CN112960689A - Preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure - Google Patents
Preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure Download PDFInfo
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- CN112960689A CN112960689A CN202110225605.0A CN202110225605A CN112960689A CN 112960689 A CN112960689 A CN 112960689A CN 202110225605 A CN202110225605 A CN 202110225605A CN 112960689 A CN112960689 A CN 112960689A
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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention relates to a preparation method of a cuprous oxide @ tin dioxide heterogeneous core-shell structure polyhedral structure, and belongs to the technical field of nano material preparation. According to the method, polyhedral cuprous oxide is used as a precursor, a layer of amorphous tin dioxide grows on the surface of the precursor through coordination etching, and a cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure with a P-N junction is formed. The shape of the cuprous oxide polyhedron can be regulated and controlled by regulating the amount of PVP. The method has the advantages of simple process, low cost, simple and convenient operation, environmental friendliness and the like, and the prepared cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron is not easy to agglomerate and has uniform size, good gas-sensitive property and potential gas-sensitive application value.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure.
Background
Design and fine control of nanocrystal shape have been one of the most important issues in nanoscience, chemistry, and physics, since surface morphology is closely related to electronic structure, bonding, surface energy, and chemical reactivity. Facets with different crystallographic features have unique surface atomic structures, reconstruction structures and atomic termination features that have been shown to have corresponding relationships to light sensitivity, gas and chemical reactivity and field emission characteristics. Understanding, predicting and controlling the exposed surface is critical to elucidating and exploring shape-related chemical and physical properties.
Cuprous oxide, a p-type semiconductor with a narrow band gap of 2.17eV, has attracted considerable attention in the fields of solar energy conversion, electrode materials, sensors, and catalytic decomposition. In recent years, since the physical and chemical properties of nanomaterials are largely dependent on their size and shape, many efforts have been made to develop a synthesis of Cu with different morphologies and sizes2O crystals such as cubes, spheres, octahedrons, and rhombohedrons, etc. Huang et al by changing NH added to the reaction system2Amount of OH & HCl, preparing Cu from cubic to rhombohedral2O nanostructures (w.c. huang, l.m.lyu, y.c. yang, m.h.huang, j.am.chem.soc.134(2012) 1261); li et al found that by using microwave radiation, ionic liquids ([ BMIM)]BF4) To obtain flower-like Cu2O structure (s.k.li, x.guo, y.wang, f.z.huang, y.h.shen, x.m.wang, a.j.xie, dalton trans.40(2011) 6745).
Tin dioxide, which is a wide band gap n-type semiconductor (Eg 3.6eV), has been widely used as a gas sensitive material since the last 60 years, because of its good chemical stability, strong corrosion resistance, short gas adsorption/desorption time, and high sensitivity. Composite materials generally have better sensing performance than single materials due to the presence of heterojunctions, where core-shell materials have the largest number of interfaces between the core and the shell and heterojunctions and are widely used in sensing research. Thus Cu2O@SnO2Core-shell structures have wide application in the sensing field. Kim et al prepared Cu by electrospinning2O@SnO2Core-shell nanowires (Kim, J. -H.; Lee, J. -H.; Kim, J. -Y.; Mirzaei, A.; Kim, H.W.; Kim, S.S. journal of Hazardous Materials 2019,376, 68-82). However, the above Cu2O@SnO2Core-shell structural speciesLess, limiting its application.
Disclosure of Invention
The problem to be solved by the invention is that the physical and chemical properties and the structure of the nano material are related, so that the Cu is the Cu2O@SnO2The diversity of the core-shell structure is poor, and the application potential of the core-shell structure is limited by fewer structures. Thus providing a method for preparing Cu2O@SnO2The heterogeneous core-shell polyhedron method enriches the types of core-shell structures, exposes specific crystal faces and improves the potential application value.
The invention adopts the following specific technical scheme:
cu2O@SnO2The preparation method of the heterogeneous core-shell polyhedral structure comprises the following steps:
dissolving a copper source in deionized water, and then adding polyvinylpyrrolidone to form a solution A;
dissolving sodium hydroxide in deionized water to form a solution B;
slowly dripping the solution B into the solution A to form a solution C, and heating and stirring in a water bath for a certain time;
dissolving ascorbic acid in deionized water to form a solution D;
slowly dripping the solution D into the solution C, aging for a certain time, centrifuging the product, washing with water and ethanol, and drying in a vacuum drying oven to obtain cuprous oxide polyhedral powder;
step (6), dissolving the obtained cuprous oxide polyhedral powder in ethanol, and adding NaCl solution;
step (7), dropwise adding SnCl into the solution prepared in the step (6)4And stirring the solution for 8-12 min, preferably 10min, centrifugally separating the product, respectively washing with water and ethanol, and drying in vacuum to obtain the cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure.
Preferably, the copper source in step (1) is copper chloride dihydrate.
Preferably, the concentration of the copper source in the step (1) is 0.01-0.03 mol-1Preferably 0.02mol-1。
Preferably, the ratio of polyvinylpyrrolidone to copper source in step (1) is 0-24, preferably 0, 3, 6, 12, 18, 24.
Preferably, the concentration of the sodium hydroxide solution in the step (2) is 4-6 mol L-1Preferably 5.0mol L-1。
Preferably, the stirring time in the step (3) is 30-40 min, preferably 40min, the water bath temperature is 60-70 ℃, preferably 75 ℃, and the mixing ratio of the solution A and the solution B is 9-10.
Preferably, the concentration of the ascorbic acid solution in the step (4) is 0.5-0.7 mol L-1Preferably 0.4mol L-1。
Preferably, the aging time in the step (5) is 3-4 h, preferably 4h, and the mixing ratio of the solution C and the solution D is 10-11.
Preferably, the concentration of the NaCl solution in the step (6) is 0.1-0.2 mol L-1Preferably 0.1mol L-1。
Preferably, the temperature of the vacuum drying oven in steps (5) and (7) is 40 ℃.
The invention has the following beneficial effects:
(1) the prepared cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral nano particle has various shapes and exposes different crystal faces. The tin dioxide shell layer is of an amorphous structure and has excellent application potential.
(2) The variety of core-shell structure materials is enriched, and the application of the variety of the core-shell materials is expanded.
(3) Simple process, simple operation, controllable reaction process and non-harsh reaction conditions.
Drawings
FIG. 1 is an X-ray diffraction pattern of the cuprous oxide polyhedral structure prepared in examples 1-6.
FIGS. 2a-f are scanning electron micrographs of the cuprous oxide polyhedral structure prepared in examples 1-6.
FIG. 3 is an X-ray diffraction pattern of the cuprous oxide @ tin dioxide heterocore-shell polyhedral structure prepared in examples 1-6.
FIGS. 4a-f are scanning electron microscope images of cuprous oxide @ tin dioxide heterocore-shell polyhedral structures prepared in examples 1-6.
FIG. 5 is a transmission electron micrograph of a heterogeneous core-shell truncated cube structure of cuprous oxide @ tin dioxide prepared in example 1.
Fig. 6a-d are X-ray spectral analysis plots of the cuprous oxide @ tin dioxide heterogeneous core-shell truncated cube structure prepared in example 1.
FIG. 7 is an X-ray photoelectron spectrum of tin element in a heterogeneous core-shell truncated pyramid structure of cuprous oxide @ tin dioxide prepared in example 1.
Fig. 8 is a graph of the sensitivity of the cuprous oxide truncated cubes and cuprous oxide @ tin dioxide truncated cubes prepared in example 1 to dimethyl ether gas.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. The following examples are presented merely to further understand and practice the present invention and are not to be construed as further limiting the claims of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention provides a Cu2O@SnO2The preparation method of the heterogeneous core-shell truncated pyramid structure comprises the following steps:
(1) 85.25mg of CuCl2·2H2Dissolving O in 25ml of deionized water, and dropwise adding 5.0mol L of the solution-12.5ml of NaOH solution, and stirring for 40 min; then dropwise adding 0.4mol L of water-12.5ml of ascorbic acid solution and aging for 4 hours. All the steps are carried out in a water bath at 75 ℃.
(2) And (2) centrifugally separating the product obtained in the step (1), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain the cuprous oxide powder with the truncated pyramid cubic structure.
(3) 30mg of Cu prepared in the step (2)2The O powder was dissolved in 25ml of ethanol,adding 0.1mol L of the solution-10.5ml of NaCl solution to form solution A; 1.7mg of SnCl4Dissolving in 25ml ethanol to form solution B; adding the solution B into the solution A, and stirring to react for 20 min.
(4) Centrifugally separating the product obtained in the step (3), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain Cu2O@SnO2Heterogeneous core-shell truncated cube structures.
Example 2
The invention provides a Cu2O@SnO2The preparation method of the heterogeneous core-shell truncated corner truncated cube structure comprises the following steps:
(1) 85.25mg of CuCl2·2H2Dissolving O in 25ml of deionized water, adding 167mg of PVP and uniformly stirring; the dropping concentration is 5.0mol L-12.5ml of NaOH solution, and stirring for 40 min; then dropwise adding 0.4mol L of water-12.5ml of ascorbic acid solution and aging for 4 hours. All the steps are carried out in a water bath at 75 ℃.
(2) And (2) centrifugally separating the product obtained in the step (1), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain the cuprous oxide powder with the truncated-angle truncated-edge cubic structure.
(3) 30mg of Cu prepared in the step (2)2Dissolving O powder in 25ml ethanol, adding 0.1mol L-10.5ml of NaCl solution to form solution A; 1.7mg of SnCl4Dissolving in 25ml ethanol to form solution B; adding the solution B into the solution A, and stirring to react for 20 min.
(4) Centrifugally separating the product obtained in the step (3), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain Cu2O@SnO2The heterogeneous core-shell truncated corner truncated cube structure.
Example 3
The invention provides a Cu2O@SnO2The preparation method of the heterogeneous core-shell truncated semi-octahedral structure comprises the following steps:
(1) 85.25mg of CuCl2·2H2Dissolving O in 25ml deionized water, adding 333.3mg PVP and stirring uniformly; the dropping concentration is5.0mol L-12.5ml of NaOH solution, and stirring for 40 min; then dropwise adding 0.4mol L of water-12.5ml of ascorbic acid solution and aging for 4 hours. All the steps are carried out in a water bath at 75 ℃.
(2) And (2) centrifugally separating the product obtained in the step (1), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain the cuprous oxide powder with the truncated octahedral structure.
(3) 30mg of Cu prepared in the step (2)2Dissolving O powder in 25ml ethanol, adding 0.1mol L-10.5ml of NaCl solution to form solution A; 1.7mg of SnCl4Dissolving in 25ml ethanol to form solution B; adding the solution B into the solution A, and stirring to react for 20 min.
(4) Centrifugally separating the product obtained in the step (3), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain Cu2O@SnO2Heterogeneous core-shell truncated hemi-octahedral structures.
Example 4
The invention provides a Cu2O@SnO2The preparation method of the heterogeneous core-shell truncated octahedral structure comprises the following steps:
(1) 85.25mg of CuCl2·2H2Dissolving O in 25ml of deionized water, adding 667mg of PVP and stirring uniformly; the dropping concentration is 5.0mol L-12.5ml of NaOH solution, and stirring for 40 min; then dropwise adding 0.4mol L of water-12.5ml of ascorbic acid solution and aging for 4 hours. All the steps are carried out in a water bath at 75 ℃.
(2) And (2) centrifugally separating the product obtained in the step (1), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain the cuprous oxide powder with the truncated octahedral structure.
(3) 30mg of Cu prepared in the step (2)2Dissolving O powder in 25ml ethanol, adding 0.1mol L-10.5ml of NaCl solution to form solution A; 1.7mg of SnCl4Dissolving in 25ml ethanol to form solution B; adding the solution B into the solution A, and stirring to react for 20 min.
(4) Centrifugally separating the product obtained in the step (3), washing with water and ethanol, and drying in a vacuum drying oven at 40 DEG CTo obtain Cu2O@SnO2Heterogeneous core-shell truncated octahedral structures.
Example 5
The invention provides a Cu2O@SnO2The preparation method of the heterogeneous core-shell truncated octahedral structure comprises the following steps:
(1) 85.25mg of CuCl2·2H2Dissolving O in 25ml of deionized water, adding 1000mg of PVP and uniformly stirring; the dropping concentration is 5.0mol L-12.5ml of NaOH solution, and stirring for 30 min; then dropwise adding 0.4mol L of water-12.5ml of ascorbic acid solution and aging for 4 hours. All the steps are carried out in a water bath at 75 ℃.
(2) And (2) centrifugally separating the product obtained in the step (1), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain the cuprous oxide powder with the truncated octahedral structure.
(3) 30mg of Cu prepared in the step (2)2Dissolving O powder in 25ml ethanol, adding 0.1mol L-10.5ml of NaCl solution to form solution A; 1.7mg of SnCl4Dissolving in 25ml ethanol to form solution B; adding the solution B into the solution A, and stirring to react for 20 min.
(4) Centrifugally separating the product obtained in the step (3), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain Cu2O@SnO2Heterogeneous core-shell truncated octahedral structures.
Example 6
The invention provides a Cu2O@SnO2The preparation method of the heterogeneous core-shell regular octahedral structure comprises the following steps:
(1) 85.25mg of CuCl2·2H2Dissolving O in 25ml of deionized water, adding 1334mg of PVP and uniformly stirring; the dropping concentration is 5.0mol L-12.5ml of NaOH solution, and stirring for 40 min; then dropwise adding 0.6mol L of water-12.5ml of ascorbic acid solution and aging for 4 hours. All the steps are carried out in a water bath at 75 ℃.
(2) And (2) centrifugally separating the product obtained in the step (1), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain the cuprous oxide powder with the octahedral structure.
(3) 30mg of Cu prepared in the step (2)2Dissolving O powder in 25ml ethanol, adding 0.1mol L-10.5ml of NaCl solution to form solution A; 1.7mg of SnCl4Dissolving in 25ml ethanol to form solution B; adding the solution B into the solution A, and stirring to react for 20 min.
(4) Centrifugally separating the product obtained in the step (3), washing with water and ethanol, and drying in a vacuum drying oven at 40 ℃ to obtain Cu2O@SnO2A heterogeneous core-shell regular octahedral structure.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art. It is therefore intended that the invention not be limited to the exact details and illustrations described and illustrated herein, but fall within the scope of the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure is characterized in that the material is prepared by the following method:
dissolving a copper source in deionized water, and then adding polyvinylpyrrolidone to form a solution A;
dissolving sodium hydroxide in deionized water to form a solution B;
slowly dripping the solution B into the solution A to form a solution C, and heating and stirring in a water bath for a certain time;
dissolving ascorbic acid in deionized water to form a solution D;
slowly dripping the solution D into the solution C, aging for a certain time, centrifuging the product, washing with water and ethanol, and drying in a vacuum drying oven to obtain cuprous oxide polyhedral powder;
step (6), dissolving the obtained cuprous oxide polyhedral powder in ethanol, and adding NaCl solution;
step (ii) of(7) Dropwise adding SnCl into the solution prepared in the step (6)4And stirring the solution for 8-12 min, centrifugally separating the product, respectively washing with water and ethanol, and drying in vacuum to obtain the cuprous oxide @ tin dioxide heterogeneous core-shell polyhedral structure.
2. A process for the preparation of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedra as claimed in claim 1 wherein said copper source in step (1) is cupric chloride dihydrate.
3. The preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron of claim 1, wherein the concentration of copper source in step (1) is 0.01-0.03 mol L-1。
4. The preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron of claim 1, wherein the ratio of polyvinylpyrrolidone to copper source in step (1) is 0-24.
5. The preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron of claim 1, wherein concentration of sodium hydroxide solution in step (2) is 4-6 mol L-1。
6. The preparation method of a cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron according to claim 1, wherein in step (3), the water bath heating and stirring time is 30-40 min, the water bath temperature is 60-70 ℃, and the mixing ratio of the solution A and the solution B is 9-10.
7. The preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron of claim 1, wherein concentration of ascorbic acid solution in step (4) is 0.5-0.7 mol L-1。
8. The preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron of claim 1, wherein aging time in step (5) is 3-4 h, and the mixing ratio of solution C and solution D is 10-11.
9. The preparation method of cuprous oxide @ tin dioxide heterogeneous core-shell polyhedron of claim 1, wherein concentration of NaCl solution in step (6) is 0.1-0.2 mol L-1。
10. A copper (i) oxide @ tin dioxide heterogeneous core-shell polyhedron preparation method as claimed in claim 1, wherein the temperature of the vacuum drying oven used in step (5) and step (7) is 40 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115463688A (en) * | 2022-08-15 | 2022-12-13 | 湖南工商大学 | Copper-based metal organic framework composite material and preparation method and application thereof |
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| CN101348275A (en) * | 2008-09-11 | 2009-01-21 | 北京航空航天大学 | Preparation of polyhedral cuprous oxide nano particle |
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