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CN-121406243-B - Anticorrosive paint composition and preparation method and application thereof

CN121406243BCN 121406243 BCN121406243 BCN 121406243BCN-121406243-B

Abstract

The invention relates to the technical field of anti-corrosion coating compositions, in particular to an anti-corrosion coating composition, a preparation method and application thereof. The coating composition comprises three layers which are sequentially arranged, wherein an anti-corrosion bottom layer is formed by dynamically crosslinking epoxy soybean oil, polyethylene glycol and silane borate modified microcrystalline cellulose and has a humidity triggering self-repairing function, a conductive middle layer is formed by physically compounding PEDOT (polyether-urethane-styrene) aqueous dispersion liquid, sodium magnesium lithium silicate and ionic liquid in an aqueous gel network and has strain self-adaptive conductivity, and a wear-resistant surface layer is formed by ultraviolet triggering mercaptan-alkene clicking crosslinking of an alkenyl fluorinated polyurethane prepolymer and polyfunctional mercaptan and can realize fixed-point light repairing. The composition has the advantages of long-acting corrosion resistance, stable conduction, high wear resistance and damage self-repairing capability through three-layer function cooperation, is particularly suitable for surface protection of semiconductor manufacturing process equipment parts such as electrostatic chucks, and meets the long-acting service requirement under extreme working conditions.

Inventors

  • WANG YONGDONG
  • HU CHAO
  • LIU JIACHENG
  • ZHOU MENG

Assignees

  • 合肥升滕半导体技术有限公司

Dates

Publication Date
20260508
Application Date
20251104

Claims (10)

  1. 1. An anticorrosive coating composition, characterized in that the coating composition comprises three layers of coatings which are sequentially arranged, wherein the three layers of coatings are respectively as follows: the anti-corrosion bottom layer is formed by dynamically crosslinking bottom layer slurry containing epoxidized soybean oil, polyethylene glycol and silane borate modified microcrystalline cellulose; the conductive intermediate layer is formed by physical gelation of intermediate layer slurry containing PEDOT, PSS aqueous dispersion, sodium magnesium lithium silicate and ionic liquid; The wear-resistant surface layer is formed by light-triggered click crosslinking of surface layer slurry containing an alkenyl fluoride polyurethane prepolymer and a polyfunctional thiol compound.
  2. 2. A method of preparing an anticorrosive coating composition according to claim 1, comprising the steps of: s1, dispersing silane borate modified microcrystalline cellulose in a mixture of epoxidized soybean oil and polyethylene glycol, adding a compatilizer to form a bottom sizing agent, coating the bottom sizing agent on a substrate, and carrying out dynamic crosslinking and curing in a wet environment to obtain an anti-corrosion bottom layer; s2, dispersing PEDOT (polyether-ether-ketone) PSS aqueous dispersion and ionic liquid in an aqueous gel network formed by sodium magnesium lithium silicate to form middle-layer slurry, coating the middle-layer slurry on the anti-corrosion bottom layer, and drying and gelling to form a conductive middle layer; s3, mixing the alkenyl fluoride polyurethane prepolymer with a polyfunctional mercaptan compound and a photoinitiator to form surface layer slurry, coating the surface layer slurry on the conductive intermediate layer, and carrying out mercaptan-alkene click crosslinking curing by ultraviolet irradiation to obtain the wear-resistant surface layer.
  3. 3. The method of preparing an anticorrosive coating composition according to claim 2, wherein in step S1, the silane borate modified microcrystalline cellulose is prepared by: Dispersing microcrystalline cellulose in a mixed solvent of ethanol and water, adding a silane coupling agent KH-560, and carrying out reflux reaction for 4-6 hours at 70-80 ℃ to realize silanization modification of the microcrystalline cellulose; then, reacting the silanized microcrystalline cellulose with 4-formylphenylboric acid in methanol solvent at 50-60 ℃ for 8-10 hours, reacting Jing Xifu alkali to form C=N bond, and then adding sodium borohydride for reductive amination to obtain stable silane borate modified microcrystalline cellulose; wherein the molar ratio of the microcrystalline cellulose to the silane coupling agent KH-560 to the 4-formylphenylboric acid is 1 (1.0-1.2) to 1.0-1.2.
  4. 4. A method of preparing an anticorrosive coating composition according to claim 2, characterized in that in step S1: in the bottom layer slurry, the mass ratio of the epoxidized soybean oil to the polyethylene glycol to the silane borate modified microcrystalline cellulose is (40-50): 5-10): 1; The compatilizer is silane coupling agent KH-560, and the addition amount of the compatilizer is 0.1% -0.5% of the total mass of the bottom layer slurry; The coating is spin coating, and spin coating parameters are that the first stage lasts for 8-12 seconds at 400-600rpm, and the second stage lasts for 25-35 seconds at 1800-2200 rpm; The dynamic cross-linking and curing environment conditions are that the temperature is 20-25 ℃, the relative humidity is 50-60%, and the curing time is 20-28 hours.
  5. 5. A method of preparing an anticorrosive coating composition according to claim 2, characterized in that in step S2: The ionic liquid is 1-ethyl-3-methylimidazole NTF2; The sodium magnesium lithium silicate is synthesized sodium magnesium lithium silicate; In the middle layer slurry, 4-6 parts by mass of sodium magnesium lithium silicate, 4-6 parts by mass of PEDOT (sodium silicate) and PSS aqueous dispersion liquid, 35-45 parts by mass of ionic liquid and 45-55 parts by mass of water are calculated, and the solid content of the PEDOT and PSS aqueous dispersion liquid is 1.0% -1.5%; The preparation of the slurry comprises dissolving sodium magnesium lithium silicate in water, stirring at 800-1000rpm for 1.5-2.5 hours to form pregel, adding PEDOT, PSS aqueous dispersion and ionic liquid, and grinding for 2-4 times by a three-roller grinder with a roller gap of 5-20 μm; The coating is spray coating, the spray coating pressure is 0.2-0.4MPa, the spray distance is 12-18cm, and the conductive intermediate layer is formed by drying for 1.5-2.5 hours at the temperature of 20-25 ℃ and the relative humidity of less than 60% after spray coating.
  6. 6. A method of preparing an anticorrosive coating composition according to claim 2 wherein in step S3, the alkenylated fluorinated polyurethane prepolymer is prepared and used with a polyfunctional thiol compound by: a. Reacting hydroxyl-terminated perfluoropolyether with excessive isophorone diisocyanate to generate an isocyanate-terminated prepolymer, adding an active hydrogen compound hydroxyethyl methacrylate containing alkenyl, and introducing the alkenyl into the end of a polymer chain by reaction to obtain an alkenyl fluorinated polyurethane prepolymer; b. Mixing the prepolymer with pentaerythritol tetra-3-mercaptopropionate and 1wt% of 1173 type photoinitiator, directly carrying out ultraviolet light irradiation after coating, and carrying out high-efficiency mercaptan-alkene click reaction on the mercaptan group and alkenyl on the prepolymer under photoinitiation to form a C-S bond crosslinked network.
  7. 7. The method of producing an anticorrosive coating composition according to claim 6, wherein in step S3: The feeding mole ratio of the hydroxyl-terminated perfluoropolyether, isophorone diisocyanate and hydroxyethyl methacrylate is 1 (2.0-2.2): 2.0-2.2; the solid content of the surface layer slurry is 25% -35%; The coating is dip-coating, and the pulling speed is 3-6mm/s; The ultraviolet light wavelength adopted by the light-triggered crosslinking curing is 360-370nm, the irradiation intensity is 18-22mW/cm 2 , and the irradiation time is 45-75 seconds; after curing, the residual solvent was removed by vacuum drying at 75-85 ℃ below-0.09 MPa for 40-80 minutes.
  8. 8. A method of preparing an anticorrosive coating composition according to claim 2, characterized in that prior to step S1, it further comprises a pretreatment of the substrate: the substrate is sequentially placed in acetone and isopropanol for ultrasonic cleaning for 10-15 minutes respectively, and after nitrogen is blown dry, the substrate is treated in a plasma cleaning machine with the power of 80-120W and the oxygen flow of 20-25sccm for 5-10 minutes.
  9. 9. Use of the anticorrosive coating composition according to claim 1 in a component of semiconductor manufacturing process equipment.
  10. 10. Use of the anticorrosive coating composition according to claim 9 in a semiconductor manufacturing process equipment component, wherein the semiconductor manufacturing process equipment component is an electrostatic chuck.

Description

Anticorrosive paint composition and preparation method and application thereof Technical Field The invention relates to the technical field of anti-corrosion coating compositions, in particular to an anti-corrosion coating composition, a preparation method and application thereof. Background The corrosion-resistant coating technology is used as a core means for guaranteeing the safe service of major engineering equipment, the development level of the corrosion-resistant coating technology is directly related to the long-acting performance and reliability of strategic industries such as aerospace, ocean engineering, new energy, microelectronics and the like, the traditional coating is mainly used for blocking corrosive media through physical shielding, and advanced coating facing high-end equipment is required to realize the cooperation and integration of the multifunctional characteristics such as corrosion resistance, electric conduction, wear resistance, heat insulation and the like under the complex and harsh service conditions, so that the material system design and preparation process of the coating are challenged unprecedentedly. Particularly in the field of semiconductor manufacturing, the electrostatic chuck is used as a key bearing and temperature control component in the wafer processing process, the coating performance of the electrostatic chuck has a decisive influence on the chip yield and the production line stability, the electrostatic chuck coating needs to work for a long time under the conditions of high-frequency plasma bombardment, strong corrosive gas environment and extremely multiple physical field coupling of transient thermal load, the coating is required to have ultrahigh corrosion resistance, insulativity and low outgassing rate, the surface potential stable for a long time, the accurate heat conductivity coefficient and excellent particle impact resistance are also required to be maintained, and the wafer slip, thermal runaway or fatal faults such as process chamber pollution and the like can be caused by the degradation of any performance. In order to cope with the challenges, researchers try to construct a composite coating of 'structure-function integration' by using a functional nano material organic polymer matrix, however, most of the prior art relies on a simple mechanical blending and physical superposition process, and the 'stacking' strategy has intrinsic limitations that on one hand, nano materials are extremely easy to agglomerate due to high specific surface energy to form stress concentration points and defect channels in the coating, and on the other hand, poor compatibility of an organic/inorganic two-phase interface, weak interface combination is easy to become a preferential path for initiation and expansion of microcracks under thermal cycle and particle bombardment, so that the coating is early peeled off and fails, and the contradiction in a deep level is that the traditional method is difficult to realize cooperative regulation and control on properties such as corrosion resistance, conductivity, mechanics and the like on a molecular scale, so that a novel coating construction method capable of realizing accurate distribution of functional components, strengthening interaction of phase interfaces and finally realizing high-efficiency synergy of various properties is explored, and has become an urgent topic of breaking through the requirements of the current technology and meeting the next-generation semiconductor equipment. Disclosure of Invention In order to solve the problems mentioned in the background art, the invention provides an anticorrosive coating composition, a preparation method and application thereof. In order to achieve the above purpose, the present invention adopts the following technical scheme: an anticorrosive coating composition comprising three layers of coating layers arranged in sequence, respectively: the anti-corrosion bottom layer is formed by dynamically crosslinking bottom layer slurry containing epoxidized soybean oil, polyethylene glycol and silane borate modified microcrystalline cellulose; the conductive intermediate layer is formed by physical gelation of intermediate layer slurry containing PEDOT, PSS aqueous dispersion, sodium magnesium lithium silicate and ionic liquid; The wear-resistant surface layer is formed by light-triggered click crosslinking of surface layer slurry containing an alkenyl fluoride polyurethane prepolymer and a polyfunctional thiol compound. Further, the method comprises the following steps: s1, dispersing silane borate modified microcrystalline cellulose in a mixture of epoxidized soybean oil and polyethylene glycol, adding a compatilizer to form a bottom sizing agent, coating the bottom sizing agent on a substrate, and carrying out dynamic crosslinking and curing in a wet environment to obtain an anti-corrosion bottom layer; s2, dispersing PEDOT (polyether-ether-ketone) PSS aqueous dispersion and i