CN114850785B - Method for preparing super-hydrophobic coating by utilizing reaction wetting - Google Patents
Method for preparing super-hydrophobic coating by utilizing reaction wetting Download PDFInfo
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- CN114850785B CN114850785B CN202210389730.XA CN202210389730A CN114850785B CN 114850785 B CN114850785 B CN 114850785B CN 202210389730 A CN202210389730 A CN 202210389730A CN 114850785 B CN114850785 B CN 114850785B
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Abstract
A method for preparing a super-hydrophobic coating by utilizing reaction wetting relates to a method for preparing a super-hydrophobic coating. The invention aims to solve the technical problems of complex preparation process, small application range and poor mechanical stability of the existing super-hydrophobic surface. According to the invention, agCuTi alloy containing active element Ti is infiltrated into the porous anodic alumina template, the molten AgCuTi has better wetting and joint filling capacity for metal oxide, and the anodic alumina template is easy to remove by subsequent alkali solution; and then, the heated anodic alumina template can be effectively removed by adopting a hydrothermal mode, and on the other hand, the growth of a nano structure is facilitated in the hydrothermal process, so that a complex microstructure with multilevel roughness can be finally obtained, and the super-hydrophobic coating can be obtained on the substrate after modification. The method disclosed by the invention is simple and effective to operate, and the obtained super-hydrophobic coating is excellent in long-term stability, good in mechanical stability and good in application prospect.
Description
Technical Field
The invention relates to a method for preparing a super-hydrophobic coating.
Background
The super-hydrophobic property requires that the static contact angle (WCA) of a water drop on the surface of a material is more than 150 degrees, and the dynamic rolling angle (SA) is less than 10 degrees. Due to the special performance of the super-hydrophobic material, the super-hydrophobic material has wide application prospects in the fields of life and industry. Generally, superhydrophobicity requires both large surface roughness and low surface energy. When an organic material with low surface energy is adopted, the super-hydrophobic property can be realized only by preparing a micro-nano structure on the surface of the organic material, but the material selection during the preparation of the super-hydrophobic surface is greatly limited. When a material with high surface energy per se is adopted to realize the super-hydrophobic function, for example, inorganic materials such as metal, non-metal ceramic and the like need to prepare a complex multi-stage micro-nano structure on the surface, and then a low surface energy modifier is adopted for processing. At present, a plurality of methods are available for preparing a multistage micro-nano structure on the surface of an inorganic material, such as chemical corrosion, electroplating, electrodeposition, chemical vapor deposition, electrostatic spinning and the like. However, most of the super-hydrophobic surfaces have the problems of complex preparation process, small application range, poor mechanical stability, reduced long-term service performance and the like, and practical application and development of the super-hydrophobic surfaces are restricted.
Disclosure of Invention
The invention provides a method for preparing a super-hydrophobic coating by utilizing reaction wetting, aiming at solving the technical problems of complex preparation process, small application range and poor mechanical stability of the existing super-hydrophobic surface.
The method for preparing the super-hydrophobic coating by utilizing the reaction wetting is carried out according to the following steps:
1. reaction wetting: grinding AgCuTi foils by using abrasive paper of 400#, 600#, 800#, 1200# and 1500# in sequence, then ultrasonically cleaning the AgCuTi foils for 5-15 min by using absolute ethyl alcohol, naturally airing the AgCuTi foils, then placing the AgCuTi alloy foils between a porous anodic alumina template and a substrate to form a sandwich structure, wherein the substrate is positioned at the lowest part, then heating the AgCuTi alloy foils from room temperature to 800-880 ℃ at a heating rate of 5-15 ℃/min under the protection of vacuum or inert gas, preserving the heat for 5-15 min, and then cooling the AgCuTi alloy foils to the room temperature under the condition that the cooling rate is 5-15 ℃/min;
2. hydrothermal treatment: putting the sample prepared in the first step into a hydrothermal reaction kettle, adding NaOH aqueous solution with the concentration of 0.3-0.7 mol/L, and completely immersing the sample, wherein the volume filling degree of the NaOH aqueous solution in the hydrothermal reaction kettle is 50-52%; raising the temperature from room temperature to 200-280 ℃ under the condition that the temperature raising rate is 5-10 ℃/min, preserving the heat for 30-90 min, cooling to the room temperature along with the furnace, taking out a sample, cleaning by using deionized water, and naturally drying;
3. modification: sealing the sample obtained in the step two and the dust-free cloth soaked with 5-10 drops of the modifier in a culture dish, leaving a gap between the sample and the dust-free cloth, naturally standing for 5-24 h at room temperature, and taking out to obtain a super-hydrophobic coating on the substrate; the modifier is volatile liquid with low surface energy. And step three, in order to reduce the surface energy of the sample, the modifier on the non-woven fabric is firstly evaporated and then is subjected to vapor deposition on the sample.
The design principle of the invention is as follows:
the super-hydrophobic surface needs to be prepared with multilevel roughness and has a structure with two dimensions of micron and nanometer. Reaction wetting is often used in the aspects of brazing connection and composite material preparation, and the alloy containing the active metal elements has a good wetting and joint filling effect after being melted and can permeate into a complex micro-nano structure, so that the wetting of the active metal has the capability of preparing the micro-nano structure.
In the first step, agCuTi alloy containing active element Ti is adopted to permeate into the porous anodic alumina template, the molten AgCuTi has better wetting joint filling capability on metal oxide, and the anodic alumina template is easy to be removed by subsequent alkali solution; in the second step of the invention, the heated anodic aluminum oxide template can be effectively removed by adopting a hydrothermal mode, and on the other hand, the growth of the nano structure is facilitated in the hydrothermal process, so that a complex microstructure with multilevel roughness can be finally obtained, and the super-hydrophobic coating can be obtained on the substrate after modification.
In addition, because AgCuTi can realize better wetting and spreading on the surfaces of a plurality of base materials, different bases can be selected, the super-hydrophobic coating can be directly prepared on a target base, and the super-hydrophobic coating has higher bonding strength with the base.
The invention has the following beneficial effects:
1. the method is simple and effective in operation, and the AgCuTi and the porous anodic alumina template are sequentially stacked from bottom to top and then pressurized and heated in vacuum or protective atmosphere, so that the AgCuTi can be infiltrated into the porous anodic alumina template;
2. the AgCuTi adopted by the invention can realize good connection with the matrix while permeating into the anodic alumina template, and the bonding force of the super-hydrophobic coating and the matrix is ensured;
3. according to the method, the removal of the anodic aluminum oxide template and the growth of the nano structure are simultaneously realized by adopting hydrothermal treatment, and the operation is simple and convenient;
4. the AgCuTi adopted by the invention can realize good wetting with a plurality of substrate materials, so that super-hydrophobic coatings can be prepared on the surfaces of different substrates, and the application range is wide.
The invention provides a method for preparing a super-hydrophobic coating on different base materials by utilizing reaction wetting, the operation is simple and effective, and the obtained super-hydrophobic coating has excellent long-term stability, good mechanical stability and good application prospect.
Drawings
FIG. 1 is a schematic diagram of step three of experiment one, wherein 1 is a sample, 2 is a non-woven fabric, 3 is a modifier, and 4 is a culture dish;
FIG. 2 is an SEM image of the surface topography of the sample after hydrothermal treatment in step two of experiment one;
FIG. 3 is a water droplet static contact angle (WCA) image of a superhydrophobic coating prepared on a substrate at step three of test one;
FIG. 4 is a water droplet dynamic roll angle (SA) image of a superhydrophobic coating prepared on a substrate at step three of experiment one;
FIG. 5 is a graph of the contact angle of a water drop after a prolonged period of test two;
FIG. 6 is a graph of the contact angle of a water droplet on the surface of a sample after the pressure is unloaded in test three;
FIG. 7 is a graph of contact angles for a test four of superhydrophobic coatings prepared on a stainless steel substrate;
FIG. 8 is a contact angle plot of a superhydrophobic coating prepared on a Cu substrate for test five;
FIG. 9 is a contact angle plot of a superhydrophobic coating prepared on a SiC substrate for test six;
fig. 10 is a contact angle diagram of the superhydrophobic coating prepared on the graphite substrate for test seven.
Detailed Description
The first specific implementation way is as follows: the embodiment is a method for preparing a super-hydrophobic coating by utilizing reaction wetting, which is specifically carried out according to the following steps:
1. reaction wetting: grinding AgCuTi foils by using abrasive paper of 400#, 600#, 800#, 1200# and 1500# in sequence, then ultrasonically cleaning the AgCuTi foils for 5-15 min by using absolute ethyl alcohol, naturally airing the AgCuTi foils, then placing the AgCuTi alloy foils between a porous anodic alumina template and a substrate to form a sandwich structure, wherein the substrate is positioned at the lowest part, then heating the AgCuTi alloy foils from room temperature to 800-880 ℃ at a heating rate of 5-15 ℃/min under the protection of vacuum or inert gas, preserving the heat for 5-15 min, and then cooling the AgCuTi alloy foils to the room temperature under the condition that the cooling rate is 5-15 ℃/min;
2. hydrothermal treatment: putting the sample prepared in the first step into a hydrothermal reaction kettle, adding NaOH aqueous solution with the concentration of 0.3-0.7 mol/L to completely immerse the sample, wherein the volume filling degree of the NaOH aqueous solution in the hydrothermal reaction kettle is 50-52%; raising the temperature from room temperature to 200-280 ℃ under the condition that the temperature raising rate is 5-10 ℃/min, preserving the heat for 30-90 min, cooling to the room temperature along with the furnace, taking out a sample, cleaning by using deionized water, and naturally drying;
3. modification: sealing the sample obtained in the step two and the dust-free cloth soaked with 5-10 drops of the modifier in a culture dish, leaving a gap between the sample and the dust-free cloth, naturally standing for 5-24 hours at room temperature, and taking out to obtain a super-hydrophobic coating on the substrate; the modifier is volatile liquid with low surface energy.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the vacuum degree is 1 x 10 -3 Pa～5×10 -3 Pa. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the substrate in the first step is a metal material which is stable under the conditions of vacuum high temperature and alkali solution. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the third difference between the present embodiment and the specific embodiment is that: the substrate in the first step is copper, titanium, steel or platinum. The rest is the same as the third embodiment.
The fifth concrete implementation mode is as follows: the fourth difference between the present embodiment and the specific embodiment is that: the matrix in the step one is a non-metallic material which is stable under the conditions of vacuum high temperature and alkali solution. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fifth embodiment is different from the specific embodiment in that: the matrix in the first step is graphite, silicon carbide, alumina, diamond or carbon composite material. The rest is the same as the fifth embodiment.
The seventh concrete implementation mode: the present embodiment differs from the first to sixth embodiments in that: the aperture of the anodic aluminum oxide template in the step one is 400nm, the anodic aluminum oxide template is of a two-pass structure, and the shape of the nanopore is circular, triangular or square. The rest is the same as the first to sixth embodiments.
The specific implementation mode eight: the present embodiment differs from the first to seventh embodiments in that: the AgCuTi alloy foil in the first step has the composition of Ag-Cu28-Ti1.5 (wt.%). The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the inert gas in the first step is argon. The others are the same as in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from the first to ninth embodiments in that: the modifier in the third step is heptadecafluorodecyltrimethoxysilane. The others are the same as in the first to ninth embodiments.
The invention was verified with the following tests:
the first test: the test is a method for preparing a super-hydrophobic coating by utilizing reaction wetting, and is specifically carried out according to the following steps:
1. reaction wetting: grinding AgCuTi foils by using abrasive paper of 400#, 600#, 800#, 1200# and 1500# in sequence, then ultrasonically cleaning the AgCuTi foils for 5-15 min by using absolute ethyl alcohol, naturally airing the AgCuTi foils, then placing the AgCuTi alloy foils between a porous anodic alumina template and a substrate to form a sandwich structure, wherein the substrate is positioned at the lowest part, then heating the AgCuTi alloy foils from room temperature to 850 ℃ at a heating rate of 10 ℃/min in vacuum, preserving the temperature for 10min, and then cooling the AgCuTi alloy foils to the room temperature under the condition that the cooling rate is 10 ℃/min; vacuum degree of 2X 10 -3 Pa; the substrate is solid alumina ceramic, the surface area is 12mm multiplied by 18mm, and the thickness is 0.6mm;
the aperture of the anodic aluminum oxide template in the step one is 400nm, the anodic aluminum oxide template is of a two-pass structure, the shape of a nanopore is circular, and the surface area is 10mm multiplied by 10mm;
the AgCuTi alloy foil in the first step has the components of Ag-Cu28-Ti1.5 (wt.%), and the surface area of 10mm multiplied by 10mm;
2. hydrothermal treatment: putting the sample prepared in the first step into a hydrothermal reaction kettle, adding a 0.5mol/L NaOH aqueous solution to completely immerse the sample, wherein the volume filling degree of the NaOH aqueous solution in the hydrothermal reaction kettle is 50%; heating to 250 ℃ from room temperature under the condition that the heating rate is 7 ℃/min, preserving heat for 60min, cooling to room temperature along with the furnace, taking out a sample, cleaning by using deionized water, and naturally drying;
3. modification: placing the sample obtained in the step two and the dust-free cloth (5 layers in total, stacked up and down) soaked with 10 drops of the modifying agent in a culture dish, sealing, leaving a gap (as shown in figure 1) between the sample and the dust-free cloth, naturally placing for 12 hours at room temperature, and taking out to obtain a super-hydrophobic coating on the substrate; the modifier is heptadecafluorodecyltrimethoxysilane; the length and the width of the non-woven fabric are both 1cm.
Fig. 2 is an SEM image of the surface topography of the sample after hydrothermal treatment in step two of the first test, from which it can be seen that the surface prepared by reaction wetting and hydrothermal treatment in this test has a multi-level roughness structure.
Fig. 3 is a water drop static contact angle (WCA) image of the superhydrophobic coating prepared on the substrate in step three of the first test, fig. 4 is a water drop dynamic rolling angle (SA) image of the superhydrophobic coating prepared on the substrate in step three of the first test, and it can be seen from the images that the static contact angle (WCA) of the water drop is greater than 150 ° and the dynamic rolling angle (SA) is less than 10 °, which proves that the superhydrophobic coating is obtained on the substrate by the present test.
And (2) testing II: the sample of the superhydrophobic coating prepared on the substrate in the step three of the test one is placed in the air for 60 days, fig. 5 shows the contact angle condition of a water drop after long-time placement, the left pillar in each time period is a static contact angle, and the right pillar is a dynamic rolling angle, so that the superhydrophobic surface still keeps good superhydrophobicity after 60 days of placement, and the superhydrophobic surface is proved to have good long-term stability.
And (3) test III: and (3) pressurizing the super-hydrophobic coating prepared on the substrate in the step three of the test I by adopting a hydraulic press, wherein the pressure is 4 tons, and FIG. 6 shows a water drop contact angle of the surface of the sample after the pressure is unloaded.
And (4) testing: the test differs from the first test in that the base material used in the first step is stainless steel. The rest were the same as test one.
And (5) testing five: the test is different from the first test in that the base material adopted in the first step is Cu. The rest were the same as test one.
And (6) test six: the present test differs from the first test in that the matrix material used in the first step is SiC. The rest were the same as test one.
Test seven: the difference between the test and the first test is that the matrix material used in the first step is graphite. The rest were the same as test one.
Fig. 7 is a contact angle diagram of a superhydrophobic coating prepared on a stainless steel substrate in test four, fig. 8 is a contact angle diagram of a superhydrophobic coating prepared on a Cu substrate in test five, fig. 9 is a contact angle diagram of a superhydrophobic coating prepared on a SiC substrate in test six, and fig. 10 is a contact angle diagram of a superhydrophobic coating prepared on a graphite substrate in test seven.
Claims (10)
1. A method for preparing a super-hydrophobic coating by utilizing reactive wetting is characterized by comprising the following steps of:
1. reaction wetting: sequentially polishing AgCuTi foils by using abrasive paper of 400#, 600#, 800#, 1200# and 1500#, then ultrasonically cleaning for 5-15 min by using absolute ethyl alcohol, naturally airing, then placing the AgCuTi alloy foils between a porous anodic aluminum oxide template and a substrate to form a sandwich structure, wherein the substrate is positioned at the lowest part, then heating to 800-880 ℃ from room temperature at a heating rate of 5-15 ℃/min under the protection of vacuum or inert gas, preserving heat for 5-15 min, and then cooling to room temperature at a cooling rate of 5-15 ℃/min;
2. hydrothermal treatment: putting the sample prepared in the first step into a hydrothermal reaction kettle, adding NaOH aqueous solution with the concentration of 0.3-0.7 mol/L to completely immerse the sample, wherein the volume filling degree of the NaOH aqueous solution in the hydrothermal reaction kettle is 50-52%; raising the temperature from room temperature to 200-280 ℃ under the condition that the temperature raising rate is 5-10 ℃/min, preserving the heat for 30-90 min, cooling to the room temperature along with the furnace, taking out a sample, cleaning by using deionized water, and naturally drying;
3. modification: sealing the sample obtained in the step two and the dust-free cloth soaked with 5-10 drops of the modifier in a culture dish, leaving a gap between the sample and the dust-free cloth, naturally standing for 5-24 h at room temperature, and taking out to obtain a super-hydrophobic coating on the substrate; the modifier is volatile liquid with low surface energy.
2. The method for preparing superhydrophobic coating using reactive wetting according to claim 1, wherein the degree of vacuum in the first step is 1 x 10 -3 Pa～5×10 -3 Pa。
3. The method for preparing superhydrophobic coating using reactive wetting according to claim 1, wherein the substrate in the first step is a metal material stable under vacuum at high temperature and under alkaline solution condition.
4. The method for preparing superhydrophobic coating using reactive wetting according to claim 3, wherein the substrate in the first step is copper, titanium, steel or platinum.
5. The method for preparing superhydrophobic coating using reactive wetting according to claim 1, wherein the substrate in the first step is a non-metallic material stable under vacuum at high temperature and under alkaline solution.
6. The method for preparing superhydrophobic coating using reactive wetting according to claim 5, wherein the substrate in the first step is graphite, silicon carbide, alumina, diamond or carbon composite.
7. The method for preparing a superhydrophobic coating using reactive wetting according to claim 1, wherein the pore size of the anodized aluminum template in the first step is 400nm, and the anodized aluminum template has a double-pass structure, and the shape of the nano-pores is circular, triangular or square.
8. The method for preparing a superhydrophobic coating using reactive wetting according to claim 1, wherein the composition of the AgCuTi alloy foil in the first step is Ag-Cu28-ti1.5.
9. The method of claim 1, wherein the inert gas in the first step is argon.
10. The method of claim 1, wherein the modifying agent is heptadecafluorodecyltrimethoxysilane in step three.
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| US8603703B2 (en) * | 2006-07-26 | 2013-12-10 | GM Global Technology Operations LLC | Method for making super-hydrophilic and electrically conducting surfaces for fuel cell bipolar plates |
| KR100927729B1 (en) * | 2008-03-14 | 2009-11-18 | 포항공과대학교 산학협력단 | Manufacturing Method of 3D Shaped Structure with Hydrophobic Surface Using Immersion |
| DE102008051883A1 (en) * | 2008-10-16 | 2010-04-22 | Nano-X Gmbh | Coating for cathodic corrosion protection of metal, method for producing the coating and use of the coating. |
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| CN114000138A (en) * | 2021-11-05 | 2022-02-01 | 哈尔滨工业大学 | Method for preparing super-hydrophobic surface by utilizing nano metal hot pressing |
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