Anticorrosive coating composition as well as preparation method and application thereof
By employing a three-layer coating structure and dynamic crosslinking and photo-triggered click crosslinking technologies, the problems of nanomaterial agglomeration and poor interfacial compatibility were solved, achieving a synergistic improvement in the coating's self-healing, conductivity stability, and wear resistance, thus meeting the needs of high-end semiconductor manufacturing.
Patent Information
- Application Number
- CN202511597175.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-04
- Publication Date
- 2026-01-27
- Estimated Expiration
- 2045-11-04
AI Technical Summary
Existing technologies struggle to achieve the synergistic integration of multiple properties such as corrosion resistance, conductivity, wear resistance, and heat insulation under complex and demanding service conditions. Nanomaterials are prone to agglomeration and have poor interfacial compatibility, leading to premature peeling and failure of the coating, making it difficult to achieve synergistic regulation of performance at the molecular scale.
The coating adopts a three-layer structure, including an anti-corrosion base layer, a conductive intermediate layer, and a wear-resistant top layer, which are respectively formed by epoxidized soybean oil and silane borate modified microcrystalline cellulose, PEDOT:PSS aqueous dispersion and ionic liquid, alkenylated fluorinated polyurethane prepolymer and multifunctional thiol compound. The synergistic effect of each layer is achieved through dynamic crosslinking and photo-triggered click crosslinking technology.
It achieves the synergistic improvement of coating's self-healing, conductivity stability and wear resistance. The coating exhibits excellent performance in terms of salt spray corrosion resistance life, surface resistivity stability, hardness and flexibility, meeting the stringent requirements of high-end semiconductor manufacturing.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of anti-corrosion coating composition technology, and in particular to an anti-corrosion coating composition, its preparation method and application. Background Technology
[0002] As a core means to ensure the safe operation of major engineering equipment, the development level of anti-corrosion coating technology is directly related to the long-term effectiveness and reliability of strategic industries such as aerospace, marine engineering, new energy, and microelectronics. Traditional coatings mainly block corrosive media through physical shielding, while advanced coatings for high-end equipment need to achieve the synergistic integration of multiple functions such as corrosion resistance, conductivity, wear resistance, and heat insulation under complex and harsh service conditions. This poses unprecedented challenges to the material system design and preparation process of coatings.
[0003] Especially in the semiconductor manufacturing field, electrostatic chucks, as key support and temperature control components in wafer processing, have a decisive impact on chip yield and production line stability due to the quality of their coating performance. Electrostatic chuck coatings need to operate for extended periods under extreme multi-physics coupling conditions, including high-frequency plasma bombardment, highly corrosive gas environments, and transient thermal loads. This requires the coating to not only possess extremely high corrosion resistance, insulation, and low gas release rate, but also maintain a long-term stable surface potential, precise thermal conductivity, and excellent resistance to particle impact. Any performance degradation can lead to fatal failures such as wafer slippage, thermal runaway, or process chamber contamination.
[0004] To address these challenges, researchers have attempted to construct "structure-function integrated" composite coatings using functional nanomaterials as organic polymer matrices. However, most existing technologies rely on simple mechanical blending and physical stacking processes. This "stacking" strategy has inherent limitations: on the one hand, nanomaterials, due to their high specific surface energy, are prone to aggregation, forming stress concentration points and defect channels within the coating, which accelerates localized corrosion; on the other hand, the poor interfacial compatibility between the organic and inorganic phases means that weak interfacial bonding easily becomes a preferred path for microcrack initiation and propagation under thermal cycling and particle bombardment, leading to premature coating peeling and failure. A deeper contradiction lies in the fact that traditional methods struggle to achieve synergistic control of corrosion resistance, conductivity, and mechanical properties at the molecular scale, often resulting in compromises. Therefore, exploring a novel coating construction method that can achieve precise distribution of functional components, enhance interfacial interactions, and ultimately achieve efficient synergy of multiple properties has become an urgent issue for overcoming current technological bottlenecks and meeting the needs of next-generation semiconductor equipment. Summary of the Invention
[0005] To address the problems mentioned in the background section, the present invention provides an anti-corrosion coating composition, its preparation method, and its application.
[0006] To achieve the above objectives, the present invention adopts the following technical solution: An anti-corrosion coating composition comprising three layers sequentially arranged as follows: The anti-corrosion base layer is formed by dynamic cross-linking of a base slurry containing epoxidized soybean oil, polyethylene glycol, and silanoborate-modified microcrystalline cellulose; The conductive intermediate layer is formed by physical gelation of an intermediate layer slurry containing PEDOT:PSS aqueous dispersion, sodium magnesium lithium silicate, and ionic liquid; The wear-resistant surface layer is formed by photo-triggered click crosslinking of a surface slurry containing an alkenylated fluorinated polyurethane prepolymer and a multifunctional thiol compound.
[0007] Furthermore, this includes the following steps: S1. Silanoborate-modified microcrystalline cellulose is dispersed in a mixture of epoxidized soybean oil and polyethylene glycol, and a compatibilizer is added to form a bottom slurry. After being coated onto a substrate, the slurry is dynamically cross-linked and cured in a humid environment to obtain an anti-corrosion bottom layer. S2. A PEDOT:PSS aqueous dispersion and an ionic liquid are dispersed in an aqueous gel network formed by sodium magnesium lithium silicate to form an intermediate layer slurry, which is then coated onto the anti-corrosion underlayer and dried to gel, forming a conductive intermediate layer. S3. The alkenylated fluorinated polyurethane prepolymer is mixed with a multifunctional thiol compound and a photoinitiator to form a surface slurry, which is then coated onto the conductive intermediate layer. The thiol-alkene click crosslinking is then performed by ultraviolet irradiation to obtain a wear-resistant surface layer.
[0008] Furthermore, in step S1, the silanoborate-modified microcrystalline cellulose is prepared by the following method: Microcrystalline cellulose was dispersed in a mixed solvent of ethanol and water, and silane coupling agent KH-560 was added. The mixture was refluxed at 70-80℃ for 4-6 hours to achieve silanization modification of microcrystalline cellulose. Subsequently, silanized microcrystalline cellulose and 4-formylphenylboronic acid were reacted in methanol solvent at 50-60°C for 8-10 hours to form C=N bonds via Schiff base reaction. Sodium borohydride was then added for reductive amination to obtain stable silaneboronic acid ester modified microcrystalline cellulose.
[0009] The molar ratio of the microcrystalline cellulose, silane coupling agent KH-560, and 4-formylphenylboronic acid is 1:(1.0-1.2):(1.0-1.2).
[0010] Furthermore, in step S1: In the bottom slurry, the mass ratio of epoxidized soybean oil, polyethylene glycol and silane borate modified microcrystalline cellulose is (40-50):(5-10):1; The compatibilizer is silane coupling agent KH-560, and its addition amount is 0.1%-0.5% of the total mass of the bottom layer slurry; The coating is spin coating, and the spin coating parameters are: first stage 400-600 rpm / 8-12 seconds, second stage 1800-2200 rpm / 25-35 seconds; The environmental conditions for dynamic cross-linking curing are: temperature 20-25℃, relative humidity 50%-60%, and curing time 20-28 hours.
[0011] Furthermore, in step S2: The ionic liquid is 1-ethyl-3-methylimidazolium NTF2; The sodium magnesium lithium silicate is a synthetic sodium magnesium lithium silicate. In the intermediate layer slurry, by mass, there are 4-6 parts of sodium magnesium lithium silicate, 4-6 parts of PEDOT:PSS aqueous dispersion, 35-45 parts of ionic liquid, and 45-55 parts of water. The solid content of the PEDOT:PSS aqueous dispersion is 1.0%-1.5%. The preparation of the slurry includes: first dissolving sodium magnesium lithium silicate in water, stirring at 800-1000 rpm for 1.5-2.5 hours to form a pregel, then adding PEDOT:PSS aqueous dispersion and ionic liquid, and grinding 2-4 times with a three-roll mill with a roller gap of 5-20 μm. The coating is applied by spraying at a pressure of 0.2-0.4 MPa and a distance of 12-18 cm. After spraying, the coating is dried for 1.5-2.5 hours at a temperature of 20-25°C and a relative humidity of <60% to form a conductive intermediate layer.
[0012] Furthermore, in step S3, the alkenylated fluorinated polyurethane prepolymer and the multifunctional thiol compound are prepared and used by the following method: a. React hydroxyl-terminated perfluoropolyether with excess isophorone diisocyanate to generate a terminal isocyanate prepolymer, and then add hydroxyethyl methacrylate, an active hydrogen compound containing an alkenyl group. The reaction introduces the alkenyl group into the end of the polymer chain to obtain an alkenylated fluorinated polyurethane prepolymer. b. The prepolymer described above is mixed with pentaerythritol tetra-3-mercaptopropionate and 1 wt% of type 1173 photoinitiator, coated, and then directly subjected to ultraviolet irradiation. The thiol groups and the alkenyl groups on the prepolymer undergo a highly efficient thiol-alkene click reaction under photoinitiation to form a CS bond crosslinking network.
[0013] Furthermore, in step S3: The molar ratio of the terminal hydroxyl perfluoropolyether, isophorone diisocyanate and hydroxyethyl methacrylate is 1:(2.0-2.2):(2.0-2.2); The solid content of the surface slurry is 25%-35%; The coating is a dip coating, with a lifting speed of 3-6 mm / s; The photo-triggered crosslinking curing uses ultraviolet light with a wavelength of 360-370nm, an irradiation intensity of 18-22mW / cm2, and an irradiation time of 45-75 seconds. After curing, vacuum dry at 75-85℃ and below -0.09MPa for 40-80 minutes to remove residual solvent.
[0014] Furthermore, prior to step S1, a pretreatment of the substrate is included: The substrate was ultrasonically cleaned in acetone and isopropanol for 10-15 minutes each, dried with nitrogen, and then treated in a plasma cleaner with a power of 80-120W and an oxygen flow rate of 20-25 sccm for 5-10 minutes.
[0015] Furthermore, the application of the aforementioned anti-corrosion coating composition in semiconductor manufacturing process equipment components. Furthermore, the semiconductor manufacturing process equipment component is an electrostatic chuck.
[0016] The beneficial effects of this invention are: 1. This invention innovatively employs a dynamic crosslinking system based on epoxidized soybean oil and borate-modified microcrystalline cellulose in the anti-corrosion substrate. When microcracks appear in the coating, the borate bonds at the cracks can be reversibly broken; under the influence of ambient humidity, the borate groups and adjacent vicinal diol structures can be re-coordinated, achieving self-repair at room temperature, effectively blocking the penetration path of corrosive media, and minimizing the impact of local damage.
[0017] 2. In this invention, a pair of photo-clicking reactive groups composed of alkenyl and thiol groups is introduced into the wear-resistant surface layer. When the coating surface fails due to wear, localized ultraviolet irradiation can stimulate a highly efficient photo-clicking chemical reaction between the thiol and olefin, achieving rapid, targeted photo-triggered repair of the worn area of the surface layer and restoring the wear resistance and hydrophobic properties of the coating.
[0018] 3. This invention utilizes a unique physical gel network of lithium saponite to encapsulate PEDOT:PSS and a specific ionic liquid in a conductive intermediate layer. This gel network exhibits dynamic reversibility; under external stress or thermal cycling, the conductive filler network can be reconstructed rather than destroyed, demonstrating strain-adaptive conductive stability and ensuring the reliability of the electrostatic adsorption function.
[0019] 4. The dynamic cross-linking network at the bottom layer and the photo-click cross-linking network at the top layer of this invention can both form chemical bonds or strong interactions with the substrate or adjacent layers at the interface, rather than simple physical adhesion, thereby giving the coating excellent interlayer bonding and overall structural integrity, and significantly enhancing its anti-peeling ability.
[0020] 5. In the technical solution of this invention, the bottom layer curing does not require any traditional toxic curing agents, but relies on environmentally friendly dynamic covalent reactions. The surface layer curing is based on efficient and clean thiol-ene photoclick chemistry. The core raw materials, such as epoxidized soybean oil and microcrystalline cellulose, are derived from renewable resources, which is in line with the development trend of green chemistry.
[0021] 6. In the technical solution of this invention, the three-layer structure performs its own function while working together: the bottom layer actively repairs, the middle layer provides stable conductivity, and the top layer is wear-resistant and photo-repairable. The resulting coating exhibits excellent performance in terms of salt spray corrosion resistance, surface resistivity stability, hardness, wear resistance, and flexibility, far exceeding the performance limits of traditional single-function coatings, and can meet the stringent requirements of high-end semiconductor manufacturing for the surface protection of key components. Detailed Implementation
[0022] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0023] Unless otherwise specified, the raw materials used in this invention are all from commercially available conventional products.
[0024] Example 1 A method for preparing an anti-corrosion coating composition includes the following steps: S1. Substrate pretreatment: The substrate was ultrasonically cleaned in acetone and isopropanol for 12 minutes each, dried with nitrogen, and then treated in a plasma cleaner with a power of 100W and an oxygen flow rate of 22sccm for 8 minutes to obtain a pretreated substrate.
[0025] S2. Preparation of the anti-corrosion base layer: a. Preparation of silaneborate-modified microcrystalline cellulose: Weigh 1.0 g of microcrystalline cellulose and disperse it in 100 mL of ethanol / water mixed solvent. Add 1.2 g of 3-aminopropyltriethoxysilane (APTES) and reflux at 75 °C for 5 hours. After the reaction is complete, centrifuge and wash with ethanol to obtain silanized microcrystalline cellulose. Disperse the silanized microcrystalline cellulose in 50 mL of methanol and add 0.8 g of 4-formylphenylboronic acid. React at 55 °C for 9 hours. After the reaction solution cools to room temperature, add 0.2 g of sodium borohydride and continue stirring for 2 hours for reduction. Finally, wash with methanol and vacuum dry to obtain silaneborate-modified microcrystalline cellulose.
[0026] b. Formation of the base slurry and coating: Under nitrogen protection, 45g of epoxidized soybean oil and 5g of polyethylene glycol 6000 (PEG6000) were added to a mixing tank and heated to 60℃ to ensure uniform mixing. 1.0g of the above-mentioned silane borate modified microcrystalline cellulose and 0.15g of silane coupling agent KH-560 were added as compatibilizers, and the mixture was mechanically stirred at 300rpm for 40 minutes to obtain a uniform and stable base slurry.
[0027] c. Dynamic crosslinking curing: Spin-coat 2 mL of the slurry onto the pretreated substrate. Then, cure the coating at 23°C and 55% relative humidity for 24 hours. Under these conditions, the boric acid groups on the modified microcrystalline cellulose form reversible borate ester bonds with the vicinal diol structure on the PEG chain, constituting a dynamic crosslinking network. Simultaneously, the silane end groups of the modified microcrystalline cellulose can hydrolyze and form strong Si-OM covalent bonds with the substrate surface, enhancing adhesion. Compatibilizer KH-560 ensures good compatibility between the components.
[0028] S3. Preparation of a conductive intermediate layer: Add 5g of synthetic sodium magnesium lithium silicate to 50g of deionized water and stir at 900rpm for 2 hours to form a transparent pregel.
[0029] Add 5g of PEDOT:PSS aqueous dispersion and 40g of 1-ethyl-3-methylimidazolium NTF2 ionic liquid to the gel, and grind it three times with a three-roll mill to obtain the intermediate layer slurry.
[0030] The slurry is applied to the substrate by spraying (pressure 0.3MPa, spray distance 15cm), and then left to dry for 2 hours at 23℃ and 55% relative humidity to form a conductive gel layer.
[0031] S4. Prepare the wear-resistant surface layer: a. Synthesis of alkenylated fluorinated polyurethane prepolymer: In a dry glove box, 1 mol of terminal hydroxyl perfluoropolyether was reacted with 2.1 mol of isophorone diisocyanate at 70°C for 2 hours to generate a prepolymer. 2.1 mol of hydroxyethyl methacrylate (HEMA) was added, and the reaction continued for 1 hour to introduce alkenyl groups, yielding the alkenylated fluorinated polyurethane prepolymer.
[0032] b. Formation of surface layer slurry and photo-click crosslinking: The above prepolymer is diluted with DMF to a solid content of 30%, and then mixed with 0.15 mol pentaerythritol tetra-3-mercaptopropionate and 1 wt% of type 1173 photoinitiator to obtain surface layer slurry.
[0033] After being coated using the dip-coating method, it is directly applied at a wavelength of 365nm and an intensity of 20mW / cm. 2Irradiate with ultraviolet light for 60 seconds. Ultraviolet light excites the click reaction of thiol-alkene, rapidly forming a dense three-dimensional cross-linked network. Finally, dry under vacuum at 80°C and -0.095 MPa for 1 hour.
[0034] Example 2 The difference from Example 1 is that in step S2, the mass ratio of epoxidized soybean oil to borate-modified microcrystalline cellulose is 52:1. In step S3, the amount of PEDOT:PSS aqueous dispersion is 4.5g, and the amount of ionic liquid is 42g.
[0035] Example 3 The difference from Example 1 is that in step S2, the mass ratio of epoxidized soybean oil to borate-modified microcrystalline cellulose is 48:1. In step S3, the amount of PEDOT:PSS aqueous dispersion is 5.5g, and the amount of ionic liquid is 38g.
[0036] Comparative Example 1 The difference from Example 1 is that the anti-corrosion undercoating process in step S2 is omitted, and the conductive intermediate layer in step S3 is directly coated onto the pretreated substrate.
[0037] Comparative Example 2 The difference from Example 1 is that in step S3, an equal mass of ordinary polyaniline / carbon black mixture (mass ratio 9:1) is used instead of the PEDOT:PSS aqueous dispersion / ionic liquid / sodium magnesium lithium silicate system.
[0038] Comparative Example 3 The difference from Example 1 is that in step S4, ordinary fluorinated polyurethane without the introduction of alkenyl groups is used, and 2 wt% of type 1173 photoinitiator is added for UV curing, and pentaerythritol tetra-3-mercaptopropionate is not added.
[0039] Performance testing methods and results To verify the effectiveness of the present invention, performance tests were conducted on the coatings obtained in Examples 1-3 and Comparative Examples 1-3. Five parallel samples were prepared for each group of samples, and the average value was taken after testing.
[0040] Test method: Neutral salt spray resistance: According to GB / T 10125-2021, the test was conducted in a 5% NaCl solution at 35℃, and the time (h) for the coating to develop red rust was recorded as the corrosion protection life.
[0041] Surface resistivity: Refer to GB / T 1410-2006 and use a high-resistivity meter to measure the surface resistivity (Ω·sq) of the coating.
[0042] Scratch repair efficiency: Standard scratches were created on the coating surface using a nanoindenter. The surface scratches in Examples 1-3 were examined under ultraviolet light (365nm, 20mW / cm²). 2 Irradiate for 5 minutes. Measure the scratch depth using an optical profilometer and calculate the repair efficiency (%) = (initial depth - post-repair depth) / initial depth × 100%. The results are shown in Table 1:
[0043]
[0044] Test method: Adhesion: Perform cross-cut adhesion test according to ASTM D3359, rated from 0B (worst) to 5B (best).
[0045] Pencil hardness: Refer to ASTM D3363.
[0046] Abrasion resistance: According to ASTM D4060, the Taber abrasion tester was used with a CS-10 grinding wheel and a 1kg load to record the mass loss (mg) after 1000 abrasion cycles. The results are shown in Table 2:
[0047]
[0048] As shown in Table 1, the coatings prepared in Examples 1-3 exhibit significant advantages in corrosion resistance, electrical properties, and self-healing ability. Their salt spray lifetime all exceed 1380 hours, and their surface resistivity remains stable at 10⁻⁶. 5 The results show a scratch repair efficiency on the order of Ω·sq, exceeding 90%, and adhesion at the highest level (5B). This fully demonstrates the effectiveness of the three-layer structure design of this invention: the dynamic covalent bonds in the anti-corrosion layer enable self-repair of microcracks, effectively delaying the penetration of corrosive media; the gel network in the conductive intermediate layer ensures uniform and stable charge transport; and the photo-triggering chemical reaction in the wear-resistant surface layer achieves targeted and efficient repair of damage. In contrast, Comparative Example 1 exhibits the worst performance due to the lack of a key anti-corrosion layer; Comparative Example 2 uses traditional conductive materials, resulting in excessively high resistivity and poor adhesion; and Comparative Example 3 lacks a photo-triggered repair mechanism, thus almost completely losing its self-repair capability.
[0049] As shown in Table 2, the coatings of Examples 1-3 also possess excellent mechanical properties, with pencil hardness reaching 3H-4H and wear resistance far superior to the comparative examples. This is mainly attributed to the rigid support provided by the dense cross-linked network formed by photoclick chemistry in the wear-resistant surface layer, while the microcrystalline cellulose in the bottom layer and the sodium magnesium lithium silicate nanosheets in the middle layer play a crucial reinforcing role. Comparative Example 1 suffers from decreased hardness and wear resistance due to its incomplete structure; Comparative Example 2, due to the use of soft carbon black filler, severely disrupts the continuity of the matrix, resulting in the worst hardness and wear resistance; Comparative Example 3 has insufficient cross-linking density in its surface layer, and its performance is also significantly lower than that of the examples.
[0050] In summary, the anti-corrosion coating composition provided by this invention successfully solves the core problems of traditional composite coatings, such as single function, weak interfacial bonding, and poor durability, through a synergistic mechanism of "dynamic self-healing of the bottom layer, adaptive conductivity of the intermediate layer, and photo-triggered repair of the top layer." Experimental data fully demonstrate that this coating system achieves breakthrough improvements in key performance aspects such as corrosion protection life, electrical stability, self-healing efficiency, and mechanical strength. All performance indicators can meet the long-term protection requirements of electrostatic chucks under extreme working conditions, and it has broad application prospects in the field of high-end semiconductor equipment manufacturing.
[0051] In the description of this specification, the terms "preparation example," "example," "various examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that example or preparation example, which are included in at least one example or preparation example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same example or preparation example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more examples or preparation examples.
[0052] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. An anti-corrosion coating composition, characterized in that, The coating composition comprises three layers arranged sequentially: The anti-corrosion base layer is formed by dynamic cross-linking of a base slurry containing epoxidized soybean oil, polyethylene glycol, and silanoborate-modified microcrystalline cellulose; The conductive intermediate layer is formed by physical gelation of an intermediate layer slurry containing PEDOT:PSS aqueous dispersion, sodium magnesium lithium silicate, and ionic liquid; The wear-resistant surface layer is formed by photo-triggered click crosslinking of a surface slurry containing an alkenylated fluorinated polyurethane prepolymer and a multifunctional thiol compound.
2. The method for preparing an anti-corrosion coating composition according to claim 1, characterized in that, Includes the following steps: S1. Silanoborate-modified microcrystalline cellulose is dispersed in a mixture of epoxidized soybean oil and polyethylene glycol, and a compatibilizer is added to form a bottom slurry. After being coated onto a substrate, the slurry is dynamically cross-linked and cured in a humid environment to obtain an anti-corrosion bottom layer. S2. A PEDOT:PSS aqueous dispersion and an ionic liquid are dispersed in an aqueous gel network formed by sodium magnesium lithium silicate to form an intermediate layer slurry, which is then coated onto the anti-corrosion underlayer and dried to gel, forming a conductive intermediate layer. S3. The alkenylated fluorinated polyurethane prepolymer is mixed with a multifunctional thiol compound and a photoinitiator to form a surface slurry, which is then coated onto the conductive intermediate layer. The thiol-alkene click crosslinking is then performed by ultraviolet irradiation to obtain a wear-resistant surface layer.
3. The method for preparing an anti-corrosion coating composition according to claim 2, characterized in that, In step S1, the silaneborate-modified microcrystalline cellulose is prepared by the following method: Microcrystalline cellulose was dispersed in a mixed solvent of ethanol and water, and silane coupling agent KH-560 was added. The mixture was refluxed at 70-80℃ for 4-6 hours to achieve silanization modification of microcrystalline cellulose. Subsequently, silanized microcrystalline cellulose and 4-formylphenylboronic acid were reacted in methanol solvent at 50-60°C for 8-10 hours, forming C=N bonds via a Schiff base reaction. Sodium borohydride was then added for reductive amination to obtain stable silaneboronic acid ester modified microcrystalline cellulose. The molar ratio of the microcrystalline cellulose, silane coupling agent KH-560, and 4-formylphenylboronic acid was 1:(1.0-1.2):(1.0-1.2).
4. The method for preparing an anti-corrosion coating composition according to claim 2, characterized in that, In step S1: In the bottom slurry, the mass ratio of epoxidized soybean oil, polyethylene glycol and silane borate modified microcrystalline cellulose is (40-50):(5-10):1; The compatibilizer is silane coupling agent KH-560, and its addition amount is 0.1%-0.5% of the total mass of the bottom layer slurry; The coating is spin coating, and the spin coating parameters are: first stage 400-600 rpm / 8-12 seconds, second stage 1800-2200 rpm / 25-35 seconds; The environmental conditions for dynamic cross-linking curing are: temperature 20-25℃, relative humidity 50%-60%, and curing time 20-28 hours.
5. The method for preparing an anti-corrosion coating composition according to claim 2, characterized in that, In step S2: The ionic liquid is 1-ethyl-3-methylimidazolium NTF2; The sodium magnesium lithium silicate is a synthetic sodium magnesium lithium silicate. In the intermediate layer slurry, by mass, there are 4-6 parts of sodium magnesium lithium silicate, 4-6 parts of PEDOT:PSS aqueous dispersion, 35-45 parts of ionic liquid, and 45-55 parts of water. The solid content of the PEDOT:PSS aqueous dispersion is 1.0%-1.5%. The preparation of the slurry includes: first dissolving sodium magnesium lithium silicate in water, stirring at 800-1000 rpm for 1.5-2.5 hours to form a pregel, then adding PEDOT:PSS aqueous dispersion and ionic liquid, and grinding 2-4 times with a three-roll mill with a roller gap of 5-20 μm. The coating is applied by spraying at a pressure of 0.2-0.4 MPa and a distance of 12-18 cm. After spraying, the coating is dried for 1.5-2.5 hours at a temperature of 20-25°C and a relative humidity of <60% to form a conductive intermediate layer.
6. The method for preparing an anti-corrosion coating composition according to claim 2, characterized in that, In step S3, the alkenylated fluorinated polyurethane prepolymer and the multifunctional thiol compound are prepared and used by the following method: a. React hydroxyl-terminated perfluoropolyether with excess isophorone diisocyanate to generate a terminal isocyanate prepolymer, and then add hydroxyethyl methacrylate, an active hydrogen compound containing an alkenyl group. The reaction introduces the alkenyl group into the end of the polymer chain to obtain an alkenylated fluorinated polyurethane prepolymer. b. The prepolymer described above is mixed with pentaerythritol tetra-3-mercaptopropionate and 1 wt% of type 1173 photoinitiator, coated, and then directly subjected to ultraviolet irradiation. The thiol groups and the alkenyl groups on the prepolymer undergo a highly efficient thiol-alkene click reaction under photoinitiation to form a CS bond crosslinking network.
7. The method for preparing an anti-corrosion coating composition according to claim 6, characterized in that, In step S3: The molar ratio of the terminal hydroxyl perfluoropolyether, isophorone diisocyanate and hydroxyethyl methacrylate is 1:(2.0-2.2):(2.0-2.2); The solid content of the surface slurry is 25%-35%; The coating is a dip coating, with a lifting speed of 3-6 mm / s; The photo-triggered crosslinking curing uses ultraviolet light with a wavelength of 360-370nm, an irradiation intensity of 18-22mW / cm2, and an irradiation time of 45-75 seconds. After curing, vacuum dry at 75-85℃ and below -0.09MPa for 40-80 minutes to remove residual solvent.
8. The method for preparing an anti-corrosion coating composition according to claim 2, characterized in that, Prior to step S1, a pretreatment of the substrate is also included: The substrate was ultrasonically cleaned in acetone and isopropanol for 10-15 minutes each, dried with nitrogen, and then treated in a plasma cleaner with a power of 80-120W and an oxygen flow rate of 20-25 sccm for 5-10 minutes.
9. The application of the anti-corrosion coating composition as described in claim 1 in components of semiconductor manufacturing process equipment.
10. The application of the anti-corrosion coating composition according to claim 9 in semiconductor manufacturing process equipment components, characterized in that, The semiconductor manufacturing process equipment component is an electrostatic chuck.
Citation Information
Patent Citations
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