CN113277514A - Transition metal carbide Mo2Preparation method of material C - Google Patents
Transition metal carbide Mo2Preparation method of material C Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 32
- 229910052723 transition metal Inorganic materials 0.000 title claims description 8
- 150000003624 transition metals Chemical class 0.000 title claims description 8
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000002086 nanomaterial Substances 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 229930006000 Sucrose Natural products 0.000 claims abstract description 13
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000005720 sucrose Substances 0.000 claims abstract description 13
- 238000001291 vacuum drying Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 10
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 10
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 10
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 229910003178 Mo2C Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 150000001720 carbohydrates Chemical class 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000000643 oven drying Methods 0.000 claims 1
- 230000007704 transition Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 230000003197 catalytic effect Effects 0.000 description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052750 molybdenum Inorganic materials 0.000 description 8
- 239000011733 molybdenum Substances 0.000 description 8
- 239000011261 inert gas Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 5
- 229910039444 MoC Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 150000001247 metal acetylides Chemical class 0.000 description 3
- 238000003775 Density Functional Theory Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
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- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229960004424 carbon dioxide Drugs 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
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- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910001009 interstitial alloy Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- -1 molybdenum carbide Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum 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
- 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
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- B01J35/23—
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- B01J35/33—
-
- B01J35/39—
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/40—Electric properties
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention discloses Mo2The simple preparation method of the C nano material comprises the following specific steps: s1: respectively adding 0.3g of ammonium molybdate and 0.5g of sucrose into 20ml of deionized water; s2: drying the solution obtained in the step S1 in a vacuum drying oven at the temperature of 80 ℃, and collecting a powder sample obtained after drying; s3: sintering the powder material collected by S2 in a tube furnace at 800 ℃ for 5h at a heating rate of 5 ℃ for min‑1Finally obtaining Mo2And C, nano-materials. Compared with the other Mo preparations2The raw materials are cheap and easy to obtain; the conditions are simple and easy to control in the synthesis process; the preparation efficiency is high, and the method has good application and industrialization prospects.
Description
Technical Field
The invention relates to the field of synthesis and energy of nano materials, in particular to Mo2A simple preparation method of the C nano material.
Background
Energy problems are the times of development and industrialization of human society, and the environmental problems caused by the use of traditional fossil energy are becoming more and more serious, so that the demand of people for novel, sustainable development, environment-friendly and efficient new energy is more and more urgent. Hydrogen energy is favored due to the characteristics that the combustion product is water and the like because of high combustion value, however, most of hydrogen at the present stage is derived from traditional fossil energy sources such as coal, petroleum, natural gas and the like, and the influence on the environment is self-evident, and an effective way is provided for solving the problem by utilizing sunlight to catalyze and produce hydrogen. However, the problem of low conversion efficiency from solar energy to hydrogen energy still exists in the sunlight catalytic hydrogen production, and the separation of the photo-generated charges is the key point for determining the conversion efficiency. The problem can be effectively solved by loading a proper cocatalyst, and the traditional noble metal hydrogen production cocatalyst such as Pt has the characteristics of higher work function and strong hydrogen production capability by catalyzing proton reduction, but the industrialized application of the traditional noble metal hydrogen production cocatalyst is limited due to the high price of the traditional noble metal hydrogen production cocatalyst. Therefore, the development of a non-noble metal catalyst which is cheap and has high cocatalyst activity has extremely important significance.
Transition metal carbide is a kind of interstitial compound with metal property generated by carbon atoms entering crystal lattices of transition metals, has special chemical and physical properties such as high melting point, high hardness and the like, and is widely concerned and applied in the fields of energy, catalysis and the like. In the 90 s of the 20 th century, Ledoux et al reported that metal carbides have noble metal-like characteristics, and it is believed that in metal carbides, carbon atoms fill in the metal lattice, resulting in a change in electron density, an increase in lattice parameter, an increase in lattice spacing, a contraction of the d-band, and Fermi energyThe state d electron density increases and thus has surface properties and absorption characteristics similar to those of noble metals. In recent years, carbides, particularly molybdenum carbide, have attracted much attention as a new class of catalytic materials. The molybdenum carbide is formed by embedding carbon atoms into the layers of the metal molybdenum, so that the interlayer spacing of the metal molybdenum is increased, and the molding device has good catalytic performance. Density Functional Theory (DFT) calculations show that when a carbon atom is intercalated between layers of molybdenum, the d-band of molybdenum and the s-and p-orbitals of the carbon atom hybridize, resulting in a broadening of the d-band, causing the molybdenum to exhibit a d-band structure similar to Pt; moreover, the movement of the d-band can cause the change of the adsorption energy of hydrogen atoms, so that the molybdenum carbide shows excellent electrocatalytic hydrogen evolution performance (PNAS, 2011, 108, 937). Mo2C has been widely used in thermal catalysis, electrocatalysis and photoelectrocatalysis because of its characteristics of extremely high thermal stability, corrosion resistance at room temperature, high catalytic activity, etc. The material of molybdenum carbide also has better energy storage characteristics due to the advantages of good conductivity, high hardness and the like.
From the prior literature reports, Mo is currently available2The main synthesis methods of the C catalytic material include the following methods: 1) preparation of Mo by propanol reduction method2C (CN201711238001.X preparation of Mo by reduction of propanol2C powder method) uses cheap propanol as a reduction raw material, propanol steam taking argon as a carrier directly contacts and reacts with molybdenum oxide powder at a low temperature of 800-1150 ℃ to produce Mo2C powder products greatly improve the reduction efficiency and simultaneously carry out carbonization, but the method cannot ensure the purity of molybdenum carbide; 2) chemical vapor deposition (ACS appl. mater. interfaces,2011,3,517) gasifies a molybdenum source and a carbon source by using a chemical vapor deposition method and then deposits the molybdenum source and the carbon source into nano particles, and the method has the main defects that the method has higher requirements on temperature and atmosphere, is expensive in cost and is not suitable for industrial production; 3) high temperature carbonization (Energy)&Environmental Science,2013,6,943) carbonization of oxides of metal species, mainly molybdenum, with carbon or carbon monoxide at high temperature, as in the CVD process, which produces Mo2C, the reaction temperature is high; 4) temperature Programmed Reaction (TPR), (Catalysis Letters,2015,145,875) from molybdenum oxides (nitrides)The method is the method which is most applied in the existing carbide synthesis literature, and because the method uses hydrogen as one of reaction gases, uncertain safety hazards exist when the method is used for synthesizing carbide. In addition to the above-mentioned methods, there are a carbothermic method, a solvothermal reduction method, a metal precursor cracking method, an ultrasonic method, a microwave method, a hydrothermal method and the like, but Mo cannot be solved by these methods as well2The yield in the production process is low, the preparation method is complex and the like.
Therefore, a novel Mo preparation method which is simple in process, low in cost, environment-friendly and good in safety performance is sought2The method of the C nanometer material is very necessary.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a transition metal carbide Mo which is simple and convenient in method, free of pollution and low in cost2And C, a preparation method of the material. The method has the advantages of short reaction time, simple process conditions and easy batch production.
The technical scheme is as follows: mo of the invention2The simple preparation method of the material C is characterized by comprising the following steps: the method comprises the following steps:
s1: adding molybdate and sucrose into deionized water, and stirring until the molybdate and the sucrose are completely dissolved;
s2: drying the solution obtained in the step S1 in a vacuum drying oven at 80 ℃, and collecting precursor powder;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with argon at 5 ℃ for min-1Heating to 800 ℃ and preserving the temperature for 5 hours, cooling to room temperature and collecting the obtained powder sample, namely Mo2C。
As a preferred embodiment of the above technical solution, the sucrose in step S1 may also be selected from other sugars as a carbon source;
preferably, in the step S2, the drying method is drying in a vacuum drying oven at 80 ℃;
as a preferable aspect of the above technical meansThe temperature increase rate in the step S3 is 5 ℃ min-1；
Preferably, in the step S3, the roasting temperature is 700-900 ℃, and the roasting time is 4-10 h;
has the advantages that: compared with the prior art, the invention has the following beneficial effects:
(1) mo of the invention2The preparation method of the C nano material has low requirement on preparation conditions, and the used raw materials are cheap and easy to obtain. Not only solves the problem of environmental pollution, but also obtains a cheap catalyst with high catalytic performance, and has the prospect of large-scale commercial application;
(2) prepared Mo2The C nano material has rich pore structure and large specific surface area, and is beneficial to the diffusion of reactants and the exposure of active sites;
(3) mo prepared by the method2The C nano material is expected to be applied to the fields of electrode catalytic materials of lithium-sulfur batteries, photocatalytic materials and the like.
Drawings
FIG. 1 shows Mo synthesized in example 2 of the present invention2XRD pattern of material C;
FIG. 2 shows Mo synthesized in example 2 of the present invention2SEM image of material C;
FIG. 3 shows Mo synthesized in example 2 of the present invention2Raman plot of material C;
FIG. 4 shows Mo synthesized in example 2 of the present invention2C, a nitrogen absorption and desorption curve chart of the material C;
FIG. 5 shows Mo synthesized in example 2 of the present invention2Pore size distribution of material C.
Detailed Description
The invention prepares Mo through simple process design2The preparation conditions of the C nano material are mild, the used raw materials are cheap and easy to obtain, the problem of environmental pollution is solved, the cheap catalyst with high catalytic performance is prepared, and the C nano material has a prospect of large-scale commercial application. Produced Mo2The C nano material has abundant pore structures and large specific surface area, which is beneficial to rapid diffusion of reactants and exposure of active sites. At the same time, preparedMo2The C nano material is expected to be applied to electrode catalytic materials and photocatalytic materials of lithium-sulfur batteries.
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments and the drawings, and it is obvious that the described embodiments are some, not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.3g of ammonium molybdate and 0.5g of sucrose are dissolved and dispersed in 20ml of deionized water;
s2: drying the dispersed solution of S1 in a vacuum drying oven at 80 ℃, and collecting powder materials;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 5 ℃ for a period of min-1The temperature is raised to 700 ℃ and roasted for 5 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely the sample 1;
example 2:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.3g of ammonium molybdate and 0.5g of sucrose are dissolved and dispersed in 20ml of deionized water;
s2: drying the dispersed solution of S1 in a vacuum drying oven at 80 ℃, and collecting powder materials;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 5 ℃ for a period of min-1The temperature is raised to 800 ℃ and roasted for 5 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely the sample 2;
mo prepared in this example2The XRD pattern of the C nano material is shown in figure 1. The results show that: mo2The micro-nano material C has a stronger diffraction peak at the 2 theta-40 DEG positionAnd other strong peaks (angle of 2 theta 35 deg., 61.2 deg., 69.8 deg.) and Mo2The peaks of the C standard card (JCPDS NO.35-0787) are identical, thereby proving that the method successfully prepares the hexagonal Mo2And C, material. Prepared Mo2SEM image of C material is shown in FIG. 2, and is composed of Mo2C, nano-particles.
Mo prepared in this example2Raman diagram of the micro-nano material C is shown in FIG. 3, and the obtained material is 872 cm and 788cm-1Generates a Raman peak with larger intensity corresponding to the generated Mo2C nano material proves that Mo is successfully prepared by the method2And C, material.
Mo prepared in this example2The nitrogen adsorption and desorption curves and the pore size distribution diagram of the material C are shown in FIGS. 4 and 5. According to the analysis of FIG. 4, Mo is obtained2The specific surface area of the C material is 10.1m2g-1This result exhibits a large specific surface area. From Mo2On the pore size distribution diagram of C, we see that the size of pores is mainly concentrated near 1.8nm, which is beneficial to exposing more active sites and improving the electrochemical energy storage performance.
Example 3:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.3g of ammonium molybdate and 0.5g of sucrose are dissolved and dispersed in 20ml of deionized water;
s2: drying the dispersed solution of S1 in a vacuum drying oven at 80 ℃, and collecting powder materials;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 5 ℃ for a period of min-1The temperature is raised to 800 ℃ and roasted for 10 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely a sample 3;
example 4:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.6g of ammonium molybdate and 0.5g of sucrose are dissolved and dispersed in 20ml of deionized water;
s2: drying the dispersed solution of S1 in a vacuum drying oven at 80 ℃, and collecting powder materials;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 5 ℃ for a period of min-1The temperature is raised to 800 ℃ and roasted for 5 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely a sample 4;
example 5:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.3g of ammonium molybdate and 0.5g of sucrose are dissolved and dispersed in 20ml of deionized water;
s2: carrying out spray drying on the solution dispersed in the S1 to obtain a powder material, wherein the spray drying parameters are set to 120 ℃ at an inlet temperature and 500ml h at a flow rate-1；
S3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 5 ℃ for a period of min-1The temperature is raised to 800 ℃ and roasted for 5 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely the sample 5;
example 6:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.3g of ammonium molybdate and 0.5g of sucrose are dissolved and dispersed in 20ml of deionized water;
s2: drying the dispersed solution of S1 in a vacuum drying oven at 80 ℃, and collecting powder materials;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 2 ℃ for 2 min-1The temperature is raised to 800 ℃ and roasted for 5 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely the sample 6;
example 7:
the embodiment discloses a Mo2The simple preparation method of the C nano material comprises the following steps:
s1: 0.3g of ammonium molybdate and 0.5g of glucose were dissolved and dispersed in 20ml of deionized water;
s2: drying the dispersed solution of S1 in a vacuum drying oven at 80 ℃, and collecting powder materials;
s3: a sample of the powder obtained in S2 was placed in a tube furnace filled with inert gas at 5 ℃ for a period of min-1The temperature is raised to 800 ℃ and roasted for 5 hours at the temperature, and the obtained powder sample is collected after being cooled to room temperature, namely the sample 7.
Claims (6)
1. Mo2The simple preparation method of the C nano material is characterized by comprising the following steps: the method comprises the following steps:
s1: respectively adding ammonium molybdate and sucrose into deionized water, and stirring until the ammonium molybdate and the sucrose are completely dissolved;
s2: drying the solution obtained in the step S1 in a vacuum drying oven at the temperature of 80 ℃, and collecting precursor powder;
s3: the precursor material obtained in S2 was placed in a tube furnace filled with argon at 5 ℃ for min-1The temperature rise rate is increased to 800 ℃, the mixture is sintered for 5 hours at 800 ℃, and the obtained powder sample is collected after the mixture is cooled to room temperature, namely Mo2C。
2. The transition metal carbide Mo of claim 12The preparation method of the C nano material is characterized by comprising the following steps: the sucrose in step S1 may also be selected from other saccharides as carbon source.
3. The transition metal carbide Mo of claim 12The preparation method of the C nano material is characterized by comprising the following steps: the drying mode in the step S2 is vacuum drying oven drying at 80 ℃.
4. The transition metal carbide Mo of claim 12The preparation method of the C nano material is characterized by comprising the following steps: the temperature rise rate in the step S3 is 5 ℃ min-1。
5. The transition gold according to claim 1Metal carbide Mo2The preparation method of the C nano material is characterized by comprising the following steps: the roasting temperature in the step S3 is 700-900 ℃, and the constant temperature time is 4-6 h.
6. Mo obtainable by a synthesis process according to one of claims 1 to 52And C, nano-materials.
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