CN114713836A - Synthetic method of Cu-Ag sheet-shaped nano composite material - Google Patents
Synthetic method of Cu-Ag sheet-shaped nano composite material Download PDFInfo
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- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 9
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- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims description 3
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- 238000001878 scanning electron micrograph Methods 0.000 description 8
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention relates to a method for synthesizing a Cu-Ag sheet nano composite material, which comprises the following steps: preparing a Cu nano material precursor: respectively dispersing the template and the copper source into a solvent for uniform dispersion to obtain a first dispersion liquid; mixing the reducing agent and the first dispersion liquid in sequence and heating to obtain a Cu nano material; synthesizing a Cu-Ag sheet nano composite material: separating and washing the prepared Cu nano material, dispersing the Cu nano material into a solvent, and adding a certain amount of template agent to obtain a second dispersion liquid; and dispersing a silver source in a solvent to form a silver source dispersion liquid, adding the silver source dispersion liquid into the second dispersion liquid, and continuously stirring to obtain the Cu-Ag flaky nano composite material. Compared with the prior art, the invention has the advantages of forming a specific interface, generating a unique catalytic site, having strong light absorption performance and the like.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a synthetic method of a Cu-Ag sheet nano composite material.
Background
In recent years, with the development of nano-characterization technology, people have more deep understanding on the microstructure and composition of nano-materials. Among them, metal, semiconductor and metal oxide nanomaterials have special physical and chemical properties due to their nano-size effect, especially in the field of catalysis, and at present, reduction catalysts commonly used for catalysis are based on metal materials.
However, at present, the materials mainly used in this field are precious metals and alloys, and therefore, it is imperative to find a high-efficiency and stable catalyst based on a large amount of non-precious metals. The silver and copper nanoparticles are widely concerned due to high conductivity and catalytic activity, and the copper nanoparticles are ideal catalysts for carbon dioxide reduction, catalytic degradation of pollutants, preparation of methanol by catalyzing glycerol, selective preparation of benzaldehyde by catalyzing toluene and the like.
However, research shows that a specific interface can be formed by doping with other metals, so that a unique catalytic site can be generated, and the catalytic efficiency is improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for synthesizing a Cu-Ag sheet-shaped nano composite material which can form a specific interface, generate a unique catalytic site and has strong light absorption performance.
The purpose of the invention can be realized by the following technical scheme:
a method for synthesizing a Cu-Ag sheet nano composite material comprises the following steps:
preparing a Cu nano material precursor: respectively dispersing the template and the copper source into a solvent for uniform dispersion to obtain a first dispersion liquid;
mixing the reducing agent and the first dispersion liquid in sequence and heating to obtain a Cu nano material;
synthesizing a Cu-Ag sheet nano composite material: separating and washing the prepared Cu nano material, dispersing the Cu nano material into a solvent, and adding a certain amount of template agent to obtain a second dispersion liquid;
and dispersing a silver source in a solvent to form a silver source dispersion liquid, adding the silver source dispersion liquid into the second dispersion liquid, and continuously stirring to obtain the Cu-Ag flaky nano composite material.
Furthermore, the molar ratio of copper to silver in the copper source and the silver source is 1 (0-10), preferably 1 (0-2), and is not 0.
Furthermore, the dosage ratio of the copper source, the template agent and the solvent in the first dispersion liquid is (1-2) mmol, (0-1) g:30mL, and 0 is not taken.
Further, in the second dispersion, the amount ratio of the template to copper was (0.08-0.12) g:1 mmol. The amount of the template in the second dispersion may be 0.08 to 0.12 g.
Furthermore, the molar ratio of the reducing agent to the copper source is (1-3): 1.
Furthermore, in the solution for preparing the Cu nano material, the dosage ratio of the reducing agent to the copper in the copper source to the solvent is (1.8-2.2) mmol to 1mmol to 10 mL.
Further, the ratio of silver to the solvent in the silver source dispersion was (0-2) mmol:10mL, not 0.
Further, the temperature of the heating treatment is 140-180 ℃, and the time is 10min-2 h.
Further, the continuous stirring time is 30min-2 h.
Further, the template agent comprises polyvinylpyrrolidone; the reducing agent comprises fructose.
Further, the copper source comprises copper acetate monohydrate, copper nitrate or copper sulfate; the silver source comprises silver acetate, silver nitrate or silver sulfate.
Further, the solvent comprises ethylene glycol or water.
Furthermore, the material can be applied to the fields of water catalytic decomposition, solar batteries, super capacitors, lithium ion batteries, fuel cells, catalysis and the like.
Compared with the prior art, the invention has the following advantages:
(1) the synthesis method has simple process conditions, safe experimental method and strong experimental result controllability, and can synthesize a large amount of Cu-Ag sheet-shaped nano composite materials;
(2) by controlling the ratio of copper to silver, composite materials with different shapes can be synthesized;
(3) the Cu-Ag sheet nano composite material obtained by the invention is a novel semiconductor nano material and has application prospects in the fields of carbon dioxide catalytic reduction, pollutant degradation, alkaline fuel cell cathode materials and the like.
Drawings
FIG. 1 is an XRD pattern of the materials prepared in examples 1-5;
FIG. 2 is an SEM image of materials prepared in examples 1-5;
FIG. 3 is a TEM image of a material prepared in example 5;
FIG. 4 is a CV image of the material prepared in example 5;
fig. 5 is an SEM image of comparative example 1.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.
A method for synthesizing Cu-Ag sheet-shaped nano composite material comprises the following steps:
preparing a Cu nano material precursor: respectively dispersing the template and the copper source into a solvent for uniform dispersion to obtain a first dispersion liquid; the molar ratio of copper and silver in the copper source and the silver source is 1 (0-10), preferably 1 (0-2), and is not 0. In the first dispersion, the mass-to-volume ratio of the copper source, the template agent and the solvent is (1-2) mmol, (0-1) g, 30mL, and 0 is not selected. Dispersing a reducing agent into a solvent, and mixing the reducing agent and the first dispersion liquid, wherein the molar mass ratio of the reducing agent to the copper source is (1-3): 1. In the solution for preparing the Cu nano material, the molar volume ratio of the reducing agent to the copper in the copper source to the solvent is (1.8-2.2) mmol to 1mmol to 10 mL. The molar mass ratio of the reducing agent, the copper source and the template agent is (1.8-2.2) mmol to 1mmol (0.1-1) g.
Mixing the reducing agent and the first dispersion liquid in sequence and heating to obtain a Cu nano material; the temperature of the heating treatment is 130-. The template agent comprises polyvinylpyrrolidone; the reducing agent comprises fructose. The copper source comprises copper acetate monohydrate, copper nitrate or copper sulfate; the solvent comprises ethylene glycol or water.
Synthesizing a Cu-Ag sheet nano composite material: separating and washing the prepared Cu nano material, dispersing the Cu nano material into a solvent, and adding a certain amount of template agent to obtain a second dispersion liquid; the continuous stirring time is 30min-2 h; in the silver source dispersion, the ratio of silver to the solvent was (0-2) mmol:10mL, not 0. The continuous stirring time is 30min-2 h. The silver source comprises silver acetate, silver nitrate or silver sulfate. The mass molar ratio of the template agent to the copper source is (0.08-0.12) g:1 mmol.
Dispersing a silver source in a solvent to form a silver source dispersion liquid, adding the silver source dispersion liquid into the second dispersion liquid, and continuously stirring for 30min-2 h; the Cu-Ag sheet nano composite material can be applied to the fields of water catalytic decomposition, solar batteries, super capacitors, lithium ion batteries, fuel batteries, catalysis and the like.
Example 1
Under the conditions that the temperature is 160 ℃ and the proportion of Ag and Cu elements is 0:1, the method for synthesizing the Cu nano material comprises the following steps:
(1) dispersing 0.66g of polyvinylpyrrolidone (PVP) and 1mmol of copper acetate into 30mL of ethylene glycol, placing on a magnetic stirrer, and stirring for 30min until the two are completely dispersed into the solvent;
(2) 2mmol of fructose was weighed out and dispersed in 10mL of ethylene glycol and both were dispersed uniformly using a magnetic stirrer. After the dispersion is uniform, pouring the dispersion liquid in the step (1) and the dispersion liquid into a three-neck flask, and then placing the three-neck flask on a magnetic stirrer to heat and stir at the temperature of 160 ℃ for 30 min;
(3) centrifuging the substance obtained after heating in the step (2), washing the substance by deionized water and alcohol, and drying the substance at normal temperature;
in fig. 1, a is an XRD spectrum of example 1, and in fig. 2, b is an SEM image of the material prepared in example 1, from which it can be seen that the sample mainly consists of copper and consists of polyhedrons having a particle size of about 500 nm.
Example 2
The method for synthesizing the Cu-Ag sheet nano composite material comprises the following steps:
(1) dispersing 0.66g of polyvinylpyrrolidone (PVP) and 1mmol of copper acetate into 30ml of ethylene glycol, placing on a magnetic stirrer, and stirring for 30min until the two are completely dispersed into the solvent;
(2) 2mmol of fructose was weighed out and dispersed in 10mL of ethylene glycol and both were dispersed uniformly using a magnetic stirrer. After the dispersion is uniform, pouring the dispersion liquid in the step (1) and the dispersion liquid into a three-neck flask, and then placing the three-neck flask on a magnetic stirrer to heat and stir at the temperature of 160 ℃ for 30 min;
(3) centrifuging the substance obtained in the step (2) to obtain a copper nano material, washing the copper nano material by deionized water and alcohol, dispersing the copper nano material into 20mL of deionized water, adding 0.1g of PVP, and stirring at normal temperature for 30 min;
(4) 0.1mmol of silver acetate was weighed, mixed with 10mL of deionized water, and the silver acetate was dispersed uniformly in the deionized water by stirring and sonication. Then adding the silver acetate dispersion liquid into the solution obtained in the step (3), continuously stirring at normal temperature for 50min, and standing for 24h to obtain the Cu-Ag sheet nano composite material;
in fig. 1, b is the XRD spectrum of example 2, and in fig. 2, b is the SEM image of the material prepared in example 2, which shows that the sample mainly consists of copper and silver, and the morphology appears as a combination of flakes and particles.
Example 3
The method for synthesizing the Cu-Ag sheet nano composite material comprises the following steps:
(1) dispersing 0.66g of polyvinylpyrrolidone (PVP) and 1mmol of copper acetate into 30ml of ethylene glycol, placing on a magnetic stirrer, and stirring for 30min until the two are completely dispersed into the solvent;
(2) 2mmol of fructose was weighed out and dispersed in 10mL of ethylene glycol and both were dispersed uniformly using a magnetic stirrer. After the dispersion is uniform, pouring the dispersion liquid in the step (1) and the dispersion liquid into a three-neck flask, and then placing the three-neck flask on a magnetic stirrer to heat and stir at the temperature of 160 ℃ for 30 min;
(3) centrifuging the substance obtained in the step (2) to obtain a copper nano material, washing the copper nano material by using alcohol and deionized water, dispersing the copper nano material into 20mL of deionized water, adding 0.1g of PVP, and stirring the mixture at normal temperature for 30 min;
(4) 0.5mmol of silver acetate was weighed, mixed with 10mL of deionized water, and the silver acetate was dispersed uniformly in the deionized water by stirring. Then adding the silver acetate dispersion liquid into the solution obtained in the step (3), continuously stirring at normal temperature for 50min, and standing for 24h to obtain a Cu-Ag sheet nano composite material;
in fig. 1, c is the XRD pattern of example 3, in fig. 2, c is the SEM image of the material prepared in example 3, from which it can be seen that the sample mainly consists of copper and silver, and the morphology appears as a morphology in which platelets are combined with a few particles, and in fig. 3, a is the TEM image of example 3, which is seen to partially evolve into platelets.
Example 4
The method for synthesizing the Cu-Ag sheet nano composite material comprises the following steps:
(1) dispersing 0.66g of polyvinylpyrrolidone (PVP) and 1mmol of copper acetate into 30mL of ethylene glycol, placing on a magnetic stirrer, and stirring for 30min until the two are completely dispersed into the solvent;
(2) 2mmol of fructose was weighed out and dispersed in 10mL of ethylene glycol and both were dispersed uniformly using a magnetic stirrer. After the dispersion is uniform, pouring the dispersion liquid in the step (1) and the dispersion liquid into a three-neck flask, and then placing the three-neck flask on a magnetic stirrer to heat and stir at the temperature of 160 ℃ for 30 min;
(3) centrifuging the substance obtained in the step (2) to obtain a copper nano material, washing the copper nano material by deionized water and alcohol, dispersing the copper nano material into 20mL of deionized water, adding 0.1g of PVP, and stirring at normal temperature for 30 min;
(4) 1mmol of silver acetate was weighed, mixed with 10mL of deionized water, and the silver acetate was uniformly dispersed in the deionized water by stirring and sonication. Then adding the silver acetate dispersion liquid into the solution obtained in the step (3), continuously stirring at normal temperature for 50min, and standing for 24h to obtain the Cu-Ag sheet nano composite material;
in fig. 1, d is the XRD spectrum of example 4, and d is the SEM image of the material prepared in example 4, which shows that the sample mainly consists of copper and silver, and the morphology shows a combination of plate-like and particle-like morphology.
Example 5
(1) Dispersing 0.66g of polyvinylpyrrolidone (PVP) and 1mmol of copper acetate into 30ml of ethylene glycol, placing on a magnetic stirrer, and stirring for 30min until the two are completely dispersed into the solvent;
(2) 2mmol of fructose was weighed out and dispersed in 10mL of ethylene glycol and both were dispersed uniformly using a magnetic stirrer. After the dispersion is uniform, pouring the dispersion liquid in the step (1) and the dispersion liquid into a three-neck flask, and then placing the three-neck flask on a magnetic stirrer to heat and stir at the temperature of 160 ℃ for 30 min;
(3) centrifuging the substance obtained in the step (2) to obtain a copper nano precursor, washing the copper nano precursor by deionized water and alcohol, dispersing the copper nano precursor into 20ml of deionized water, adding 0.1g of PVP, and stirring at normal temperature for 30 min;
(4) 2mmol of silver acetate was weighed, mixed with 10mL of deionized water, and the silver acetate was dispersed uniformly in the deionized water by stirring and sonication. Then adding the silver acetate dispersion liquid into the solution obtained in the step (3), continuously stirring at normal temperature for 50min, and standing for 24h to obtain the Cu-Ag sheet nano composite material;
in FIG. 1, e is the XRD pattern of example 5, and in FIG. 2, e is the SEM image of the material prepared in example 5, and it can be seen that the sample mainly consists of copper and silver, and the morphology appears as a complete plate-like morphology. In fig. 3, b is the TEM image of example 4, and the synthesized material package shows uniform distribution of Cu and Ag elements and a sheet structure.
In FIG. 4, a-e are CV curves of examples 1-5, which clearly show stronger oxidation and reduction peaks around 1.2V and 1.0V as the proportion of Ag increases.
Comparative example 1
(1) 0.66g of polyvinylpyrrolidone (PVP) and 1mmol of copper acetate were dispersed in 30ml of ethylene glycol;
(2) weighing 1.5mmol of fructose and dispersing into 10ml of ethylene glycol;
(3) pouring the two into a three-neck flask, and then placing the three-neck flask on a magnetic stirrer to heat and stir at the temperature of 160 ℃ for 2 hours;
(4) 1mmol of silver acetate was weighed to be dispersed into 10ml of ethylene glycol solution and added to the solution of step (2), and stirring was continued with heating at 160 ℃ for 2 hours, followed by obtaining a sample by centrifugation and washing.
Fig. 5 is an SEM image of comparative example 1, and it can be seen that the microstructure of the substance is significantly different from the above-described plate-like nanostructure.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for synthesizing a Cu-Ag sheet nano composite material is characterized by comprising the following steps:
preparing a Cu nano material precursor: respectively dispersing the template and the copper source into a solvent for uniform dispersion to obtain a first dispersion liquid;
mixing the reducing agent and the first dispersion liquid in sequence and heating to obtain a Cu nano material;
synthesizing a Cu-Ag sheet nano composite material: separating and washing the prepared Cu nano material, dispersing the Cu nano material into a solvent, and adding a certain amount of template agent to obtain a second dispersion liquid;
and dispersing a silver source in a solvent to form a silver source dispersion liquid, adding the silver source dispersion liquid into the second dispersion liquid, and continuously stirring to obtain the Cu-Ag flaky nano composite material.
2. The method for synthesizing a Cu-Ag plate-shaped nano composite material according to claim 1, wherein the molar ratio of copper to silver in the copper source to the silver source is 1 (0-10).
3. The method for synthesizing the Cu-Ag sheet nano composite material according to claim 1, wherein the first dispersion liquid contains the copper source, the template and the solvent in a ratio of (1-2) mmol (0-1) g:30 mL.
4. The method for synthesizing the Cu-Ag flake nano composite material according to claim 1, wherein the molar ratio of the reducing agent to the copper source is (1-3): 1.
5. The method for synthesizing a Cu-Ag flake nano composite material according to claim 1, wherein the ratio of the amount of silver to the amount of the solvent in the silver source dispersion is (0-2) mmol:10 mL.
6. The method for synthesizing a Cu-Ag plate-like nanocomposite material as claimed in claim 1, wherein the temperature of the heat treatment is 140-180 ℃ and the time is 10min-2 h.
7. The method for synthesizing a Cu-Ag plate-shaped nano composite material according to claim 1, wherein the stirring is continued for 30min to 2 h.
8. The method for synthesizing a Cu-Ag flake nano composite material according to claim 1, wherein the mass molar ratio of the template to the copper in the second dispersion is (0.08-0.12) g:1 mmol.
9. The method for synthesizing a Cu-Ag platelet nanocomposite material according to claim 1, wherein the templating agent comprises polyvinylpyrrolidone; the reducing agent comprises fructose, and the solvent comprises glycol or water.
10. The method of claim 1, wherein the copper source comprises copper acetate monohydrate, copper nitrate or copper sulfate; the silver source comprises silver acetate, silver nitrate or silver sulfate.
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