CN114023934A - Preparation method and application of metal/carbide/oxide composite nano material - Google Patents

Preparation method and application of metal/carbide/oxide composite nano material Download PDF

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CN114023934A
CN114023934A CN202111177687.2A CN202111177687A CN114023934A CN 114023934 A CN114023934 A CN 114023934A CN 202111177687 A CN202111177687 A CN 202111177687A CN 114023934 A CN114023934 A CN 114023934A
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metal
carbide
oxide composite
temperature
preparation
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乔秀清
王紫昭
胡杰杰
侯东芳
李东升
兰亚乾
张其春
刘彬
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China Three Gorges University CTGU
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    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method and application of a metal/carbide/oxide composite nano material, belonging to the field of nano material preparation. The invention adopts a one-step in-situ thermal decomposition reduction method, firstly, a carbonaceous organic complex is adopted to prepare a precipitate of high-melting-point metal through a complex reaction, then the prepared complex precipitate of the high-melting-point metal is subjected to in-situ thermal decomposition at high temperature, C generated by high-temperature pyrolysis of the organic complex has strong reducibility at high temperature, an oxide generated by the high-temperature pyrolysis can be gradually reduced into a carbide and a metal, and the composition of the product can be regulated and controlled by controlling the reaction temperature and time, so that the metal-carbide-oxide nano particle composite material is obtained. The invention adopts a one-step method to prepare the refractory metal and the carbon oxide composite material thereof, has simple process, economy and environmental protection compared with the prior high-temperature smelting method, and is suitable for batch production.

Description

Preparation method and application of metal/carbide/oxide composite nano material
Technical Field
The invention relates to a preparation method and application of a high-melting-point metal-carbide-oxide composite nano material, belonging to the field of nano material preparation.
Background
The refractory metal is a metal element with a melting point higher than 1650 ℃, has excellent mechanical property, conductivity, high-temperature strength, corrosion resistance, oxidation resistance and the like, and is widely applied to the technical fields of aerospace, national defense, ferrous metallurgy and other modern industries. At present, the refractory metals in the periodic table include 10 metals such as tungsten, molybdenum, niobium, vanadium, zirconium, etc. Because the melting point of metal is higher, the preparation process of the material is complex, and the preparation of refractory metal nano particles with good dispersity and uniform size is difficult. Meanwhile, the industrial cost for preparing the nano particles is high, the continuity is poor, and the wide application of the metal is restricted. Therefore, a simple and low-cost preparation method is developed to obtain the refractory metal nanoparticles, and the industrial application of the refractory metal can be promoted.
In recent years, attention has been paid to a refractory metal, and a carbide, an oxide, a nitride and the like thereof, in the fields of catalysis, a supercapacitor, a lithium ion battery and the like. For example, metal carbides have recently proven to be an effective material for electrocatalytic decomposition of water to produce hydrogen. However, the preparation process of the refractory metal compound is relatively complex, the research on the compound is less, and the relationship between the structure and the performance of the material is still unclear. Meanwhile, as the valence state of the refractory compound is more, different valence states have different influences on the material performance. Therefore, the controllable preparation of the refractory compound components with different valence states can be helpful for analyzing the influence of the structure and chemical valence of the material on the material performance.
Disclosure of Invention
The invention aims to provide a preparation method and application of a novel high-melting-point metal-carbide-oxide composite nano material.
The high melting point metal can be any one or any combination of tungsten, molybdenum, niobium, tantalum, vanadium, zirconium and the like. The relative contents of metal, carbide and oxide can be controlled by changing the process flow of in-situ thermal decomposition reduction.
The composite nano material is prepared by adopting a one-step in-situ thermal decomposition reduction method, and the nano materials have stronger interface contact.
A composite nano-class refractory metal-carbide-oxide material is prepared from the refractory metal, metal carbide and metal oxide through regular arrangement and in-situ thermal decomposing reduction.
The preparation method of the high-melting-point metal-carbide-oxide composite nano material adopts an in-situ pyrolysis reduction method, and comprises the following steps of:
(1) mixing a certain amount of carbon-containing organic complex such as dicyandiamide, sodium alginate, aniline, hexamethylenetetramine, melamine or glucose with the prepared metal anion oxygen-containing salt solution according to a molar ratio of 20: 1-15: 1, preparing a mixed solution, and stirring the mixed solution in a water bath at the temperature of 40-70 ℃ for 4-12 hours to obtain a precipitate;
(2) drying the obtained precipitate in vacuum, and then carrying out high-temperature in-situ thermal decomposition reduction reaction for 1-5 h at the temperature of 920-1020 ℃ in the inert atmosphere of nitrogen to obtain the high-melting-point metal-carbide-oxide composite nano material.
In the method, in step 1, the concentration of the carbon-containing organic complex is preferably 0.5 to 1.2 mol/L, and the concentration of the anionic oxysalt is preferably 0.02 to 0.1 mmol/L.
The metal salt solution comprises any one of ammonium molybdate, sodium tungstate and ammonium tungstate as an anion salt.
The high-melting-point metal-carbide-oxide composite nano material prepared by the invention has a regularly arranged structure.
The photocatalyst material accelerant prepared by the invention promotes photocatalytic separation of photocatalytic reagentThe photocatalyst comprises CdS and TiO2、C3N4、ZnIn2S4Any one of them.
The addition amount of the photocatalyst material accelerant is 20-30wt% of the mass of the photocatalyst, and the toxic pollutants comprise one or more of metal cations, organic dyes, rhodamine B, polychlorinated biphenyl and nitenpyram.
The prepared photocatalytic material accelerant is applied to preparation of an electrocatalytic hydrogen evolution material.
The prepared photocatalytic material accelerant is applied to the preparation of lithium ion battery cathode materials.
Compared with the prior art, the high-melting-point metal-carbide-oxide composite nano material prepared by the invention has the beneficial effects that:
the composite nano material is composed of three materials with different chemical valence states of refractory metal, the nano material inherits the appearance of a precursor and has better regular arrangement, nano particles are generated by in-situ carbonization-reduction, the particles have better interface structure contact, and the dispersibility of the nano particles is better. The preparation method is simple, can be obtained by a one-step thermal decomposition reduction method, has low cost of raw materials and high yield, and is suitable for industrial production. The nano-particles obtained by the method have many active sites and strong interface contact, and have great advantages when being used in the fields of catalysis, supercapacitors, lithium ion batteries and the like.
Drawings
FIG. 1: the XRD pattern of the refractory metal-carbide-oxide composite nanomaterial prepared in example 1 is shown.
FIG. 2: is a scanning electron microscope picture of the refractory metal-carbide-oxide composite nanomaterial prepared in example 1.
FIG. 3: a graph of hydrogen produced by photocatalytic decomposition of water for the high melting point molybdenum-molybdenum carbide-molybdenum oxide-CdS composite nanomaterial prepared in example 4.
FIG. 4: is a performance test chart of the battery material prepared in example 6.
FIG. 5: the gas sensitive material prepared for example 7 was used to measure the performance of ethanol.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present disclosure and fall within the scope of the appended claims.
Example 1
The preparation method of the metal/carbide/oxide composite nano material comprises the following steps:
(1) mixing 36 mmol aniline solution with concentration of 0.8mol/L with 2mmol prepared ammonium molybdate solution with concentration of 0.05mol/L, and stirring the mixed solution in water bath at 50 ℃ for 8h to obtain precipitate;
(2) drying the obtained precipitate in vacuum for 8h, and then carrying out high-temperature in-situ thermal decomposition reduction reaction at 950 ℃ in nitrogen atmosphere for 3h to obtain the final product, namely the high-melting-point metal-carbide-oxide composite nano material.
XRD diffraction pattern analysis of the prepared high-melting-point metal-carbide-oxide composite nano material proves that the prepared composite nano material contains molybdenum oxide, molybdenum carbide and metal molybdenum. The scanning electron microscope is shown in fig. 1, and it can be seen from the figure that the composite nano material is formed by regularly arranging nano particles.
Example 2
The preparation method of the metal/carbide/oxide composite nano material comprises the following steps:
(1) mixing 36 mmol alginic acid solution with concentration of 0.8mol/L with 2mmol prepared ammonium molybdate solution with concentration of 0.05mol/L, and stirring the mixed solution in water bath at 50 ℃ for 8h to obtain precipitate;
(2) drying the obtained precipitate in vacuum for 8h, and then carrying out high-temperature in-situ thermal decomposition reduction reaction at 950 ℃ in nitrogen atmosphere for 3h to obtain the final product, namely the high-melting-point molybdenum-molybdenum carbide-molybdenum oxide composite nano material.
Example 3
The preparation method of the metal/carbide/oxide composite nano material comprises the following steps:
(1) mixing 36 mmol of 0.8mol/L hexamethylenetetramine and 2mmol of 0.05mol/L prepared sodium tungstate solution, and stirring the mixed solution in a water bath at the temperature of 60 ℃ for 8 hours to obtain a precipitate;
(2) drying the obtained precipitate in vacuum for 8h, and then carrying out high-temperature in-situ thermal decomposition reduction reaction for 5h at 950 ℃ in nitrogen atmosphere to obtain the final product high-melting-point tungsten-tungsten carbide-tungsten oxide composite nano material.
Example 4
The high-melting-point molybdenum-molybdenum carbide-molybdenum oxide composite nano material prepared in the embodiment 1 and a CdS photocatalytic material prepared in advance are ultrasonically mixed in a methanol solution, and the CdS photocatalytic material is mixed according to the mass percentage of 20-40%. The preparation process of the CdS comprises the following steps: 16.2 mmol of thiourea containing 48.6 mmol of cadmium nitrate tetrahydrate is dissolved in 80ml of ethylenediamine and stirred vigorously to obtain a transparent light green solution, then 40ml of the solution is put into a reaction kettle to react for 24h at 160 ℃, and finally the faint yellow CdS photocatalytic material is obtained. And (3) ultrasonically dispersing 100mg of CdS photocatalytic material and 30mg of metal-carbide-oxide composite nano material in 50ml of methanol solution, and ultrasonically treating for 30min to obtain the composite material. And (3) placing 30mg of the compounded material in a reaction container, adding 8ml of lactic acid and 80ml of aqueous solution into the reaction container, and carrying out a photocatalytic hydrogen production test under a xenon lamp light source with a 420nm optical filter. The hydrogen production performance is shown in FIG. 3. It can be seen that when the mass of the molybdenum-molybdenum carbide-molybdenum oxide composite nano material is different, the photocatalytic hydrogen production activity is different, and when the mass percentage is 20%, the photocatalytic hydrogen production activity of the composite material is 20 mmol/h*g, more than 9 times that of pure CdS.
Example 5
The refractory metal-carbide-oxide composite nanomaterial prepared in example 2 was used for electrocatalytic hydrogen evolution. The electrode was prepared as follows: dispersing 4 mg of catalyst in 500. mu.L of 0.5 wt% Nafion solution, ultrasonically dispersing for 1h, and dropwise adding 4. mu.L of the uniform solution to platinum with diameter of 3mmThe loading of the catalyst on the carbon electrode was about 0.453 mg cm−2And drying the obtained electrode in the air to obtain a working electrode, wherein the Pt wire is used as a counter electrode, and the saturated calomel electrode is used as a reference electrode. Electrocatalytic hydrogen evolution at 0.5M H2SO4In solution. The test result shows that the nano composite material has lower initial over potential (eta) when being used for electrocatalytic hydrogen evolution10=140 mV) and small tafel slope (72 mV dec)−1)。
Example 6
The refractory metal-carbide-oxide composite nanomaterial prepared in example 2 was used in a lithium ion battery material. The electrode was prepared as follows: the nanocomposite was mixed with carbon black and poly (vinyl difluoride) in a mass ratio of 80:10:10 and then attached to a copper foil to a thickness of about 50 um. Pure lithium foil as counter electrode, polypropylene membrane as separator, electrolyte of 1M LiPF6Dissolved in ethylene carbonate/dimethyl carbonate (volume ratio 1: 1), the cell was assembled in a glove box, and then a charge-discharge test was performed. FIG. 4a is 0.2 mV s-1CV curve at the scan rate of (a). FIG. 4b shows the current density at 0.1A cm-2In the case of (3), the 1 st, 2 nd, and 3 rd constant current charge/discharge curves. The coulomb efficiency can reach 95 percent after the circulation is carried out for 200 times under the current density of 50 mA/g.
Example 7
The prepared high-melting-point metal-carbide-oxide composite nano-material prepared in example 3 is used as a gas-sensitive sensing material for detecting ethanol. The gas sensor device was made as follows: a certain amount of powder and ethanol are prepared into uniform paste according to the mass ratio of 9: 1. The paste was brushed on the electrode coated with an Ag-Pd electrode with a distance of 1mm, and the electrode coated with the paste was dried and then used for detecting ethanol gas. The detection limit can reach 5ppm, and the sensitivity of the ethanol with the concentration of 200ppm at 100 ℃ is 26.

Claims (10)

1. The preparation method of the metal/carbide/oxide composite nano material is characterized by comprising the following steps of:
(1) stirring a certain amount of carbon-containing organic complex and a metal salt solution in a water bath for a period of time to obtain a complex precipitate;
(2) and drying the obtained complex precipitate in vacuum, and then carrying out high-temperature in-situ thermal decomposition reduction reaction in an inert atmosphere to obtain the metal/carbide/oxide composite nano material.
2. The method for preparing metal/carbide/oxide composite nanomaterial according to claim 1, wherein the carbon-containing organic complex comprises any one or more of dicyandiamide, sodium alginate, aniline, hexamethylenetetramine, melamine or glucose.
3. The method for preparing a metal/carbide/oxide composite nanomaterial according to claim 1, wherein the concentration of the carbon-containing organic complex is 0.5 to 1.2 mol/L, the concentration of the anion oxysalt is 0.02 to 0.1mmol/L, and the oxygen-containing molar ratio of the carbon-containing organic complex to the anion is 20: 1-15: 1, the water bath stirring temperature is 40-70 ℃, and the stirring time is 4-12 h.
4. The method of claim 1, wherein the metal salt solution comprises an anion salt selected from ammonium molybdate, sodium tungstate and ammonium tungstate.
5. The method for preparing the metal/carbide/oxide composite nanomaterial according to claim 1, wherein the complex precipitate is subjected to high-temperature in-situ thermal decomposition reduction reaction in an inert atmosphere, the inert atmosphere is nitrogen, the temperature of the high-temperature in-situ thermal decomposition reaction is 920-1020 ℃, and the reaction time is 1-5 hours.
6. Use of the metal/carbide/oxide composite nanomaterial prepared according to any one of claims 1 to 5 in promoting photocatalytic reagent to carry out photocatalytic water decomposition to produce hydrogen and degrading toxic pollutants, wherein the photocatalyst comprises CdS and TiO2、C3N4、ZnIn2S4Any one of them.
7. The use according to claim 6, wherein the metal/carbide/oxide composite nanomaterial is added in an amount of 20-30wt% relative to the mass of the photocatalyst, and the toxic contaminant comprises one or more of metal cations, organic dyes, rhodamine B, polychlorinated biphenyl, and nitenpyram.
8. Use of the metal/carbide/oxide composite nanomaterial prepared according to any one of claims 1 to 5 in the preparation of an electrocatalytic hydrogen evolution material.
9. Use of the metal/carbide/oxide composite nanomaterial prepared according to any one of claims 1 to 5 in preparation of a negative electrode material of a lithium ion battery.
10. The application of the metal/carbide/oxide composite nano material prepared according to any one of claims 1 to 5 in preparing a gas-sensitive sensing material, wherein the gas for which the gas-sensitive material aims comprises any one of methanol, ethanol and acetonitrile.
CN202111177687.2A 2021-10-09 2021-10-09 Preparation method and application of metal/carbide/oxide composite nano material Pending CN114023934A (en)

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CN114772646A (en) * 2022-04-29 2022-07-22 福州大学 Preparation method of tungsten oxide nano material and application of tungsten oxide nano material in photocatalytic desulfurization
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