CN111533160A - Method for preparing super-hydrophobic cuprous sulfide micro-nano particle surface based on copper - Google Patents
Method for preparing super-hydrophobic cuprous sulfide micro-nano particle surface based on copper Download PDFInfo
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Abstract
The invention belongs to the technical field of solid surfaces, and particularly relates to a method for preparing a super-hydrophobic cuprous sulfide micro-nano particle surface based on copper, which comprises the following specific steps: 1) treating the copper-based material for later use; 2) and (2) placing the copper-based material treated in the step 1) in a thioacetamide solution at 10-40 ℃ for reacting for 0.5-8 d, taking out, cleaning with deionized water, naturally airing, and heating the obtained sample at 60-100 ℃ for 3-48 h to obtain the super-hydrophobic cuprous sulfide micro/nano particle surface on the surface of the copper-based material. The size of the cuprous sulfide micro-nano particles is 0.1-1 mu m, the surface has super-hydrophobic performance, and the static contact angle of the cuprous sulfide micro-nano particles to water in the air is larger than 160 degrees. The method is simple and convenient, is easy to operate, uses instruments and reagents with low cost, is beneficial to large-scale industrial production, and does not need additional chemical modification of low-surface-energy substances.
Description
Technical Field
The invention belongs to the technical field of solid surfaces, and particularly relates to a method for preparing a super-hydrophobic cuprous sulfide micro-nano particle surface based on copper.
Background
With the development of nanotechnology, people have conducted a great deal of research on semiconductor materials with micro-nano structures. As a narrow-band-gap semiconductor material, the forbidden band width of cuprous sulfide is about 1.2eV, and the cuprous sulfide is widely applied to the fields of supercapacitors, solar cells, lithium ion batteries, biosensing and the like. In order to increase the specific surface area of the cuprous sulfide and obtain better performance, attempts have been made to prepare cuprous sulfide in various shapes.
The metal copper is often used as an electrode material due to good conductivity, and the preparation of the cuprous sulfide on the surface of the metal copper is generally carried out solid-gas reaction by a copper sheet and a sulfur source such as sulfur powder, a mixed gas of hydrogen sulfide and oxygen, and the like, and the reaction is difficult to operate due to the need of gas sealing equipment. The method for preparing the cuprous sulfide micro-nano structure on the surface of the copper-based material has the problems that the cuprous sulfide micro-nano structure is not completely converted and the like, and the currently reported method is to react precursors such as copper oxide, copper hydroxide and cuprous oxide with a certain micro-nano structure with a sulfur source. For the preparation of micro-nano granular cuprous sulfide on a copper substrate by a solution method, the following reports exist at present: applied Surface Science,2017,422, 456-468 published a paper entitled "A Surface adaptation for the simulation of 3D flow-like Cu2Snanostructure on glass mesh with an improved-property-induced wetting for oil-water separation" (Lei Niu, Zhixin Kang), a cuprous sulfide cauliflower-like particle accumulation structure is prepared on the Surface of a copper mesh by an electrodeposition method with the copper mesh as a substrate, copper sulfate as a copper source and thioacetamide as a sulfur source for oil-water separation. The cuprous sulfide micro-nano particles are prepared by adopting an electrodeposition method, electrodeposition equipment is needed in the preparation process, influence factors are more, and the process is more complex.
Aiming at the problems, the invention provides a method for preparing the surface of the super-hydrophobic cuprous sulfide micro-nano particle based on copper, the method can complete the preparation of the cuprous sulfide micro-nano particle in aqueous solution, the operation is simple, the repeatability is good, the cost is low, the method is suitable for large-area industrial production, the hydrophobic treatment of the surface of the cuprous sulfide particle does not need to additionally perform chemical modification of substances with low surface energy, and the cost is saved.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing the surface of the super-hydrophobic cuprous sulfide micro-nano particle based on copper, aiming at the defects in the prior art, and the size of the particle and the thickness of a deposited film are regulated and controlled through a preparation process so as to regulate the hydrophobic property of the surface of the cuprous sulfide micro-nano particle. The preparation method is simple to operate, good in repeatability, low in cost, suitable for large-area preparation, and free of additional hydrophobic chemical modification by using low-surface-energy substances.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the method for preparing the surface of the super-hydrophobic cuprous sulfide micro-nano particle based on copper comprises the following specific steps:
1) sequentially polishing the copper-based material by using sand paper, scrubbing by using an alcohol cotton ball, ultrasonically cleaning, and drying for later use;
2) and (2) placing the copper-based material treated in the step 1) in a thioacetamide solution at 10-40 ℃ for reacting for 0.5-8 d, taking out, cleaning with deionized water, naturally airing, and heating the obtained sample at 60-100 ℃ for 3-48 h to obtain the super-hydrophobic cuprous sulfide micro/nano particle surface on the surface of the copper-based material.
According to the scheme, the copper-based material in the step 1) is a copper sheet with the thickness of 0.05-5 mm and the purity of 95-99.99%.
According to the scheme, step 2) The concentration of the thioacetamide solution is 0.01-1.5 mol.L-1More preferably 0.02 to 0.5 mol.L-1。
Preferably, the copper-based material in the step 2) is placed in a thioacetamide solution for reaction at a temperature of 14-32 ℃ for 1-8 days.
The invention further comprises the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface material prepared by the method, wherein the size of the cuprous sulfide micro-nano particle is 0.1-1 mu m, and the static contact angle of the surface material to water in the air is larger than 160 degrees.
And the application of the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface material as a semiconductor material.
This application uses metallic copper as the base and as the copper source, uses thioacetamide as the sulfur source, through the slow oxidation of copper surface (the dissolved oxygen of copper-based material and aqueous solution slowly reacts, releases the copper ion) through the chemical bath deposition method, then slowly react with the slowly controlled temperature of the sulfur ion that thioacetamide slowly-released comes out, can guarantee that the cuprous sulfide granule that deposits is tiny, obtain cuprous sulfide micro-nano particle, then through thermal treatment, obtain the super hydrophobic cuprous sulfide micro-nano particle surface material that has bigger surface roughness, the hydrophobicity can be better.
According to the invention, the size of the cuprous sulfide micro-nano particles and the thickness, roughness and the like of a deposition film of the cuprous sulfide particles are regulated and controlled by regulating the concentration and reaction time of thioacetamide in a reaction system, so that the preparation of the surface of the cuprous sulfide micro-nano particles with excellent hydrophobic property is realized, and the regulation and control of the hydrophobic property are realized.
The invention has the beneficial effects that:
1. the existing preparation method of cuprous sulfide mostly adopts a vapor deposition method or an electrodeposition method, the size of the prepared material is limited, the preparation method has simple process and easy operation, the cuprous sulfide can react in aqueous solution at room temperature, the cuprous sulfide is suitable for large-area preparation, the surface modification is only carried out by a heating treatment method, the additional use of chemical modification of low surface energy substances is avoided, and the cost is saved. 2. The cuprous sulfide micro-nano particle surface prepared by the method has super-hydrophobicity, has good application prospects in the fields of gas detection, gas-solid catalysis, supercapacitors, solar cells and the like, and can prevent the surface of a material from being polluted.
Drawings
FIG. 1 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particle prepared in example 1;
fig. 2 is a contact angle picture of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particle prepared in example 1;
FIG. 3 is an XRD spectrum of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particle prepared in example 1;
FIG. 4 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particle prepared in example 2;
FIG. 5 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particles prepared in example 3;
FIG. 6 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particles prepared in example 4;
FIG. 7 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particles prepared in example 5;
FIG. 8 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particles prepared in example 6;
fig. 9 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particles prepared in example 7;
fig. 10 is an SEM photograph of the surface of the copper-based superhydrophobic cuprous sulfide micro-nano particles prepared in example 8;
FIG. 11 is an SEM photograph of the surface of copper-based cuprous sulfide micro/nano particles prepared in comparative example 1;
FIG. 12 is an SEM photograph of the surface of copper-based cuprous sulfide micro/nano particles prepared in comparative example 2;
fig. 13 is an SEM photograph of the surface of the copper-based cuprous sulfide micro/nano particles prepared in comparative example 3.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1
The method comprises the following steps of preparing a copper-based super-hydrophobic cuprous sulfide micro-nano particle surface material:
(1) polishing copper-based material (copper sheet with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in acetone for 10min, ultrasonic cleaning in deionized water for 5min, and air drying.
(2) Placing the copper-based material treated in the step 1) at 0.5 mol.L at 14 DEG C-1Reacting in the thioacetamide solution for 4d, taking out, cleaning with deionized water, naturally drying, heating the obtained sample at 70 ℃ for 24h, and obtaining the super-hydrophobic cuprous sulfide micro-nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 1. As can be seen from FIG. 1: the size of the cuprous sulfide micro-nano particles in the sample is 0.1-0.3 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 171.15 °, and the contact angle is shown in the picture of fig. 2. The XRD spectrum of the surface of the copper-based super-hydrophobic cuprous sulfide micro-nano particle prepared by the embodiment is shown in an attached figure 3, as can be seen from the attached figure 3, besides the diffraction peak (marked by a hollow triangle symbol) of the copper substrate, the XRD spectrum also has the diffraction peak (marked by a solid diamond), and the number of a corresponding standard card is 83-1462.
Example 2
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) polishing copper-based material (copper sheet with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in acetone for 10min, ultrasonic cleaning in deionized water for 5min, and air drying.
(2) Placing the copper-based material treated in the step 1) at 0.5 mol.L at 14 DEG C-1Reacting in thioacetamide solution for 1d, taking out, cleaning with deionized water, naturally drying, and addingAnd (3) heating the obtained sample at 70 ℃ for 24h to obtain the super-hydrophobic cuprous sulfide micro/nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 4. As can be seen from FIG. 4: the size of the cuprous sulfide micro-nano particles in the sample is 0.1-0.2 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 160.47 °.
Example 3
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) polishing copper-based material (copper sheet with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in acetone for 10min, ultrasonic cleaning in deionized water for 5min, and air drying.
(2) Placing the copper-based material treated in the step 1) at 0.5 mol.L at 14 DEG C-1Reacting in the thioacetamide solution for 3d, taking out, cleaning with deionized water, naturally drying, and heating the obtained sample at 60 ℃ for 48h to obtain the super-hydrophobic cuprous sulfide micro-nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 5. As can be seen from FIG. 5: the size of the cuprous sulfide micro-nano particles in the sample is 0.1-0.3 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 166.81 °.
Example 4
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) polishing copper-based material (copper sheet with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in acetone for 10min, ultrasonic cleaning in deionized water for 5min, and air drying.
(2) Placing the copper-based material treated in the step 1) at 0.5 mol.L at 14 DEG C-1Reacting in thioacetamide solution for 5d, taking out, cleaning with deionized water, naturally drying, heating the obtained sample at 80 deg.C for 12h to obtain superhydrophobic material on the surface of copper-based materialAnd (4) cuprous sulfide micro-nano particle surfaces.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 6. As can be seen in FIG. 6: the size of the cuprous sulfide micro-nano particles in the sample is 0.2-0.3 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 168.66 °.
Example 5
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) polishing copper-based material (copper sheet with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in acetone for 10min, ultrasonic cleaning in deionized water for 5min, and air drying.
(2) Placing the copper-based material treated in the step 1) at 0.5 mol.L at 14 DEG C-1Reacting in the thioacetamide solution for 6d, taking out, cleaning with deionized water, naturally drying, heating the obtained sample at 100 ℃ for 3h, and obtaining the super-hydrophobic cuprous sulfide micro-nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 7. As can be seen in FIG. 7: the size of the cuprous sulfide micro-nano particles in the sample is 0.2-0.4 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 169.49 °.
Example 6
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) polishing copper-based materials (copper sheets with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in acetone for 10min, ultrasonic cleaning in deionized water for 5min, and blowing with blower for use.
(2) Placing the copper-based material treated in the step 1) at 0.02 mol.L at 15 DEG C-1Reacting in the thioacetamide solution for 3.5d, taking out, cleaning with deionized water, naturally drying, heating the obtained sample at 80 ℃ for 6h, and obtaining the super-hydrophobic cuprous sulfide micro-nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 8. As can be seen in fig. 8: the size of the cuprous sulfide micro-nano particles in the sample is 0.1-0.4 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 165.81 °.
Example 7
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) sequentially polishing copper-based materials (copper sheets with thickness of 0.1mm and purity of 99.9%) with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning in deionized water for 10min, and blowing with blower for use.
(2) Placing the copper-based material treated in the step 1) at the temperature of 17 ℃ in a place of 0.05 mol.L-1Reacting in the thioacetamide solution for 8d, taking out, cleaning with deionized water, naturally drying, heating the obtained sample at 90 ℃ for 5h, and obtaining the super-hydrophobic cuprous sulfide micro-nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 9. As can be seen in fig. 9: the size of the cuprous sulfide micro-nano particles in the sample is 0.3-1 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 161.72 °.
Example 8
The method comprises the following steps of preparing the copper-based super-hydrophobic cuprous sulfide micro-nano particle surface:
(1) and sequentially polishing the copper-based material by using sand paper and scrubbing by using an alcohol cotton ball, then placing the copper-based material in deionized water for ultrasonic cleaning for 10min, washing the copper-based material by using the deionized water, and blow-drying the copper-based material by using a blower for later use.
(2) Placing the copper-based material treated in the step 1) at 0.05 mol.L at 32 DEG C-1Reacting in the thioacetamide solution for 3d, taking out, cleaning with deionized water, naturally drying, heating the obtained sample at 70 ℃ for 24h, and obtaining the super-hydrophobic cuprous sulfide micro-nano particle surface on the surface of the copper-based material.
The SEM image of the surface of the sample obtained in this example is shown in FIG. 10. As can be seen from fig. 10: the size of the cuprous sulfide micro-nano particles in the sample is 0.2-0.9 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 161.21 °.
Comparative example 1
The preparation method of the copper-based hydrophobic cuprous sulfide micro-nano particle surface comprises the following specific steps:
(1) and sequentially polishing the copper-based material by using sand paper and scrubbing by using an alcohol cotton ball, then placing the copper-based material in deionized water for ultrasonic cleaning for 10min, washing the copper-based material by using the deionized water, and blow-drying the copper-based material by using a blower for later use.
(2) Placing the copper-based material treated in the step 1) at 0.005 mol.L at 18 DEG C-1Reacting in thioacetamide solution for 4d, taking out, cleaning with deionized water, naturally drying, and heating the obtained sample at 70 ℃ for 24 h.
The scanning electron micrograph of the surface of the sample obtained in this comparative example is shown in FIG. 11. As can be seen in FIG. 11: the cuprous sulfide micro-nano particles in the sample are rare, and the size of the sample is small and is about 0.05-0.2 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 141.6 °.
Comparative example 2
The preparation method of the copper-based hydrophobic cuprous sulfide micro-nano particle surface comprises the following specific steps:
(1) and sequentially polishing the copper-based material by using sand paper and scrubbing by using an alcohol cotton ball, then placing the copper-based material in deionized water for ultrasonic cleaning for 10min, washing the copper-based material by using the deionized water, and blow-drying the copper-based material by using a blower for later use.
(2) Placing the copper-based material treated in the step 1) at 2.0 mol.L at 15 DEG C-1Reacting in thioacetamide solution for 3.5d, taking out, cleaning with deionized water, naturally drying, and heating the obtained sample at 70 ℃ for 24 h.
The scanning electron micrograph of the surface of the sample obtained in this comparative example is shown in FIG. 12. As can be seen in fig. 12: the cuprous sulfide micro-nano particles in the sample are rare, and the size of the cuprous sulfide micro-nano particles is about 0.1-0.3 mu m. The resulting sample surface was measured to have a static contact angle of 145.5 ° with water in air.
Comparative example 3
The preparation method of the copper-based hydrophobic cuprous sulfide micro-nano particle surface comprises the following specific steps:
(1) and sequentially polishing the copper-based material by using sand paper and scrubbing by using an alcohol cotton ball, then placing the copper-based material in deionized water for ultrasonic cleaning for 10min, washing the copper-based material by using the deionized water, and blow-drying the copper-based material by using a blower for later use.
(2) Placing the copper-based material treated in the step 1) at 2.0 mol.L at 15 DEG C-1Reacting in thioacetamide solution for 8.5d, taking out, cleaning with deionized water, naturally drying, and heating the obtained sample at 70 ℃ for 24 h.
The scanning electron micrograph of the surface of the sample obtained in this comparative example is shown in FIG. 13. As can be seen from fig. 13: the surface of the sample is almost free of cuprous sulfide micro-nano particles, and only has protrusions with the size of about 1-2 mu m. The static contact angle of the surface of the obtained sample to water in air was measured to be 135.5 °.
According to the invention, the size of the cuprous sulfide micro-nano particles and the thickness, roughness and the like of a deposition film of the cuprous sulfide particles are regulated and controlled by regulating the concentration and reaction time of thioacetamide in a reaction system, so that the preparation of the surface of the cuprous sulfide micro-nano particles with excellent hydrophobic property can be realized, and the regulation and control of the hydrophobic property can be realized. The concentration of thioacetamide is too low, cuprous sulfide particles generated by the reaction are few, the roughness does not meet the super-hydrophobic requirement, and the hydrophobic property is poor; the cuprous sulfide is easy to fall off due to excessive thickness, particles are too large, the roughness of the surface is reduced, the cuprous sulfide cannot be obtained even, and only protrusions with the size of about 1-2 mu m are formed, so that the hydrophobic property of the heated surface is reduced.
The above embodiments of the present invention are merely representative embodiments of the present invention, and are not intended to limit the embodiments of the present invention. Any modifications, equivalents, improvements and the like which come within the spirit and scope of the invention are desired to be protected by the following claims.
Claims (7)
1. A method for preparing a super-hydrophobic cuprous sulfide micro-nano particle surface based on copper is characterized by comprising the following steps: the method comprises the following specific steps:
1) treating the copper-based material for later use;
2) and (2) placing the copper-based material treated in the step 1) in a thioacetamide solution at 10-40 ℃ for reacting for 0.5-8 d, taking out, cleaning with deionized water, naturally airing, and heating the obtained sample at 60-100 ℃ for 3-48 h to obtain the super-hydrophobic cuprous sulfide micro/nano particle surface on the surface of the copper-based material.
2. The method of claim 1, wherein: the copper-based material in the step 1) is a copper sheet with the thickness of 0.05-5 mm and the purity of 95-99.99%.
3. The method of claim 1, wherein: the copper-based material is processed as follows: sequentially polishing with sand paper, scrubbing with alcohol cotton ball, ultrasonic cleaning, and drying.
4. The method of claim 1, wherein: the concentration of the thioacetamide solution in the step 2) is 0.01-1.5 mol.L-1。
5. The method of claim 1, wherein: the concentration of the thioacetamide solution is 0.02-0.5 mol.L-1。
6. The method of claim 1, wherein: and 2) placing the copper-based material in a thioacetamide solution, wherein the reaction temperature is 14-32 ℃, and the reaction time is 1-8 d.
7. The copper-based super-hydrophobic cuprous sulfide micro-nano particle surface material prepared by the method according to any one of claims 1-6, wherein the size of the cuprous sulfide micro-nano particle is 0.1-1 μm, and the static contact angle of the surface material to water in the air is more than 160 °.
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