CN113735157B - Preparation method of petal-shaped copper oxide nanosheet and application of petal-shaped copper oxide nanosheet - Google Patents
Preparation method of petal-shaped copper oxide nanosheet and application of petal-shaped copper oxide nanosheet Download PDFInfo
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- CN113735157B CN113735157B CN202111109932.6A CN202111109932A CN113735157B CN 113735157 B CN113735157 B CN 113735157B CN 202111109932 A CN202111109932 A CN 202111109932A CN 113735157 B CN113735157 B CN 113735157B
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Abstract
The invention provides a preparation method of petaloid copper oxide nanosheets, which comprises the following steps: step S1: dissolving copper salt into ethanol to prepare copper salt solution, and dissolving sulfide into deionized water to prepare sulfide solution; step S2: mixing a copper salt solution and a sulfide solution to obtain a mixed solution; step S3: heating the mixed solution at 120-180 ℃ for 1-2 h to obtain a dry gray black intermediate product, and cooling to room temperature; step S4: pouring the intermediate product into deionized water, dripping ammonia water for secondary reaction, and then filtering, washing and drying to obtain the petal-shaped copper oxide nanosheet. According to the invention, the preparation of the petal-shaped copper oxide nanosheets is realized by introducing ammonia water to carry out instantaneous secondary reaction, and the product has the characteristics of good petal shape and small size.
Description
Technical Field
The invention belongs to the field of preparation methods of semiconductor nano materials, and particularly relates to a preparation method of petal-shaped copper oxide nanosheets.
Background
Copper oxide (CuO) is an important p-type transition metal oxide, has a narrow band gap (Eg ═ 1.2-1.9 eV), is abundant in natural resources, low in price, non-toxic, and simple in synthesis, and has attracted attention in various applications such as gas sensors, solar photovoltaics, lithium ion batteries, and photocatalysts due to its unique properties such as light, heat, and electricity.
Although there are many reports on the preparation method of copper oxide, such as hydrothermal method, chemical precipitation method, sol-gel method, electrochemical method, calcination method, etc., many methods have disadvantages of high temperature and high pressure, long reaction time, and the need for special environment (such as high temperature and high pressure, special gas, additives, etc.), complicated equipment, complicated process, etc. Such as: a preparation method and application (CN110436508A) of flake nano copper oxide disclosed by the Royal et al, mentions a calcination method, has the characteristics of simple process flow and the like, but needs high temperature of 300-600 ℃; in a synthesis method and application (CN111517358A) of a flower-shaped copper oxide nanosphere disclosed by Wangcai, et al, a cold-hot reflux method is mentioned, and the reaction is carried out at normal temperature and normal pressure, but special cold-hot reflux equipment is required, and an additive is required. Therefore, the development of the method has the advantages of simple flow, low requirement on reaction conditions, no need of additives, no need of high temperature and high pressure, no need of special gas environment and easy large-scale application and also has important significance.
Disclosure of Invention
Aiming at the problems in the background art, the invention provides a preparation method of petal-shaped copper oxide nanosheets.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of petal-shaped copper oxide nanosheets is characterized by comprising the following steps:
step S1: dissolving copper salt into ethanol to prepare copper salt solution, and dissolving sulfide into deionized water to prepare sulfide solution;
step S2: mixing a copper salt solution and a sulfide solution to obtain a mixed solution;
step S3: heating the mixed solution at 120-180 ℃ for 1-2 h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: pouring the intermediate product into deionized water, dripping ammonia water for secondary reaction, and then filtering, washing and drying to obtain the petal-shaped copper oxide nanosheets.
Further, in step S1, the copper salt is copper nitrate or copper carbonate.
Further, in step S1, the sulfide is sodium sulfide or potassium sulfide.
Further, in step S1, the concentration of the copper salt solution is 0.1-0.2 mol/L, and the concentration of the sulfide solution is 0.1-0.2 mol/L; in step S2, the volume ratio of the dosage of the copper salt solution to the dosage of the sulfide solution is (1-2): 1.
further, in the step S4, the mass concentration of the ammonia water is 25.0-28.0%, and the ratio of the intermediate product to the ammonia water is 10 mg: (1-4) ml.
Further, in step S4, immediately after completion of the addition of ammonia water, a filtration operation is performed. The secondary reaction is used for converting the intermediate product into copper oxide, is an instant reaction, and can be carried out in the subsequent steps after ammonia water is dropped.
Further, in step S4, the drying temperature is 50-60 ℃ and the drying time is 0.5-1 h.
Further, in step S4, washing is performed by deionized water and acetone in this order.
The petal-shaped copper oxide nanosheet obtained by the preparation method is applied to the field of photoelectric and photo-thermal materials.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) according to the invention, instantaneous secondary reaction is carried out by introducing ammonia water, so that the preparation of the petal-shaped copper oxide nanosheet is realized, and the product has a good petal shape and the characteristic of small size, and the thickness is less than 50nm and even 20 nm.
(2) The controllable preparation of the petal-shaped copper oxide nanosheets assembled into the spheroidal structure and the film is realized by controlling the heating temperature, the whole body has the characteristics of higher specific surface area and higher active sites, and therefore, the petal-shaped copper oxide nanosheets have higher performances in the aspects of photo-thermal, catalysis and the like.
(3) The method has simple flow, easy operation and low reaction requirement condition, can be realized in an open system exposed in the air, and does not need high temperature and high pressure or special gas. Meanwhile, other components such as any active agent and the like are not added, the reaction period is short, the energy consumption is low, and the method is suitable for industrial popularization and application and is superior to the existing methods.
Drawings
Fig. 1 is a scanning electron micrograph of petaloid copper oxide nanoplates prepared in example 1;
fig. 2 is a transmission electron micrograph of petaloid copper oxide nanoplates prepared in example 1;
fig. 3 is an XRD pattern of petal-shaped copper oxide nanosheets prepared in example 1;
fig. 4 is a scanning electron micrograph of petaloid copper oxide nanoplates prepared in example 2;
fig. 5 is a scanning electron micrograph of petaloid copper oxide nanoplates prepared in example 3;
FIG. 6 is a scanning electron micrograph of a gray black product prepared in comparative example 1;
FIG. 7 is an XRD pattern of a gray black product prepared in comparative example 1;
fig. 8 is a scanning electron micrograph of copper oxide nanoplates prepared in comparative example 2.
Detailed Description
Example 1
Step S1: dissolving copper nitrate into ethanol to prepare a copper nitrate solution with the concentration of 0.15mol/L, and dissolving sodium sulfide into deionized water to prepare a sodium sulfide solution with the concentration of 0.15 mol/L;
step S2: copper nitrate solution and sodium sulfide solution are mixed according to the volume ratio of 1.5: 1 mixing to obtain a mixed solution;
step S3: heating the mixed solution at 130 ℃ for 1.5h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: pouring the intermediate product into deionized water, and dripping ammonia water with the mass concentration of 26% for secondary reaction, wherein the ratio of the intermediate product to the ammonia water is 10 mg: 2ml, then filtering, washing with deionized water and acetone in turn, and drying at 55 ℃ for 0.7h to obtain the petal-shaped copper oxide nanosheet.
FIGS. 1 and 2 are a scanning electron microscope image and a transmission electron microscope image of the petal-shaped copper oxide nanosheet prepared in example 1, respectively, and it can be seen that the petal-shaped copper oxide nanosheet has good dispersibility, the thickness of the middle part is greater than that of the edge, and the thickness of the copper oxide nanosheet is less than 50 nm; fig. 3 is an XRD pattern of the petal-shaped copper oxide nanosheets prepared in example 1, and it can be seen that the composition is copper oxide.
Example 2
Step S1: dissolving copper nitrate into ethanol to prepare a copper nitrate solution with the concentration of 0.15mol/L, and dissolving sodium sulfide into deionized water to prepare a sodium sulfide solution with the concentration of 0.15 mol/L;
step S2: copper nitrate solution and sodium sulfide solution are mixed according to the volume ratio of 1.5: 1 mixing to obtain a mixed solution;
step S3: heating the mixed solution at 150 ℃ for 1.5h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: pouring the intermediate product into deionized water, and dripping ammonia water with the mass concentration of 26% for secondary reaction, wherein the ratio of the intermediate product to the ammonia water is 10 mg: 2ml, then filtering, washing with deionized water and acetone in turn, and drying at 55 ℃ for 0.7h to obtain the petal-shaped copper oxide nanosheet.
FIG. 4 is a scanning electron microscope image of the petal-shaped copper oxide nanosheets prepared in example 2, the copper oxide nanosheets being petal-shaped and self-assembled into a quasi-spherical structure, and the copper oxide nanosheets being less than 20nm thick.
Example 3
Step S1: dissolving copper nitrate into ethanol to prepare a copper nitrate solution with the concentration of 0.15mol/L, and dissolving sodium sulfide into deionized water to prepare a sodium sulfide solution with the concentration of 0.15 mol/L;
step S2: copper nitrate solution and sodium sulfide solution are mixed according to the volume ratio of 1.5: 1 mixing to obtain a mixed solution;
step S3: heating the mixed solution at 170 ℃ for 1.5h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: pouring the intermediate product into deionized water, and dripping ammonia water with the mass concentration of 26% for secondary reaction, wherein the ratio of the intermediate product to the ammonia water is 10 mg: 2ml, then filtering, washing with deionized water and acetone in turn, and drying at 55 ℃ for 0.7h to obtain the petal-shaped copper oxide nanosheet.
Fig. 5 is a scanning electron micrograph of the petal-shaped copper oxide nanosheets prepared in example 3, and it can be seen that the petal-shaped copper oxide nanosheets have formed a thin film.
Comparative example 1
Step S1: dissolving copper nitrate into ethanol to prepare a copper nitrate solution with the concentration of 0.15mol/L, and dissolving sodium sulfide into deionized water to prepare a sodium sulfide solution with the concentration of 0.15 mol/L;
step S2: copper nitrate solution and sodium sulfide solution are mixed according to the volume ratio of 1.5: 1 mixing to obtain a mixed solution;
step S3: heating the mixed solution at 130 ℃ for 1.5h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: then, the mixture is filtered, washed by deionized water and acetone in turn and dried at 55 ℃ for 0.7h to obtain a gray black product.
FIG. 6 is a scanning electron micrograph of the gray-black product prepared in comparative example 1, showing no petal-like morphology; fig. 7 is an XRD pattern of the gray black product prepared in comparative example 1, which can be seen as a non-copper oxide component.
Comparative example 2
Step S1: dissolving copper nitrate into ethanol to prepare a copper nitrate solution with the concentration of 0.15mol/L, and dissolving sodium sulfide into deionized water to prepare a sodium sulfide solution with the concentration of 0.15 mol/L;
step S2: copper nitrate solution and sodium sulfide solution are mixed according to the volume ratio of 1.5: 1 mixing to obtain a mixed solution;
step S3: heating the mixed solution at 100 ℃ for 1.5h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: pouring the intermediate product into deionized water, and dripping ammonia water with the mass concentration of 26% for secondary reaction, wherein the ratio of the intermediate product to the ammonia water is 10 mg: 2ml, then filtered, washed with deionized water and acetone in sequence, and dried at 55 ℃ for 0.7h to obtain copper oxide nanosheets.
Fig. 8 is a scanning electron microscope image of the copper oxide nanosheets prepared in comparative example 2, showing that the copper oxide nanosheets no longer exhibit petal-like morphology.
Comparative example 1 is different from example 1 only in that comparative example 1 does not perform the secondary reaction of the intermediate product with the introduced aqueous ammonia of step S4. The gray black product prepared in comparative example 1 has neither petal-like morphology nor copper oxide component. It can be seen that the importance of the instantaneous secondary reaction of ammonia water on the form and components of the final product is provided by the invention.
The only difference between examples 1 to 3 and comparative example 2 is that the heating temperature in step S3 is different, and the heating temperatures in examples 1 to 3 were 130 ℃, 150 ℃, 170 ℃ and the heating temperature in comparative example 2 was 100 ℃. When the heating temperature is 130 ℃ in the example 1, monodisperse petal-shaped copper oxide nanosheets are obtained; when the heating temperature is 150 ℃ in the embodiment 2, the petal-shaped copper oxide nanosheet self-assembled into the spheroidal structure is obtained; when the heating temperature is 170 ℃ in the embodiment 3, the copper oxide nano-sheets further form a film; on the other hand, in comparative example 2, when the heating temperature was 100 ℃, the copper oxide nanoplate having a petal-like morphology could not be obtained, but the component was still copper oxide. From the above, it can be seen that the appropriate temperature range as well as the different temperatures play an important role in the formation of the petal morphology and the controlled preparation of the further assembly.
It should be noted that, according to the implementation requirement, each step described in the present application can be divided into more steps, and two or more steps or partial operations of the steps can be combined into a new step to achieve the purpose of the present invention.
It should be understood that parts of the specification not set forth in detail are well within the prior art.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A preparation method of petal-shaped copper oxide nanosheets is characterized by comprising the following steps:
step S1: dissolving copper salt into ethanol to prepare copper salt solution, and dissolving sulfide into deionized water to prepare sulfide solution; the copper salt is copper nitrate or copper carbonate, the sulfide is sodium sulfide or potassium sulfide, the concentration of the copper salt solution is 0.1-0.2 mol/L, and the concentration of the sulfide solution is 0.1-0.2 mol/L;
step S2: mixing a copper salt solution and a sulfide solution to obtain a mixed solution; the volume ratio of the dosage of the copper salt solution to the dosage of the sulfide solution is (1-2): 1;
step S3: heating the mixed solution at 120-150 ℃ for 1-2 h to obtain a dry gray black intermediate product, and cooling to room temperature;
step S4: pouring the intermediate product into deionized water, dripping ammonia water for secondary reaction, and then filtering, washing and drying to obtain petal-shaped copper oxide nanosheets; the mass concentration of the ammonia water is 25.0-28.0%, and the ratio of the intermediate product to the ammonia water is 10 mg: (1-4) ml.
2. The method for producing petal-shaped copper oxide nanosheets according to claim 1, wherein in step S4, filtration is performed immediately after completion of dropwise addition of aqueous ammonia.
3. The method for producing petaloid copper oxide nanosheets according to claim 1, wherein in step S4, the drying temperature is 50 to 60 ℃ and the drying time is 0.5 to 1 hour.
4. The method for producing petaloid copper oxide nanosheets according to claim 1, wherein in step S4, the washing is performed sequentially with deionized water and acetone.
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