CN111761074B - Preparation method of carbon-loaded nano high-entropy alloy particle composite material - Google Patents
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Abstract
The invention belongs to the field of novel material preparation processes, and provides a preparation method of a carbon-supported nano high-entropy alloy particle composite material, which is simple in operation process and capable of reducing production cost. Specifically, an organic network precursor containing multiple metal ions is obtained by adopting a metal complex polymerization reaction, and the carbon-loaded nano high-entropy alloy particle composite material with high purity and uniformly dispersed alloy particles is obtained after the organic network precursor is subjected to a high-temperature reduction reaction. The invention can realize the adjustment of the components of the high-entropy alloy through the selection of the metal nitrate, and then realize the size control of the nano high-entropy alloy through the regulation of the molar ratio of the metal salt to the organic polymer and the selection of the complexing agent.
Description
Technical Field
The invention belongs to the field of novel material preparation processes, and particularly relates to a preparation method of a carbon-loaded nano high-entropy alloy particle composite material.
Background
The high-entropy alloy is a novel alloy material, and compared with the traditional alloy, the high-entropy alloy has the characteristic of adjustable performance due to the unique composition, and opens up a new design method for improving the performances of high temperature resistance, corrosion resistance, irradiation resistance, oxidation resistance and the like of the alloy material. Therefore, the high-entropy alloy has important application prospects in the fields of nuclear energy, high and low temperature resistant devices, solar heat utilization devices and the like.
The preparation of the high-entropy alloy powder has very important significance for the performance research and application of the alloy. Chinese patent 201710819270.9 adopts gas atomization method and mechanical alloying method to prepare high-entropy alloy powder, and the average grain diameter of the alloy powder is 10-20 microns. Chinese patent 201910028042.9 also adopts gas atomization method to prepare high-entropy alloy powder, and the average grain diameter of the alloy is tens of microns. Chinese patent 201911267043.5 discloses a method for preparing high-entropy alloy powder by fused salt electrodeposition, wherein the grain size of the alloy is less than 100 microns. The size of the material affects the properties of the material, especially in the field of catalysis. However, the prepared high-entropy alloy powder has larger size, and the development of the performance of the high-entropy alloy powder is influenced, so that the preparation of the nano high-entropy alloy and the composite material thereof has very important application value in the research and industrial fields.
At present, a group of the Hulian (Science 359.6383(2018): 1489-. Nirmal (Journal of Materials Science 53.19(2018): 13411-. Schuhmann (Advanced Energy Materials 8.34(2018):1802269) prepares a nano high-entropy alloy material by sputtering metal into ionic liquid, the work is important contribution to the research and application of the nano high-entropy alloy and the composite material thereof, but the work needs expensive special equipment, and the research and application of the nano high-entropy alloy and the composite material thereof are greatly limited, so that the preparation of the nano high-entropy alloy and the composite material thereof with adjustable components and controllable sizes by adopting a method with low cost and simple operation is necessary for the research and application of the nano high-entropy alloy and the composite material thereof.
Disclosure of Invention
Aiming at the defects of the existing novel material preparation technology, the invention provides a preparation method of a carbon-loaded nano high-entropy alloy particle composite material.
The technical scheme adopted by the invention is as follows:
a preparation method of a carbon-supported nano high-entropy alloy particle composite material is characterized by comprising the following steps:
step one, dissolving a complexing agent in water or ethanol according to the concentration of 0.01-10g/mL, adding polyhydric alcohol, and stirring at 50-90 ℃ to obtain a uniform and transparent mixed solution 1;
step two, adding metal salts into the mixed solution 1 one by one, and stirring to obtain a mixed solution 2;
stirring the mixed solution 2 at a set temperature for 1-48 hours to obtain an organic network precursor containing multiple metal ions;
and step four, carrying out high-temperature reduction reaction on the organic network precursor in a protective or reducing atmosphere according to a set temperature rise system to obtain the carbon-loaded nano high-entropy alloy particle composite material.
Further, in the first step, the complexing agent may be one or a combination of several of citric acid, oxalic acid, tartaric acid, lactic acid, and salicylic acid.
Further, in the first step, the polyhydric alcohol may be one or a combination of ethylene glycol, propylene glycol, glycerol and polyethylene glycol.
Further, in the first step, the molar amount of the polyhydric alcohol in the mixed solution 1 is 1 to 10 times of the molar amount of the complexing agent.
Further, In the second step, the metal salts may be 5 to 11 kinds of nitrates or alkoxides containing Mg, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ba, In.
Further, in the second step, the molar total amount of the metal ions in the mixed solution 2 is 0.005-0.5 times of the molar amount of the complexing agent, and the content of each metal ion is 5% -35% of the total amount of the metal ions.
Further, in the third step, the set temperature is 100-.
Further, in the third step, the multi-element metal ions are 5-11 of Mg, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu and Zn.
Further, in the fourth step, the protective reducing gas is one of nitrogen, argon, a hydrogen-argon mixture and hydrogen.
Further, in the fourth step, the temperature-raising rate in the temperature-raising system is 1-20 ℃/min, the reaction temperature is 600-1200 ℃, and the reaction time is 1-12 hours.
The principle of the invention is as follows: according to the invention, an organic network precursor containing multiple metal ions is obtained by adopting a metal complex polymerization reaction, the carbon-loaded nano high-entropy alloy particle composite material with high purity and uniform dispersion of alloy particles is obtained by the organic network precursor through a high-temperature reduction reaction, the components of the high-entropy alloy particles are adjustable by selecting metal nitrate, and the size of the nano high-entropy alloy particles is controllable by regulating the molar ratio of metal salt to organic polymer and the selection of a complexing agent.
The invention has the beneficial effects that:
1. the components of the nano high-entropy alloy particles are adjusted by adjusting and controlling the selection of the metal salt, so that the components of the nano high-entropy alloy particles are controllable;
2. the controllable size of the nanometer high-entropy alloy particles is realized by regulating and controlling the ratio of the metal salt to the complexing agent and the selection of the complexing agent;
3. the prepared carbon-loaded nano high-entropy alloy particle composite material has the advantages that the nano high-entropy alloy particles are uniformly distributed on the surface of the carbon material, the particle size can be controlled to be several nanometers to hundreds of nanometers, and more possibilities are provided for developing the application of the nano high-entropy alloy material;
4. the preparation process of the invention has simple operation and low cost.
Drawings
Fig. 1 is the XRD phase results for the carbon-supported nano high-entropy alloy particle composite prepared in example 1.
Fig. 2 is a transmission electron microscope picture of the carbon-supported nano high-entropy alloy particle composite material prepared in example 1.
Fig. 3 is a transmission electron microscope picture of the carbon-supported nano high-entropy alloy particle composite material prepared in example 3.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which a person skilled in the art can, without any creative effort, fully implement the present invention.
The specific embodiment of the invention is as follows:
example 1
A preparation method of a carbon-supported nano high-entropy alloy particle composite material comprises the following steps: (1) dissolving citric acid in water according to the concentration of 0.01g/mL, adding glycerol according to 6 times of the molar weight of the citric acid, and stirring at 90 ℃ to obtain a uniform and transparent mixed solution 1; (2) adding nitrates of Al, Fe, Co, Ni and Cu into the mixed solution 1 one by one according to the molar weight of 0.02 of citric acid, wherein the molar ratio of Al, Fe, Co, Ni and Cu is 1:1:1:0.8, and stirring to obtain a mixed solution 2; (3) stirring the mixed solution 2 at 300 ℃ for 1 hour to obtain an organic network precursor containing multiple metal ions; (4) and heating the precursor to 900 ℃ at the speed of 5 ℃/min under the hydrogen atmosphere, preserving the heat for 2 hours, and carrying out high-temperature reduction reaction to obtain the carbon-loaded nano high-entropy alloy particle composite material. The main components of the prepared sample are shown in figure 1, the sample is a high-entropy alloy with carbon and FCC structures, a transmission electron microscope photo is shown in figure 2, the nano high-entropy alloy is uniformly distributed on the surface of carbon, and the size of the nano high-entropy alloy is 5-20 nm.
Example 2
A preparation method of a carbon-supported nano high-entropy alloy particle composite material comprises the following steps: (1) dissolving oxalic acid in ethanol according to the concentration of 2g/mL, adding polyethylene glycol according to 2 times of the molar weight of the oxalic acid, and stirring at 80 ℃ to obtain a uniform and transparent mixed solution 1; (2) adding isopropoxides of Mg, Al, Fe, Ni, Cu and Ti into the mixed solution 1 one by one according to the molar weight of 0.02 of oxalic acid, wherein the molar ratio of Mg, Al, Fe, Ni, Cu and Ti is 0.5:0.5:1: 0.5:0.3, and stirring to obtain a mixed solution 2; (3) stirring the mixed solution 2 at 250 ℃ for 24 hours to obtain an organic network precursor containing multiple metal ions; (4) and (3) heating the precursor to 1200 ℃ at the speed of 3 ℃/min under the atmosphere of hydrogen-argon mixed gas, preserving the temperature for 12 hours, and carrying out high-temperature reduction reaction to obtain the carbon-loaded nano high-entropy alloy particle composite material.
Example 3
A preparation method of a carbon-supported nano high-entropy alloy particle composite material comprises the following steps: (1) dissolving malic acid in water according to the concentration of 5g/mL, adding ethylene glycol according to 10 times of the molar weight of the malic acid, and stirring at 70 ℃ to obtain a uniform and transparent mixed solution 1; (2) adding nitrates of Mg, Al, Fe, Ni and Co into the mixed solution 1 one by one according to the molar weight of 0.05 of the malic acid, wherein the molar ratio of Mg, Al, Fe, Ni and Co is 0.5:1:1:1, and stirring to obtain a mixed solution 2; (3) stirring the mixed solution 2 at 100 ℃ for 8 hours to obtain an organic network precursor containing multiple metal ions; (4) and heating the precursor to 700 ℃ at a speed of 20 ℃/min under the argon atmosphere, preserving the heat for 4 hours, and carrying out high-temperature reduction reaction to obtain the carbon-loaded nano high-entropy alloy particle composite material. The transmission electron microscope photograph of the prepared sample is shown in fig. 3, the nano high-entropy alloy is uniformly distributed on the surface of the carbon, and the size of the nano high-entropy alloy is 5-50 nm.
Example 4
A preparation method of a carbon-supported nano high-entropy alloy particle composite material comprises the following steps: (1) dissolving malic acid in ethanol according to the concentration of 10g/mL, adding propylene glycol according to 3 times of the molar weight of the malic acid, and stirring at 90 ℃ to obtain a uniform and transparent mixed solution 1; (2) adding isopropoxides of Ti, V, Cr, Ni and Zn into the mixed solution 1 one by one according to 0.1 time of the molar weight of malic acid, wherein the molar ratio of Ti, V, Cr, Ni and Zn is 0.3:0.3:0.5:1:1, and stirring to obtain a mixed solution 2; (3) stirring the mixed solution 2 at 160 ℃ for 4 hours to obtain an organic network precursor containing multiple metal ions; (4) and heating the precursor to 800 ℃ at a speed of 10 ℃/min under the nitrogen atmosphere, preserving the heat for 8 hours, and carrying out high-temperature reduction reaction to obtain the carbon-loaded nano high-entropy alloy particle composite material.
Example 5
A preparation method of a carbon-supported nano high-entropy alloy particle composite material comprises the following steps: (1) dissolving salicylic acid in water according to the concentration of 0.01g/mL, adding glycol according to 3 times of the molar weight of the salicylic acid, and stirring at 60 ℃ to obtain a uniform and transparent mixed solution 1; (2) adding isopropoxides of Cr, Mn, Fe, Co and Ni into the mixed solution 1 one by one according to the molar weight of 0.03 of salicylic acid, wherein the molar ratio of Cr, Mn, Fe, Co and Ni is 0.5:1:1:1, and stirring to obtain a mixed solution 2; (3) stirring the mixed solution 2 at 140 ℃ for 16 hours to obtain an organic network precursor containing multiple metal ions; (4) and heating the precursor to 600 ℃ at the speed of 3 ℃/min under the hydrogen atmosphere, preserving the heat for 1 hour, and carrying out high-temperature reduction reaction to obtain the carbon-supported nano high-entropy alloy particle composite material.
While the preferred embodiments of the invention have been described, it is to be understood that the invention is not limited to the precise embodiments described, and that equipment and structures not described in detail are understood to be practiced as commonly known in the art; any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention by those skilled in the art can be made without departing from the technical scope of the present invention, and still fall within the protection scope of the technical solution of the present invention.
Claims (7)
1. A preparation method of a carbon-supported nano high-entropy alloy particle composite material is characterized by comprising the following steps:
step one, dissolving a complexing agent in water or ethanol according to the concentration of 0.01-10g/mL, adding polyhydric alcohol, and stirring at 50-90 ℃ to obtain a uniform and transparent mixed solution 1;
step two, adding metal salts into the mixed solution 1 one by one, and stirring to obtain a mixed solution 2;
stirring the mixed solution 2 at a set temperature for 1-48 hours to obtain an organic network precursor containing multiple metal ions;
performing high-temperature reduction reaction on the organic network precursor in a protective or reducing atmosphere according to a set temperature rise system to obtain the carbon-loaded nano high-entropy alloy particle composite material;
in the first step, the complexing agent is one or a combination of more of citric acid, oxalic acid, tartaric acid, lactic acid and salicylic acid;
in the third step, the set temperature is 100-250 ℃;
in the fourth step, the heating rate in the heating system is 1-20 ℃/min, the reaction temperature is 600-1200 ℃, and the reaction time is 1-12 hours.
2. The method for preparing the carbon-supported nano high-entropy alloy particle composite material as claimed in claim 1, wherein in the first step, the polyhydric alcohol is one or a combination of ethylene glycol, propylene glycol, glycerol and polyethylene glycol.
3. The method for preparing the carbon-supported nano high-entropy alloy particle composite material as claimed in claim 1, wherein, in the first step, the molar amount of the polyhydric alcohol in the mixed solution 1 is 1-10 times of that of the complexing agent.
4. The method for preparing the carbon-supported nano high-entropy alloy particle composite material as claimed In claim 1, wherein In the second step, the metal salt is 5 to 11 of nitrates or alkoxides containing Mg, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ba and In.
5. The method for preparing the carbon-supported nano high-entropy alloy particle composite material according to claim 1, wherein, in the second step, the molar total amount of the metal ions in the mixed solution 2 is 0.005-0.5 times of the molar amount of the complexing agent, and the content of each metal ion is 5% -35% of the total amount of the metal ions.
6. The method for preparing the carbon-supported nano high-entropy alloy particle composite material of claim 1, wherein in the third step, the multi-element metal ions are 5-11 of Mg, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu and Zn.
7. The method for preparing the carbon-supported nano high-entropy alloy particle composite material according to claim 1, wherein in the fourth step, the protective or reducing atmosphere is one of nitrogen, argon, a hydrogen-argon mixture and hydrogen.
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