CN110760191B

CN110760191B - Template for repeated carving of hydrophobic coating

Info

Publication number: CN110760191B
Application number: CN201910664171.7A
Authority: CN
Inventors: 张衍; 朱鑫睿; 刘育建
Original assignee: East China University of Science and Technology
Current assignee: East China University of Science and Technology
Priority date: 2019-07-23
Filing date: 2019-07-23
Publication date: 2021-06-04
Anticipated expiration: 2039-07-23
Also published as: CN110760191A

Abstract

The invention discloses a template for re-engraving a hydrophobic coating, which is prepared by the following method: firstly, preparing a template material: the template comprises the raw materials of 40-70 parts of silicone resin, 0.01-10 parts of flatting agent, 0.01-10 parts of defoaming agent, 0.01-5 parts of catalyst and 20-50 parts of solvent. Dissolving the silicone resin into a solvent according to the proportion, adding a defoaming agent, a flatting agent and a catalyst, uniformly stirring, and preserving heat at the temperature of 40-100 ℃ for 1-8 hours to obtain a template material for repeated etching of a hydrophobic coating; and then etching the surface of the template material: soluble salt is embedded in the surface layer of the template material in a multi-time spraying mode, and salt particles are etched, so that a multi-stage rough structure is simply, conveniently and quickly constructed on the surface of a substrate, and the template for re-etching the hydrophobic coating is prepared. The preparation method is simple in preparation process, low in production cost, green and environment-friendly, and the template can be repeatedly used.

Description

Template for repeated carving of hydrophobic coating

Technical Field

The invention relates to a template for hydrophobic coating repeated engraving. Belongs to the technical field of materials.

Background

Hydrophobic materials have important applications in many applications, for example, they can be used for stain resistance, self-cleaning, ice adhesion, corrosion protection, oxidation resistance, and prevention of current conduction. Based on the lotus leaf hydrophobic self-cleaning effect, the super-hydrophobic surface based on bionics has become a research hotspot at present. When preparing hydrophobic surface, firstly reducing the free energy of the surface of the material; secondly, the roughness of the surface of the material is improved, the contact area between water drops and the surface is reduced, the contact angle of the surface can be effectively improved, and the hydrophobicity is increased.

However, the current method for constructing the surface roughness has the problems of complex process, high cost and the like. For example: the invention with the publication number of CN106809795A and the name of 'a super-hydrophobic microstructure and a preparation method' takes colloid crystal grains as an etching mask, adopts a colloid crystal grain etching technology and utilizes an inductive coupling plasma etching technology to carry out etching, thereby forming a nano-scale or micron-scale microstructure on the surface of a silicon wafer. The surface roughness of the material can be well controlled by utilizing a photoetching method, but the instrument is expensive, the preparation process is complex, and the method is not suitable for large-scale production; the invention with the publication number of CN103409754A and the name of 'super-hydrophobicity treatment process for the surface of aluminum material based on etching method' reports that the super-hydrophobicity performance is obtained by etching the surface of a polished aluminum sample by using a hydrochloric acid solution with a certain concentration and then performing low-surface-energy modification by using a stearic acid ethanol solution. The roughness can be constructed by etching the porous aluminum template, but the selectable substrates are limited, and the etching effect is not easy to control.

Disclosure of Invention

The invention aims to provide a template for hydrophobic coating re-engraving, which has the advantages of simple process and low cost and can be repeatedly used, so as to overcome the defects in the prior art.

In order to achieve the purpose, the invention provides the following technical scheme:

a template for hydrophobic coating replication, said template being prepared by the method comprising:

1) preparing a template material:

the template comprises the following raw materials in parts by weight:

dissolving silicone resin in a solvent according to the proportion, adding a defoaming agent, a flatting agent and a catalyst, uniformly stirring, and preserving heat at the temperature of 40-100 ℃ for 1-8 hours to obtain the template material for repeated etching of the hydrophobic coating;

the silicone resin is at least one of phenyl silicone resin, methyl phenyl silicone resin, polyaryl silicone resin, vinyl silicone resin and vinyl phenyl silicone resin,

the catalyst is an organotin carboxylate.

2) Etching the surface of the template material:

dissolving soluble salt in deionized water with the mass concentration of 1-35%; adjusting the pressure of an air compressor to 0.2-0.8MPa, atomizing the solution by a spray gun, spraying 1-8 times on the surface of the template material, heating the template material to 150-.

In step 1):

the leveling agent is at least one of polyethylacrylate, polybutyl acrylate, poly (2-ethylhexyl acrylate), ethyl acrylate-butyl acrylate copolymer or organic silicon modified polyacrylate.

The defoaming agent is emulsified silicone oil or polydimethylsiloxane.

The solvent is at least one of xylene, toluene, acetone, isopropanol, n-butanol and ethyl acetate.

The catalyst is preferably dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, dioctyltin mercaptide and alkyl tin mercaptide.

In step 2):

the soluble inorganic salt is at least one of sodium salt, potassium salt and ammonium salt, preferably sodium carbonate, potassium carbonate, sodium chloride, potassium chloride, sodium sulfate, potassium sulfate and ammonium chloride.

By adopting the technical scheme, the invention has the following advantages and beneficial effects:

according to the template for re-engraving the hydrophobic coating, the silicone resin is selected as the matrix, so that the template has good high-temperature resistance and low cost. In addition, when the template material is etched, the surface roughness of the template can be regulated and controlled by changing the spraying pressure, and finally the template for repeated etching of the hydrophobic coating is obtained. The template can be used for simply, conveniently and quickly constructing rough structures on the surfaces of different matrixes, so that the hydrophobicity of the coating is greatly enhanced, and the hydrophobic or super-hydrophobic performance is achieved. Meanwhile, the template can be reused, so that the cost is further reduced, and the method has a good industrial application prospect.

Drawings

FIG. 1 is a SEM illustration of a template for hydrophobic coating replication in example 1 of the present invention.

FIG. 2 is a SEM illustration of an epoxy coating replicated with the prepared template in example 1 of the present invention.

Fig. 3 is a schematic water contact angle of an epoxy coating without repeated engraving.

FIG. 4 is a schematic water contact angle of an epoxy coating replicated with the prepared template in example 1 of the present invention.

Detailed Description

In order to more clearly illustrate the present invention, the present invention will be further described with reference to the following examples and the accompanying drawings.

Example 1

And (2) dissolving 30g of vinyl silicone resin in 70.5g of dimethylbenzene, uniformly stirring, adding 0.06g of defoaming agent (BYK-306), 0.06g of flatting agent (BYK-333) and 0.2g of dibutyltin dilaurate, uniformly stirring again, placing in a 90 ℃ oven, and preserving heat for 4 hours to pre-cure the mixture to obtain the template material.

20g of ammonium chloride and 15g of sodium chloride were dissolved in 200g of deionized water. Adjusting the pressure of an air compressor to 0.2MPa, atomizing the solution by a spray gun, spraying for 2 times on the surface of the template material, and after salt particles are crystallized, heating the template material to 170 ℃ and preserving heat for 2 hours. And after the curing is completed, placing the template material in deionized water to etch and remove the salt particles, and finally obtaining the template for re-etching the hydrophobic coating.

E51 epoxy resin coating with the thickness of about 1mm is poured on the surface of the template, and after the epoxy resin coating is cured and demoulded, the epoxy resin coating with the hydrophobic property can be obtained.

The epoxy coating was tested with a contact angle measuring instrument and the contact angle with water was found to be 130 °.

Example 2

Dissolving 10g of phenyl silicone resin and 15g of vinyl silicone resin in 74.4g of dimethylbenzene, uniformly stirring, adding 0.2g of defoaming agent (BYK-A535), 0.2g of flatting agent (BYK-380N) and 0.2g of dioctyl tin mercaptide, uniformly stirring again, and placing in an oven at 80 ℃ for heat preservation for 8 hours to pre-cure to obtain the template material.

35g of potassium carbonate were dissolved in 100g of deionized water. Adjusting the pressure of an air compressor to 0.8MPa, atomizing the solution by a spray gun, spraying the solution on the surface of the resin for 4 times, and crystallizing the potassium carbonate. The template material is heated to 220 ℃ and is kept warm for 2 h. And after the curing is completed, placing the template material in deionized water to etch and remove the salt particles, and finally obtaining the template for re-etching the hydrophobic coating.

And pouring a polydimethylsiloxane coating with the thickness of about 1mm on the surface of the template, and demolding after curing to obtain the polydimethylsiloxane coating with the super-hydrophobic property.

The coating was tested with a contact angle measuring instrument and the contact angle with water was 152 °.

As shown in fig. 1 to 4, fig. 1 is a SEM view of a template for re-etching a hydrophobic coating layer in example 1 of the present invention, fig. 2 is a SEM view of an epoxy coating layer re-etched with the prepared template in example 1 of the present invention, fig. 3 is a water contact angle view of an epoxy coating layer without re-etching, and fig. 4 is a water contact angle view of an epoxy coating layer re-etched with the prepared template in example 1 of the present invention.

The template for the hydrophobic coating repeated engraving of the invention can simply, conveniently and quickly construct rough structures (as shown in figure 2) on the surfaces of different substrates, so that the hydrophobicity of the coating is greatly enhanced (as shown in figure 4), and the hydrophobic or super-hydrophobic performance is achieved.

Claims

1. A template for hydrophobic coating replication, said template being prepared by the method comprising:

1) preparing a template material:

the template comprises the following raw materials in parts by weight:

the silicone resin is at least one of phenyl silicone resin, methyl phenyl silicone resin, vinyl silicone resin and vinyl phenyl silicone resin,

the catalyst is organic tin carboxylate;

2) etching the surface of the template material:

dissolving soluble inorganic salt in deionized water with the mass concentration of 1-35%, adjusting the pressure of an air compressor to 0.2-0.8MPa, atomizing the solution by a spray gun, spraying for 1-8 times on the surface of the template material, heating the template material to 150-phase and 250 ℃ for heat preservation for 1-12h, and removing salt particles by using deionized water after curing to obtain the template for re-etching the hydrophobic coating.

2. The stencil for lithographically reorganizing a hydrophobic coating as claimed in claim 1, wherein the leveling agent in step 1) is at least one of polyethylacrylate, polybutylacrylate, poly-2-ethylhexyl acrylate, copolymer of ethylacrylate and butylacrylate, or silicone modified polyacrylate.

3. The stencil for hydrophobic coating imprinting according to claim 1, wherein in step 1), the anti-foaming agent is silicone emulsion or polydimethylsiloxane.

4. The template for hydrophobic coating counterengraving of claim 1, wherein in the step 1), the solvent is at least one of xylene, toluene, acetone, isopropanol, n-butanol and ethyl acetate.

5. The template for hydrophobic coating re-engraving of claim 1, wherein in the step 1), the catalyst is one of dibutyltin dilaurate, stannous octoate, dibutyltin diacetate, dioctyltin mercaptide and alkyltin mercaptide.

6. The template for hydrophobic coating imprinting according to claim 1, wherein in step 2), the soluble inorganic salt is at least one of a sodium salt, a potassium salt, and an ammonium salt.

7. The template for hydrophobic coating counterengraving of claim 6, wherein in the step 2), the soluble inorganic salt is one or more of sodium carbonate, potassium carbonate, sodium chloride, potassium chloride, sodium sulfate, potassium sulfate and ammonium chloride.