Antistatic wafer cutting adhesive tape and preparation method thereof
By introducing functionalized reducing graphene oxide into the antistatic acrylate pressure-sensitive adhesive, the problem of electrostatic discharge in the semiconductor wafer cutting process is solved, and wafer cutting tape with excellent antistatic properties is prepared, which improves the reliability and yield of the product.
Patent Information
- Application Number
- CN202311157327.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-08
- Publication Date
- 2025-03-11
AI Technical Summary
In the semiconductor wafer cutting process, electrostatic discharge problems between the cutting tape and the silicon wafer lead to static accumulation, affecting the chip quality on the wafer and the reliability of the final product.
Functional reduced graphene oxide and antistatic acrylate pressure-sensitive adhesive system were used to prepare antistatic wafer cutting tape. This method enhances the antistatic properties of the tape by hydrolysis and reduction of graphene oxide by aminosilane, introducing organic segments and amino groups, thereby enhancing the anti-static properties of the tape.
It realizes excellent antistatic and comprehensive performance of wafer cutting tape, meets application needs in the wafer cutting field, and improves product reliability and yield.
Smart Images
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Abstract
Description
Technical Field
[0001] The invention relates to the field of antistatic methods for semiconductor wafer dicing tapes, and in particular to an antistatic wafer dicing tape and a preparation method thereof. Background Art
[0002] Electrostatic discharge (ESD) is the rapid transfer of charge between two objects, usually generated when two objects with different electrical potentials come into direct contact with each other. With the development of electronic packaging technology and the continuous miniaturization of transistor circuits, electronic devices have become increasingly susceptible to ESD. Therefore, strict control of ESD phenomena is required in semiconductor manufacturing processes. Among them, in the semiconductor wafer dicing process, since the dicing tape and silicon wafer are insulators and semiconductors respectively, static charges will be generated on the surface and potential will accumulate. Therefore, a large amount of static electricity may be generated during the peeling process of the release film and the adhesive layer of the dicing tape, the bonding process of the dicing tape and the wafer, and the separation process of the tape and the chip after dicing. Even if these static electricity that may be generated is very small, it may cause various problems for the chips on the wafer, such as causing the circuit in the chip to be destroyed, thereby causing chip defects or damage, or electrostatic adsorption causing the circuit to be contaminated by foreign matter, etc. These problems will affect the reliability and yield of the final product, so the wafer dicing tape itself needs to have anti-static properties. Summary of the invention
[0003] In order to solve the deficiencies of the prior art, the purpose of the present invention is to provide a method for synthesizing an antistatic acrylic pressure-sensitive adhesive and a method for preparing a wafer dicing tape containing functionalized reduced graphene oxide. The functionalized reduced graphene oxide prepared by the present invention has good dispersibility and compatibility in an acrylic ester system, and the prepared wafer dicing tape has excellent antistatic properties and other comprehensive properties, meeting the application requirements of dicing tape in the field of wafer dicing.
[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is:
[0005] A method for preparing an antistatic wafer dicing tape, characterized in that the specific steps include diluting the antistatic acrylic pressure-sensitive adhesive solution, mixing with a curing agent and functionalized reduced graphene oxide, coating on a substrate film, drying the adhesive layer, pressing a release film onto the adhesive layer, and aging.
[0006] Preferably, the method for preparing functionalized graphene oxide comprises the following steps:
[0007] (1) dispersing graphene oxide and alcohol in hydrolyzed aminosilane for reaction, washing and drying to obtain functionalized graphene oxide;
[0008] (2) Reducing the functionalized graphene oxide in the presence of a reducing agent to obtain functionalized reduced graphene oxide.
[0009] Preferably, the structural formula of aminosilane is as shown in Formula I,
[0010]
[0011] Wherein, R1 is methyl or ethyl; n1 is 1 to 20; n2 is 0 to 20; and R2 is selected from any one of methyl, amino, phenyl, and hydrogen atom.
[0012] Preferably, the aminosilane is selected from at least one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-n-butyl-3-aminopropyltrimethoxysilane and N-aminoethyl-aminopropyltrimethoxysilane.
[0013] Preferably, in step (1), the lateral size of the graphene oxide is ≤10 μm; for example, it can be 9 μm, 7 μm, 6 μm, 4 μm, 2 μm, or 1 μm, and more preferably ≤5 μm; too large a size is not conducive to the preparation of functionalized graphene oxide, and the dicing tape prepared by synthesizing functionalized reduced graphene oxide using graphene oxide of too large a size has the problem of unstable peeling force.
[0014] Preferably, the hydrolysis solution used for aminosilane is a mixture of ethanol and deionized water, wherein the ratio of ethanol to deionized water is 9:1 to 7:3, for example, 9:1, 8:2 or 7:3;
[0015] Preferably, in step (1), the hydrolysis time is 0.5 to 2 h, for example, 0.5 h, 1 h or 1.5 h, etc.; the hydrolysis temperature is 20 to 50 ° C, for example, 25 ° C, 30 ° C or 40 ° C, etc.; if the hydrolysis time is too short, the hydrolysis is insufficient, and if the time is too long, the aminosilane hydrolysis product will self-polymerize too much, which will be unfavorable for the reaction with graphene oxide.
[0016] Preferably, in step (1), the reaction time is 1 to 4 h, for example, 1.5 h, 2 h, 3 h or 4 h; the reaction temperature is 75 to 85 ° C, for example, 77 ° C, 79 ° C, 81 ° C, 83 ° C or 85 ° C; the reaction is carried out in an inert atmosphere, preferably a nitrogen atmosphere.
[0017] Preferably, the alcohol includes any one of methanol, ethanol, isopropanol, or a combination of at least two of them.
[0018] Preferably, in step (2), the reducing agent is an amino- or hydroxy-containing reducing agent;
[0019] Preferably, the reducing agent is hydrazine, polyol, more preferably L-ascorbic acid;
[0020] Preferably, in step (2), the temperature of the reduction reaction is 85-95°C, for example, 87°C, 89°C, 91°C, 93°C or 95°C; the time of the reduction reaction is 1-5h, for example, 1h, 3h or 5h; the reduction is carried out in an inert atmosphere, preferably a nitrogen atmosphere.
[0021] Preferably, the mass ratio of aminosilane, graphene oxide, alcohol and reducing agent is (5-15):1:(100-1000):(5-15); for example, the mass ratio of graphene oxide to alcohol can be 1:200, 1:300, 1:500, 1:800 or 1:1000, etc.; the mass ratio of graphene oxide to aminosilane can be 1:5, 1:6, 1:8, 1:10, 1:12 or 1:15, etc.; the mass ratio of graphene oxide to reducing agent can be 1:5, 1:6, 1:8, 1:10, 1:12 or 1:15, etc.
[0022] Preferably, the dispersion method is ultrasonic dispersion, and the dispersion time is 1 to 2 hours, for example, 1.2 hours, 1.6 hours or 2 hours.
[0023] Preferably, the reduction further includes post-treatment, which includes filtration, washing and drying; the washing agent includes deionized water and acetone.
[0024] Preferably, the cleaning method comprises cleaning with water and acetone 2 to 3 times respectively.
[0025] Preferably, the drying method is freeze drying, and the drying time is 24 to 72 hours, for example, 24 hours, 32 hours or 40 hours.
[0026] Preferably, the preparation method of the antistatic acrylic pressure-sensitive adhesive is: mixing monomers with a thermal initiator and a solvent for reaction, wherein the monomers include soft monomers, hard monomers and reactive functional monomers.
[0027] Preferably, the reaction first mixes the soft monomer and the hard monomer and 1 / 3 of the solvent into the reaction container, and then dissolves the thermal initiator in the remaining 2 / 3 of the solvent for standby use. When the reaction container is heated to 70°C, begin to drip 1 / 2 of the total amount of the thermal initiator solution, control the dripping speed to complete the dripping within 2 hours, and keep warm for 2 hours. Then heat to 74°C, continue to drip 1 / 3 of the total amount of the thermal initiator solution, drip it within 1 hour, and keep warm for 1.5 hours. Finally, drip the remaining thermal initiator solution within 0.5 hours, and keep warm for 2 hours to obtain the antistatic acrylate pressure-sensitive adhesive solution.
[0028] Preferably, the speed of the stirring paddle during the reaction is 100 to 200 rpm / min, for example, 100 rpm / min, 150 rpm / min or 200 rpm / min, etc.; the reaction is carried out in an inert atmosphere, preferably a nitrogen atmosphere.
[0029] Preferably, the soft monomer is selected from one or more of formula II and / or formula III,
[0030]
[0031] Wherein, R3 and R4 are independently methyl or hydrogen atoms; n3 and n4 are independently 0 to 30;
[0032] Preferably, the hard monomer is selected from one or more of formula IV, formula V, vinyl acetate, styrene, and acrylamide.
[0033]
[0034] wherein R5 and R6 are independently methyl or hydrogen atoms; n5 and n6 are independently 0 to 30;
[0035] Preferably, the reactive functional monomer is selected from at least one of glycidyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, acrylic acid, and methacrylic acid.
[0036] Preferably, the mass ratio of the soft monomer, the hard monomer and the reactive functional monomer is (55-90): (5-30): (1-15);
[0037] Preferably, the mass ratio of monomer, thermal initiator and solvent is 1:(0.001-0.003):(1-4);
[0038] Preferably, the mass ratio of the curing agent, the functionalized reduced graphene oxide, and the monomer (the sum of the soft monomer, the hard monomer, and the reactive functional monomer) is (0.4-3):(0.1-3):100.
[0039] Preferably, the thermal initiator is one or more of azobisisobutyronitrile and benzoyl peroxide.
[0040] Preferably, the solvent is one or more of toluene, ethyl acetate and methanol.
[0041] Preferably, the curing agent is one or more of toluene diisocyanate (TDI), TDI trimer, diphenylmethane diisocyanate (MDI), MDI trimer, hexamethylene diisocyanate (HDI), HDI trimer, isophorone diisocyanate (IPDI) and IPDI trimer.
[0042] Preferably, the coating method is a coater or a four-sided coater.
[0043] Preferably, the coating thickness is 25 to 75 μm, for example, 30 μm, 45 μm or 70 μm.
[0044] Preferably, the substrate film is one of polyethylene, polypropylene, polybutylene, ethylene-vinyl acetate copolymer, ethylene-butylene copolymer and polyvinyl chloride.
[0045] Preferably, the release film is polyethylene terephthalate.
[0046] Preferably, the dilution is specifically: diluting with ethyl acetate to a solid content of 15-25%, for example, 16%, 21% or 24%.
[0047] Preferably, the drying temperature is 90-100° C., for example, 92° C., 96° C. or 100° C., etc.; the drying time is 100-150 s, for example, 110 s, 130 s or 140 s, etc.
[0048] Preferably, the aging temperature is 30-50°C, for example, 35°C, 40°C or 45°C, etc.; the aging time is 48-72h, for example, 50h, 60h or 70h, etc.
[0049] Compared with the prior art, the present invention has the following innovations and beneficial effects:
[0050] In the functionalized reduced graphene oxide provided by the present invention, aminosilane is hydrolyzed, and the silanol groups in the hydrolyzate react with the hydroxyl groups on the graphene oxide to undergo a dehydration condensation reaction to obtain the functionalized graphene oxide, and an organic segment and an amino group are introduced. The introduction of the amino group enables it to react with an isocyanate crosslinking agent, and the synergistic effect of the organic segment and the chemical bonding improves its dispersibility and compatibility in the polymer system. At the same time, a reducing agent is used to reduce the functionalized reduced graphene oxide, and the conjugated structure of a part of the graphene is restored, thereby improving its conductivity, and the functionalized reduced graphene oxide can be used as an antistatic component in an acrylic pressure-sensitive adhesive system and a wafer dicing tape.
[0051] The present invention adopts functionalized reduced graphene oxide as an antistatic component to copolymerize with an acrylate system, thereby solving the incompatibility problem between graphene and pressure-sensitive adhesive. The chemical bond connection method has a good dispersion effect, and only a small amount needs to be added to achieve an antistatic effect. The present invention can be used to prepare an antistatic wafer dicing tape that has both peeling force and antistatic performance. DETAILED DESCRIPTION
[0052] The disclosure below provides many different embodiments or examples to implement different contents of the present invention. In order to simplify the disclosure of the present invention, the settings of specific examples are described below. Of course, they are only examples, and the purpose is not to limit the present invention. In addition, the present invention can repeat reference numbers and / or reference letters in different examples, and this repetition is for the purpose of simplification and clarity, which itself does not indicate the relationship between the various embodiments and / or settings discussed.
[0053]
[0054] Formula VI is a reaction chemical formula of a base acrylic polymer with a reactive group, a curing agent and functionalized reduced graphene oxide. is a basic acrylic ester polymer with a reactive group, R1 is a reactive group (carboxyl or hydroxyl), As a curing agent, For functionalized reduced graphene oxide, R2 is a structure obtained by the reaction of the reactive group R1 and the isocyanate group.
[0055] Example 1
[0056] (1) Preparation of functionalized reduced graphene oxide:
[0057] 10 g of 3-aminopropyltrimethoxysilane was dispersed in 36 ml of ethanol and 4 ml of aqueous solution and hydrolyzed at 20°C for 2 h. Then, 1 g of graphene oxide and the hydrolyzate were mixed with 200 ml of ethanol. The suspension was homogenized by ultrasound at room temperature for 2 h. The mixture was stirred and heated at 80°C at a speed of 200 ppm for 2 h in a nitrogen atmosphere. Then, 5 g of L-ascorbic acid was added to the suspension and heated at 90°C for 2 h. After filtration, the product was washed several times with acetone and deionized water, and then freeze-dried for 48 h to obtain functionalized reduced graphene oxide.
[0058] (2) Preparation of basic acrylic pressure-sensitive adhesive:
[0059] First, 23.4g butyl acrylate (soft monomer), 3.6g vinyl acetate (hard monomer), 3g 2-hydroxyethyl acrylate (reactive functional monomer) and 23.34g ethyl acetate (solvent) were mixed and added to a four-necked flask, and then 0.06g azobisisobutyronitrile (thermal initiator) was dissolved in 46.66g ethyl acetate (solvent) for standby use. When the four-necked flask was heated to 70°C, 1 / 2 of the total amount of azobisisobutyronitrile solution was added dropwise, and the addition speed was controlled to be completed within 2h, and the mixture was kept warm for 2h. Then, the temperature was raised to 74°C, and 1 / 3 of the total amount of azobisisobutyronitrile solution was continued to be added dropwise, and the addition was completed within 1h, and the mixture was kept warm for 1.5h. Finally, the remaining azobisisobutyronitrile solution was added dropwise within 0.5h, and the mixture was kept warm for 2h to obtain the basic acrylic pressure-sensitive adhesive solution.
[0060] (3) Preparation of antistatic wafer dicing tape:
[0061] First, add 20g of acrylic pressure-sensitive adhesive liquid to 0.135g of TDI trimer and 0.03375g of functionalized reduced graphene oxide, mix and dilute with ethyl acetate to a solid content of 20%, use a four-sided coater to coat a 50μm thick adhesive layer on the polyvinyl chloride base film, dry in an oven at 100℃ for 120s, use a laminator to laminate the polyethylene terephthalate film onto the adhesive layer, and put it in a 40℃ oven for aging for 72h to obtain an antistatic wafer dicing tape.
[0062] Example 2
[0063] (1) The preparation of functionalized reduced graphene oxide is the same as in Example 1.
[0064] (2) The preparation of the basic acrylic pressure-sensitive adhesive is the same as in Example 1.
[0065] (3) Preparation of antistatic wafer dicing tape:
[0066] The specific preparation method is different from that in Example 1 only in that the mass of the functionalized reduced graphene oxide is increased to 0.0675 g; other materials, amounts and specific preparation methods are the same as those in Example 1.
[0067] Example 3
[0068] (1) The preparation of functionalized reduced graphene oxide is the same as in Example 1.
[0069] (2) The preparation of the basic acrylic pressure-sensitive adhesive is the same as in Example 1.
[0070] (3) Preparation of antistatic wafer dicing tape:
[0071] The specific preparation method is different from that in Example 1 only in that the mass of the functionalized reduced graphene oxide is increased to 0.135 g; other materials, amounts and specific preparation methods are the same as those in Example 1.
[0072] Example 4
[0073] (1) Preparation of functionalized reduced graphene oxide:
[0074] 15 g of N-phenyl-3-aminopropyltrimethoxysilane was dispersed in 40 ml of ethanol and 6 ml of aqueous solution and hydrolyzed at 35°C for 1 h. Then, 1 g of graphene oxide and the hydrolysis product were mixed with 200 ml of ethanol. The suspension was homogenized by ultrasound at room temperature for 2 h. The mixture was stirred and heated at 80°C at a speed of 200 ppm for 2 h in a nitrogen atmosphere. Then, 6 g of hydrazine hydrate was added to the suspension and heated at 90°C for 2 h. After filtration, the product was washed several times with acetone and deionized water, and then freeze-dried for 48 h to obtain functionalized reduced graphene oxide.
[0075] (2) Preparation of basic acrylic pressure-sensitive adhesive:
[0076] First, add 26.4g of isooctyl acrylate (soft monomer), 5.6g of ethyl methacrylate (hard monomer), 3g of 2-hydroxyethyl methacrylate (reactive functional monomer) and 25g of ethyl acetate (solvent) into a four-necked flask, and then dissolve 0.08g of azobisisobutyronitrile (thermal initiator) in 40g of ethyl acetate for later use. When the four-necked flask is heated to 70°C, begin to drip 1 / 2 of the total amount of azobisisobutyronitrile solution, control the dripping speed to complete the dripping within 2h, and keep warm for 2h. Then heat to 74°C, continue to drip 1 / 3 of the total amount of azobisisobutyronitrile solution, drip it within 1h, and keep warm for 1.5h. Finally, drip the remaining azobisisobutyronitrile solution within 0.5h, and keep warm for 2h to obtain the basic acrylic pressure-sensitive adhesive solution.
[0077] (3) Preparation of antistatic wafer dicing tape:
[0078] First, add 18g of acrylic pressure-sensitive adhesive liquid to 0.135g of MDI trimer and 0.1g of functionalized reduced graphene oxide, mix and dilute with ethyl acetate to a solid content of 20%, use a four-sided coater to coat a 50μm thick adhesive layer on the polyvinyl chloride base film, dry in an oven at 100℃ for 120s, use a laminator to laminate the polyethylene terephthalate film onto the adhesive layer, and put it in a 40℃ oven for aging for 72h to obtain an antistatic wafer dicing tape.
[0079] Example 5
[0080] (1) Preparation of functionalized reduced graphene oxide:
[0081] 13.5 g of N-n-butyl-3-aminopropyltrimethoxysilane was dispersed in 40 ml of ethanol and 6 ml of aqueous solution and hydrolyzed at 50°C for 0.5 h. Then, 1 g of graphene oxide and the hydrolysis product were mixed with 200 ml of ethanol. The suspension was homogenized by ultrasound at room temperature for 1.5 h. The mixture was stirred and heated at 80°C for 2 h at a speed of 200 ppm. Then, 6 g of hydrazine hydrate was added to the suspension and heated at 90°C for 2 h. After filtration, the product was washed several times with acetone and deionized water, and then freeze-dried for 48 h to obtain functionalized reduced graphene oxide.
[0082] (2) Preparation of basic acrylic pressure-sensitive adhesive:
[0083] First, 27g of n-hexyl acrylate (soft monomer), 5g of methyl methacrylate (hard monomer), 4g of 2-hydroxyethyl methacrylate (reactive functional monomer) and 26g of ethyl acetate (solvent) were mixed and added to a four-necked flask, and then 0.08g of azobisisobutyronitrile (thermal initiator) was dissolved in 38g of ethyl acetate for use. When the four-necked flask was heated to 70°C, 1 / 2 of the total amount of azobisisobutyronitrile solution was added dropwise, and the addition speed was controlled to be completed within 2h, and the mixture was kept warm for 2h. Then, the temperature was raised to 74°C, and 1 / 3 of the total amount of azobisisobutyronitrile solution was continued to be added dropwise, and the addition was completed within 1h, and the mixture was kept warm for 1.5h. Finally, the remaining azobisisobutyronitrile solution was added dropwise within 0.5h, and the mixture was kept warm for 2h to obtain a basic acrylic pressure-sensitive adhesive solution.
[0084] (3) Preparation of antistatic wafer dicing tape:
[0085] First, add 15g of acrylic pressure-sensitive adhesive liquid to 0.138g of IPDI trimer and 0.1g of functionalized reduced graphene oxide, mix and dilute with ethyl acetate to a solid content of 20%, use a four-sided coater to coat a 50μm thick adhesive layer on the polyvinyl chloride base film, dry in an oven at 100℃ for 120s, use a laminator to laminate the polyethylene terephthalate film onto the adhesive layer, and put it in a 40℃ oven for aging for 72h to obtain an antistatic wafer dicing tape.
[0086] Comparative Example 1
[0087] (1) The preparation of functionalized reduced graphene oxide is the same as in Example 1.
[0088] (2) The preparation of the basic acrylic pressure-sensitive adhesive is the same as in Example 1.
[0089] (3) Preparation of antistatic wafer dicing tape:
[0090] The specific preparation method is different from that in Example 1 only in that no functionalized reduced graphene oxide is added; other materials, amounts and specific preparation methods are the same as those in Example 1.
[0091] Determination of surface resistance: The surface resistance value of the prepared antistatic wafer dicing tape was measured using a SIMCO-ST4 surface resistance tester. The measurement method was to apply voltage to the surface and measure a comprehensive surface resistance value.
[0092] Peel force: 180° peel force is tested according to GB / 2792-1998.
[0093] The results of Examples 1 to 5 and Comparative Example 1 are shown in Table 1:
[0094] Performance Tests of Examples 1 to 5 and Comparative Example 1
[0095] Surface resistance / Ω Peel force / gf Example 1 3.2E+11 50 Example 2 1E+11 46 Example 3 2.0E+10 37 Example 4 1.6E+10 53 Example 5 1.5E+10 49 Comparative Example 1 ＞1E+13 56
[0096] It can be seen from the examples and comparative examples in the table that the anti-static pressure-sensitive adhesive prepared by the present invention containing functionalized reduced graphene oxide can be used to prepare a wafer dicing tape having both peeling force and anti-static performance.
[0097] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate a functionalized reduced graphene oxide, an antistatic cutting tape and a preparation method thereof, but the present invention is not limited to the above-mentioned process steps, that is, it does not mean that the present invention must rely on the above-mentioned process steps to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.
[0098] Those skilled in the art will readily appreciate other embodiments of the invention after considering the specification and practicing the invention herein. The invention is intended to cover any variations, uses or adaptations of the invention that follow the general principles of the invention and include common knowledge or customary techniques in the art of the invention. The specification and examples are to be considered exemplary only, and the true scope and spirit of the invention are indicated by the claims.
[0099] It should be understood that the present invention is not limited to what has been described above and that various modifications and changes may be made without departing from its scope. The scope of the present invention is limited only by the appended claims.
Claims
1. A method for preparing an antistatic wafer dicing tape, characterized in that: The specific steps include adding antistatic acrylic pressure-sensitive adhesive liquid to a curing agent and functionalized reduced graphene oxide, mixing and diluting, coating on a substrate film, drying the adhesive layer, pressing a release film onto the adhesive layer, and ripening.
2. The preparation method according to claim 1, characterized in that: The preparation method of the functionalized graphene oxide comprises the following steps: (1) dispersing graphene oxide and alcohol in hydrolyzed aminosilane for reaction, washing and drying to obtain functionalized graphene oxide; (2) reducing the functionalized graphene oxide in the presence of a reducing agent to obtain functionalized reduced graphene oxide.
3. The preparation method according to claim 2, characterized in that: The structural formula of the aminosilane is shown in Formula I, Wherein, R1 is methyl or ethyl; n1 is 1 to 20; n2 is 0 to 20; and R2 is selected from any one of methyl, amino, phenyl, and hydrogen atom.
4. The preparation method according to claim 3, characterized in that: The aminosilane is selected from at least one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-n-butyl-3-aminopropyltrimethoxysilane and N-aminoethyl-aminopropyltrimethoxysilane.
5. The preparation method according to claim 2, characterized in that: In step (1), the lateral size of the graphene oxide is ≤10 μm; Preferably, in step (1), the hydrolysis time is 0.5 to 2 hours, and the hydrolysis temperature is 20 to 50° C.; Preferably, in step (1), the reaction time is 1 to 4 hours, and the reaction temperature is 75 to 85°C.
6. The preparation method according to claim 2, characterized in that: In step (2), the reducing agent is an amino- or hydroxyl-containing reducing agent; Preferably, in step (2), the temperature of the reduction reaction is 85 to 95° C., and the time of the reduction reaction is 1 to 5 hours.
7. The preparation method according to claim 2, characterized in that: The mass ratio of the aminosilane, the graphene oxide, the alcohol and the reducing agent is (5-15):1:(100-1000):(5-15).
8. The preparation method according to claim 1, characterized in that: The preparation method of the antistatic acrylate pressure-sensitive adhesive solution is: mixing monomers with a thermal initiator and a solvent for reaction, wherein the monomers include soft monomers, hard monomers and reactive functional monomers.
9. The preparation method according to claim 8, characterized in that: The soft monomer is selected from one or more of formula II and / or formula III, Wherein, R3 and R4 are independently methyl or hydrogen atoms; n3 and n4 are independently 0 to 30; Preferably, the hard monomer is selected from one or more of formula IV, formula V, vinyl acetate, styrene, and acrylamide. wherein R5 and R6 are independently methyl or hydrogen atoms; n5 and n6 are independently 0 to 30; Preferably, the reactive functional monomer is selected from at least one of glycidyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, acrylic acid, and methacrylic acid.
10. The preparation method according to claim 8, characterized in that: The dilution specifically comprises: diluting with ethyl acetate to a solid content of 15-25%; Preferably, the mass ratio of the soft monomer, the hard monomer and the reactive functional monomer is (55-90): (5-30): (1-15); Preferably, the mass ratio of the monomer, the thermal initiator and the solvent is 1:(0.001-0.003):(1-4); Preferably, the mass ratio of the curing agent, the functionalized reduced graphene oxide, and the monomer is (0.4-3):(0.1-3):100.