CN111468740A - Method for preparing hexagonal elemental copper nanosheet by using polyol method - Google Patents
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- CN111468740A CN111468740A CN202010263505.2A CN202010263505A CN111468740A CN 111468740 A CN111468740 A CN 111468740A CN 202010263505 A CN202010263505 A CN 202010263505A CN 111468740 A CN111468740 A CN 111468740A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for preparing hexagonal elementary copper nanosheets by using a polyol method, belongs to the technical field of metal nano materials, and particularly relates to a method for preparing hexagonal elementary copper nanosheets by mixing a copper salt solution, a polyol solvent and an organic acid solution, heating and stirring to form a uniform mixed solution; adding long-chain alkylamine into the mixed solution, and uniformly stirring; heating, and then continuing heating to obtain the copper nanosheet with the hexagonal structure. According to the invention, a polyol method is adopted, long-chain alkylamine is mixed with a copper salt solution, a nano copper simple substance with a sheet structure is obtained by induction in a reduction system of organic acid and polyol, and a hexagonal copper nanosheet is obtained by regulating and controlling the proportion of the organic acid and the polyol. The invention has the advantages of simple raw materials, mild reaction conditions, simple and convenient preparation method and the like. In addition, the side length of the hexagonal elemental copper nanosheet prepared by the method is easy to regulate and control, the specific surface area is large, and the hexagonal elemental copper nanosheet can be well applied to the field of electrochemistry and SERS spectral analysis.
Description
Technical Field
The invention belongs to the technical field of metal nano materials, and particularly relates to a method for preparing hexagonal elemental copper nanosheets by using a polyol method.
Background
With the development of society, the quality of human life is continuously improved, and various chemical and biological materials need to be continuously, rapidly and sensitively monitored in the fields of food safety, clinical detection, drug production and the like. Under such a background, electrochemical detection methods are attracting much attention because of their simplicity of operation, high sensitivity, easy miniaturization, and on-line analysis. Since a common solid electrode does not have a molecular recognition function and many electroactive substances have a high active potential on a bare electrode, chemical modification needs to be performed on the surface of the electrode to improve the selectivity of an electrochemical analysis process.
The metal nano material has the characteristics of more surface active centers, high surface reaction activity, good selectivity and the like. And the metal nano material has properties which are not possessed by the material such as: interface effect, size distribution effect, quantum confinement effect, and the like. Due to this different physicochemical property, the metal nanoparticles can be used as a modification material and a catalyst. When the metal nano material is used as a modified electrode, the metal nano material has large specific surface area and excellent adsorption performance. Thereby reducing the electrode potential of the chemical reaction, and improving the speed of the electrochemical reaction, the sensitivity of the measurement and the selectivity of the electrode.
In addition, metal nanomaterials also play an important role in SERS spectroscopy. The SERS phenomenon occurs on metal surfaces with a certain degree of roughness. Compared with bulk metal, the metal nanoparticles have special surface plasmon resonance property, and the resonance property can enable molecules on the surface of the particles and nearby to generate strong Raman enhancement signals. The nano particles with various morphologies can be prepared by controlling different reaction conditions, and the anisotropic nano particles have stronger enhancement effect than spherical particles. The metal nanoparticles with more corners have an additional enhancement effect when being used as the SERS substrate.
The nano copper has higher stability and lower cost price. When being used as an electrode modification material, the copper nanoparticles have the advantages of large specific surface area, wide response range, strong selectivity, high reaction activity and the like. Compared with a bare electrode, the electrode modified by the copper nanoparticles has higher catalytic efficiency on certain substances because the copper nanoparticles can generate higher active surface area. Meanwhile, biological enzyme, protein and cells can keep better biological activity on the copper nanoparticles, so the copper nanoparticles also have good biocompatibility. The copper nanoparticles have various shapes, such as lines, sheets, blocks and the like, wherein the sheets have larger specific surface area and the shapes are easy to regulate, so the copper nanoparticles are ideal materials for modifying electrodes. In the prior art, the operation flow is complex when the hexagonal elemental copper nanosheet is prepared, and the prepared copper nanosheet is large in thickness, small in specific surface area and irregular in shape, and cannot be widely applied to the field of electrochemistry and SERS substrate analysis.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for preparing hexagonal elemental copper nanosheets by using a polyol method.
The invention is realized by the following technical scheme:
a method for preparing hexagonal elemental copper nanosheets by using a polyol method comprises the following specific steps:
(1) mixing a copper salt solution, a polyalcohol solvent and an organic acid solution, heating to T1 temperature, and stirring to form a uniform mixed solution;
(2) adding long-chain alkylamine into the mixed solution prepared in the step (1), and uniformly stirring;
(3) and (3) heating the mixed solution prepared in the step (2) to T2 constant temperature, and then continuously heating to T3 constant temperature to obtain the copper nanosheet with the hexagonal structure.
Further, the mass ratio of the long-chain alkylamine to the copper salt solution is 1:1-10: 1; the volume ratio of the copper salt solution to the polyhydric alcohol solvent to the organic acid solution is 1:10: 1-1: 20: 1; the temperature of the T1 is 60-80 ℃; the T2 temperature is 100-150 ℃, and the constant temperature time is 1-12 h; the T3 temperature is 150 ℃ and 250 ℃, and the constant temperature time is 1-12 h.
Further, the long-chain alkylamine is one or a composition of more than two of tetradecylamine, hexadecylamine or octadecylamine.
Further, the copper salt is one or a composition of more than two of cuprous chloride, cupric chloride, copper sulfate, cupric bromide or basic cupric carbonate.
Further, the polyalcohol solvent is one or a composition of more than two of propylene glycol, 1, 2-butanediol, pentaerythritol, diethylene glycol or polyethylene glycol.
Further, the organic acid solution is one or a composition of more than two of acetic acid, oxalic acid, α -hydracrylic acid, pyruvic acid and benzoic acid solution, and the mass fraction of the organic acid solution is 40-42%.
Compared with the prior art, the invention has the following advantages:
according to the invention, a polyol method is adopted, long-chain alkylamine is mixed with a copper salt solution, a nano copper simple substance with a sheet structure is obtained by induction in a reduction system of organic acid and polyol, and a hexagonal copper nanosheet is obtained by regulating and controlling the proportion of the organic acid and the polyol. The invention has the advantages of simple raw materials, mild reaction conditions, simple and convenient preparation method and the like. In addition, the side length of the hexagonal elemental copper nanosheet prepared by the method is easy to regulate and control, the specific surface area is large, and the hexagonal elemental copper nanosheet can be well applied to the field of electrochemistry and SERS spectral analysis.
Drawings
Fig. 1 is a scanning electron microscope image of hexagonal elemental copper nanosheets prepared in example 1 of the present invention;
fig. 2 is an XRD pattern of hexagonal-shaped elemental copper nanoplates prepared in example 1 of the present invention;
fig. 3 is a scanning electron microscope image of hexagonal elemental copper nanosheets prepared in example 2 of the present invention;
fig. 4 is a scanning electron microscope image of hexagonal elemental copper nanosheets prepared in example 3 of the present invention;
fig. 5 is a scanning electron microscope image of hexagonal elemental copper nanosheets prepared in example 4 of the present invention;
fig. 6 is a scanning electron microscope image of hexagonal elemental copper nanosheets prepared in example 5 of the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
Example 1
A method for preparing hexagonal elemental copper nanosheets by using a polyol method comprises the specific steps of measuring 30m of L propylene glycol solvent, sequentially adding 2mmol of cuprous chloride and 2ml of benzoic acid, heating to 60 ℃, stirring for 10min to form a uniform mixed solution, adding 10mmol of octadecylamine into the solution, reacting for a period of time to obtain a mixed solution, heating the mixed solution to 125 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1h, heating to 240 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1.5h to obtain the elemental copper nanosheets, and measuring the specific surface area of the elemental copper nanosheets to be 124.31m as shown in figure 12/g。
Fig. 2 is an XRD pattern of hexagonal-shaped elemental copper nanoplates prepared in example 1. According to a spectrogram, the hexagonal nanosheets forming the target product are elemental copper nanosheets.
Example 2
A method for preparing hexagonal elemental copper nanosheets by using a polyol method comprises the specific steps of measuring 30m of L propylene glycol solvent, sequentially adding 3mmol of copper chloride and 3ml of benzoic acid, heating to 60 ℃, stirring for 10min to form a uniform mixed solution, adding 8mmol of octadecylamine into the solution, reacting for a period of time to obtain a mixed solution, heating the mixed solution to 130 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1h, heating to 240 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1.5h to obtain the elemental copper nanosheets, and measuring the specific surface area of the elemental copper nanosheets to be 93.78m as shown in figure 32/g。
Example 3
A method for preparing hexagonal elemental copper nanosheets by using a polyol method comprises the specific steps of measuring 40m L1, 2-butanediol solvent, and thenSequentially adding 2mmol of copper sulfate and 2ml of α -hydroxypropionic acid, heating to 70 ℃, stirring for 10min to form a uniform mixed solution, adding 10mmol of octadecylamine into the solution, reacting for a period of time to obtain a mixed solution, heating the mixed solution, heating to 110 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 1h, heating to 220 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 1.5h to obtain the elemental copper nanosheet, and measuring the specific surface area of the elemental copper nanosheet to be 87.69m as shown in figure 42/g。
Example 4
A method for preparing hexagonal elemental copper nanosheets by using a polyol method comprises the specific steps of measuring 30m of L propylene glycol solvent, sequentially adding 2mmol of copper bromide and 2ml of pyruvic acid, heating to 60 ℃, stirring for 10min to form a uniform mixed solution, adding 6mmol of octadecylamine into the solution, reacting for a period of time to obtain a mixed solution, heating the mixed solution to 130 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1h, heating to 250 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1.5h to obtain the elemental copper nanosheets, and measuring the specific surface area of the elemental copper nanosheets to be 68.34m as shown in figure 52/g。
Example 5
A method for preparing hexagonal elemental copper nanosheets by using a polyol method comprises the specific steps of measuring 20m L propylene glycol solvent, sequentially adding 2mmol of basic copper carbonate and 2ml of oxalic acid, heating to 60 ℃, stirring for 10min to form a uniform mixed solution, adding 10mmol of octadecylamine into the solution, reacting for a period of time to obtain a mixed solution, heating the mixed solution to 120 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1h, heating to 220 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 1.5h to obtain the elemental copper nanosheets, and measuring the specific surface area of the elemental copper nanosheets to be 47.97m as shown in figure 62/g。
As can be seen from the figure, the shapes of the prepared hexagonal copper nanosheets are different due to different types of copper salt solutions. The hexagonal copper nanosheet prepared in the embodiment 1 is regular in shape, free of byproducts, largest in specific surface area and highest in raw material utilization rate, and can be widely applied to the field of electrochemistry and SERS spectral analysis. Compared with the copper nanosheet prepared in the example 1, the copper nanosheets prepared in the examples 2-5 have slightly smaller specific surface areas and have shapes without the rule of the copper nanosheet prepared in the example 1, because the types and the use amounts of the polyhydric alcohol and the organic acid have important influence on the shapes of the elemental copper nanosheets. In a polyol system, the organic acid can be selectively adsorbed on a specific copper crystal face to realize kinetic control growth, and in examples 2 to 5, the growth of the copper crystal face is inhibited by the selective adsorption of the organic acid on the copper crystal face, so that the copper nanosheet with irregular shape and anisotropy is finally formed.
The preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (6)
1. A method for preparing hexagonal elemental copper nanosheets by using a polyol method is characterized by comprising the following specific steps:
(1) mixing a copper salt solution, a polyalcohol solvent and an organic acid solution, heating to T1 temperature, and stirring to form a uniform mixed solution;
(2) adding long-chain alkylamine into the mixed solution prepared in the step (1), and uniformly stirring;
(3) and (3) heating the mixed solution prepared in the step (2) to T2 constant temperature, and then continuously heating to T3 constant temperature to obtain the copper nanosheet with the hexagonal structure.
2. The method for preparing hexagonal elemental copper nanosheets using the polyol process of claim 1, wherein the mass ratio of the long chain alkylamine to the copper salt solution is from 1:1 to 10: 1; the volume ratio of the copper salt solution to the polyhydric alcohol solvent to the organic acid solution is 1:10: 1-1: 20: 1; the temperature of the T1 is 60-80 ℃; the T2 temperature is 100-150 ℃, and the constant temperature time is 1-12 h; the T3 temperature is 150 ℃ and 250 ℃, and the constant temperature time is 1-12 h.
3. The method for preparing hexagonal elemental copper nanosheets using the polyol process of claim 1, wherein the long chain alkylamine is one or a combination of two or more of tetradecylamine, hexadecylamine, or octadecylamine.
4. The method for preparing hexagonal elemental copper nanosheets using the polyol process of claim 1, wherein the copper salt is one or a combination of two or more of cuprous chloride, cupric sulfate, cupric bromide, or basic cupric carbonate.
5. The method for preparing hexagonal elemental copper nanosheets by the polyol process of claim 1, wherein the polyol solvent is one or a combination of two or more of propylene glycol, 1, 2-butanediol, pentaerythritol, diethylene glycol, or polyethylene glycol.
6. The method for preparing hexagonal elemental copper nanosheets by using the polyol method according to claim 1, wherein the organic acid solution is one or a combination of two or more of acetic acid, oxalic acid, α -hydroxypropionic acid, pyruvic acid and benzoic acid, and the mass fraction of the organic acid solution is 40% -42%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112517921A (en) * | 2020-11-23 | 2021-03-19 | 延边大学 | Preparation method and system of hollow copper nanosheet |
| CN113500202A (en) * | 2021-07-14 | 2021-10-15 | 哈尔滨理工大学 | Preparation method of high-purity hexagonal Cu nanocrystalline |
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2020
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| WO2009112046A1 (en) * | 2008-03-10 | 2009-09-17 | Jacobs University Bremen Gmbh | Nio nanosheet structure possessing the (111) crystallographic planes with hexagonal holes, method for preparing the same and uses thereof |
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Cited By (3)
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| CN112517921A (en) * | 2020-11-23 | 2021-03-19 | 延边大学 | Preparation method and system of hollow copper nanosheet |
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| CN113500202A (en) * | 2021-07-14 | 2021-10-15 | 哈尔滨理工大学 | Preparation method of high-purity hexagonal Cu nanocrystalline |
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Application publication date: 20200731 |