preparation method of pomegranate-shaped molybdenum carbide/carbon MoC/C nano-particles | |
| CN109616626B (en) | Low-temperature macro preparation method of carbon-coated ferroferric oxide nanocrystal | |
| CN111715209B (en) | Gas phase preparation method of tungsten trioxide/graphite felt composite material | |
| Negahdari et al. | Synthesis and characterization of nanocrystalline microwave dielectric LaAlO3 powder via sucrose method | |
| CN108640144A (en) | A kind of yttrium oxide twin-stage nanosphere and preparation method thereof | |
| CN103276476A (en) | Method for preparing nano-carbon fibers by T-ZnOw surface in-situ polymerization | |
| CN111203249A (en) | Preparation method of graphene-coated transition metal carbide nanocapsules and application of nanocapsules in microwave catalysis field | |
| CN112591754A (en) | Preparation method of carbon nanocage coupled molybdenum carbide quantum dot nanocomposite | |
| CN110756205A (en) | Nickel-based cerium dioxide coated silicon carbide catalyst and preparation method and application thereof | |
| CN111875454B (en) | Ammonium perchlorate catalyst, preparation method and application | |
| WO2022213423A1 (en) | Phosphorus-doped bismuth tungstate photocatalyst, preparation method therefor and use thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |