Polydimethylsiloxane amphiphobic coating, preparation method therefor, and use thereof

Abstract

The present invention relates to the field of preparation of self-cleaning materials, and particularly relates to a polydimethylsiloxane amphiphobic coating, a preparation method therefor, and the use thereof. Disclosed in the present invention are the polydimethylsiloxane amphiphobic coating, the preparation method therefor, and the use thereof. Raw materials of the polydimethylsiloxane amphiphobic coating provided in the present invention comprise: hydroxyl polydimethylsiloxane, a sulfhydryl compound, a fluorine-containing acrylate, a curing agent and an initiator. Provided in the present invention is the preparation method of the polydimethylsiloxane amphiphobic coating, which comprises the following steps: mixing hydroxyl polydimethylsiloxane, a sulfydryl compound, a fluorine-containing acrylate and an initiator with a solvent to obtain a mixed solution, performing light irradiation on the mixed solution, adding a curing agent to obtain a coating solution, coating a surface of a substrate with the coating solution, and curing same to obtain the polydimethylsiloxane amphiphobic coating. The coating prepared in the present invention has a water contact angle of 145°-159°, and an oil contact angle of 134°-149°.

Description

A polydimethylsiloxane amphiphobic coating, preparation method and application

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] The present invention claims the priority of the Chinese patent application entitled “A polydimethylsiloxane amphiphobic coating, preparation method and application” filed on September 4, 2023, with application number CN202311129901.6, and claims the priority of the Chinese patent application entitled “A preparation method of an amphiphobic coating, the prepared amphiphobic coating and application” filed on December 5, 2023, with application number 202311648286.X. Technical Field

[0003] The present invention relates to the field of self-cleaning material preparation, and in particular to a polydimethylsiloxane amphiphobic coating, a preparation method and applications thereof. Background Art

[0004] Chemical mechanical planarization (CMP), one of the most critical technologies for achieving multi-level metallization and gate and channel material incorporation during integrated circuit (IC) manufacturing, is an essential planarization process in semiconductor manufacturing. However, the polishing slurry used in the CMP process contains a certain amount of abrasive nanoparticles (such as SiO2 and CeO2). As the polishing process progresses, the mechanical abrasion causes the slurry to evaporate due to temperature increases, increasing the abrasive concentration and leading to localized supersaturation of the nanoabrasive particles. This temperature increase also accelerates the movement of the colloidal particles, causing the nanoparticles to agglomerate and adhere to the surface of the polishing equipment, forming white crystals that are difficult to clean and severely impact subsequent processes and production. Furthermore, because the polishing equipment is made of metal, long-term use of the polishing slurry can also cause a certain degree of corrosion. However, there is currently no clear solution to the problem of nanoparticle agglomeration in the polishing slurry system. Therefore, applying an amphiphobic coating to the polishing equipment with both anti-corrosion and self-cleaning properties has become an effective solution.

[0005] Polydimethylsiloxane (PDMS) resin is a polymer with low surface energy, good mechanical properties, thermal stability, and chemical stability, making it a promising candidate for amphiphobic anti-corrosion coatings. However, PDMS's lack of oleophobicity and strong adsorption to non-polar substances hinder its application in amphiphobic coatings, necessitating surface modification of the PDMS.

[0006] Currently, methods for modifying the surface of PDMS include plasma treatment, UV irradiation and ozone radiation treatment, and surfactant treatment. Plasma treatment is only a temporary treatment; UV irradiation and ozone radiation treatment require strict environmental conditions and long reaction times; and surfactants can bind to the PDMS surface, reducing hydrophobicity and bonding strength, and affecting the mechanical properties of PDMS.

[0007] Therefore, there is an urgent need in the prior art for an amphiphobic coating that has good amphiphobic effect, strong durability and a simple preparation method to keep the surface of the polishing equipment clean.

[0008] Summary of the Invention

[0009] In order to solve the above problems in the prior art, the present invention proposes a polydimethylsiloxane amphiphobic coating, a preparation method and an application thereof.

[0010] In a first aspect, the present invention provides a polydimethylsiloxane amphiphobic coating, wherein the raw materials of the polydimethylsiloxane amphiphobic coating include: hydroxy polydimethylsiloxane, a mercapto compound, a fluorine-containing acrylate, a curing agent, and an initiator.

[0011] Specifically, the hydroxy polydimethylsiloxane is a hydroxyl-terminated polydimethylsiloxane with a viscosity of 90-100 cp (25° C.) and a hydroxyl content of (1.03±0.03) wt %.

[0012] As a first embodiment of the first aspect of the present invention, the mass ratio of hydroxypolydimethylsiloxane, mercapto compound and curing agent is 1-3:1:0.1-0.4; the mass ratio of mercapto compound, fluorinated acrylate and initiator is 1:0.6-3:0.01-0.3.

[0013] As a specific embodiment of the present invention, the raw materials for preparing the polydimethylsiloxane amphiphobic coating further include filler particles, and the mass ratio of hydroxy polydimethylsiloxane to filler particles is 1:0.5-2.5.

[0014] As a specific embodiment of the present invention, the filler particles include micron-sized particles and nano-sized particles;

[0015] The diameter of the micron-sized particles is 2 to 10 μm, and the diameter of the nano-sized particles is 10 to 30 nm; the mass ratio of the micron-sized particles to the nano-sized particles is 1:(1 to 5);

[0016] The micron-sized particles and nano-sized particles are independently selected from one or more of hydrophobically modified SiO2, TiO2, Al2O3, polytetrafluoroethylene, graphite fluoride, and hollow micro-glass spheres.

[0017] Specifically, the hydrophobically modified SiO2 in the present invention comprises placing SiO2 in a mixture comprising 95% by volume ethanol and 5% by volume deionized water, adding a fluorosilicone to the mixture, adjusting the pH to a weakly acidic or weakly alkaline pH of 5 or 9, and hydrophobically modifying the SiO2 with the fluorosilicone. The mass ratio of SiO2 to fluorosilicone is 1:0.15 to 0.2.

[0018] Specifically, the mass ratio of SiO2 to fluorinated silicone is 1:0.15.

[0019] Specifically, the pH of the mixed solution is adjusted to 5.

[0020] As a specific embodiment of the present invention, the water contact angle of the polydimethylsiloxane amphiphobic coating is 132° to 154°, and the oil contact angle of the polydimethylsiloxane amphiphobic coating is 114° to 129°.

[0021] As a second embodiment of the first aspect of the present invention, based on the mass of hydroxy polydimethylsiloxane as 100%, the mass of the mercapto compound is 1% to 10%, the mass of the fluorinated acrylate is 2% to 20%, the mass of the initiator is 0.01% to 1%, and the mass of the curing agent is 10% to 30%.

[0022] Preferably, based on 100% by mass of hydroxypolydimethylsiloxane, the mass of the mercapto compound is 3% to 7%, the mass of the fluorinated acrylate is 5% to 10%, the mass of the initiator is 0.05 to 0.5%, and the mass of the curing agent is 15% to 25%.

[0023] As a specific embodiment of the present invention, the raw materials for preparing the polydimethylsiloxane amphiphobic coating further include filler particles, and the mass ratio of hydroxy polydimethylsiloxane to filler particles is 1:0.1-1.

[0024] As a specific embodiment of the present invention, the filler particles include micron-sized particles and nano-sized particles;

[0025] Specifically, the particle size of the micron-sized particles is 5 to 15 μm, and the particle size of the nano-sized particles is 10 to 30 nm; the mass ratio of the micron-sized particles to the nano-sized particles is 1:(1 to 5);

[0026] Specifically, the micron-sized particles and nano-sized particles are independently selected from one or more of hydrophobically modified SiO2, TiO2, Al2O3, polytetrafluoroethylene, graphite fluoride, and hollow micro-glass spheres.

[0027] Specifically, the hydrophobically modified SiO2 in the present invention comprises placing SiO2 in a mixture comprising 95% by volume ethanol and 5% by volume deionized water, adding a fluorosilicone to the mixture, adjusting the pH to a weakly acidic or weakly alkaline pH of 5 or 9, and hydrophobically modifying the SiO2 with the fluorosilicone. The mass ratio of SiO2 to fluorosilicone is 1:0.15 to 0.2.

[0028] Specifically, the mass ratio of SiO2 to fluorinated silicone is 1:0.15.

[0029] Specifically, the pH of the mixed solution is adjusted to 5.

[0030] As a specific embodiment of the present invention, the performance of the amphiphobic coating prepared according to the second embodiment of the first aspect of the present invention was tested.

[0031] The water contact angle of the polydimethylsiloxane amphiphobic coating is 145° to 159°, and the oil contact angle of the polydimethylsiloxane amphiphobic coating is 134° to 149°.

[0032] The wear resistance of the polydimethylsiloxane amphiphobic coating was tested by a weight movement method, and the wear resistance of the coating was 122 g to 200 g.

[0033] The hardness of the polydimethylsiloxane amphiphobic coating was tested by the pencil hardness method, and the hardness of the coating was 4H.

[0034] The adhesion of the polydimethylsiloxane amphiphobic coating was tested using the GB / T 9286-1998 standard, and the adhesion of the coating was 4B.

[0035] In a second aspect, the present invention provides a method for preparing the polydimethylsiloxane amphiphobic coating provided in the first embodiment of the first aspect of the present invention, comprising the following steps:

[0036] (1) Hydroxypolydimethylsiloxane, a thiol compound, a curing agent, and a solvent I are configured to form a mixed solution I, wherein the hydroxypolydimethylsiloxane in the mixed solution I reacts with the thiol compound, and the mixed solution I is coated on the surface of the substrate and cured; the coating may include spin coating, spray coating, dip coating, or drop coating.

[0037] (2) preparing a mixed solution II by mixing fluorinated acrylate, an initiator and a solvent II, immersing the substrate cured in step (1) in the mixed solution II, irradiating the substrate with light, causing the mercapto compound to react with the fluorinated acrylate, and aging the substrate to obtain a polydimethylsiloxane amphiphobic coating.

[0038] In hydroxyl-terminated polydimethylsiloxane, thiol groups are introduced into the polydimethylsiloxane coating through a condensation reaction between hydroxyl groups and thiol groups. A curing agent is then added for cross-linking and curing. After complete curing, the remaining thiol groups on the film surface serve as reactive sites. Through a thiol-double bond click reaction, a fluorinated acrylate is introduced onto the film surface to create a low surface energy, thus imparting the PDMS coating with both hydrophobic and oleophobic properties.

[0039] As a specific embodiment of the present invention, the raw materials used in the preparation process of the polydimethylsiloxane amphiphobic coating further include filler particles, and the filler particles include micron-sized particles and nano-sized particles.

[0040] The diameter of micron-sized particles is 2 to 10 μm, and the diameter of nano-sized particles is 10 to 30 nm.

[0041] The micron-sized particles and nano-sized particles are independently selected from one or more of hydrophobically modified SiO2, TiO2, Al2O3, polytetrafluoroethylene, graphite fluoride, and hollow micro-glass spheres.

[0042] In step (1), hydroxy polydimethylsiloxane, a thiol compound, filler particles, a curing agent, and a solvent I are prepared into a mixed solution I. After the filler particles are added, the filler particles can simulate the papillary structure of the lotus leaf surface and construct a fine micro-nano surface secondary structure, thereby increasing the water-oil contact angle of the coating and simultaneously improving the mechanical properties of the coating;

[0043] The mass of the filler particles is 5% to 20% of the mass of the mixed solution I.

[0044] As a specific embodiment of the present invention, step (1) further includes pre-treating the substrate before applying the mixed solution I on the substrate surface. The pre-treatment includes rinsing the substrate to clean the substrate surface.

[0045] Specifically, acetone, ethanol, and deionized water are used to rinse the substrate during the pretreatment process of the present invention.

[0046] As a specific embodiment of the present invention, the mass of hydroxy polydimethylsiloxane is 10% to 20% of the mass of solvent I.

[0047] As a specific embodiment of the present invention, the mass of the fluorine-containing acrylate is 20% to 30% of the mass of the mixed solution II.

[0048] As a specific embodiment of the present invention, the mass of the initiator is 0.1% to 3% of the mass of the mixed solution II.

[0049] As a specific embodiment of the present invention, the mixed solution I in step (1) is stirred and degassed before being coated on the surface of the substrate.

[0050] As a specific embodiment of the present invention, the curing conditions in step (1) include: a curing time of 8 to 12 hours.

[0051] As a specific embodiment of the present invention, the illumination conditions in step (2) include: ultraviolet irradiation with a wavelength of 300 to 380 nm, a power of 8 to 12 W, and an irradiation time of 2 to 8 hours. Under the action of light, the mercapto group can react with the fluorinated acrylate.

[0052] The aging conditions in step (2) include: a temperature of 40 to 60° C. and a time of 1 to 5 hours. During the aging process, the mercapto group reacts more fully with the fluorinated acrylate.

[0053] As a specific embodiment of the present invention, the thiol compound includes at least one or more of tetrakis(3-mercaptopropionic acid)pentaerythritol ester, dipentaerythritol hexa(3-mercaptopropionate), trimethylolpropane tris(3-mercaptopropionate), four-arm polyethylene glycol thiol, 3-mercapto-1-propanol, 1,4-butanediol di(thioglycolate), di(2-mercaptoethyl) adipate, diisopropyl 2,3-dimercaptosuccinate, 1,4-butanediol and di(thioglycolate)ethylene glycol ester.

[0054] Preferably, the mercapto compound is pentaerythritol tetrakis(3-mercaptopropionate).

[0055] As a specific embodiment of the present invention, the curing agent includes at least one or more of isocyanate, acetic acid, diaminodiphenylamine, butanone oxime and methyl ethyl ketone oxime.

[0056] Specifically, the isocyanate is polyhexamethylene diisocyanate.

[0057] As a specific embodiment of the present invention, the fluorine-containing acrylate includes at least one or more of 1H,1H,2H,2H-perfluorodecyl acrylate, 1H,1H,2H,2H-perfluorooctyl methacrylate, 2-(perfluorohexyl)ethyl methacrylate, 2-(perfluorooctyl)ethyl methacrylate, perfluoroalkylethyl methacrylate, tridecafluorooctyl acrylate, perfluoroundecyl acrylate and 2-(perfluorobutyl)ethyl methacrylate.

[0058] Preferably, the fluorine-containing acrylate is 1H,1H,2H,2H-perfluorodecyl acrylate.

[0059] As a specific embodiment of the present invention, the initiator includes at least one or more of benzoin dimethyl ether, dimethylbenzene ketone and photoinitiator 184.

[0060] As a specific embodiment of the present invention, the substrate includes at least one of glass, steel, wood, paper, marble and cotton.

[0061] As a specific embodiment of the present invention, solvent I is selected from one or more of dichloromethane, chloroform, N,N-dimethylformamide, tetrahydrofuran, acetone and n-hexane.

[0062] As a specific embodiment of the present invention, solvent II is selected from one or more of acetone, anhydrous ethanol, isopropanol, n-butanol, dichloromethane, n-hexane, toluene, tetrahydrofuran, ethyl acetate and N,N-dimethylformamide.

[0063] The present invention provides a method for preparing a polydimethylsiloxane amphiphobic coating provided by the second embodiment of the first aspect of the present invention, comprising the following steps:

[0064] A hydroxy polydimethylsiloxane, a mercapto compound, a fluorinated acrylate, an initiator, and a solvent are mixed to obtain a mixed solution. After the mixed solution is irradiated with light, a curing agent is added to obtain a coating solution. The coating solution is applied to the surface of a substrate and cured to obtain a polydimethylsiloxane amphiphobic coating. The coating may include spin coating, spray coating, dip coating, or drop coating.

[0065] In the preparation method provided by the present invention, hydroxy polydimethylsiloxane is mixed with a mercapto compound and a fluorinated acrylate in a solvent. After sufficient reaction, a curing agent is added to obtain a coating, which is sprayed on the surface of a substrate. After complete curing, a uniform and stable super-amphiphobic coating is obtained.

[0066] Hydroxyl-terminated polydimethylsiloxane is grafted with a mercapto compound to obtain an organic resin intermediate (using the condensation reaction between hydroxyl and mercapto groups to obtain mercapto-grafted silicone resin segments), and then a fluorinated acrylate with low surface energy is chemically grafted to the end of the silicone resin chain through a light-induced mercapto-ene click reaction.

[0067] In the preparation method of the present invention, the mercapto compound, serving as an intermediate polymer segment, can react simultaneously with hydroxypolydimethylsiloxane and a fluorinated acrylate. The curing agent is added only after the three have fully reacted, thus eliminating the need for curing agent addition. Furthermore, the fluorinated acrylate is chemically bonded and uniformly present in the coating, ensuring the stability of the coating's performance.

[0068] As a specific embodiment of the present invention, the raw materials used in the preparation process of the polydimethylsiloxane amphiphobic coating also include filler particles.

[0069] The preparation method further comprises: adding filler particles to the mixed solution after the mixed solution is irradiated with light and before the curing agent is added;

[0070] The mass of the filler particles is 1% to 3% of the mass of the mixed liquid.

[0071] After adding filler particles, the filler particles can simulate the papillary structure of the lotus leaf surface and construct a fine micro-nano surface secondary structure, thereby increasing the water-oil contact angle of the coating and increasing the mechanical properties of the coating.

[0072] As a specific embodiment of the present invention, before applying the coating to the substrate surface, the substrate is pretreated, and the pretreatment includes rinsing the substrate to clean the substrate surface. Specifically, acetone, ethanol, and deionized water are used to rinse the substrate during the pretreatment process of the present invention.

[0073] As a specific embodiment of the present invention, the mass of hydroxy polydimethylsiloxane is 9% to 20% of the mass of the solvent;

[0074] As a specific embodiment of the present invention, the mass of the thiol compound is 0.4% to 1% of the mass of the solvent.

[0075] As a specific embodiment of the present invention, the mass of the fluorine-containing acrylate is 0.5% to 2% of the mass of the solvent.

[0076] As a specific embodiment of the present invention, the preparation method further includes: after adding a curing agent, ultrasonicating and degassing to obtain a coating, and coating the coating on the surface of a substrate.

[0077] As a specific embodiment of the present invention, the conditions of illumination include: ultraviolet irradiation, the wavelength of ultraviolet irradiation is 300-380nm, the power is 8-12W, and the ultraviolet irradiation time is 2-8h.

[0078] Specifically, the mixed liquid is irradiated with light while being stirred at a stirring speed of 500 to 1000 rpm.

[0079] As a specific embodiment of the present invention, the curing conditions include: room temperature, time of 8 to 12 hours;

[0080] As a specific embodiment of the present invention, the curing conditions include: 50°C, time is 3 to 5h;

[0081] As a specific embodiment of the present invention, the curing conditions include: 80° C., and a curing time of 30 min to 1 h.

[0082] Among the raw materials used in the present invention, the thiol compound includes at least one or more of tetrakis(3-mercaptopropionic acid)pentaerythritol ester, dipentaerythritol hexa(3-mercaptopropionate), trimethylolpropane tris(3-mercaptopropionate), four-arm polyethylene glycol thiol, 3-mercapto-1-propanol, 1,4-butanediol di(thioglycolate), di(2-mercaptoethyl)adipate, diisopropyl 2,3-dimercaptosuccinate, 1,4-butanediol and ethylene glycol di(thioglycolate).

[0083] Preferably, the mercapto compound is pentaerythritol tetrakis(3-mercaptopropionate).

[0084] As a specific embodiment of the present invention, the curing agent includes at least one or more of isocyanate, acetic acid, diaminodiphenylamine, butanone oxime and methyl ethyl ketone oxime.

[0085] Specifically, the isocyanate is polyhexamethylene diisocyanate.

[0086] As a specific embodiment of the present invention, the fluorine-containing acrylate includes at least one or more of 1H,1H,2H,2H-perfluorodecyl acrylate, 1H,1H,2H,2H-perfluorooctyl methacrylate, 2-(perfluorohexyl)ethyl methacrylate, 2-(perfluorooctyl)ethyl methacrylate, perfluoroalkylethyl methacrylate, tridecafluorooctyl acrylate, perfluoroundecyl acrylate and 2-(perfluorobutyl)ethyl methacrylate.

[0087] Preferably, the fluorine-containing acrylate is 1H,1H,2H,2H-perfluorodecyl acrylate.

[0088] As a specific embodiment of the present invention, the initiator includes at least one or more of benzoin dimethyl ether, dimethylbenzene ketone and photoinitiator 184.

[0089] As a specific embodiment of the present invention, the substrate includes at least one of glass, steel, wood, paper, marble and cotton.

[0090] As a specific embodiment of the present invention, solvent I is selected from one or more of dichloromethane, chloroform, N,N-dimethylformamide, tetrahydrofuran, acetone and n-hexane.

[0091] As a specific embodiment of the present invention, solvent II is selected from one or more of acetone, anhydrous ethanol, isopropanol, n-butanol, dichloromethane, n-hexane, toluene, tetrahydrofuran, ethyl acetate and N,N-dimethylformamide.

[0092] In a third aspect, the present invention provides an application of the polydimethylsiloxane amphiphobic coating provided in the first aspect of the present invention or the polydimethylsiloxane amphiphobic coating prepared by the preparation method provided in the second aspect of the present invention in cleaning polishing equipment during chemical mechanical planarization.

[0093] The amphiphobic coating provided by the first embodiment of the first aspect of the present invention and the amphiphobic coating prepared by the method for preparing the amphiphobic coating provided by the first embodiment of the first aspect of the present invention in the second aspect have the following beneficial effects.

[0094] (1) The coating prepared by the present invention has a water contact angle greater than 132° and an oil contact angle greater than 114°, and has strong amphiphobic properties. After being coated on polishing equipment, it can largely prevent the nanoabrasive particles in the polishing liquid from adhering to the surface of the polishing equipment, and can keep the surface of the polishing equipment clean.

[0095] (2) The in situ self-assembly of the fluorinated acrylate in the present invention is based on a thiol-ene click reaction, which is simple and efficient with a high conversion rate. The prepared polydimethylsiloxane amphiphobic coating has a large water-oil contact angle.

[0096] (3) The polydimethylsiloxane amphiphobic coating prepared by the present invention has strong chemical corrosion resistance, strong adhesion and wear resistance, and can be used in chemical mechanical polishing (CMP) processes or other harsh operating environments.

[0097] (4) The polydimethylsiloxane amphiphobic coating prepared by the present invention also has good thermal stability and can be applied to higher operating temperatures.

[0098] (5) The present invention adds filler particles during the coating preparation process. The filler particles can mimic the papillary structure of the lotus leaf surface in the coating, constructing a fine micro-nano surface secondary structure, thereby increasing the water-oil contact angle of the coating. The filler particles in the present invention can be selected from hydrophobically modified SiO2 particles, polytetrafluoroethylene particles, or other particles. Changing the type of nanoparticles has little effect on the hydrophobic oil properties of the coating.

[0099] (6) The hydroxy polydimethylsiloxane used in the present invention contains hydroxyl groups, which can make the hydroxy polydimethylsiloxane adhere well to the surface of the substrate, so that the prepared coating does not need to be pretreated with a pretreatment agent before being applied to the substrate surface.

[0100] (7) The modified polydimethylsiloxane amphiphobic coating material provided by the present invention has a wide range of applications and is expected to be used in equipment corrosion protection, oil-water separation, clothing and accessories, electronic product protection and other fields.

[0101] The amphiphobic coating provided by the second embodiment of the first aspect of the present invention and the amphiphobic coating prepared by the method for preparing the amphiphobic coating provided by the second embodiment of the first aspect of the present invention have the following beneficial effects.

[0102] (1) The coating prepared by the present invention has a water contact angle of 145° to 159° and an oil contact angle of 134° to 149°. It has strong amphiphobic properties. When applied to polishing equipment, it can largely prevent the nanoabrasive particles in the polishing liquid from adhering to the polishing equipment surface, thereby maintaining the cleanliness of the polishing equipment surface.

[0103] (2) The present invention grafts hydroxy polydimethylsiloxane, a mercapto compound, and a fluorinated acrylate by a one-step method to obtain a siloxane polymer segment modified with a long fluorocarbon chain group at the end. The mercapto compound can react with the hydroxy polydimethylsiloxane and the fluorinated acrylate at the same time, the reaction process is sufficient, and the amount of fluorine introduced into the coating is not limited by the amount of mercapto groups grafted with the hydroxyl group, nor by the reaction time of the hydroxy polydimethylsiloxane and the mercapto compound. In addition, based on the reversible mercapto-ene click reaction between the mercapto compound and the fluorinated acrylate, the amphiphobic coating is given certain self-healing properties.

[0104] (3) The hydroxyl groups in the hydroxy polydimethylsiloxane used in the present invention have strong polarity, which facilitates bonding with the substrate material, ensuring strong adhesion of the coating. This eliminates the need for pre-treatment of the substrate surface with a pre-treatment agent before application. Furthermore, after grafting with the fluorinated acrylate, the hydroxyl groups have lower surface energy and are therefore more likely to migrate to the coating surface, imparting excellent hydrophobic and oleophobic properties to the coating.

[0105] (4) The polydimethylsiloxane amphiphobic coating prepared by the present invention has strong chemical corrosion resistance, strong adhesion and wear resistance, and can be used in chemical mechanical polishing (CMP) processes or other harsh operating environments.

[0106] (5) The polydimethylsiloxane amphiphobic coating prepared by the present invention also has good thermal stability and can be applied to higher operating temperatures.

[0107] (6) The present invention adds filler particles during the coating preparation process. The filler particles can mimic the papillary structure of the lotus leaf surface in the coating, constructing a fine micro-nano surface secondary structure, thereby increasing the water-oil contact angle of the coating. The filler particles in the present invention can be selected from hydrophobically modified SiO2 particles, polytetrafluoroethylene particles, or other particles. Changing the type of nanoparticles has little effect on the hydrophobic oil properties of the coating.

[0108] (7) The modified polydimethylsiloxane amphiphobic coating material provided by the present invention has a wide range of applications and is expected to be used in equipment corrosion protection, oil-water separation, clothing and accessories, electronic product protection and other fields. BRIEF DESCRIPTION OF THE DRAWINGS

[0109] FIG1 is a graph showing the water contact angle of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0110] FIG2 is a graph showing the contact angle of n-hexadecane of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0111] FIG3 is a graph showing the contact angle of the CMP polishing solution of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0112] FIG4 is an infrared test spectrum of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0113] FIG5 is a roughness test diagram of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0114] FIG6 is a thermogravimetric graph of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0115] FIG7 is a SEM image of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention;

[0116] FIG8 is an SEM image of the modified polydimethylsiloxane amphiphobic coating prepared in Example 1 of the present invention.

[0117] FIG9 is a graph showing the water contact angle of the modified polydimethylsiloxane amphiphobic coating prepared in Example 11 of the present invention;

[0118] FIG10 is a graph showing the contact angle of n-hexadecane of the modified polydimethylsiloxane amphiphobic coating prepared in Example 11 of the present invention;

[0119] FIG11 is a graph showing the contact angle of the CMP polishing solution of the modified polydimethylsiloxane amphiphobic coating prepared in Example 11 of the present invention;

[0120] FIG12 is an infrared test spectrum of the modified polydimethylsiloxane amphiphobic coating prepared in Example 11 of the present invention;

[0121] FIG13 is a roughness test graph of the modified polydimethylsiloxane amphiphobic coating prepared in Example 11 of the present invention;

[0122] FIG14 is an SEM image of the modified polydimethylsiloxane amphiphobic coating prepared in Example 11 of the present invention. DETAILED DESCRIPTION

[0123] The present invention will be further described below with reference to specific examples, but they do not constitute any limitation to the present invention.

[0124] The raw materials used in the embodiments of the present invention are all commercially available, among which:

[0125] Liquid reagents such as ethanol, acetone, and dichloromethane were purchased from Kermiou Reagents;

[0126] Hydroxylated polydimethylsiloxane and polyhexamethylene diisocyanate curing agent were purchased from Shenzhen Jipeng Silicon Fluoride Materials Co., Ltd.; the viscosity of hydroxylated polydimethylsiloxane was 90 mm 2 / s (25℃), specific gravity is 0.99 (25℃), refractive index is 1.413, and functional group equivalent is 30000g / mol;

[0127] Pentaerythritol tetrakis(3-mercaptopropionate) was purchased from Shanghai Titan Technology Co., Ltd.

[0128] 1H,1H,2H,2H-Perfluorodecyl acrylate was purchased from Shanghai Titan Technology Co., Ltd.

[0129] Benzoin dimethyl ether and dimethylbenzene ketone were purchased from Jizhi Chemical

[0130] Example 1

[0131] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0132] Dissolve 2g of hydroxypolydimethylsiloxane in 12mL of dichloromethane, add 2g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.3g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0133] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0134] The water contact angle of the amphiphobic coating was tested to be 153.58°, and the n-hexadecane contact angle was 128.69°. Contact angle test photos are shown in Figures 1 and 2.

[0135] Example 2

[0136] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0137] Dissolve 2g of hydroxypolydimethylsiloxane in 12mL of acetone, add 2g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm, respectively (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.3g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0138] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0139] The tested water contact angle of the amphiphobic coating was 132.26°, and the n-hexadecane contact angle was 114.75°.

[0140] Example 3

[0141] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0142] 2 g of hydroxypolydimethylsiloxane was dissolved in 12 mL of dichloromethane, 0.9 g of pentaerythritol tetrakis(3-mercaptopropionate) was added and stirred for 1 h, and then 0.3 g of isocyanate was added and stirred for 30 min. After ultrasonic degassing for 10 min, the mixture was spin-coated on a glass slide and cured at room temperature for 8 h.

[0143] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0144] The tested water contact angle of the amphiphobic coating was 139.81°, and the n-hexadecane contact angle was 117.62°.

[0145] Example 4

[0146] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0147] Dissolve 2g of hydroxypolydimethylsiloxane in 12mL of dichloromethane, add 1g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm, respectively (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.3g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0148] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0149] The tested water contact angle of the amphiphobic coating was 143.55°, and the n-hexadecane contact angle was 122.89°.

[0150] Example 5

[0151] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0152] 2 g of hydroxypolydimethylsiloxane was dissolved in 12 mL of dichloromethane, and 2 g of polytetrafluoroethylene with average particle sizes of 4 μm and 20 nm were added (the mass ratio of polytetrafluoroethylene particles of 4 μm and 20 nm was 1:5). The mixture was stirred at 1200 r / min for 20 min, and 0.9 g of pentaerythritol tetrakis(3-mercaptopropionate) was added and stirred for 1 h. Then, 0.3 g of isocyanate was added and stirred for 30 min. After ultrasonic degassing for 10 min, the mixture was spin-coated on a glass slide and cured at room temperature for 8 h.

[0153] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0154] The tested water contact angle of the amphiphobic coating was 152.33°, and the n-hexadecane contact angle was 127.44°.

[0155] Example 6

[0156] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0157] Dissolve 2g of hydroxypolydimethylsiloxane in 12mL of dichloromethane, add 2g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.3g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0158] 0.018 g of xylene ketone and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution. After being irradiated under a UV lamp with a wavelength of 365 nm and a power of 10 W for 3 hours, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0159] The tested water contact angle of the amphiphobic coating was 149.66°, and the n-hexadecane contact angle was 126.93°.

[0160] Example 7

[0161] A 304 stainless steel piece with a size of 2 cm × 5 cm × 0.3 cm was cleaned with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0162] Dissolve 2g of hydroxypolydimethylsiloxane in 12mL of dichloromethane, add 2g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.3g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0163] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0164] The tested water contact angle of the amphiphobic coating was 151.15°, and the n-hexadecane contact angle was 128.74°.

[0165] Example 8

[0166] A cotton cloth with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0167] Dissolve 2g of hydroxypolydimethylsiloxane in 12mL of dichloromethane, add 2g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.3g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0168] 0.018 g of benzoin dimethyl ether and 1.8 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 9 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0169] The tested water contact angle of the amphiphobic coating was 153.39°, and the n-hexadecane contact angle was 128.23°.

[0170] Example 9

[0171] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0172] Dissolve 1.4 g of hydroxypolydimethylsiloxane in 10 mL of dichloromethane, add 2 g of hydrophobically modified silica filler particles with average particle sizes of 5 μm and 20 nm, respectively (mass ratio of 5 μm and 20 nm silica filler particles is 1:5), and stir at 1200 rpm for 20 minutes. Add 0.9 g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1 hour. Then, add 0.09 g of isocyanate and continue stirring for 30 minutes. After ultrasonic degassing for 10 minutes, the mixture is spin-coated on a glass slide and cured at room temperature for 8 hours. The silica filler particles are hydrophobically modified silica filler particles.

[0173] 0.008 g of benzoin dimethyl ether and 1.1 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 7 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. Then, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0174] The tested water contact angle of the amphiphobic coating was 150.22°, and the n-hexadecane contact angle was 127.67°.

[0175] Example 10

[0176] A glass piece with a size of 2 cm × 5 cm × 0.3 cm was washed with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0177] Dissolve 2.7g of hydroxypolydimethylsiloxane in 15mL of dichloromethane, add 2g of hydrophobically modified silica filler particles with average particle sizes of 5μm and 20nm, respectively (mass ratio of 5μm and 20nm silica filler particles is 1:5), and stir at 1200r / min for 20min. Add 0.9g of pentaerythritol tetrakis(3-mercaptopropionate) and stir for 1h. Then add 0.36g of isocyanate and continue stirring for 30min. After ultrasonic degassing for 10min, the mixture is spin-coated on a glass slide and cured at room temperature for 8h. The silica filler particles are hydrophobically modified silica filler particles.

[0178] 0.27 g of benzoin dimethyl ether and 2.7 g of 1H,1H,2H,2H-perfluorodecyl acrylate were dissolved in 12 mL of ethanol solution, and the above-mentioned completely cured glass slide was immersed in the solution and kept under ultraviolet light with a wavelength of 365 nm and a power of 10 W for 3 hours. After that, the glass slide was taken out and placed in an oven at 50°C for 2 hours. After rinsing the surface with anhydrous ethanol, an amphiphobic coating attached to the surface of the glass slide was obtained.

[0179] The tested water contact angle of the amphiphobic coating was 148.31°, and the n-hexadecane contact angle was 126.04°.

[0180] Application Example 1

[0181] The contact angle of the polishing liquid of the present invention on the surface of the coating prepared in Example 1 was tested, and the test results are shown in Figure 3. The contact angle of the coating polishing liquid was measured to be 140.7°. After the coating prepared by the present invention is applied to the surface of the polishing equipment, it can avoid the polishing liquid residue on the surface of the polishing equipment, so that the surface of the polishing equipment is kept clean. The polishing liquid used in the test was produced by Dalian Zhengyun Technology Co., Ltd. The ingredients of the polishing liquid are: water, 20nm silica filler, potassium permanganate, polyethylene glycol, N-(p-aminoethyl)-r-aminopropyltrimethoxysilane, ethylenediamine, and triethanolamine.

[0182] It can be seen from the contact angles of water and n-hexadecane of the substrate surface modified polydimethylsiloxane amphiphobic coating measured in the above examples.

[0183] Comparison of Example 1 and Example 2 shows that dissolving hydroxypolydimethylsiloxane in dichloromethane is more polar than dissolving hydroxypolydimethylsiloxane in acetone. Dichloromethane has a greater polarity than acetone, which can achieve uniform dispersion of siloxane and pentaerythritol tetrakis(3-mercaptopropionic acid), effectively avoiding the occurrence of phase separation, and is more conducive to obtaining a uniform and stable coating, so that the water-oil contact angle of the prepared coating is larger.

[0184] Comparison of Example 1 with Examples 3-4 demonstrates that filler particles can mimic the papillary structure of a lotus leaf surface, constructing a fine micro-nano surface secondary structure, thereby increasing the water-oil contact angle of the coating. The degree of increase in the water-oil contact angle of the prepared coating is also reduced when no filler particles are added or when a smaller amount of filler particles is used.

[0185] Comparison between Example 1 and Example 5 shows that the filler particles in the present invention can be selected from hydrophobically modified SiO2 particles or polytetrafluoroethylene particles, and the change in the type of nanoparticles has little effect on the hydrophobicity of the coating.

[0186] Comparison between Example 1 and Example 6 shows that benzoin dimethyl ether and dimethyl acetone are used as photoinitiators for the thiol-ene click reaction. Although the initiation mechanisms are different, benzoin dimethyl ether is based on a cracking mechanism and dimethyl ketone is based on a hydrogen abstraction mechanism, both can effectively catalyze the thiol-ene reaction and achieve chemical bonding of fluorinated acrylate on the coating surface.

[0187] Comparison between Example 1 and Examples 7-8 shows that the amphiphobic coating prepared in the present invention can be widely applied to various substrates.

[0188] Comparison between Example 1 and Examples 9-10 shows that the raw material composition for preparing the amphiphobic coating in the present invention can be adjusted within the composition defined in the present invention, with little effect on the water-oil contact angle of the coating.

[0189] The present invention uses an infrared tester (Bruker Alpha II) to perform infrared testing on the coating, raw materials and intermediate reaction products prepared in Example 1. The test results are shown in Figure 4.

[0190] PDMS stands for hydroxypolydimethylsiloxane.

[0191] 2955cm -1 The infrared absorption peak at 1260 cm is attributed to the asymmetric stretching vibration of CH3. -1 The infrared absorption peak at 1070 cm is attributed to the symmetrical bending vibration of the -CH3 group, while the -1 The strong absorption at 905cm is caused by the asymmetric stretching vibration of the -Si-O-Si- bond in the hydroxy polydimethylsiloxane polymer. -1 The weak infrared absorption at 790 cm is attributed to the stretching vibration of Si-OH. -1 The strong absorption is attributed to the stretching vibration of the Si-C bond.

[0192] PDMS-SH represents the coating formed after the mixed solution I is cured

[0193] By adding pentaerythritol tetrakis(3-mercaptopropionic acid) ester into PDMS, thiol groups were introduced as reactive sites. After the thiol groups were introduced into the curing system, the infrared spectrum showed that the 2955cm -1 There is still asymmetric stretching vibration characteristic absorption of CH3, which is found at 2565cm -1 There is an obvious S-H characteristic absorption at 1730cm -1 There is a characteristic absorption of C=O at 1140cm -1 The characteristic absorption of the CO bond at indicates that pentaerythritol tetrakis(3-mercaptopropionate) successfully participates in the curing of PDMS, and the remaining –SH can undergo a thiol-double bond click reaction with the fluorinated acrylate.

[0194] PDMS-SH-F represents the amphiphobic coating prepared in Example 1

[0195] The infrared spectrum test after depositing fluorinated acrylate on the surface of the film with mercapto groups showed that the -1 The obvious S-H characteristic absorption disappears at 1202 cm -1 There is an obvious C-F characteristic absorption peak at 1620-1680 cm -1There is no characteristic absorption of C=C, indicating that perfluorodecyl acrylate is deposited on the film surface in the form of chemical bonding. -1 There are characteristic absorptions of C=O and 1140cm -1 The characteristic absorption of the C-O bond at the position is attributed to the stretching vibration of the ester group of perfluorodecyl acrylate.

[0196] The present invention uses an atomic force microscope (Park NX20) to test the roughness of the amphiphobic coating prepared in Example 1. The test results are shown in Figure 5, and the roughness calculation results are shown in Table 1.

[0197] Table 1 Roughness results of the coating in Example 1

[0198] It can be seen from Table 1 that the line roughness of the coating prepared in Example 1 is Ra=54.354 nm.

[0199] The thermal stability of the coating prepared in Example 1 was tested using a thermogravimetric analyzer (NETZSCH TG209F3). The test graph is shown in Figure 6. As shown in Figure 6, the coating prepared in Example 1 exhibited no significant weight change below 230°C. This indicates that the coating prepared in the present invention can function normally within temperatures of at least 230°C.

[0200] The present invention uses a scanning electron microscope (Tescan AMBER) to observe the morphology of the coating prepared in Example 1, and the SEM images are shown in Figures 7 and 8. As shown in Figures 7 and 8, the coating prepared in Example 1 of the present invention forms a micro-nano secondary structure.

[0201] The present invention conducted a chemical resistance test on the coating prepared in Example 1, and the test results are shown in Table 2.

[0202] Table 2 Test results of chemical resistance of coating in Example 1

[0203] Three identical steel materials were used as substrates. The coating prepared in Example 1 of the present invention was applied to the entire surface of the substrates. The three substrates were then immersed in a 1M HCl solution for 48 h, a 1M NaOH solution for 48 h, and a 1M NaCl solution for 48 h to test the corrosion resistance of the coatings.

[0204] It was observed that there was no damage to the coating on the surface of the substrate, and the hydrophobicity and oleophobicity angles of the coating were measured, and the results are shown in Table 2. The results show that the coating prepared in Example 1 has good corrosion resistance.

[0205] The present invention conducted mechanical property tests on the coatings prepared in Examples 1-10, and the test results are shown in Table 3.

[0206] (1) Wear resistance test:

[0207] A substrate coated with the polydimethylsiloxane amphiphobic coating prepared by the present invention is placed horizontally, and a piece of 320-grit sandpaper with an area of ​​approximately 1 / 3 of the polydimethylsiloxane amphiphobic coating is placed on its surface. A glass plate with an area equivalent to the sandpaper is placed on the adhesive backing of the sandpaper, and the sandpaper and the glass plate are adhered together by the adhesive backing to prevent relative sliding between the two. Finally, a weight is placed on the glass plate to ensure that the polydimethylsiloxane amphiphobic coating is in contact with the sandpaper surface. The sandpaper is moved at a speed of v = 0.5 mm / s, and the minimum weight corresponding to the scratch depth of the polydimethylsiloxane amphiphobic coating surface ≥ 1 μm is recorded to measure the wear resistance of the coating.

[0208] (2) Hardness test:

[0209] The hardness of the wear-resistant coating on the surface of the polydimethylsiloxane amphiphobic coating prepared by the present invention was tested by a pencil hardness method.

[0210] (3) Testing:

[0211] The adhesion between the polydimethylsiloxane amphiphobic coating prepared in this invention and the substrate was tested using the GB / T 9286-1998 standard. A 10x10 grid array was cut into the coating surface using a blade. 3M tape was applied to the cut grid surface. The tape surface was vigorously rubbed with an eraser to ensure adhesion. The tape was then grasped at one end and torn off at a 90-degree angle to test the coating's adhesion.

[0212] Table 3 Mechanical properties test results of the coatings in Examples 1-10

[0213] Comparison of Example 1 and Example 2 shows that dissolving the hydroxypolydimethylsiloxane in dichloromethane in Example 1 is more polar than dissolving the hydroxypolydimethylsiloxane in acetone. Dichloromethane is more polar than acetone, which can achieve uniform dispersion of siloxane and pentaerythritol tetrakis(3-mercaptopropionic acid), effectively avoiding the occurrence of phase separation, and is conducive to obtaining a uniform and stable coating. The mechanical properties of the amphiphobic coating prepared in Example 1 are better than those of the amphiphobic coating prepared in Example 2.

[0214] Comparison between Example 1 and Examples 3-4 shows that the presence of a certain amount of filler particles in the coating can simulate the papillary structure on the lotus leaf surface, construct a fine micro-nano surface secondary structure, and enhance the mechanical properties of the coating.

[0215] Comparison between Example 1 and Example 5 shows that the filler particles in the present invention can be selected from hydrophobically modified SiO2 particles or polytetrafluoroethylene particles, and the change in the type of nanoparticles has little effect on the mechanical properties of the coating.

[0216] Comparison between Example 1 and Example 6 shows that the selection of benzoin dimethyl ether or dimethyl acetone as the photoinitiator for the thiol-ene click reaction has little effect on the mechanical properties of the prepared coating.

[0217] Comparison between Example 1 and Examples 7-8 shows that the amphiphobic coating prepared in the present invention can be widely applied to various substrates without significant changes in mechanical properties.

[0218] Comparison between Example 1 and Examples 9-10 shows that the raw material composition of the amphiphobic coating of the present invention can be adjusted within the composition defined in the present invention, with little effect on the mechanical properties of the prepared coating.

[0219] Example 11

[0220] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence, and dried for later use.

[0221] 5g of hydroxypolydimethylsiloxane was dissolved in 34mL of dichloromethane, and 0.25g of pentaerythritol tetrakis(3-mercaptopropionic acid) was added and stirred for 30 minutes. Then, 0.5g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.005g of benzoin dimethyl ether were added to obtain a mixed solution. The mixture was stirred (500rpm) and reacted for 5 hours under a 365nm wavelength and 10W power ultraviolet lamp. To the mixture, 0.9g of hydrophobically modified silica filler particles (10μm and 20nm silica filler particles, mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 1g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was obtained. The obtained coating was brush-coated on the surface of the substrate and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0222] The water contact angle of the amphiphobic coating was tested to be 158.5°, and the n-hexadecane contact angle was 148.5°. Contact angle test photos are shown in Figures 9 and 10.

[0223] Example 12

[0224] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence, and dried for later use.

[0225] 5g of hydroxypolydimethylsiloxane was dissolved in 34mL of acetone, 0.25g of pentaerythritol tetrakis(3-mercaptopropionic acid) was added, and the mixture was stirred for 30 minutes. Then, 0.5g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.005g of benzoin dimethyl ether were added to obtain a mixed solution. The mixture was stirred (500rpm) and reacted for 5 hours under a 10W ultraviolet lamp with a wavelength of 365nm. To the mixture, 0.9g of hydrophobically modified silica filler particles (10μm and 20nm silica filler particles with a mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 1g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was obtained. The obtained coating was brush-coated on the surface of the substrate and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0226] The tested water contact angle of the amphiphobic coating was 158.36°, and the n-hexadecane contact angle was 147.2°.

[0227] Example 13

[0228] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence, and dried for later use.

[0229] 5g of hydroxy polydimethylsiloxane was dissolved in 34mL of dichloromethane, 0.25g of pentaerythritol tetrakis (3-mercaptopropionic acid) was added and stirred for 30min, and then 0.5g of 1H, 1H, 2H, 2H-perfluorodecyl acrylate and 0.005g of benzoin dimethyl ether were added to obtain a mixed solution. The mixed solution was stirred (500rpm) for 5h under irradiation with a UV lamp having a wavelength of 365nm and a power of 10w. 1g of polyhexamethylene diisocyanate was added to the mixed solution, and ultrasonic dispersion was continued for 10min. After degassing, a coating was obtained. The obtained coating was brush-coated on the surface of the substrate and cured at room temperature for 8h to obtain a double-repellent coating.

[0230] The tested water contact angle of the amphiphobic coating was 145.7°, and the n-hexadecane contact angle was 134.2°.

[0231] Example 14

[0232] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence, and dried for later use.

[0233] 5g of hydroxypolydimethylsiloxane was dissolved in 34mL of dichloromethane, 0.25g of pentaerythritol tetrakis(3-mercaptopropionic acid) was added, and the mixture was stirred for 30 minutes. Then, 0.5g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.005g of dimethylbenzene were added to obtain a mixed solution. The mixed solution was stirred (500rpm) and reacted for 5 hours under a 10W ultraviolet lamp with a wavelength of 365nm. To the mixed solution, 0.9g of hydrophobically modified silica filler particles (10μm and 20nm silica filler particles with a mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 1g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was obtained. The obtained coating was brush-coated on the surface of the substrate and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0234] The tested water contact angle of the amphiphobic coating was 157.9°, and the n-hexadecane contact angle was 146.6°.

[0235] Example 15

[0236] A stainless steel sheet of 2 cm*5 cm*0.3 cm was cleaned with acetone, ethanol and deionized water in sequence, and then dried for later use.

[0237] 5g of hydroxypolydimethylsiloxane was dissolved in 34mL of dichloromethane, and 0.25g of pentaerythritol tetrakis(3-mercaptopropionic acid) was added and stirred for 30 minutes. Then, 0.5g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.005g of benzoin dimethyl ether were added to obtain a mixed solution. The mixture was stirred (500rpm) and reacted for 5 hours under a 365nm wavelength and 10W power ultraviolet lamp. To the mixture, 0.9g of hydrophobically modified silica filler particles (10μm and 20nm silica filler particles, mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 1g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was obtained. The obtained coating was brush-coated on the surface of the substrate and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0238] The tested water contact angle of the amphiphobic coating was 157.2°, and the n-hexadecane contact angle was 148.1°.

[0239] Example 16

[0240] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence, and dried for later use.

[0241] 5g of hydroxypolydimethylsiloxane was dissolved in 34mL of dichloromethane, and 0.25g of pentaerythritol tetrakis(3-mercaptopropionic acid) was added and stirred for 30 minutes. Then, 0.5g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.005g of benzoin dimethyl ether were added to obtain a mixed solution. The mixed solution was stirred (500rpm) and reacted for 5 hours under a 365nm wavelength and 10W power ultraviolet lamp. To the mixed solution, 0.9g of polytetrafluoroethylene (10μm and 20nm silica filler particles were in a mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 1g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was obtained. The obtained coating was brush-coated on the surface of the substrate and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0242] The tested water contact angle of the amphiphobic coating was 156.9°, and the n-hexadecane contact angle was 147.3°.

[0243] Example 17

[0244] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence, and dried for later use.

[0245] 4.5g of hydroxypolydimethylsiloxane was dissolved in 34mL of dichloromethane, and 0.25g of pentaerythritol tetrakis(3-mercaptopropionate) was added and stirred for 30 minutes. Then, 0.25g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.025g of benzoin dimethyl ether were added to form a mixture. The mixture was stirred (500rpm) under irradiation with a 10W UV lamp at a wavelength of 365nm for 5 hours. To the mixture, 0.9g of hydrophobically modified silica filler particles (10μm to 20nm silica filler particles in a mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 0.75g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was applied to the substrate surface and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0246] The tested water contact angle of the amphiphobic coating was 156.32°, and the n-hexadecane contact angle was 146.9°.

[0247] Example 18

[0248] A glass piece of 2 cm*5 cm*0.3 cm in size was washed with acetone, ethanol and deionized water in sequence and dried for later use.

[0249] 6.25g of hydroxypolydimethylsiloxane was dissolved in 34mL of dichloromethane, and 0.25g of pentaerythritol tetrakis(3-mercaptopropionate) was added and stirred for 30 minutes. Then, 0.625g of 1H,1H,2H,2H-perfluorodecyl acrylate and 0.0315g of benzoin dimethyl ether were added to form a mixture. The mixture was stirred (500rpm) under irradiation with a 10W UV lamp at a wavelength of 365nm for 5 hours. To the mixture, 0.9g of hydrophobically modified silica filler particles (10μm to 20nm silica filler particles in a mass ratio of 1:2) was added. After ultrasonic dispersion for 30 minutes, 1.5g of polyhexamethylene diisocyanate was added and ultrasonic dispersion was continued for 10 minutes. After degassing, the coating was applied to the substrate surface by brush and cured at room temperature for 8 hours to obtain an amphiphobic coating.

[0250] The tested water contact angle of the amphiphobic coating was 155.1°, and the n-hexadecane contact angle was 146.7°.

[0251] Application Example 2

[0252] The contact angle of the polishing liquid of the present invention on the surface of the coating prepared in Example 11 was tested, and the test results are shown in Figure 11. The contact angle of the coating polishing liquid was measured to be 152.61°. After the coating prepared by the present invention is applied to the surface of the polishing equipment, it can avoid the polishing liquid residue on the surface of the polishing equipment, so that the surface of the polishing equipment is kept clean. The polishing liquid used in the test was produced by Dalian Zhengyun Technology Co., Ltd. The ingredients of the polishing liquid are: water, 20nm silica filler, potassium permanganate, polyethylene glycol, N-(p-aminoethyl)-r-aminopropyltrimethoxysilane, ethylenediamine, and triethanolamine.

[0253] Application Example 3

[0254] In the coating surface prepared in Example 11, microcracks were artificially created with sandpaper, a knife, or other hard materials to obtain a micro-damaged surface, and then the damaged surface was irradiated with 365nm ultraviolet light. After 30 minutes, the damaged microcracks healed themselves. After the self-healing test, the water contact angle at this position was 157.1°, and the contact angle of n-hexadecane was 148.3°. The coating prepared by the method provided by the present invention has certain self-healing properties, which is attributed to the SC bonds contained in the coating. After the thiol-ene click reaction is induced by ultraviolet irradiation, the SC bonds at the damaged position are rebonded to obtain a silicone elastomer with a dynamic cross-linking network, so that the micro-damage of the coating can be repaired.

[0255] The present invention uses an infrared tester (Bruker Alpha II) to perform infrared testing on the coating, raw materials and intermediate reaction products prepared in Example 11. The test results are shown in Figure 12.

[0256] PDMS-OH represents the infrared spectrum of the coating after curing with hydroxy polydimethylsiloxane.

[0257] 2955cm -1 The infrared absorption peak at 1260 cm is attributed to the asymmetric stretching vibration of CH3. -1 The infrared absorption peak at 1070 cm is attributed to the symmetrical bending vibration of the -CH3 group, while the -1 The strong absorption at 905cm is caused by the asymmetric stretching vibration of the -Si-O-Si- bond in hydroxy polydimethylsiloxane. -1 The weak infrared absorption at 789 cm is attributed to the stretching vibration of Si-OH. -1 The strong absorption is attributed to the stretching vibration of the Si-C bond.

[0258] PDMS-OH / PETMP represents the IR spectrum of the cured coating obtained by adding pentaerythritol tetrakis(3-mercaptopropionate) (PETMP) to hydroxy polydimethylsiloxane.

[0259] Pentaerythritol tetrakis(3-mercaptopropionic acid) (PETMP) was added to PDMS-OH resin. The infrared spectrum of the cured coating is: 2955 cm -1 There is still asymmetric stretching vibration characteristic absorption of CH3, which is found at 2580cm -1 There is an obvious S-H characteristic absorption at 1730cm -1 There is a characteristic absorption of C=O at 1147cm -1 The characteristic absorption of the C-O bond at the positions indicated that pentaerythritol tetrakis(3-mercaptopropionate) was successfully grafted onto hydroxypolydimethylsiloxane, and the remaining -SH groups could undergo a mercapto-double bond click reaction with fluorinated acrylates.

[0260] PDMS / PETMP / FMA represents the amphiphobic coating prepared in Example 11

[0261] Infrared spectrum of the coating after adding pentaerythritol tetrakis(3-mercaptopropionate) (PETMP) and fluorinated acrylate (FMA) to PDMS-OH resin and curing: at 2580 cm -1 The obvious S-H characteristic absorption disappears at 1202 cm -1 There is an obvious C-F characteristic absorption peak at 1620-1680cm -1 There is no C=C characteristic absorption, indicating that perfluorodecyl acrylate is grafted onto the silicone resin polymer chain in the form of chemical bonding. -1 There are characteristic absorptions of C=O and 1147cm -1The characteristic absorption of the C-O bond at the position is attributed to the ester stretching vibration of perfluorodecyl acrylate, which proves that the fluorinated acrylate has been successfully grafted into the thiol-modified silicone resin segment.

[0262] The present invention uses an atomic force microscope (Park NX20) to test the roughness of the amphiphobic coating prepared in Example 11. The test results are shown in Figure 13, and the roughness calculation results are shown in Table 4.

[0263] Table 4 Roughness results of the coating in Example 11

[0264] It can be seen from Table 1 that the line roughness of the coating prepared in Example 11 is Ra=5.437±1.61 μm.

[0265] The surface roughness of the prepared coating is 5.437 μm ( FIG13 ), and the micronized particles are distributed in an island-like manner, and the nanoparticles are aggregated on the surface of the micronized particles (further demonstrated in FIG14 ). At this time, the contact model of the droplet on the coating surface is similar to the Cassie model, with high water and oil contact angles.

[0266] The present invention conducted mechanical property tests on the coatings prepared in Examples 11-18, and the test results are shown in Table 5.

[0267] (1) Wear resistance test:

[0268] A substrate coated with the polydimethylsiloxane amphiphobic coating prepared by the present invention is placed horizontally, and a piece of 320-grit sandpaper with an area of ​​approximately 1 / 3 of the polydimethylsiloxane amphiphobic coating is placed on its surface. A glass plate with an area equivalent to the sandpaper is placed on the adhesive backing of the sandpaper, and the sandpaper and the glass plate are adhered together by the adhesive backing to prevent relative sliding between the two. Finally, a weight is placed on the glass plate to ensure that the polydimethylsiloxane amphiphobic coating is in contact with the sandpaper surface. The sandpaper is moved at a speed of v = 0.5 mm / s, and the minimum weight corresponding to the scratch depth of the polydimethylsiloxane amphiphobic coating surface ≥ 1 μm is recorded to measure the wear resistance of the coating.

[0269] (2) Hardness test:

[0270] The hardness of the wear-resistant coating on the surface of the polydimethylsiloxane amphiphobic coating prepared by the present invention was tested by a pencil hardness method.

[0271] (3) Testing:

[0272] The adhesion between the polydimethylsiloxane amphiphobic coating prepared in this invention and the substrate was tested using the GB / T 9286-1998 standard. A 10x10 grid array was cut into the coating surface using a blade. 3M tape was applied to the cut grid surface. The tape surface was vigorously rubbed with an eraser to ensure adhesion. The tape was then grasped at one end and torn off at a 90-degree angle to test the coating's adhesion.

[0273] Table 5 Mechanical properties test results of the coatings in Examples 11-18

[0274] The present invention conducted a chemical resistance test on the coating prepared in Example 11, and the test results are shown in Table 6.

[0275] Table 6 Test results of chemical resistance of coating in Example 11

[0276] Three identical steel materials were used as substrates. The coating prepared in Example 11 of the present invention was applied to the entire surface of the substrates. The three substrates were then immersed in a 1M HCl solution for 48 h, a 1M NaOH solution for 48 h, and a 1M NaCl solution for 48 h to test the corrosion resistance of the coatings.

[0277] It was observed that there was no damage to the coating on the surface of the substrate, and the hydrophobicity and oleophobicity angles of the coating were measured, and the results are shown in Table 6. The results show that the coating prepared in Example 11 has good corrosion resistance.

[0278] It should be noted that the embodiments described above are intended to illustrate the present invention only and are not intended to limit the present invention in any way. While the present invention has been described with reference to exemplary embodiments, it should be understood that the terms used herein are intended to be descriptive and explanatory, rather than limiting. The present invention may be modified as specified within the scope of the claims and revised without departing from the scope and spirit of the present invention. Although the present invention is described herein with reference to specific methods, materials, and embodiments, it is not intended that the present invention be limited to the specific examples disclosed herein; rather, the present invention extends to all other methods and applications having the same functions. It should be noted that the embodiments described above are intended to illustrate the present invention only and are not intended to limit the present invention in any way. While the present invention has been described herein with reference to exemplary embodiments, it should be understood that the terms used herein are intended to be descriptive and explanatory, rather than limiting. The present invention may be modified as specified within the scope of the claims and revised without departing from the scope and spirit of the present invention. Although the present invention is described herein with reference to specific methods, materials, and embodiments, it is not intended that the present invention be limited to the specific examples disclosed herein; rather, the present invention extends to all other methods and applications having the same functions.

Claims

1. A polydimethylsiloxane amphiphobic coating, characterized in that: The raw materials of the polydimethylsiloxane amphiphobic coating include: hydroxy polydimethylsiloxane, mercapto compound, fluorine-containing acrylate, curing agent and initiator.

2. The polydimethylsiloxane amphiphobic coating according to claim 1, characterized in that: The mass ratio of hydroxy polydimethylsiloxane, mercapto compound and curing agent is 1-3:1:0.1-0.4; The mass ratio of the mercapto compound, the fluorinated acrylate and the initiator is 1:0.6-3:0.01-0.

3.

3. The polydimethylsiloxane amphiphobic coating according to claim 2, characterized in that: The raw materials for preparing the polydimethylsiloxane amphiphobic coating also include filler particles, and the mass ratio of the hydroxy polydimethylsiloxane to the filler particles is 1:0.5-2.

5.

4. The polydimethylsiloxane amphiphobic coating according to claim 3, characterized in that: The filler particles include micron-sized particles and nano-sized particles; The particle size of the micron-sized particles is 2 to 10 μm, and the particle size of the nano-sized particles is 10 to 30 nm; The micron-sized particles and the nano-sized particles are independently selected from one or more of hydrophobically modified SiO2, TiO2, Al2O3, polytetrafluoroethylene, graphite fluoride, and hollow micro glass spheres.

5. The polydimethylsiloxane amphiphobic coating according to claim 4, characterized in that: The water contact angle of the polydimethylsiloxane amphiphobic coating is 132° to 154°, and the oil contact angle of the polydimethylsiloxane amphiphobic coating is 114° to 129°.

6. The polydimethylsiloxane amphiphobic coating according to claim 1, characterized in that: Taking the mass of the hydroxy polydimethylsiloxane as 100%, the mass of the mercapto compound is 1% to 10%, the mass of the fluorine-containing acrylate is 2% to 20%, the mass of the initiator is 0.01% to 1%, and the mass of the curing agent is 10% to 30%.

7. The polydimethylsiloxane amphiphobic coating according to claim 1 or 6, characterized in that: The raw materials for preparing the polydimethylsiloxane amphiphobic coating also include filler particles, and the mass ratio of the hydroxy polydimethylsiloxane to the filler particles is 1:0.1-1.

8. The polydimethylsiloxane amphiphobic coating according to claim 7, characterized in that: The filler particles include micron-sized particles and nano-sized particles; Preferably, the particle size of the micron-sized particles is 5 to 15 μm, and the particle size of the nano-sized particles is 10 to 30 nm; the mass ratio of the micron-sized particles to the nano-sized particles is 1:(1 to 5); Preferably, the micron-sized particles and the nano-sized particles are independently selected from one or more of hydrophobically modified SiO2, TiO2, Al2O3, polytetrafluoroethylene, graphite fluoride, and hollow micro glass spheres.

9. The polydimethylsiloxane amphiphobic coating according to claim 8, characterized in that: The water contact angle of the polydimethylsiloxane amphiphobic coating is 145° to 159°, and the oil contact angle of the polydimethylsiloxane amphiphobic coating is 134° to 149°; and / or, the wear resistance is 122g to 200g; and / or, the hardness of the coating is 4H; and / or, the adhesion of the coating is 4B.

10. A method for preparing the polydimethylsiloxane amphiphobic coating according to any one of claims 1 to 5, characterized in that: The steps include: (1) preparing a mixed solution I with hydroxy polydimethylsiloxane, a mercapto compound, a curing agent and a solvent I, applying the mixed solution I on a surface of a substrate, and curing; (2) preparing a mixed solution II with a fluorinated acrylate, an initiator and a solvent II, immersing the substrate cured by the mixed solution I in step (1) in the mixed solution II, irradiating the substrate with light, and aging the substrate to obtain a polydimethylsiloxane amphiphobic coating.

11. The preparation method according to claim 10, characterized in that: The raw materials used in the preparation process of the polydimethylsiloxane amphiphobic coating also include filler particles. In step (1), hydroxy polydimethylsiloxane, mercapto compound, filler particles, curing agent and solvent I are prepared into a mixed solution I; The mass of the filler particles is 5% to 20% of the mass of the mixed solution I.

12. The preparation method according to claim 11, characterized in that: The mass of the hydroxy polydimethylsiloxane is 10% to 20% of the mass of the solvent I; The mass of the fluorinated acrylate is 20% to 30% of the mass of the mixed solution II; The mass of the initiator is 0.1% to 3% of the mass of the mixed solution II.

13. The method for preparing the polydimethylsiloxane amphiphobic coating according to claim 12, characterized in that: In step (1), the mixed solution I is stirred and degassed before being coated on the surface of the substrate; And / or, the curing conditions in step (1) include: a time of 8 to 12 hours; And / or, the conditions of illumination in step (2) include: using ultraviolet irradiation, the wavelength of the ultraviolet irradiation is 300 to 380 nm, the power is 8 to 12 W, and the ultraviolet irradiation time is 2 to 8 hours; And / or, the aging conditions in step (2) include: temperature of 40 to 60° C. and time of 1 to 5 hours.

14. A method for preparing the polydimethylsiloxane amphiphobic coating according to any one of claims 6 to 9, characterized in that: The steps include: Hydroxypolydimethylsiloxane, mercapto compounds, fluorine-containing acrylates, initiators and solvents are mixed to obtain a mixed solution. After the mixed solution is exposed to light, a curing agent is added to obtain a coating. The coating is coated on the surface of a substrate and cured to obtain a polydimethylsiloxane amphiphobic coating.

15. The preparation method according to claim 14, characterized in that: The raw materials used in the preparation process of the polydimethylsiloxane amphiphobic coating also include filler particles, and the preparation method further includes: adding filler particles to the mixed solution after the mixed solution is irradiated with light and before adding the curing agent; Preferably, the mass of the filler particles is 1% to 3% of the mass of the mixed liquid.

16. The preparation method according to claim 14 or 15, characterized in that: The mass of the hydroxy polydimethylsiloxane is 9% to 20% of the mass of the solvent; And / or, the mass of the thiol compound is 0.4% to 1% of the mass of the solvent; And / or, the mass of the fluorine-containing acrylate is 0.5% to 2% of the mass of the solvent.

17. The preparation method according to any one of claims 14 to 16, characterized in that: The preparation method further comprises: after adding a curing agent, performing ultrasound and degassing to obtain a coating, and coating the coating on the surface of a substrate; And / or, the conditions of illumination include: using ultraviolet irradiation, the wavelength of the ultraviolet irradiation is 300-380nm, the power is 5-20w, and the ultraviolet irradiation time is 2-8h; And / or, the curing conditions include: room temperature, time of 8 to 12 hours.

18. The preparation method according to any one of claims 10 to 17, characterized in that: The thiol compound includes at least one or more of tetrakis(3-mercaptopropionic acid) pentaerythritol ester, dipentaerythritol hexa(3-mercaptopropionate), trimethylolpropane tris(3-mercaptopropionate), four-arm polyethylene glycol thiol, 3-mercapto-1-propanol, 1,4-butanediol di(thioglycolate), di(2-mercaptoethyl) adipate, diisopropyl 2,3-dimercaptosuccinate, 1,4-butanedithiol and di(thioglycolate)ethylene glycol ester; The curing agent includes at least one or more of isocyanate, acetic acid, diaminobutane, butanone oxime and methyl ethyl ketone oxime; The fluorine-containing acrylate includes at least one or more of 1H, 1H, 2H, 2H-perfluorodecyl acrylate, 1H, 1H, 2H, 2H-perfluorooctyl methacrylate, 2-(perfluorohexyl) ethyl methacrylate, 2-(perfluorooctyl) ethyl methacrylate, perfluoroalkylethyl methacrylate, tridecafluorooctyl acrylate, perfluoroundecyl acrylate and 2-(perfluorobutyl) ethyl methacrylate; The initiator includes at least one or more of benzoin dimethyl ether, dimethylbenzene ketone and photoinitiator 184; The substrate is selected from one of glass, steel, wood, paper, marble and cotton cloth; The solvent is selected from one or more of dichloromethane, chloroform, N,N-dimethylformamide, tetrahydrofuran, acetone and n-hexane.

19. Use of the polydimethylsiloxane amphiphobic coating according to any one of claims 1 to 9 or the polydimethylsiloxane amphiphobic coating prepared by the preparation method according to any one of claims 10 to 18 in cleaning polishing equipment during chemical mechanical planarization.

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