Preparation method of anticorrosive electrostatic chuck coating

Abstract

The invention relates to the technical field of anti-corrosion coatings in a semiconductor manufacturing process, in particular to an anti-corrosion electrostatic chuck coating and a preparation method thereof.The preparation method includes the steps that a substrate is subjected to ultrasonic cleaning to remove greasy dirt and impurities and blow-dried with nitrogen, then plasma treatment is conducted, and a pretreated substrate is obtained; after bisphenol A type epoxy resin is heated and softened, nano zinc powder and graphene oxide are sequentially added and stirred to prepare slurry, the slurry is spin-coated on a substrate and cured, two metacrylic acid esters in a specific proportion are prepared into a copolymer, the copolymer is mixed with graphene and tin antimony oxide which are subjected to ultrasonic dispersion and stirred to obtain conductive slurry, and the conductive slurry is subjected to thermocuring after spraying to obtain the high-temperature-resistant coating. The preparation method comprises the following steps: ultrasonically dispersing nano aluminum oxide in ethyl acetate, adding perfluoroalkoxy side chain fluorinated polyurethane to prepare a suspension, dip-coating a substrate, and curing by ultraviolet irradiation to finally obtain the coating. The prepared coating has the advantages of improving the corrosion resistance, enhancing the anti-static function, prolonging the wear-resistant life, optimizing the process performance, achieving synergistic protection and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of anti-corrosion coatings in semiconductor manufacturing processes, and in particular to an anti-corrosion electrostatic chuck coating and a preparation method thereof. Background Art

[0002] As a core component of the metal etching process, the performance of the electrostatic chuck directly affects the yield and stability of wafer processing. However, traditional electrostatic chucks are susceptible to ion bombardment and erosion by corrosive process gases in a plasma environment, resulting in coating damage and shortened lifespan. To meet this challenge, the industry urgently needs to develop new coating technologies that are resistant to plasma erosion, structurally stable, and have long-term corrosion resistance. In recent years, multi-layer coating designs based on ceramics or group IIIB metal compounds have gradually become a research hotspot. By optimizing the integrated protective structure of the thin film electrode and the base plate, the corrosion resistance and service life of the electrostatic chuck have been significantly improved. At the same time, the rapid development of anti-corrosion treatment technologies such as electrostatic spraying has provided new ideas for material selection and process innovation of electrostatic chuck coatings, further promoting technological progress in this field towards high efficiency and durability.

[0003] Traditional electrostatic chucks are primarily made of alumina ceramic, with a dielectric layer formed through plasma spraying technology. High-purity, nanoscale powders are used to enhance density and insulation. For high-performance applications, aluminum nitride or silicon carbide coatings are used due to their high thermal conductivity and well-matched thermal expansion coefficients, ensuring stability in extreme environments.

[0004] However, organic coatings such as silicone and epoxy resin are prone to chemical degradation in humid or corrosive environments. Although inorganic ceramic coatings have good corrosion resistance, they may still fail due to electrochemical corrosion after long-term exposure to plasma or strong acid and alkali environments. The coating and the graphite / metal substrate have large differences in thermal expansion coefficients, which can easily cause peeling under extreme temperature changes. Traditional adhesive layers have poor resistance to plasma erosion, exacerbating the risk of interface failure. They rely on high-temperature sintering or electroplating processes, which have high energy consumption and are prone to environmental pollution. At the same time, the preparation process of multi-layer structures is complex and the cost remains high, making it difficult to meet sustained and stable quality requirements. Summary of the Invention

[0005] In order to solve the problems mentioned in the above background technology, the present invention provides an anti-corrosion electrostatic chuck coating and a preparation method thereof.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] S1. Place the substrate in an ultrasonic cleaning machine to remove oil and impurities, blow dry with nitrogen, and place it in a plasma cleaning machine for 5-10 minutes to obtain a pretreated substrate;

[0008] S2. Under nitrogen protection, bisphenol A epoxy resin is placed in a stirring kettle, nano zinc powder is added, and mechanical stirring is carried out for 30-40 minutes. Graphene oxide is slowly added and stirring is continued for 45-60 minutes to obtain an anti-corrosion base slurry, which is evenly coated by a spin coater and then cured by variable temperature;

[0009] S3. Trifluoroethyl methacrylate and hexafluorobutyl methacrylate are mixed and polymerized in a mass ratio of (4-6):(4-6), graphene and antimony tin oxide are added to N,N-dimethylacetamide, ultrasonically dispersed for 50-60 minutes, copolymer is added, mechanically stirred for 1.5-2 hours to obtain a conductive slurry, and then thermally cured after spraying;

[0010] S4. Disperse nano-alumina in ethyl acetate, sonicate for 50-60 minutes, add perfluoroalkoxy side-chain fluorinated polyurethane, mechanically stir for 25-30 minutes, immerse the substrate vertically in the coating tank, stay for 10-15 seconds, then remove it at a uniform speed, and cure it by ultraviolet radiation to finally obtain a complete suction cup coating.

[0011] Furthermore, the ultrasonic cleaning in step S1 is divided into two stages:

[0012] Stage 1: Immerse the substrate in a pure acetone-isopropyl alcohol solution for 10-15 minutes to remove oil stains;

[0013] Stage 2: Transfer the substrate to an isopropyl alcohol solution and wash for 10-15 minutes to remove residual organic matter;

[0014] After cleaning, place it in a vacuum drying oven, evacuate at -0.1MPa, and keep it at 70-80℃ for 20-25min to remove surface moisture. The plasma cleaning machine power is 100W, the oxygen flow rate is 20-25sccm, and the treatment is 5-8min to improve the surface energy. After treatment, immediately transfer it to a clean environment.

[0015] Furthermore, in step S2, the mass ratio of the anti-corrosion bottom layer bisphenol A epoxy resin, nano zinc powder and graphene oxide is 8:1:1, the stirring speed is 300-400 rpm, the graphene oxide is ultrasonically dispersed in ethanol before addition, the spin coating speed is 2000-2500 rpm, and the acceleration is 400-450 rad / s 2 , time is 30-40 seconds.

[0016] Furthermore, the copolymer in step S3 is prepared by the following steps:

[0017] Trifluoroethyl methacrylate and hexafluorobutyl methacrylate were mixed in a mass ratio of (4-6): (4-6), tetrahydrofuran as an initiator was added, and nitrogen was introduced for 30-35 minutes to remove oxygen. The temperature was raised to 70-80°C, and azobisisobutyronitrile as an initiator was slowly added dropwise with continuous stirring. After the reaction lasted for 3-4 hours, azobisisobutyronitrile was further added, and the reaction was continued for 1.5-2 hours. Finally, the mixture was cooled to room temperature, and a methanol-water solution was poured into the mixture to precipitate the polymer. The precipitate was filtered and vacuum dried to obtain a trifluoroethyl methacrylate-hexafluorobutyl methacrylate copolymer.

[0018] Furthermore, the variable temperature curing in step S2 is divided into three stages:

[0019] The first stage: keep warm at 60℃ for 25-30min;

[0020] The second stage: heat to 120℃ and maintain for 45-60min;

[0021] The third stage: Cool naturally to room temperature.

[0022] Furthermore, in step S3, the mass of the azobisisobutyronitrile initiator is 0.5% of the total mass of the monomers. The azobisisobutyronitrile initiator is dissolved in tetrahydrofuran solvent before being added, the methanol-water solution ratio is 1:1, the drying temperature is 60-70°C, and the drying time is 10-12 hours.

[0023] Furthermore, in step S3, the mass ratio of the copolymer, graphene and antimony tin oxide in the conductive slurry is 9:0.5:0.5, the dispersion power is 400W, the stirring speed is 500-600rpm for mechanical stirring, the spray gun pressure is 0.2-0.3MPa, the spray distance is 10-15cm, the wet film thickness covering the substrate surface is 10-15μm, and the thermal curing process is first kept at 70-80℃ for 25-30min to promote solvent volatilization, then heated to 240-250℃ and maintained for 50-60min to promote conductive network formation, and finally naturally cooled to room temperature to complete curing.

[0024] Furthermore, in step S4, the mass ratio of perfluoroalkoxy side chain fluorinated polyurethane to nano-alumina is 9:1, the nano-alumina particle size is 50 nm, the stirring speed is 250-300 rpm, the uniform extraction speed is 3-5 mm / s, the ultraviolet light irradiation wavelength is 365 nm, the intensity is 10 mW / cm², and after curing is completed, the residual solvent is removed by vacuum drying at 70-80°C for 25-30 minutes.

[0025] According to another aspect of the present invention, there is provided an anti-corrosion electrostatic chuck coating prepared by the above preparation method.

[0026] Beneficial effects of the present invention:

[0027] 1. In the technical solution of the present invention, after curing, the epoxy resin forms a three-dimensional network structure, which is filled with nano-zinc powder and graphene oxide to block the penetration path of the corrosive medium. The two-dimensional sheet structure of graphene can effectively extend the diffusion path of the corrosive medium. Through the sacrificial anode protection of the nano-zinc powder, it is preferentially oxidized in a corrosive environment and consumes electrons through the anodic reaction to protect the substrate from corrosion. The nano-zinc powder and graphene oxide are dispersed in the resin, increasing the diffusion resistance of the corrosive medium at the interface and delaying the initiation of local pitting corrosion.

[0028] 2. In the technical solution of the present invention, trifluoroethyl methacrylate and hexafluorobutyl methacrylate are randomly copolymerized to form a fluorinated polymer chain, forming a low surface energy layer. The rigid trifluoroethyl chain segment of trifluoroethyl methacrylate enhances the intermolecular cohesion through dipole action, and the few-layer graphene forms a continuous conductive network through π-π conjugation, providing a rapid migration channel for charges.

[0029] 3. In the technical solution of the present invention, a dense polyurethane-urethane network is formed by ultraviolet curing. The hard segment provides rigidity and the soft segment imparts toughness. The hardness reaches 3H-5H. Alumina nanoparticles are evenly dispersed in the resin, bearing the load during friction and reducing the plastic deformation of the resin matrix. The low surface energy characteristics of the CF bond enable the nano-ceramic particles to be wrapped by the fluorinated layer. During friction, a fluorinated transfer film is formed on the dual surface, reducing the shear force. The crack propagation is limited to the submicron scale, significantly improving the wear resistance life. DETAILED DESCRIPTION

[0030] The following will clearly and completely describe the technical solutions of the present invention in conjunction with the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0031] Unless otherwise specified, the raw materials used in the present invention are all conventional products purchased from the market.

[0032] Preparation Example 1

[0033] A method for preparing an anti-corrosion electrostatic chuck coating comprises the following steps:

[0034] Prepare bisphenol A epoxy resin, nano zinc powder and graphene oxide in a ratio of 8:1:1. Place bisphenol A epoxy resin in a stirring kettle and heat to 60°C to soften it. Add nano zinc powder and mechanically stir for 30 minutes. Slowly add graphene oxide and continue stirring for 50 minutes to obtain an anti-corrosion base slurry. Take 2 mL of the slurry and drop it on the center of the substrate. Evenly apply it with a spin coater and then solidify it. The mixture of trifluoroethyl methacrylate and hexafluorobutyl methacrylate was mixed in a mass ratio of 5:5, heated to 70 ° C, and azobisisobutyronitrile initiator was slowly added dropwise with continuous stirring. The mass of the initiator was 0.5% of the total mass of the monomers and dissolved in tetrahydrofuran. After the reaction for 4 hours, an appropriate amount of azobisisobutyronitrile was added to the inside, the mass of which was about 1 / 2 of the initial amount. The reaction was continued for 2 hours, and finally cooled to room temperature. A methanol-water solution with a volume ratio of 1:1 was poured into the mixture. After the precipitate was filtered and vacuum dried at 65 ° C for 11 hours, trifluoroethyl methacrylate-hexafluorobutyl methacrylate copolymer was obtained. Graphene and antimony tin oxide were added to N,N- In dimethylacetamide, ultrasonic dispersion is carried out for 1 hour, the copolymer is added, and mechanical stirring is carried out for 2 hours to obtain a conductive slurry. Finally, it is sprayed on the surface of the substrate and thermally cured. First, 75℃ / 30min, then 245℃ / 55min, the nano-alumina is dispersed in ethyl acetate, ultrasonicated for 1 hour, and perfluoroalkoxy side chain fluorinated polyurethane is added. The mass ratio of perfluoroalkoxy side chain fluorinated polyurethane to alumina is 9:1. Mechanical stirring is carried out for 30 minutes to form a uniform suspension. The substrate is vertically immersed in a coating tank containing the suspension and stayed for 10 seconds. Then it is taken out at a uniform speed and finally cured under ultraviolet irradiation for 30 seconds to obtain an anti-corrosion electrostatic suction cup coating.

[0035] Preparation Example 2

[0036] A method for preparing an anti-corrosion electrostatic chuck coating comprises the following steps:

[0037] Bisphenol A epoxy resin, nano zinc powder and graphene oxide were prepared in a ratio of 8:1:1. Bisphenol A epoxy resin was placed in a stirring kettle and heated to 63°C to soften it. Nano zinc powder was added and mechanically stirred for 33 minutes. Graphene oxide was slowly added and stirred for 45 minutes to obtain an anti-corrosion base slurry. 3 mL of the slurry was dropped on the center of the substrate and evenly coated with a spin coater and then cured. Trifluoroethyl methacrylate and hexafluorobutyl methacrylate were mixed in a mass ratio of 5:5, heated to 73°C, and azobisisobutyronitrile initiator was slowly added dropwise with continuous stirring. The initiator mass was 0.5% of the total monomer mass and dissolved in tetrahydrofuran. After reacting for 4 hours, an appropriate amount of azobisisobutyronitrile was added to the inside, the mass of which was about 1 / 2 of the first added amount. The reaction was continued for 2.3 hours, cooled to room temperature, and a methanol-water solution with a volume ratio of 1:1 was poured into the mixture. After filtration of the precipitate, it was vacuum dried at 65°C for 11 hours to obtain trifluoroethyl methacrylate-hexafluorobutyl methacrylate copolymer. Graphene and antimony tin oxide were added to N,N-dimethylacetamide at a ratio of 9:1, ultrasonically dispersed for 1.3 hours, and the copolymer was added. Mechanical stirring was performed for 1.3 hours to obtain a conductive slurry. After spraying and covering, it was first thermally cured at 75°C / 30 minutes and then at 245°C / 55 minutes. Nano-alumina was dispersed in ethyl acetate and ultrasonicated for 1.3 hours. Perfluoroalkoxy side chain fluorinated polyurethane was added. The mass ratio of perfluoroalkoxy side chain fluorinated polyurethane to alumina was 9:1. Mechanical stirring was performed for 23 minutes to form a uniform suspension. The substrate was vertically immersed in a coating tank containing the suspension and stayed for 13 seconds before being withdrawn at a uniform speed. Finally, it was cured by ultraviolet irradiation for 35 seconds to obtain a complete anti-corrosion electrostatic chuck coating.

[0038] Preparation Example 3

[0039] A method for preparing an anti-corrosion electrostatic chuck coating comprises the following steps:

[0040] Bisphenol A epoxy resin, nano zinc powder and graphene oxide were prepared in a ratio of 8:1:1. Bisphenol A epoxy resin was placed in a stirring kettle and heated to 65 °C to soften it. Nano zinc powder was added and mechanically stirred for 35 minutes. Graphene oxide was slowly added and stirred for 45 minutes to obtain an anti-corrosion bottom layer slurry. 3 mL of the slurry was dropped on the center of the substrate and evenly coated and cured by a spin coater. Trifluoroethyl methacrylate and hexafluorobutyl methacrylate were mixed in a mass ratio of 5:5 and heated to 75 °C. Azobisisobutyronitrile initiator was slowly added dropwise and stirred continuously (the mass of the initiator was 0.5% of the total mass of the monomers and was dissolved in tetrahydrofuran). After reacting for 4 hours, an appropriate amount of azobisisobutyronitrile (the mass was about 1 / 2 of the first amount added) was added to the inside and the reaction was continued for 2.5 hours. The mixture was cooled to room temperature and poured into a methanol-water solution (volume ratio 1:1). The precipitate was filtered and vacuum dried (65 ℃, 11h) to obtain trifluoroethyl methacrylate-hexafluorobutyl methacrylate copolymer. Graphene and antimony tin oxide were added to N,N-dimethylacetamide in a ratio of 9:1 and ultrasonically dispersed for 1.5h. The copolymer was added and mechanically stirred for 1.5h to obtain a conductive slurry. After spray coating, the slurry was thermally cured (first at 75℃ / 30min, then at 245℃ / 55min). Nano-alumina was dispersed in ethyl acetate and ultrasonically treated for 1.5h. Perfluoroalkoxy side-chain fluorinated polyurethane was added in a mass ratio of perfluoroalkoxy side-chain fluorinated polyurethane to alumina of 9:1. The slurry was mechanically stirred for 25min to form a uniform suspension. The substrate was vertically immersed in a coating tank containing the suspension for 15s and then withdrawn at a constant speed (4mm / s). Finally, the substrate was irradiated with ultraviolet light (365nm, 10mW / cm²) for 35s to form a wear-resistant layer, thereby obtaining an anti-corrosion electrostatic chuck coating.

[0041] Example 1 A method for preparing an anti-corrosion electrostatic chuck coating comprises the following steps:

[0042] S1. Place the silicon wafer substrate in an ultrasonic cleaning machine to remove oil and impurities, blow dry with nitrogen, and then place the substrate in a plasma cleaning machine for plasma treatment for 5 minutes to obtain a pretreated substrate;

[0043] S2. Under nitrogen protection, bisphenol A epoxy resin was placed in a stirring kettle and heated to 55°C to soften it. Nano-zinc powder was added and mechanically stirred for 30 minutes. Graphene oxide was slowly added and stirred for 45 minutes to obtain an anti-corrosion base slurry. 2 mL of the slurry was dropped on the center of the substrate and evenly coated using a spin coater. Finally, an anti-corrosion layer was formed by variable temperature curing (60°C / 30 minutes, 120°C / 50 minutes).

[0044] S3. Trifluoroethyl methacrylate and hexafluorobutyl methacrylate were mixed in a mass ratio of 5:5 to obtain a copolymer according to the method described in Preparation Example 1. Graphene and antimony tin oxide were added to N,N-dimethylacetamide in a mass ratio of 9:1, and ultrasonically dispersed for 50 minutes. The copolymer was added and mechanically stirred for 1.5 hours to obtain a conductive slurry. After spraying, the slurry was thermally cured to form a conductive layer (75°C / 30 minutes, 245°C / 55 minutes).

[0045] S4. Disperse nano-alumina in ethyl acetate, ultrasonicate for 50 minutes, add perfluoroalkoxy side chain fluorinated polyurethane, the mass ratio of perfluoroalkoxy side chain fluorinated polyurethane to alumina is 9:1, and mechanically stir for 25 minutes to form a uniform suspension (wear-resistant top coating). Vertically immerse the substrate in a coating tank containing the suspension and stay for 10 seconds, then withdraw it at a uniform speed (4mm / s). Finally, irradiate with ultraviolet light (365nm, 10mW / cm²) for 25 seconds to solidify it to form a wear-resistant layer, and finally obtain an anti-corrosion electrostatic chuck coating.

[0046] Example 2 A method for preparing an anti-corrosion electrostatic chuck coating comprises the following steps:

[0047] S1. Place the stainless steel substrate in an ultrasonic cleaning machine to remove oil and impurities, blow dry with nitrogen, and then place the substrate in a plasma cleaning machine for plasma treatment for 10 minutes to obtain a pretreated substrate;

[0048] S2. Under nitrogen protection, bisphenol A epoxy resin was placed in a stirring vessel and heated to 60°C to soften it. Nano-zinc powder was added and mechanically stirred for 40 minutes. Graphene oxide was slowly added and stirred for 60 minutes to obtain an anti-corrosion base slurry. 3 mL of the slurry was dropped on the center of the substrate and evenly coated using a spin coater. Finally, an anti-corrosion layer was formed by variable temperature curing (60°C / 25 minutes, 120°C / 60 minutes).

[0049] S3. Trifluoroethyl methacrylate and hexafluorobutyl methacrylate were mixed in a mass ratio of 5:5 to obtain a copolymer according to the method described in Preparation Example 1. Graphene and antimony tin oxide were added to N,N-dimethylacetamide in a mass ratio of 9:1, and ultrasonically dispersed for 60 minutes. The copolymer was added and mechanically stirred for 2 hours to obtain a conductive slurry. After spraying, the mixture was thermally cured to form a conductive layer (80°C / 25 minutes, 250°C / 50 minutes).

[0050] S4. Disperse nano-alumina in ethyl acetate, ultrasonicate for 60 minutes, add perfluoroalkoxy side chain fluorinated polyurethane, the mass ratio of perfluoroalkoxy side chain fluorinated polyurethane to alumina is 9:1, mechanically stir for 30 minutes to form a uniform suspension, immerse the substrate vertically in a coating tank containing the suspension, stay for 15 seconds, and then withdraw it at a uniform speed (3mm / s), and finally irradiate with ultraviolet light (365nm, 10mW / cm²) for 30 seconds to form a wear-resistant layer, and finally obtain an anti-corrosion electrostatic chuck coating.

[0051] Comparative Example 1

[0052] The difference between this comparative example and Example 1 is that the anti-corrosion layer (step S2) is eliminated, and the conductive layer (step S3) and the wear-resistant layer (step S4) are directly coated. The remaining steps are the same as those in Example 1.

[0053] Comparative Example 2

[0054] The difference between this comparative example and Example 1 is that the conductive layer (step S3) uses ordinary phenolic resin and carbon black (mass ratio 9:1) instead of the copolymer, graphene and antimony tin oxide mixture, and the remaining steps are the same as Example 1.

[0055] Comparative Example 3

[0056] The difference between this comparative example and Example 2 is that the wear-resistant layer (step S4) is replaced by pure perfluoroalkoxy side-chain fluorinated polyurethane without nanoparticles (without adding nano-aluminum oxide), and the remaining steps are the same as Example 2.

[0057] The anti-corrosion electrostatic chuck coatings prepared in Examples 1-2 and Comparative Examples 1-3 were divided into five groups and tested separately. Each group of samples had 10 test points. The first group was tested for neutral salt spray corrosion life on the surfaces of the coatings prepared in Examples 1-2 and Comparative Examples 1-3 with reference to the standard GB / T 10125-2021. The second group was tested for surface conductivity on the surfaces of the coatings prepared in Examples 1-2 and Comparative Examples 1-3 with reference to the standard GB / T 1410-2006. The test values ​​of the first and second groups were averaged. The results are shown in Table 1:

[0058] Table 1. Corrosion life and surface resistivity test results of Preparation Examples 1-3, Examples 1-2 and Comparative Examples 1-3

[0059] sample Salt spray life (h) Surface resistivity (Ω / sq) Preparation Example 1 1200±10 <![CDATA[10 6 ]]> Preparation Example 2 1100±10 <![CDATA[10 5 ]]> Preparation Example 3 1000±10 <![CDATA[10 7 ]]> Example 1 1300±10 <![CDATA[10 5 ]]> Example 2 1500±10 <![CDATA[10 6 ]]> Comparative Example 1 <200±10 <![CDATA[10 8 ]]> Comparative Example 2 1000±10 <![CDATA[10 10 ]]> Comparative Example 3 800±10 <![CDATA[10 7 ]]>

[0060] The third group tested the scratch resistance of the coatings prepared in Examples 1-2 and Comparative Examples 1-3 using the ASTM D3363 standard. The fourth group tested the wear resistance of the coatings prepared in Examples 1-2 and Comparative Examples 1-3 using the ASTM D4060 standard. The fifth group tested the flexibility of the coatings prepared in Examples 1-2 and Comparative Examples 1-3 using the ASTM D522 standard. The highest and lowest values ​​of the data from the third to fifth groups were excluded, and the average of the remaining 8 points was taken as the final result. The results are shown in Table 2:

[0061] Table 2. Hardness, abrasion resistance, and flexibility of Preparation Examples 1-3, Examples 1-2, and Comparative Examples 1-3

[0062] sample Pencil hardness (H) Taber abrasion times Flexibility (bending radius / mm) Preparation Example 1 3H <![CDATA[6×10 4 ]]> 5 (no cracks) Preparation Example 2 4H <![CDATA[8×10 4 ]]> 4.5 (slight cracks) Preparation Example 3 2H <![CDATA[5×10 4 ]]> 3 (no cracks) Example 1 3H <![CDATA[6×10 4 ]]> 5 (no damage to silicon wafer) Example 2 5H <![CDATA[7×10 4 ]]> 6 (stainless steel dent <0.1mm) Comparative Example 1 3H <![CDATA[6×10 4 ]]> 3.5 (no cracks) Comparative Example 2 1H <![CDATA[2×10 4 ]]> Fracture (>10mm) Comparative Example 3 1H <![CDATA[<5×10 3 ]]> Fracture (>10mm)

[0063] As shown in Table 1, the surface resistivity of Examples 1 and 2 is 10 5 Ω / sq, 10 6 Ω / sq, and salt spray lifespans of 1300±10h and 1500±10h, respectively. Comparative Examples 1-3 exhibit significantly higher surface resistivities and significantly lower salt spray lifespans than the examples. This demonstrates that the anti-corrosion electrostatic chuck coating prepared using the present invention exhibits both low surface resistivity and long salt spray lifespans, achieving a better balance between corrosion resistance and electrical conductivity. The anti-corrosion primer (absent in Comparative Example 1) and the specific conductive layer materials (common resin / carbon black used in Comparative Example 2) are crucial to performance.

[0064] As shown in Table 2, the surface hardness and wear resistance of Examples 1-2 demonstrate a high degree of protection and possess high protective strength. However, the surface hardness and wear resistance of Comparative Example 3 (without nanoparticles in the wear-resistant layer) are significantly lower than those of Example 2. This indicates that the addition of nano-alumina significantly improves the hardness and wear resistance of the coating. Comparative Example 2 exhibits the worst overall performance, including hardness, wear resistance, and flexibility.

[0065] Different comparative examples verify the key role of each functional layer (anti-corrosion layer, conductive layer, wear-resistant layer containing nanoparticles) in the overall performance of the present invention. The lack or replacement of any key component will lead to a significant decline in performance.

[0066] In summary, the trifluoroethyl methacrylate-hexafluorobutyl methacrylate copolymer prepared in the Preparation Example exhibits significant advantages in preparing anti-corrosion electrostatic chuck coatings. By adjusting the copolymer formulation and preparation process, it is possible to produce coatings that exhibit strong corrosion resistance, stable electrostatic adsorption, and abrasion resistance, adapting to various environments, meeting the coating performance requirements for specific application scenarios.

[0067] Throughout the specification, reference to terms such as "Preparation," "Example," or "Examples" indicates that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or preparation are included in at least one embodiment or preparation of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or preparation. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or preparations.

[0068] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A method for preparing an anti-corrosion electrostatic chuck coating, characterized in that: The following steps are involved: S1. Place the substrate in an ultrasonic cleaning machine to remove oil and impurities, blow dry with nitrogen, and place it in a plasma cleaning machine for 5-10 minutes to obtain a pretreated substrate; S2. Under nitrogen protection, bisphenol A epoxy resin is placed in a stirring kettle, nano zinc powder is added, and mechanical stirring is carried out for 30-40 minutes. Graphene oxide is slowly added and stirring is continued for 45-60 minutes to obtain an anti-corrosion base slurry, which is evenly coated by a spin coater and then cured by variable temperature; S3. Trifluoroethyl methacrylate and hexafluorobutyl methacrylate are mixed and polymerized in a mass ratio of (4-6):(4-6), graphene and antimony tin oxide are added to N,N-dimethylacetamide, ultrasonically dispersed for 50-60 minutes, copolymer is added, mechanically stirred for 1.5-2 hours to obtain a conductive slurry, and then thermally cured after spraying; S4. Disperse nano-alumina in ethyl acetate, sonicate for 50-60 minutes, add perfluoroalkoxy side-chain fluorinated polyurethane, mechanically stir for 25-30 minutes, immerse the substrate vertically in the coating tank, stay for 10-15 seconds, then remove it at a uniform speed, and cure it by ultraviolet radiation to finally obtain a complete suction cup coating.

2. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 1, characterized in that: The ultrasonic cleaning in step S1 is divided into two stages: Stage 1: Immerse the substrate in a pure acetone-isopropyl alcohol solution for 10-15 minutes to remove oil stains; Stage 2: Transfer the substrate to an isopropyl alcohol solution and wash for 10-15 minutes to remove residual organic matter; After cleaning, place it in a vacuum drying oven, evacuate at -0.1MPa, and keep it at 70-80℃ for 20-25min to remove surface moisture. The plasma cleaning machine power is 100W, the oxygen flow rate is 20-25sccm, and the treatment is 5-8min to improve the surface energy. After treatment, immediately transfer it to a clean environment.

3. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 1, wherein: In step S2, the mass ratio of the anti-corrosion bottom layer bisphenol A epoxy resin, nano zinc powder and graphene oxide is 8:1:1, the stirring speed is 300-400 rpm, the graphene oxide is ultrasonically dispersed in ethanol before addition, the spin coating speed is 2000-2500 rpm, and the acceleration is 400-450 rad / s 2 , time is 30-40 seconds.

4. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 1, wherein: In step S3, the copolymer is prepared by the following steps: Trifluoroethyl methacrylate and hexafluorobutyl methacrylate were mixed in a mass ratio of (4-6): (4-6), tetrahydrofuran as an initiator was added, and nitrogen was introduced for 30-35 minutes to remove oxygen. The temperature was raised to 70-80°C, and azobisisobutyronitrile as an initiator was slowly added dropwise with continuous stirring. After the reaction lasted for 3-4 hours, azobisisobutyronitrile was further added, and the reaction was continued for 1.5-2 hours. Finally, the mixture was cooled to room temperature, and a methanol-water solution was poured into the mixture to precipitate the polymer. The precipitate was filtered and vacuum dried to obtain a trifluoroethyl methacrylate-hexafluorobutyl methacrylate copolymer.

5. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 1, wherein: The variable temperature curing in step S2 is divided into three stages: The first stage: keep warm at 60℃ for 25-30min; The second stage: heat to 120℃ and maintain for 45-60min; The third stage: Cool naturally to room temperature.

6. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 4, wherein: In step S3, the mass of the azobisisobutyronitrile initiator is 0.5% of the total mass of the monomers. The azobisisobutyronitrile initiator is dissolved in tetrahydrofuran solvent before being added, the methanol-water solution ratio is 1:1, the drying temperature is 60-70° C., and the drying time is 10-12 hours.

7. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 1, wherein: In step S3, the mass ratio of copolymer, graphene and antimony tin oxide in the conductive slurry is 9:0.5:0.5, the dispersion power is 400W, the stirring speed is 500-600rpm for mechanical stirring, the spray gun pressure is 0.2-0.3MPa, the spray distance is 10-15cm, the wet film thickness covering the substrate surface is 10-15μm, and the thermal curing process is first kept at 70-80℃ for 25-30min to promote solvent volatilization, then heated to 240-250℃ and maintained for 50-60min to promote conductive network formation, and finally naturally cooled to room temperature to complete curing.

8. The method for preparing an anti-corrosion electrostatic chuck coating according to claim 1, wherein: In step S4, the mass ratio of perfluoroalkoxy side chain fluorinated polyurethane to nano-alumina is 9:1, the nano-alumina particle size is 50nm, the stirring speed is 250-300rpm, the uniform extraction speed is 3-5mm / s, the ultraviolet irradiation wavelength is 365nm, and the intensity is 10mW / cm 2 After curing, the residual solvent was removed by vacuum drying at 70-80°C for 25-30 minutes.

9. An anti-corrosion electrostatic chuck coating prepared by the preparation method according to any one of claims 1 to 8.